Analysis of Plastics

Rapra Review Reports
Expert overviews covering the science and

technology of rubber and plastics
ISSN: 0889-3144
Analysis of Plastics
Report 149
Volume 13, Number 5, 2002
Martin J. Forrest
RAPRA REVIEW REPORTS
A Rapra Review Report comprises three sections, as follows:
1. A commissioned expert review, discussing a key topic of current interest, and referring to the References and
Abstracts section. Reference numbers in brackets refer to item numbers from the References and Abstracts
section. Where it has been necessary for completeness to cite sources outside the scope of the Rapra Abstracts
database, these are listed at the end of the review, and cited in the text as a.1, a.2, etc.
2. A comprehensive References and Abstracts section, resulting from a search of the Rapra Polymer Library
database. The format of the abstracts is outlined in the sample record below.
3. An index to the References and Abstracts section, derived from the indexing terms which are added to the
abstracts records on the database to aid retrieval.
Item 1
Macromolecules
33, No.6, 21st March 2000, p.2171-83
EFFECT OF THERMAL HISTORY ON THE RHEOLOGICAL
BEHAVIOR OF THERMOPLASTIC POLYURETHANES
Pil Joong Yoon; Chang Dae Han
Akron,University
The effect of thermal history on the rheological behaviour of ester- and
ether-based commercial thermoplastic PUs (Estane 5701, 5707 and 5714
from B.F.Goodrich) was investigated. It was found that the injection
moulding temp. used for specimen preparation had a marked effect on the
variations of dynamic storage and loss moduli of specimens with time
observed during isothermal annealing. Analysis of FTIR spectra indicated
that variations in hydrogen bonding with time during isothermal annealing
very much resembled variations of dynamic storage modulus with time
during isothermal annealing. Isochronal dynamic temp. sweep experiments
indicated that the thermoplastic PUs exhibited a hysteresis effect in the
heating and cooling processes. It was concluded that the microphase
separation transition or order-disorder transition in thermoplastic PUs could
not be determined from the isochronal dynamic temp. sweep experiment.
The plots of log dynamic storage modulus versus log loss modulus varied
with temp. over the entire range of temps. (110-190C) investigated. 57 refs.
GOODRICH B.F.
USA
Accession no.771897
DOCUMENT DELIVERY SERVICE
Almost all of the documents which are listed in the References and Abstracts section are available in full text form,
as photocopies or pdf files from Rapra Technology Ltds Document Delivery Service. Documents can be delivered
by a variety of methods, including email, post or fax. Customers may pay for individual copies at the time of
ordering by credit card or alternatively open up a deposit account. See the back of this report for further information.
Please contact the Document Delivery Department for availability, current prices and delivery methods.
Document Delivery Department
Rapra Technology Limited, Shawbury, Shrewsbury, Shropshire SY4 4NR, United Kingdom
Telephone: +44 (0)1939 250383 Fax: +44 (0)1939 251118 Email: documents@rapra.net
Location
Companies or
organisations
mentioned
Abstract
Authors and
affiliation
Source of
original article
Title
RAPRA REVIEW REPORTS VOLUME 13
Series Editor Dr. S. Humphreys, Rapra Technology Limited
Rapra Review Reports comprise a unique source of polymer-related information with useful overviews accompanied by abstracts
from hundreds of relevant documents. A Rapra Review Report is an excellent starting point to improve subject knowledge in key
areas. Subscribers to this series build up a bank of information over each year, forming a small library at a very reasonable price. This
series would be an asset to corporate libraries, academic institutions and research associations with an interest in polymer science.
Twelve reports are published in each volume and these can be purchased individually or on a subscription basis.
Format: Soft-backed, 297 x 210 mm, ISSN: 0889-3144
Order individual published Rapra Review Reports (see the following pages for a list of available titles), or purchase a
subscription to Volume 13 (12 issues).
ORDER FORM
Remittance enclosed
Please invoice my company
Please charge my credit card

American Express / Visa / Mastercard (delete as appropriate)
Card Number:
(Please make cheques payable to Rapra
Technology Ltd. in Sterling/US$/Euros via UK
banks only or make payment direct to Account
No: 05625025, Sortcode: 55-50-05, National
Westminster Bank Plc, 8 Mardol Head,
Shrewsbury, Shropshire, SY1 1HE, UK)
Signature: ______________________ Exp. date: _________________
Issuing Bank: ______________________________________________
_________________________________________________________
Cardholders Name (as on card): _______________________________
Cardholders Address: ________________________________________
_________________________________________________________
_________________________________________________________
_________________________________________________________
Postcode: ______________________ Country: __________________
Telephone: _____________________ Fax: ______________________
Company PO#: _____________________________________________
Full Name: ________________________________________________
Company: _________________________________________________
Job Function: ______________________________________________
Delivery Address (if different from Cardholder's Address): _________
_________________________________________________________
_________________________________________________________
Telephone: _____________________ Fax: ______________________
If you would like to receive regular electronic updates informing you of
new titles and offers please enter your E-mail address below.
E-mail: ___________________________________________________
Title of Publication Price /$/
I would like to order ................ subscription(s) to Volume 13 of the Rapra Review Report Series at
630 / US$882 / 1071 each
I would like to order the following Rapra Review Report(s) at 80 / US$120 / 136 each
Report Number(s) ................................................................................................ (please state quantity if more than one)
Please add postage at the following rates: UK 5 total, Overseas 7 / US$11 / 10 per item
Subtotal:
Please add postage at the following rates: UK 35 total, Overseas 65 / US$110 / 110 per subscription
Total Order Value: All prices are subject to change and orders will be charged at the price
indicated on www.polymer-books.com on the date of processing
IMPORTANT - Value Added Tax (VAT)
The above prices do not include VAT. Customers in EU member
countries may be liable to pay VAT if their Registration Number
is not supplied. Please enter your EU Registration Number
(VAT - BTW - IVA - TVA - MWST - MOMS - FPA) below:
VAT Number:
Please Publications Sales, Rapra Technology Limited Tel. +44 (0)1939 250383
Return to: Shawbury, Shrewsbury, Shropshire Fax: +44 (0)1939 251118 www.rapra.net
SY4 4NR, United Kingdom E-mail: publications@rapra.net
Previous Titles Still Available
Volume 1
Report 3 Advanced Composites, D.K. Thomas, RAE, Farnborough.
Report 4 Liquid Crystal Polymers, M.K. Cox, ICI, Wilton.
Report 5 CAD/CAM in the Polymer Industry, N.W. Sandland
and M.J. Sebborn, Cambridge Applied Technology.
Report 8 Engineering Thermoplastics, I.T. Barrie, Consultant.
Report 11 Communications Applications of Polymers,
R. Spratling, British Telecom.
Report 12 Process Control in the Plastics Industry,
R.F. Evans, Engelmann & Buckham Ancillaries.
Volume 2
Report 13 Injection Moulding of Engineering Thermoplastics,
A.F. Whelan, London School of Polymer Technology.
Report 14 Polymers and Their Uses in the Sports and Leisure
Industries, A.L. Cox and R.P. Brown, Rapra
Technology Ltd.
Report 15 Polyurethane, Materials, Processing and
Applications, G. Woods, Consultant.
Report 16 Polyetheretherketone, D.J. Kemmish, ICI, Wilton.
Report 17 Extrusion, G.M. Gale, Rapra Technology Ltd.
Report 18 Agricultural and Horticultural Applications of
Polymers, J.C. Garnaud, International Committee for
Plastics in Agriculture.
Report 19 Recycling and Disposal of Plastics Packaging,
R.C. Fox, Plas/Tech Ltd.
Report 20 Pultrusion, L. Hollaway, University of Surrey.
Report 21 Materials Handling in the Polymer Industry,
H. Hardy, Chronos Richardson Ltd.
Report 22 Electronics Applications of Polymers, M.T.Goosey,
Plessey Research (Caswell) Ltd.
Report 23 Offshore Applications of Polymers, J.W.Brockbank,
Avon Industrial Polymers Ltd.
Report 24 Recent Developments in Materials for Food
Packaging, R.A. Roberts, Pira Packaging Division.
Volume 3
Report 25 Foams and Blowing Agents, J.M. Methven, Cellcom
Technology Associates.
Report 26 Polymers and Structural Composites in Civil
Engineering, L. Hollaway, University of Surrey.
Report 27 Injection Moulding of Rubber, M.A. Wheelans,
Consultant.
Report 28 Adhesives for Structural and Engineering
Applications, C. OReilly, Loctite (Ireland) Ltd.
Report 29 Polymers in Marine Applications, C.F.Britton,
Corrosion Monitoring Consultancy.
Report 30 Non-destructive Testing of Polymers, W.N. Reynolds,
National NDT Centre, Harwell.
Report 31 Silicone Rubbers, B.R. Trego and H.W.Winnan,
Dow Corning Ltd.
Report 32 Fluoroelastomers - Properties and Applications,
D. Cook and M. Lynn, 3M United Kingdom Plc and
3M Belgium SA.
Report 33 Polyamides, R.S. Williams and T. Daniels,
T & N Technology Ltd. and BIP Chemicals Ltd.
Report 34 Extrusion of Rubber, J.G.A. Lovegrove, Nova
Petrochemicals Inc.
Report 35 Polymers in Household Electrical Goods, D.Alvey,
Hotpoint Ltd.
Report 36 Developments in Additives to Meet Health and
Environmental Concerns, M.J. Forrest, Rapra
Technology Ltd.
Volume 4
Report 37 Polymers in Aerospace Applications, W.W. Wright,
University of Surrey.
Report 39 Polymers in Chemically Resistant Applications,
D. Cattell, Cattell Consultancy Services.
Report 41 Failure of Plastics, S. Turner, Queen Mary College.
Report 42 Polycarbonates, R. Pakull, U. Grigo, D. Freitag, Bayer
AG.
Report 43 Polymeric Materials from Renewable Resources,
J.M. Methven, UMIST.
Report 44 Flammability and Flame Retardants in Plastics,
J. Green, FMC Corp.
Report 45 Composites - Tooling and Component Processing,
N.G. Brain, Tooltex.
Report 46 Quality Today in Polymer Processing, S.H. Coulson,
J.A. Cousans, Exxon Chemical International Marketing.
Report 47 Chemical Analysis of Polymers, G. Lawson, Leicester
Polytechnic.
Volume 5
Report 49 Blends and Alloys of Engineering Thermoplastics,
H.T. van de Grampel, General Electric Plastics BV.
Report 50 Automotive Applications of Polymers II,
A.N.A. Elliott, Consultant.
Report 51 Biomedical Applications of Polymers, C.G. Gebelein,
Youngstown State University / Florida Atlantic University.
Report 52 Polymer Supported Chemical Reactions, P. Hodge,
University of Manchester.
Report 53 Weathering of Polymers, S.M. Halliwell, Building
Research Establishment.
Report 54 Health and Safety in the Rubber Industry, A.R. Nutt,
Arnold Nutt & Co. and J. Wade.
Report 55 Computer Modelling of Polymer Processing,
E. Andreassen, . Larsen and E.L. Hinrichsen, Senter for
Industriforskning, Norway.
Report 56 Plastics in High Temperature Applications,
J. Maxwell, Consultant.
Report 57 Joining of Plastics, K.W. Allen, City University.
Report 58 Physical Testing of Rubber, R.P. Brown, Rapra
Technology Ltd.
Report 59 Polyimides - Materials, Processing and Applications,
A.J. Kirby, Du Pont (U.K.) Ltd.
Report 60 Physical Testing of Thermoplastics, S.W. Hawley,
Rapra Technology Ltd.
Volume 6
Report 61 Food Contact Polymeric Materials, J.A. Sidwell,
Report 62 Coextrusion, D. Djordjevic, Klckner ER-WE-PA GmbH.
Report 63 Conductive Polymers II, R.H. Friend, University of
Cambridge, Cavendish Laboratory.
Report 64 Designing with Plastics, P.R. Lewis, The Open University.
Report 65 Decorating and Coating of Plastics, P.J. Robinson,
International Automotive Design.
Report 66 Reinforced Thermoplastics - Composition, Processing
and Applications, P.G. Kelleher, New Jersey Polymer
Extension Center at Stevens Institute of Technology.
Report 67 Plastics in Thermal and Acoustic Building Insulation,
V.L. Kefford, MRM Engineering Consultancy.
Report 68 Cure Assessment by Physical and Chemical
Techniques, B.G. Willoughby, Rapra Technology Ltd.
Report 69 Toxicity of Plastics and Rubber in Fire, P.J. Fardell,
Building Research Establishment, Fire Research Station.
Report 70 Acrylonitrile-Butadiene-Styrene Polymers,
M.E. Adams, D.J. Buckley, R.E. Colborn, W.P. England
and D.N. Schissel, General Electric Corporate Research
and Development Center.
Report 71 Rotational Moulding, R.J. Crawford, The Queens
University of Belfast.
Report 72 Advances in Injection Moulding, C.A. Maier,
Econology Ltd.
Volume 7
Report 73 Reactive Processing of Polymers, M.W.R. Brown,
P.D. Coates and A.F. Johnson, IRC in Polymer Science
and Technology, University of Bradford.
Report 74 Speciality Rubbers, J.A. Brydson.
Report 75 Plastics and the Environment, I. Boustead, Boustead
Consulting Ltd.
Report 76 Polymeric Precursors for Ceramic Materials,
R.C.P. Cubbon.
Report 77 Advances in Tyre Mechanics, R.A. Ridha, M. Theves,
Goodyear Technical Center.
Report 78 PVC - Compounds, Processing and Applications,
J.Leadbitter, J.A. Day, J.L. Ryan, Hydro Polymers Ltd.
Report 79 Rubber Compounding Ingredients - Need, Theory
and Innovation, Part I: Vulcanising Systems,
Antidegradants and Particulate Fillers for General
Purpose Rubbers, C. Hepburn, University of Ulster.
Report 80 Anti-Corrosion Polymers: PEEK, PEKK and Other
Polyaryls, G. Pritchard, Kingston University.
Report 81 Thermoplastic Elastomers - Properties and Applications,
J.A. Brydson.
Report 82 Advances in Blow Moulding Process Optimization,
Andres Garcia-Rejon,Industrial Materials Institute,
National Research Council Canada.
Report 83 Molecular Weight Characterisation of Synthetic
Polymers, S.R. Holding and E. Meehan, Rapra
Technology Ltd. and Polymer Laboratories Ltd.
Report 84 Rheology and its Role in Plastics Processing,
P. Prentice, The Nottingham Trent University.
Volume 8
Report 85 Ring Opening Polymerisation, N. Spassky, Universit
Pierre et Marie Curie.
Report 86 High Performance Engineering Plastics,
D.J. Kemmish, Victrex Ltd.
Report 87 Rubber to Metal Bonding, B.G. Crowther, Rapra
Technology Ltd.
Report 88 Plasticisers - Selection, Applications and Implications,
A.S. Wilson.
Report 89 Polymer Membranes - Materials, Structures and
Separation Performance, T. deV. Naylor, The Smart
Chemical Company.
Report 90 Rubber Mixing, P.R. Wood.
Report 91 Recent Developments in Epoxy Resins, I. Hamerton,
University of Surrey.
Report 92 Continuous Vulcanisation of Elastomer Profiles,
A. Hill, Meteor Gummiwerke.
Report 93 Advances in Thermoforming, J.L. Throne, Sherwood
Technologies Inc.
Report 94 Compressive Behaviour of Composites,
C. Soutis, Imperial College of Science, Technology
and Medicine.
Report 95 Thermal Analysis of Polymers, M. P. Sepe, Dickten &
Masch Manufacturing Co.
Report 96 Polymeric Seals and Sealing Technology, J.A. Hickman,
St Clair (Polymers) Ltd.
Volume 9
Report 97 Rubber Compounding Ingredients - Need, Theory
and Innovation, Part II: Processing, Bonding, Fire
Retardants, C. Hepburn, University of Ulster.
Report 98 Advances in Biodegradable Polymers, G.F. Moore &
S.M. Saunders, Rapra Technology Ltd.
Report 99 Recycling of Rubber, H.J. Manuel and W. Dierkes,
Vredestein Rubber Recycling B.V.
Report 100 Photoinitiated Polymerisation - Theory and
Applications, J.P. Fouassier, Ecole Nationale Suprieure
de Chimie, Mulhouse.
Report 101 Solvent-Free Adhesives, T.E. Rolando, H.B. Fuller
Company.
Report 102 Plastics in Pressure Pipes, T. Stafford, Rapra
Technology Ltd.
Report 103 Gas Assisted Moulding, T.C. Pearson, Gas Injection Ltd.
Report 104 Plastics Profile Extrusion, R.J. Kent, Tangram
Technology Ltd.
Report 105 Rubber Extrusion Theory and Development,
B.G. Crowther.
Report 106 Properties and Applications of Elastomeric
Polysulfides, T.C.P. Lee, Oxford Brookes University.
Report 107 High Performance Polymer Fibres, P.R. Lewis,
The Open University.
Report 108 Chemical Characterisation of Polyurethanes,
M.J. Forrest, Rapra Technology Ltd.
Volume 10
Report 109 Rubber Injection Moulding - A Practical Guide,
J.A. Lindsay.
Report 110 Long-Term and Accelerated Ageing Tests on Rubbers,
R.P. Brown, M.J. Forrest and G. Soulagnet,
Report 111 Polymer Product Failure, P.R. Lewis,
The Open University.
Report 112 Polystyrene - Synthesis, Production and Applications,
J.R. Wnsch, BASF AG.
Report 113 Rubber-Modified Thermoplastics, H. Keskkula,
University of Texas at Austin.
Report 114 Developments in Polyacetylene - Nanopolyacetylene,
V.M. Kobryanskii, Russian Academy of Sciences.
Report 115 Metallocene-Catalysed Polymerisation, W. Kaminsky,
University of Hamburg.
Report 116 Compounding in Co-rotating Twin-Screw Extruders,
Y. Wang, Tunghai University.
Report 117 Rapid Prototyping, Tooling and Manufacturing,
R.J.M. Hague and P.E. Reeves, Edward Mackenzie
Consulting.
Report 118 Liquid Crystal Polymers - Synthesis, Properties and
Applications, D. Coates, CRL Ltd.
Report 119 Rubbers in Contact with Food, M.J. Forrest and
J.A. Sidwell, Rapra Technology Ltd.
Report 120 Electronics Applications of Polymers II, M.T. Goosey,
Shipley Ronal.
Volume 11
Report 121 Polyamides as Engineering Thermoplastic Materials,
I.B. Page, BIP Ltd.
Report 122 Flexible Packaging - Adhesives, Coatings and
Processes, T.E. Rolando, H.B. Fuller Company.
Report 123 Polymer Blends, L.A. Utracki, National Research
Council Canada.
Report 124 Sorting of Waste Plastics for Recycling, R.D. Pascoe,
University of Exeter.
Report 125 Structural Studies of Polymers by Solution NMR,
H.N. Cheng, Hercules Incorporated.
Report 126 Composites for Automotive Applications, C.D. Rudd,
University of Nottingham.
Report 127 Polymers in Medical Applications, B.J. Lambert and
F.-W. Tang, Guidant Corp., and W.J. Rogers, Consultant.
Report 128 Solid State NMR of Polymers, P.A. Mirau,
Lucent Technologies.
Report 129 Failure of Polymer Products Due to Photo-oxidation,
D.C. Wright.
Report 130 Failure of Polymer Products Due to Chemical Attack,
D.C. Wright.
Report 131 Failure of Polymer Products Due to Thermo-oxidation,
D.C. Wright.
Report 132 Stabilisers for Polyolefins, C. Krhnke and F. Werner,
Clariant Huningue SA.
Volume 12
Report 133 Advances in Automation for Plastics Injection
Moulding, J. Mallon, Yushin Inc.
Report 134 Infrared and Raman Spectroscopy of Polymers,
J.L. Koenig, Case Western Reserve University.
Report 135 Polymers in Sport and Leisure, R.P. Brown.
Report 136 Radiation Curing, R.S. Davidson, DavRad Services.
Report 137 Silicone Elastomers, P. Jerschow, Wacker-Chemie GmbH.
Report 138 Health and Safety in the Rubber Industry, N. Chaiear,
Khon Kaen University.
Report 139 Rubber Analysis - Polymers, Compounds and
Products, M.J. Forrest, Rapra Technology Ltd.
Report 140 Tyre Compounding for Improved Performance,
M.S. Evans, Kumho European Technical Centre.
Report 141 Particulate Fillers for Polymers, Professor R.N.
Rothon, Rothon Consultants and Manchester
Metropolitan University.
Report 142 Blowing Agents for Polyurethane Foams, S.N. Singh,
Huntsman Polyurethanes.
Report 143 Adhesion and Bonding to Polyolefins, D.M. Brewis
and I. Mathieson, Institute of Surface Science &
Technology, Loughborough University.
Report 144 Rubber Curing Systems, R.N. Datta, Flexsys BV.
Volume 13
Report 145 Multi-Material Injection Moulding, V. Goodship and
J.C. Love, The University of Warwick.
Report 146 In-Mould Decoration of Plastics, J.C. Love and
V. Goodship, The University of Warwick
Report 147 Rubber Product Failure, Roger P. Brown
Report 148 Plastics Waste Feedstock Recycling, Chemical
Recycling and Incineration, A. Tukker, TNO
ISBN 1-85957-333-9
Martin J. Forrest
(Rapra Technology Limited)
1
Contents
1. Introduction.............................................................................................................................................. 3
2. Analytical Techniques ............................................................................................................................. 3
2.1 Wet Chemistry Techniques ............................................................................................................. 3
2.2 Spectroscopic Techniques ............................................................................................................... 4
2.2.1 Infrared Spectroscopy (IR) ................................................................................................. 4
2.2.2 Ultraviolet Light Spectroscopy (UV) ................................................................................. 4
2.2.3 Nuclear Magnetic Resonance Spectroscopy (NMR) ......................................................... 4
2.2.4 Atomic Absorption Spectroscopy (AAS) ........................................................................... 4
2.2.5 X-Ray Fluorescence Spectroscopy (XRF) ......................................................................... 5
2.2.6 Raman Spectroscopy .......................................................................................................... 5
2.3 Chromatographic Techniques ......................................................................................................... 5
2.3.1 Gas Chromatography-Mass Spectrometry (GC-MS) ......................................................... 5
2.3.2 Gas Chromatography (GC) ................................................................................................ 6
2.3.3 High Performance Liquid Chromatography (HPLC) ......................................................... 6
2.3.4 Liquid Chromatography-Mass Spectroscopy (LC-MS) ..................................................... 6
2.3.5 Gel Permeation Chromatography (GPC) ........................................................................... 6
2.3.6 Thin Layer Chromatography (TLC) ................................................................................... 7
2.4 Thermal Techniques ........................................................................................................................ 7
2.4.1 Differential Scanning Calorimetry (DSC) ......................................................................... 7
2.4.2 Dynamic Mechnanical Thermal Analysis (DMTA) ........................................................... 8
2.4.3 Thermogravimetric Analysis (TGA) .................................................................................. 9
2.5 Elemental Techniques ................................................................................................................... 12
2.6 Microscopy Techniques ................................................................................................................ 12
2.7 Miscellaneous Techniques ............................................................................................................ 12
3. Determination of Molecular Weight and Microstructure of Plastic Polymers................................ 12
3.1 Determination of Molecular Weight ............................................................................................. 12
3.1.1 Gel Permeation Chromatography (GPC) ......................................................................... 13
3.1.2 Viscosity ........................................................................................................................... 14
3.1.3 Osmometry ....................................................................................................................... 14
3.1.4 Light Scattering ................................................................................................................ 14
3.1.5 Other Methods .................................................................................................................. 15
3.2 Monomer Types and Microstructure ............................................................................................ 15
4. Determination of Polymer Type ........................................................................................................... 15
5. Determination of the Plasticiser and Filler in a Plastic Compound ................................................. 19
5.1 Determination of Plasticiser ......................................................................................................... 19
5.2 Determination of Fillers ................................................................................................................ 19
5.2.1 Particulate Fillers .............................................................................................................. 19
5.2.2 Fibrous Fillers ................................................................................................................... 20
6. Determination of Stabilisers in a Plastics Compound ....................................................................... 21
6.1 UV Stabilisers ............................................................................................................................... 21
6.2 Antioxidants .................................................................................................................................. 22
2
The views and opinions expressed by authors in Rapra Review Reports do not necessarily reflect those of
Rapra Technology Limited or the editor. The series is published on the basis that no responsibility or
liability of any nature shall attach to Rapra Technology Limited arising out of or in connection with any
utilisation in any form of any material contained therein.
7. Determination of Functional Additives ............................................................................................... 24
7.1 Process Aids and Lubricants ......................................................................................................... 24
7.2 Slip Additives ................................................................................................................................ 25
7.3 Pigments........................................................................................................................................ 25
7.4 Antistatic Agents ........................................................................................................................... 25
7.5 Crosslinking Agents and Co-Agents............................................................................................. 26
7.6 Blowing Agents............................................................................................................................. 27
7.7 Flame Retardants .......................................................................................................................... 28
7.8 Impact Modifiers........................................................................................................................... 28
8. Analysis of Plastics for Food Contact Use ........................................................................................... 28
8.1 Global Migration Tests ................................................................................................................. 29
8.2 Specific migration and residual monomer tests............................................................................ 30
9. Determination of Stabilisers in PVC ................................................................................................... 31
10. Analysis of Plastic Laminates and Fibres............................................................................................ 32
11. Surface Analysis of Plastics................................................................................................................... 34
11.1 X-Ray Photoelectron Spectroscopy (XPS) ................................................................................... 34
11.2 Laser Induced Mass Analysis (LIMA) ......................................................................................... 34
11.3 Secondary Ion Mass Spectroscopy (SIMS) .................................................................................. 36
12. Failure Diagnosis ................................................................................................................................... 36
12.1 Common Compositional Problems ............................................................................................... 36
12.2 Environmental Stress Cracking .................................................................................................... 37
12.3 Contamination Problems .............................................................................................................. 37
12.4 Odour and Emissions Problems .................................................................................................... 37
13. Conclusions............................................................................................................................................. 38
Additional References ................................................................................................................................... 39
Appendix 1. Solubility Parameters of Plastics, Plasticisers and Typical Solvents .................................. 41
Appendix 2. Specific Gravities of Plastics and Compound Ingredients .................................................. 43
Abbreviations and Acronyms ....................................................................................................................... 45
Abstracts from the Polymer Library Database .......................................................................................... 47
Subject Index ............................................................................................................................................... 133
3
1 Introduction
Plastics present chemical analysts with one of their most
difficult, but satisfying, challenges. In order to obtain
useful products that perform under a variety of
demanding conditions, the plastic matrix can be tailor
made by the bringing together of a wide range of
polymers and additives. There is a very wide range of
polymer types available and in some cases they are
blended together. The technology of plastics is therefore
a mature one, allowing fine tuning of a compound to fit
a number of design criteria and product requirements.
The choice of materials available means that plastics
can be used in many applications, ranging from
replacement windows to packaging materials, and
from mundane products such as disposable cutlery to
highly specialised components in electrical and
aerospace products.
The plastics analyst has therefore to bear in mind the
possible complexity of the system that confronts him
and the potential interferences that may be brought
into play. When reverse engineering a plastic
compound a considerable number of elemental,
spectroscopic, chromatographic and thermal
techniques have to be used in an integrated and
structured approach in order to accumulate and cross
check the data necessary for an accurate result. With
sufficient experience and access to the necessary
instrumental techniques, it should be possible for the
analyst to successfully elucidate a formulation. The
determination of the particular grade of plastic,
although a consistent request, is however rarely
possible. This is mainly due to the fact that a number
of manufacturers produce very similar, if not identical,
products or that the material has been specially
compounded for a particular purpose. Commercial
confidentiality can also restrict the ability to use the
analytical data to identify a particular manufacturers
product as a significant amount of compositional
information may not be disclosed.
The objective of this review is to present, as fully as is
possible within this format, an introduction to the
techniques and methods that are used to characterise
and carry out quality control work on plastics; to
investigate the failure of plastic products; and to
deformulate plastic compounds.
With respect to the last category, the analysts job when
characterising unknowns is always made much easier
if at least some information is available on the sample
and the types of species that may be present in it. Armed
with this knowledge they can work much more
efficiently and obtain better results. To assist in the
acquisition of this knowledge opportunities have been
taken within the text to not only detail the analytical
methods, but provide examples of the species that they
may be used to detect and quantify. In other words, in
order to have a full understanding of the principles
behind and surrounding the analytical methods and
approaches it is vital to have an understanding of plastic
technology itself.
Relevant books and academic papers are cited
throughout the review, but there are also a number of
general texts which will provide useful further reading
(79, 199, 315, 377, 387, 398, a.1-a7).
The appendices provide useful additional information.
Appendix 1 gives solubility parameters of a range of
materials. Appendix 2 lists the specific gravities of a
range of plastics and compounding ingredients.
2 Analytical Techniques
2.1 Wet Chemistry Techniques
Before the advent of modern instrumental techniques,
plastic analysis relied on a sequence of wet chemistry
reactions to determine information such as the generic
polymer type of a material.
The amount of wet chemistry carried out in the modern
polymer analysis laboratory in the 21st Century is
minimal. There are some tests which can still be
grouped under this heading, although even some of
these can employ an instrumental technique to provide
the final answer.
One such method is the oxygen flask combustion
method, which can be used on PVC products to
determine the amount of PVC in the formulation by
quantifying the chlorine present.
The oxygen flask method (ISO 6528.1-1992 and BS
7164 Section 23.1- 1993) uses an initial burn in oxygen
(although the sample is trapped between two platinum
gauge flags) and trapping of the volatile products in
an absorbing solution comprising 1-5 ml of 0.05M
potassium hydroxide, 0.2 ml of 30% hydrogen peroxide
and 10 ml of distilled water. Once the volatiles have
been trapped there is a choice of analytical method. A
titration can be performed, or ion chromatography can
be used to quantify the chloride ion.
4
2.2 Spectroscopic Techniques
2.2.1 Infrared Spectroscopy (IR)
Infrared spectroscopy (IR) is used extensively in the
analysis of plastics. It is a very good, relatively quick
technique for the determination of the polymer present
in a plastic product. Unlike rubbers, where the majority
of compounds contain additives such as carbon black
and plasticisers that can interfere with the infrared data
obtained, it is normally possible to record infrared spectra
directly from the plastic sample using either a surface
technique (e.g., attenuated total reflectance (ATR)
spectroscopy) or in transmission through the sample
from a film produced by pressing a specimen above its
glass transition or melting point.
Some plasticised plastics products (e.g., PVC or nylon
11) will need to be extracted with a solvent (e.g.,
methanol) first to remove the plasticiser. Products that
are filled (e.g., polypropylene/talc kettle bodies) will
require a pyrolysis technique where a pyrolysis
condensates infrared library, such as the one published
by Rapra Technology, needs to be available.
It is also possible with amorphous plastics that are soluble
in conventional solvents (e.g., chloroform) at room
temperature to record infrared spectra from films cast
from solution. This approach has the drawback that all
the solvent needs to be removed from the film if
interference bands are to be avoided.
Analysis of the solvent extract obtained to prepare the
plastic sample for an IR technique can be used to identify
the plasticiser present in a compound. IR analysis of an
ash of the compound obtained by heating at 550 C can
help to identify inorganic fillers. IR can also be used to
identify specialist additives such as fire retardants.
2.2.2 Ultraviolet Light Spectroscopy (UV)
Although not as universally used as IR, UV is another
spectroscopic technique which has a role to play in the
analysis of plastics. It is used in the qualitative and
quantitative analysis of additives, particularly
antioxidants and UV stabilisers.
2.2.3 Nuclear Magnetic Resonance Spectroscopy
(NMR)
NMR is a powerful tool for the determination of
polymer structure. It is at its most sensitive when used
on analytes in solution. Table 1 gives examples of
solvents used for NMR. Amorphous plastics, such as
polystyrene can be dissolved in deuterated chloroform,
whereas for the less soluble semi-crystalline plastics
(e.g., PET) solvents such as trichloroacetic acid have
to be used. Of the conventional instruments, both proton
and carbon 13 instruments have been used in plastics
analysis. Combinations of two solvents can be used to
achieve a good degree of solubility and elevated
temperatures (e.g., 70 C) are also common. The proton
NMR solvents can be used for carbon 13 experiments,
but the reverse is rarely the case.
Techniques are available for work on a specific plastic
type, e.g., in the analysis of polyvinylidene fluoride,
fluorine 19 NMR can be used. In this case a solvent
such as dimethylformamide is employed.
The
13
C NMR spectrum for a polypropylene-
polyethylene copolymer is shown in Figure 1. The
spectrum was obtained at 90 C in a solution of ortho-
dichlorobenzene. The major peaks at 21, 27 and 46
ppm are due to the polypropylene, with the other, minor
peaks being due to polyethylene.
2.2.4 Atomic Absorption Spectroscopy (AAS)
This technique, and the related inductively coupled
plasma (ICP), are used where it is necessary to quantify
metals in a plastic compound. Although not often
required it can be of use in the analysis of flame
retardant systems, where additives such as antimony
trioxide and zinc borate have been used.
s c i t s a l p n o k r o w R M N n i d e s u s t n e v l o s f o s e l p m a x E 1 e l b a T
R M N n o t o r P R M N 3 1 n o b r a C
m r o f o r o l h c d e t a r e t u e D o h t r O e n e z n e b o r o l h c i d
d i c a c i t e c a o r o u l f i r T e n e z n e b o r o l h c i r T
e n e z n e b d e t a r e t u e D e n a t p e h , . g . e , s n o b r a c o r d y h c i t a h p i l A
e n a h t e d e t a r e t u e d - o r o l h c a r t e T - 2 , 2 , 1 , 1
5
2.2.5 X-Ray Fluorescence Spectroscopy (XRF)
This technique is very useful for obtaining semi-
quantitative elemental data from plastic compounds and
their ashes. Among other things, it helps to identify
inorganic fillers and pigments in samples. The
technique is usually used in conjunction with IR.
When it comes to analysing small samples, sample
surfaces or contaminants in samples, the scanning
electron microscope (SEM)/XRF combination
(sometimes referred to as energy dispersive analysis
(Edax)) can be a very valuable tool.
2.2.6 Raman Spectroscopy
Until 1986 Raman spectrometers were either dispersive
long focal length double monochromators or shorter
focal length triple monochromators and required highly
trained scientists to obtain good quality data. The advent
of the Fourier Transform (FT)-Raman technique in 1986
significantly reduced data acquisition times and also
brought the technical advantage of suppressing any laser
induced fluorescence within the sample. Further
developments have enabled smaller, low cost, high
performance, quality instruments to be produced and
have led to the development of the Raman microscope -
an instrument analogous to the IR microscope.
This has enabled Raman spectroscopy to be used
routinely for the identification of polymer types and
the analysis of contaminants within polymer samples.
2.3 Chromatographic Techniques
2.3.1 Gas Chromatography-Mass Spectrometry
(GC-MS)
This powerful, versatile technique can be used to
obtain a significant amount of compositional
information on plastic samples. It is particularly useful
in identifying minor components of the sample such
as the stabiliser, antistatic agent and, where
appropriate, the crosslinking system.
It can also be used to investigate the polymer fraction
within a sample when the instrument is fitted with a
pyrolysis unit set at around 600 C.
The technique also plays a role in failure diagnosis by
being able to provide information on odours, and
Figure 1
13
C NMR spectrum of polypropylene-polyethylene copolymer
6
organic contaminants that may have degraded the
plastic matrix.
There are a variety of ways that the sample or fractions
of the sample (e.g., an extract) can be analysed by GC-
MS. These include static headspace, dynamic
headspace, solution injection and pyrolysis.
2.3.2 Gas Chromatography (GC)
This technique can also be used to obtain polymer type
information by use of a pyrolysis approach, although
the technique is less powerful because of the absence
of a mass spectrometer, and a pyrogram fingerprint
has to be used and a comparison made against a library
of known standards.
This technique is also used for the identification and
quantification of additives such as antioxidants and,
where sufficient volatility exists, plasticisers and
organic flame retardants.
2.3.3 High Performance Liquid Chromatography
(HPLC)
HPLC can be used to identify and quantify additives
that are either too involatile or insufficiently stable to
be determined by GC/GC-MS. This is particularly the
case with antioxidants such as Irganox 1010 and 1036.
HPLC also comes into its own in the quantification of
plasticisers such as dioctyl phthalate (DOP).
2.3.4 Liquid Chromatography-Mass Spectroscopy
(LC-MS)
This instrument is essentially a coupling of an HPLC
with a mass selective detector and as such offers a
significant enhancement in performance to the polymer
chemist. Although such combinations have been around
for many years, they were complex and expensive (i.e.,
effectively research tools only), and it is only within
the last five years or so that single quadrupole benchtop
LC-MS systems have become reasonably common
place due to their relative ease of use and cost.
A mass spectrometer can be the ideal detector for
liquid chromatography because it offers both
universality and the required selectivity for complex
analytical problems. For many years development
work has concentrated particular on the design of
the interface between the chromatograph and the
detector. Today, the two most popular types of
interface for the benchtop single quadrupole LC-MS
are the particle beam interface and the atmospheric
pressure ionisation (API) interface. The particle
beam interface is used to generate electron ionisation
(EI) spectra and the API interface is used to generate
either electrospray (ESI) or atmospheric pressure
chemical ionisation (APCI) spectra. A further
complexity is that the API interface can generate
ei t her posi t i ve (i . e. , mol ecul ar i on pl us one
hydrogen) spectra or negative (i.e., molecular ion
minus one hydrogen) spectra.
The particle beam interface is very good for
qualitative work because the 70 eV spectra contain
a significant amount of structural information and
can be searched against conventional mass spectra
libraries. However, in the full scan mode the
sensitivity is restricted to the low nanogram levels.
In the case of the API interface, both the electrospray
and APCI modes are soft ionisation techniques which
leave the molecular ion (or pseudomolecular ion)
intact without much fragmentation. The interface
therefore offers more sensitivity and is ideal for
quantitative work at low levels (e.g., contamination
of drug and food matrices by polymer additives/
breakdown products).
2.3.5 Gel Permeation Chromatography (GPC)
For this technique to be successful the sample must
be readily soluble in an organic solvent. It has a wide
application in the analysis of plastic samples. It is
possible to obtain molecular weight data on both
amorphous plastics and semi-crystalline plastics. In
the amorphous case (e.g., polystyrene), the system
used is set around ambient temperature (30 C) and
solvents such as THF, chloroform and toluene are
used. Wi t h semi -cryst al l i ne pl ast i cs (e. g. ,
polyolefins), more aggressive solvents such as ortho-
dichlorobenzene and meta-cresol are used at elevated
(140 C) temperatures.
In the case of some complex plastic systems (e.g.,
blends), the development of interfaces such as the
Lab Connections LC Transform, have proved very
useful in increasing the amount of information that
can be obtained in a GPC analysis by enabling IR
data to be recorded on the resultant chromatogram.
Hence, with the correct choice of separating column,
polymer blends can be separated and identified as
well as plasticisers.
7
2.3.6 Thin Layer Chromatography (TLC)
TLC is a relatively simple technique that can be used
for both the separation and identification of additives
such as antioxidants and UV stabilisers. A number of
approaches are possible using different developing
solvents and spraying agents.
It is also the case that TLC can be used in a preparative
way for the isolation of sample fractions for subsequent
chromatographic or spectroscopic analysis.
TLC does have the image of being somewhat old
fashioned and it is to be expected that the market
penetration of LC-MS systems will further erode the
standing of this technique in the modern analytical
laboratory.
2.4 Thermal Techniques
2.4.1 Differential Scanning Calorimetry (DSC)
DSC is used extensively in the analysis of plastics,
particularly those that are semi-crystalline - polyolefins,
nylons, polyesters, etc. It is sensitive enough to
differentiate between different polyethylenes (i.e.,
LDPE, LLDPE, HDPE, etc.) from their melting points
and the appearance of their melting endotherms as well
as being able to detect and, with appropriate standard
materials, quantify plastic blends, e.g., PP/PE and nylon
6/nylon 6,6.
The DSC trace for a quenched sample of PET is shown
in Figure 2. This trace shows the T
g
(around 75 C) of
the material, the exothermic formation of the crystalline
phase (at 156.9 C) and the endotherm due to the
melting of this phase (at 255 C).
The DSC trace of a plastic blend is shown in Figure 3.
The data obtained has been compared to standards and
the material has been shown to be a blend of ethylene-
vinyl acetate copolymer (EVA) and LDPE. The
approximate proportions of each is EVA 15-20%/LDPE
20-25%. In addition the EVA copolymer is thought to
contain around 20-25% of vinyl acetate (VA).
Although not as sensitive as dynamic mechanical
thermal analysis (DMTA) to glass transitions, DSC can
be used to identify a plastic from the glass transition in
its thermogram. The glass transition (T
g
) and crystalline
melting temperatures (T
m
) of a range of plastics are
given in Table 2.
Figure 2
DSC trace for a quenched sample of PET
8
Figure 3
DSC trace of a blend of EVA and LDPE
It is also possible to use DSC to provide quality control
fingerprint thermograms from which deviations in the
composition of a plastic compound can be detected.
One reason for this is that although the technique is
not capable of determining the molecular weight of a
plastic, differences in molecular weight will be apparent
in the melting endotherm region.
Using appropriate standard materials it is also
possible to use DSC to quantify the level of certain
additives, e.g., peroxides, in a sample.
DSC can also be used in thermal stability studies of
the plastic compound, and to investigate the
effectiveness of antidegradants and fire retardants.
2.4.2 Dynamic Mechnanical Thermal Analysis
(DMTA)
DMTA is very useful for generating modulus versus
temperature data on plastic compounds. The effects
of temperature on this important material property can
be obtained over a wide temperature range (typically
150 C to +200 C), along with the glass transition
temperature and information on thermal stability.
The use of DMTA to differentiate between plastic
samples that have a similar chemical composition, but
very different physical properties is shown in
Figure 4. Both of these samples are polymethyl-
methacrylate (PMMA), but the top one is crosslinked
having been prepared with a small amount of
difunctional monomer and the bottom sample is the
standard thermoplastic material. It can be seen that
the crosslinked sample does not melt and the modulus
does not fall away significantly until thermal
degradation occurs.
The sensitivity of DMTA to glass transition
temperatures (approximately 1,000 times greater than
DSC which measures heat capacity changes rather than
modulus) is very useful in the analysis of plastics and
their blends.
9
2.4.3 Thermogravimetric Analysis (TGA)
This technique is useful in the analysis of compounded
plastic samples. It is possible to obtain accurate
quantifications of the principal compound constituents
such as plasticiser, polymer and inorganic species.
This data can be obtained on small (e.g., 10 mg)
samples in a relatively short time (around 45 minutes).
By the use of the temperature maxima at which weight
events occur it is also possible to use the technique to
obtain some qualitative assignments for the plasticiser
and polymer.
A typical TGA programme would be:
Heat from ambient to 550 C in a nitrogen atmosphere
at 20 C/min until no further weight loss occurs. Then,
reduce the heat to 300 C, change the atmosphere to
air and heat at 20 C/min to 1,000 C.
It is common to plot the weight loss derivative in
conjunction with the weight loss, and this can be used
to detect the presence of a polymer blend of two or more
components. Thermal decomposition temperatures of a
range of plastics are shown in Table 3.
T ( n o i t i s n a r t s s a l G 2 e l b a T
g
T ( s e r u t a r e p m e t g n i t l e m e n i l l a t s y r c d n a )
m
s c i t s a l p f o e g n a r a f o )
e p y T s c i t s a l P T
g
( ) C T
m
( ) C
e n e l y h t e y l o P 0 2
) E P D L ( 5 0 1
) E P D M ( 5 1 1
) E P D H ( 5 3 1
e n e l y p o r p y l o P 5 0 6 1
e n e - 1 - t u b y l o P 0 2 0 2 1
e n e - 1 - t n e p y l o P 4 2 0 7
E F T P 5 1 1 7 2 3
) E F T C P ( e n e l y h t e o r o u l f i r t o r o l h c y l o P 2 5 1 2 2
l o h o c l a l y n i v y l o P 0 7 T w o l e b s e s o p m o c e D
g
e d i r o l h c l y n i v y l o P 0 8 -
e d i r o l h c e n e d i l y n i v y l o P 8 1 0 9 1
e l i r t i n o l y r c a y l o P 0 4 1 o t 0 8 -
e n e r y t s y l o p c i t c a t A 5 9 -
e n e r y t s y l o p c i t c a t o s I 0 0 1 0 3 2
T E P 7 6 6 5 2
e t a l y r c a h t e m l y h t e M 0 0 1 -
A l o n e h p s i b f o e t a n o b r a c y l o P 0 5 1 5 2 2
A l o n e h p s i b f o e n o f l u s y l o P 5 9 1 -
6 n o l y N 0 5 5 1 2
6 , 6 n o l y N 0 6 6 6 2
e d i x o e n e l y h t e y l o P 5 5 6 6
e d i x o e n e l y p o r p y l o P 2 6 5 6
r e h t e l y h t e m l y n i v y l o P 1 3 4 4 1
r e h t e l y h t e l y n i v y l o P - 6 8
l y n i v y l o P t r e h t e l y t u b - - 0 5 2
10
Figure 4
DMTA results for (a) crosslinked and (b) standard grades of PMMA
11
Other uses for the technique include the production of
compositional fingerprints for quality control purposes
and the investigation of thermal stability and the effects
that additives such as flame retardants and antioxidants
have on it.
It is possible to interface modern TGA instruments directly
to IR instruments or mass spectrometers, thus obtaining
both quantitative and qualitative data in one analytical step.
The introduction of high resolution TGA instruments
has enabled more accurate quantifications of minor
weight loss events to be made. For example, the use of
high resolution TGA to quantify the amount of residual
monomer in a sample of polymethylmethacrylate is
shown in Figure 5. The residual monomer weight loss
event peaks at 297.5 C.
s c i t s a l p f o e g n a r a f o s e r u t a r e p m e t n o i t i s o p m o c e d l a m r e h T 3 e l b a T
e p y T c i t s a l P ( * n o i t i s o p m o c e d % 0 5 e v e i h c a o t e r u t a r e p m e T ) C
e d i r o l h c l y n i v y l o P 0 6 2
e t a l y r c a h t e m l y h t e m y l o P 7 2 3
e n e l y p o r p y l o P 7 8 3
e n e l y h t e y l o P 4 1 4
- y l o P p e n e l y x - 2 3 4
E F T P 9 0 5
e r u t a r e p m e t t a h t t a g n i t a e h e r p s e t u n i m 5 y b d e d e c e r p s e t u n i m 0 3 t a o u c a v n i t h g i e w s t i f l a h s e s o l r e m y l o p e h t h c i h w t a e r u t a r e p m e t e h T *
Figure 5
High resolution TGA of polymethylmethacrylate
12
2.5 Elemental Techniques
The determination of the concentration of certain
elements can be very useful in plastic analysis work.
In particular, it is often necessary to determine the
amount of nitrogen or a halogen such as chlorine or
fluorine in the calculation of polymer content or
polymer blend proportions. Also, the targeting of
specific elements can enable the quantity of a
particular additive (e.g., phosphate flame retardant or
titanium dioxide pigment) to be calculated.
The determination of nitrogen is usually done using
carbon/hydrogen/nitrogen analysers and the technique
is relatively simple and uses small amounts (e.g., 20-
50 mg) of sample.
With the other elements, the technique will vary
according to the element being quantified. Sulfur and
chlorine, for example, can be determined using
oxygen combustion followed by ion chromatography
analysis of the products.
2.6 Microscopy Techniques
High magnification (e.g., 150x) optical microscopy
can be used to examine the dispersion of fillers within
the plastic matrix. The success of this operation is
usually dependent on the generation of high quality
microtome sections of the sample.
The technique of scanning electron microscopy has
already been briefly mentioned in Section 2.2.5 in
relation to the elemental analysis of surfaces in
conjunction with XRF. It can also be used in its own
right, where its high magnification powers can be
employed to determine the particle size of fillers and
in the detailed examination of fracture surfaces.
Transmission electron microscopy (TEM) can be used
to investigate the phase morphology of polymer
blends and the dispersion of fillers.
For other spectroscopic techniques see Section 2.2.
2.7 Miscellaneous Techniques
There are a number of other analytical techniques that
can be used to characterise plastic samples and many
of these feature in the abstracts at the back of this
Review Report. These include X-ray diffraction
(XRD) to identify between different crystalline forms
of inorganic additives (e.g., rutile and anatase forms
of titanium dioxide) and direct probe mass
spectroscopy (for the determination of high molecular
weight antioxidants).
Surface analysis techniques such as secondary ion mass
spectrometry (SIMS), laser induced mass analysis
(LIMA) and X-ray photoelectron spectroscopy (XPS)
are used for failure diagnosis work associated with such
things as poor bonding to substrates and for surface
characterisation work.
A chromatography technique that achieved prominence
in the research literature around ten to fifteen years
ago for the determination of relative high molecular
weight additives (e.g., antioxidants) and the study of
plastic oligomers is supercritical fluid chromatography
(SFC). This is essentially a liquid chromatography
technique that uses similar analytical columns to HPLC
but where the mobile phase is a substance (e.g., carbon
dioxide) that is kept in a supercritical state by a suitable
combination of temperature and pressure. One of the
benefits of the technique is that the analytes can be
easily separated from the mobile phase once the
chromatography has taken place so, for example, they
can be deposited on infrared transparent substrates for
analysis using an infrared microscope. The relatively
expensive nature of the instrumentation and the
development of other techniques (e.g., LC-MS) have
restricted its market penetration.
3 Determination of Molecular Weight
and Microstructure of Plastic
Polymers
This section covers analytical techniques that can be
applied both to uncompounded plastic resins and
compounded materials.
3.1 Determination of Molecular Weight
In common with other polymers, plastics have a
distribution of molecular weights. This distribution will
be widest for polymers produced by free radical
polymerisation (e.g., polystyrene) and narrowest for
plastics produced using specialised catalyst systems
such as metallocenes.
There are a number of ways in which the molecular
weight distribution of a plastic can be expressed:
13
Mn = Number average molecular weight = Sum nM
Sum n
Mw = Weight average molecular weight = Sum nM2
Sum nM
Mz = Z average molecular weight = Sum nM3
Sum nM2
where n = the number of molecules of molar mass M.
The Z average is very sensitive to high molecular
weight molecules within the polymer. The weight
average is always of greater value than the number
average. A measure of the breadth of the molecular
distribution of the polymer can be obtained by dividing
the weight average by the number average:
Polydispersity = Mw
Mn
As the polymer tends to monodispersity the
polydispersity approaches unity.
There are a wide variety of methods that can be used
to obtain molecular weights. The principal ones are
as follows.
3.1.1 Gel Permeation Chromatography (GPC)
This is the pre-eminent technique and has been refined
and developed extensively over the past 30 years.
It is possible to use it on both uncompounded resins
and plastic compounds and Mn, Mw and Mz values
can be obtained. GPC is essentially a liquid
chromatography technique where the sample is
dissolved in a suitable solvent (e.g., THF for
polystyrene) and injected into a system where the
molecules are separated according to their molecular
size by a column that contains a swollen, particulate,
porous gel packing.
Figure 6 shows the GPC chromatograms for two
polymers that have different molecular weight
distributions but similar calculated molecular weight
averages.
The standard detector for GPC systems is the refractive
index (RI) detector, but a feature of developments over
the past 10 years is the development of double (RI and
viscosity) or triple detector systems (RI, viscosity and
light scattering). These multiple detection systems
provide measures of true molecular weight by
obtaining the actual Mark-Houwink parameters (in the
case of the viscosity detector) for the polymer being
Figure 6
GPC chromatograms for two polymers with different molecular weight distributions but similar
molecular weight averages
14
analysed, as opposed to the polystyrene equivalent
molecular weight from the use of monodisperse
polystyrene calibrants alone. An inherent property of
the light scattering detector is that it provides true
molecular weight data.
It is also possible to use spectroscopic detectors such
as infrared and ultraviolet. One practical use of the
latter is to determine if chemical modifiers (e.g., silane
coupling agents) are bound to polymer molecules.
This is done by measuring the molecular weight
distribution of the modified plastic at a UV
wavelength where the polymer itself does not
contribute to the absorbance and comparing this to
the distribution of the unmodified plastic.
The use of the LC transform module with GPC has
extended its capabilities by allowing IR data to be
generated on the species during the course of an analysis.
This is done by impinging the species onto a germanium
disc which is then placed into a module fitted into the
sample compartment of an IR bench. IR data is collected
on the entire chromatogram using continuous collection
software, which enables the IR spectrum of any particular
section to be viewed. This technique is very useful for
plastic blends and highly compounded plastics such at
PVC, as it allows the polymers in the blend to be
identified, as well as relatively high molecular weight
additives such as plasticisers.
3.1.2 Viscosity
This is a standard procedure for molecular weight
determinations and involves the use of specially
designed viscometers to accurately measure the
viscosity of a polymer solution. From this the intrinsic
viscosity is determined and hence the molecular weight.
The time taken for the polymer solution to pass between
two marks on the viscometer is compared to that of
pure solvent and the ratio is the viscosity of the solution.
Successive dilutions give a range of concentrations and
times from which the intrinsic viscosity can be
calculated. The value for this is then entered into the
Mark-Houwink equation:
Intrinsic viscosity = KM
X
where K and X are constants for the particular solvent
being used and are referred to as the Mark-Houwink
parameters.
Depending on the source of the Mark-Houwink
parameters the molecular weight can be expressed as
either the number or weight average.
3.1.3 Osmometry
There are two principal osmometry techniques: vapour
pressure osmometry and membrane osmometry.
Vapour pressure osmometry involves the indirect
measuring of the lowering of the vapour pressure of a
solvent due to the presence of a solute. It is based on the
measurement of the temperature difference between
droplets of pure solvent and of polymer solution
maintained in an isothermal atmosphere saturated with
the solvent vapour. Calibration is by the analysis of
standards of known molecular weight and should be over
the entire range of molecular weights of interest to ensure
the best results. The technique is useful for polymers
that have molecular weights in the 500-50,000 range.
Membrane osmometry involves the use of a
membrane between the solvent and the polymer
solution that is permeable to the solvent molecules
but not to the solvated polymer molecules. This is
the major restriction on the technique and means that
it cannot be used for low molecular weight polymers
(< approximately 50,000).
3.1.4 Light Scattering
Recent developments in instrumentation have led to a
resurgence of this technique where the weight average
molecular weight is obtained from the light scattering
behaviour of polymer solutions. These developments
have centred around low angle laser light scattering
(LALLS), multi-angle laser light scattering (MALLS)
and evaporative light scattering (ELS). As well as being
stand alone instruments, light scattering detectors have
been developed for GPC systems. MALLS detectors
can provide direct information on the branching ratio
of a polymer (a.8).
Care has to be taken to ensure that the polymer solution
is clear (to reduce variability) and low cell volumes
(0.1 l) and dilute solutions help this. Solvent choice
is also critical, with the best results being with solvents
that have a very different refractive index to the
polymer, and that are low-scattering themselves.
Evaporative light scattering involves the removal of
the solvent from the solvated polymer as it elutes down
a drift tube and the isolated polymer particles then
scatter light from the light source.
Light scattering can produce precise data and has been
used successfully on polymers with molecular weights
ranging from 10,000 to 10,000,000.
15
3.1.5 Other Methods
Other methods include end group analysis (Mn),
ultracentrifugation (Mw) and, indirectly by determining
glass transition temperatures, DSC/DTA.
A review of the determination of the molecular weight
of polymers has been produced by Holding and
Meehan (396).
3.2 Monomer Types and Microstructure
The use of transmission IR, pyrolysis IR and pyrolysis
GC to determine the polymer type of a plastic is covered
in Section 2.1. Where appropriate standards are
available, it is also possible to use IR to quantify the
amounts of monomers in copolymers and terpolymers.
Another technique that is very effective at identifying
the monomers present in a plastic materials is NMR.
The NMR technique will also provide information on
the proportions of the various monomers in copolymers
and tripolymers. In contrast to IR this information can
be obtained without having to analyse standards of
known monomer composition; the areas under the
diagnostic chemical shifts being used.
NMR instruments can also be used to obtain
fundamental structural information on polymers such
as end group chemistry, branch points and structural
isomerism. It is also possible to use IR for the latter,
although some of the isomeric structures have relatively
weak absorptions which makes detection difficult when
they are at a low concentration.
4 Determination of Polymer Type
One of the most basic and useful tests to carry out on a
plastic sample is to determine its polymer type.
Due to their relative simplicity, it is usually possible to
carry out an infrared analysis of the plastic material in
the as received state and identify the plastic by reference
to a standards database. The advent of the single bounce
attenuated total reflectance (ATR) accessories for
Fourier transform infrared spectroscopy (FTIR)
instruments enables this operation to be carried out in
a matter of minutes on a sample a few millimetres in
size. Some care should be taken as the relative
intensities of the bands present in ATR spectra can vary
compared to conventional transmission spectra
(historically used to compile databases) and there is a
slight shifting in the absorption wavenumber value of
the bands.
If more traditional spectra are required, the usual
approach is to press a thin film of the samples using a
temperature which is above the T
g
or T
m
and to record
a transmission spectrum. A transmission infrared
spectrum of polypropylene produced from a film
pressed at 170 C is shown in Figure 7. Another
technique that can be used to obtain transmission
spectra is to dissolve the sample up using a suitable
solvent and to cast a film. Care has to be taken to
remove all of the solvent by drying in an oven otherwise
it can influence the data obtained. A transmission
infrared spectrum of PVC produced from a film cast
from a solution in THF is shown in Figure 8.
For those plastic compounds that contain a plasticiser
and/or organic flame retardant, a certain amount of
preparation work is required to effectively remove the
interference of these constituents. After milling or
comminuting the sample to increase surface area, a
solvent extraction is performed to remove these organic
species. It is then usually possible to record the infrared
spectrum using either an ATR technique or by
transmission through a hot pressed film.
One of the most comprehensive databases available
of plastic infrared spectra has been produced by
Hummel (a.9).
Where the plastic sample contains both a major organic
additive and a filler, it is necessary to pyrolyse the
extracted portion of the sample and then record an
infrared spectrum of the collected pyrolysis
condensates. Providing that an extensive database of
pyrolysate spectra is available (234), this method is
very successful in identifying generic polymer types
and polymer blends. In the case of blends, it is also
possible to express the results semi-quantitatively if
the appropriate standards are available.
If the plastic only contains a filler, the pyrolysis
approach can be employed without using the initial
solvent extraction step.
The pyrolysate infrared spectra of nylon 6 and low
density polyethylene are shown in Figures 9 and 10,
respectively.
Another method which enables the polymer type within
a plastic sample to be identified is pyrolysis gas
chromatography. This method can be applied to either
16
Figure 7
Transmission infrared spectrum of polypropylene produced from a film pressed at 170 C
Figure 8
Transmission infrared spectrum of unplasticised PVC produced from a film cast from a THF solution
17
Figure 9
Pyrolysate infrared spectrum of nylon 6
Figure 10
Pyrolysate infrared spectrum of low density polyethylene
18
the extracted portion of the sample or the sample as
received. In the former case any relatively low molecular
weight plasticiser elutes early on and does not have a
significant influence on the pyrogram as a whole. As
with pyrolysis IR, a database of standards needs to be
put together and then the pyrogram fingerprints of
unknowns can be matched. The temperature that the
pyrolysis unit is set at, and the design of the unit (e.g.,
Curie point or microfurnace), will affect the pyrograms
produced from a particular sample. Again, it is possible
to identify and quantify blends and blend ratios.
Typical experimental conditions for pyrolysis GC
experiments are as follows:
Sample weights 0.1-5.0 mg
Pyrolysis temperatures 400-800 C (microfurnace
and Curie point)
800-1200 C (platinum
filament)
Microfurnace type pyrolyser - specific example using
an SGE Pyrojector
Weight of sample 0.4 mg
Pyrolysis temperature 600 C
Pyrolysis gas Helium at 0.10 MPa
GC column 5% Diphenyl siloxane 30
m x 0.25 mm, 1.0 m film
GC column temperature 2 min at 50 C followed
program by 10 C/min to 280 C
and then 10 min at 280 C
GC carrier gas Helium at 0.06 MPa
GC injector temperature 320 C
Detector Flame ionisation detector
(FID) at 350 C
Adding a mass spectrometer into the system, so that
the technique becomes pyrolysis GC-MS, further
increases the usefulness of the method and the
information that can be obtained.
The principal diagnostic pyrolysis species which can
be detected in pyrograms of plastics are shown in
Table 4.
It can be seen from the above list that certain plastics
unzip to regenerate their monomers whereas other
undergo decomposition reactions to generate
characteristic breakdown products. In reality, a
certain amount of both types of reaction take place
for the majority of polymers and it is the one that
predominates that determines what the major
pyrolysis products will be.
With respect to the quantification of the polymer
component within a plastic compound, the easiest
technique to use is TGA. It is also possible to detect a
blend of polymers with TGA and to often obtain a
semi-quantification of the blend ratio by reference to
the splitting of the weight loss derivative.
Unfortunately, some plastic types (e.g., PVC) undergo
two stage weight loss processes when heated and the
first stage (loss of hydrogen chloride) will overlap
with the volatilisation of organics (e.g., plasticiser)
stage. It is therefore not possible to use TGA alone to
determine the polymer content of these samples.
Another complicating factor is that a number of plastics
(e.g., halogenated, polyamides, polyurethanes,
polyesters, other heteroatom containing systems) do
not completely pyrolyse during the nitrogen
atmosphere region and leave a carbonaceous residue
which essentially oxidises to carbon dioxide in the air
region. This carbonaceous residue, which may to an
extent overlap with any weight loss due to a carbon
black pigment, has to be included in order to obtain an
accurate polymer content.
s c i t s a l p f o s m a r g o r y p n i s e i c e p s s i s y l o r y p c i t s o n g a i D 4 e l b a T
e p y t c i t s a l P s e i c e p S
e n e r y t s y l o P e n e r y t s d n a e n e z n e b l y h t e , e n e u l o t , e n e z n e b
e t a l y r c a h t e m l y h t e m y l o P e t a r y t u b o s i l y h t e m , e t a l y r c a h t e m l y h t e m
e n e l y h t e y l o P n , e n a x e h - n s n o b r a c o r d y h n i a h c t h g i a r t s r e h t o , e n a t n e p -
e n e l y p o r p y l o P e n a t p e h l y h t e m i d - 4 , 2 s a h c u s s n o b r a c o r d y h d e h c n a r b
C V P s e n e z n e b o r o l h c , e n e z n e b , e d i r o l h c n e g o r d y h
19
5 Determination of the Plasticiser and
Filler in a Plastic Compound
5.1 Determination of Plasticiser
Mention has already been made in Section 4 of the
isolation of plasticisers from a plastic matrix by
solvent extraction. Careful choice of solvent is
required to ensure that the polymer itself doesnt
undergo dissolution and that the plasticiser is
selectively isolated. A solvent which has been found
to be useful for polymers such as PVC is methanol.
The ext ract i on i s carri ed out under Soxhl et
conditions with the weight of extract being obtained
from the weight gain of the conditioned solvent
reservoir flask once the solvent has been dried off
at 105 C.
Having quantified the plasticiser present by
ext ract i on i t i s t hen possi bl e t o obt ai n an
identification by the use of transmission IR. There
is an excellent database available (399) which
enables an identification to be made. Where the
plasticisers have distinct IR spectra (e.g., phthalates
and sulfonamides) it is possible to detect the
presence of a blend of plasticisers. If a quantification
of the blend composition is required, though, this is
usually easier to achieve by HPLC then IR.
The TGA technique can usually provide a good
quantification of plasticiser content. Plasticisers that
have higher molecular weights (e.g., so called
polymerised plasticisers) can give problems as the
weight loss event due to their volatilisation can
merge with the pyrolysis weight loss event of the
polymer. As mentioned in the above section,
pol ymers t hat l ose smal l mol ecul es by heat
degradation (e.g., HCl lost by PVC) give more
complicated TGA traces and will require a solvent
extraction step to determine their plasticiser level.
5.2 Determination of Fillers
5.2.1 Particulate Fillers
On some occasions, carbonaceous fillers such as a
conducting black (acetylene black) or graphite are
added to a plastic to enable it to meet certain
conductivity requirements. It is possible to use TGA
to quantify these types of fillers. It is also a useful
way of differentiating between these materials and
conventional carbon black; the former having a
maximum oxidation weight loss around 700 C and
the latter around 550 C.
The TGA trace for an EVA cable covering filled with
a conducting black is shown in Figure 11.
The fact that a number of rubbers (e.g., halogenated,
nitrile and polyurethane) produce carbonaceous
residues during the nitrogen atmosphere region has
already been mentioned in Section 4.1, and care must
be taken to ensure that these do not affect the
quantification of the carbonaceous filler in the air
atmosphere region. Use of a high resolution TGA
instrument will assist in this as it will improve the
separation of the two weight loss events.
TGA is also convenient for the quantification of
inorganic fillers such as barytes, silica and silicates.
The limitation of the technique is that the total
inorganic content of the plastic is obtained, with no
indication of the relative proportion if a blend of
inorganic fillers is present. It is therefore common
practice to complement the TGA data with a least a
semi-quantitative elemental technique such as XRF
in order to obtain qualitative as well as quantitative
data. A useful exception to this rule is where the
compound contains calcium carbonate (a relatively
common diluent filler), in which case the carbonate
will undergo quantitative degradation at around 680-
700 C into carbon dioxide and calcium oxide (which
remains as a residue). It is therefore possible to
quantity the amount of calcium carbonate in the
sample from the carbon dioxide weight loss (which
will represent 44% of the carbonate by mass) and
the remaining quantity of residue will indicate if any
other inorganics are present.
The ot her t echni que commonl y used for t he
quantification and isolation of inorganic materials
(both fillers and additives such as glass fibres) is
furnace ashing. This method is described in ISO
345-1 (1997) and a temperature of 500-600 C is
usually used.
Once t he ash has been obt ai ned, qual i t at i ve
information on the inorganic species present can be
obtained by IR (liquid paraffin mull technique), XRF
or, where the quantification of specific species is
required, ICP.
Some of the principal diagnostic IR absorption bands
for inorganic fillers are given in Table 5.
20
Figure 11
TGA trace for an EVA cable cover compound showing weight loss and derivative weight loss curves
s r e l l i f c i n a g r o n i r o f s d n a b n o i t p r o s b a R I c i t s o n g a i D 5 e l b a T
r e l l i F d n a B
a c i l i S m c 0 0 1 1 - 0 5 0 1 t a s k a e p h c i h w m c 0 3 3 1 - 0 5 9 t a d n a b d a o r B
s e t a c i l i S m c 0 0 1 1 - 0 5 9 t a s k a e p h c i h w m c 0 0 3 1 - 0 5 8 t a d n a b d a o r B
e t a n o b r a c m u i c l a C m c 0 1 7 d n a 0 7 8 , 0 2 4 1
e t a f l u s m u i r a B m c 0 1 6 d n a 0 8 0 1
5.2.2 Fibrous Fillers
In certain applications it is necessary to impart the
strength required to a plastic part by the use of a fibrous
fillers. The following types are among those used:
(1) Glass fibres
(2) Carbon fibres
(3) Synthetic polymer fibres (e.g., nylon)
(4) Wood flour
It is usually obvious whether a plastic contains a fibrous
filler from either a visual inspection or the use of a
relatively low powered optical microscope.
Glass fibres can be isolated and gravimetrically
determined by ashing at 600 C in a muffle furnace.
Higher temperatures (above 700 C) can cause problems
as the glass will eventually reach its melting point.
Confirmation that the fibres are glass can be carried out
using an infrared microscope. The IR microscope will
also give the cellulose spectrum which is expected for
21
the wood flour filler type, and be able to detect the type
of synthetic fibre (e.g., nylon or polypropylene) used
from its characteristic transmission spectrum.
TGA will enable the amount of carbon fibres in a
composite to be quantified. The oxidation temperature
of around 700 C (instead of the 500-600 C
experienced with carbon blacks) will also provide a
confirmation of their presence.
As mentioned above, synthetic polymeric fibres can be
identified by the IR microscope once sufficiently isolated
or, by use of their melting point, by the hot stage
microscope or DSC. In the case of DSC, some
quantification data can be obtained from the size of the
melting endotherm providing standards are available.
6 Determination of Stabilisers in a
Plastics Compound
In common with other polymer systems, to maintain
the physical properties of a plastic compound stabilisers
need to be added to stop, or at least retard, degradation
by a number of agencies (e.g., heat and UV light).
The use of an initial solvent extraction/dissolution step
is common in the analysis of a plastic matrix for
antidegradants, as these species may not be volatile
enough to be removed by heating the sample. In some
cases (e.g., butylated hydroxytoluene) heating a sample
liberates enough of the species to enable an identification
to be made using GC-MS; however quantification will
usually require removal by a solvent (to as near 100%
efficiency as possible). Analysis of the extract can then
be carried out by HPLC, UV spectroscopy, or GC if the
species is heat stable and sufficiently volatile. Relatively
non-specific solvents (i.e., having mid-range solubility
parameters) such as chloroform are good extracting
solvents. Another common approach is to dissolve up
the sample in a suitable solvent and then add a non-
solvent to precipitate the polymer. The stabiliser will
remain in the solvent phase.
If the type of organic antidegradant in a compound is
completely unknown, analysis of the solvent extract
by GC-MS or LC-MS is an excellent method for
identification. Once the identification has been
achieved, a quantification can be carried out using a
preferred method and a validated procedure if available.
Where the antidegradant is not volatile enough to be
identified using a GC based technique, direct probe
mass spectrometry or LC-MS can be used and the
antidegradant identified by reference to its molecular
ion and a database. The direct probe mass spectroscopy
technique can be carried out on samples in the as
received state as well as sample extracts, whereas LC-
MS is only used for extracts.
6.1 UV Stabilisers
There is a large range of commercial UV stabilisers
for plastic materials and a number of analytical
approaches can be used for their detection and
quantification.
The UV stabilisers can be divided into five different
groups:
(a) Benzophenone derivatives
(b) Salicyclic acid esters
(c) Resorcinol esters
(d) Benzotriazole compounds
(e) Coumarin drivatives
In a number of cases specific methods have been
developed to determine a particular stabiliser within a
particular polymer. Some representative methods are
outlined next.
In some cases (e.g., the determination of 2-hydroxy-4-
n-octoxybenzophenone in polyethylene) the stabiliser
has distinctive diagnostic bands and the relative
simplicity of the infrared characteristics of the polymer
matrix enables it to be quantified using transmission
infrared spectroscopy. A thin film of the sample is
produced by hot pressing at 120 C, along with films
of virgin polyethylene containing known amounts of
the stabiliser. The absorbance maxima of the diagnostic
band between 15.8 and 16.2 microns in the standard
films is used to produce a calibration curve from which
the amount of stabiliser in the unknown is calculated.
The method is capable of detecting the stabiliser down
to 0.02% w/w with an accuracy of +/- 5%.
A number of methods use the UV absorbing properties
of the UV stabiliser. For example, Tinuvin 326 can be
detected in polypropylene down to 0.02% w/w by using
an extraction with chloroform under reflux followed
by analysis of the extract using a UV/Vis spectrometer.
The ultraviolet absorption peak at 355 nm is used and
a calibration curve produced by dissolving known
amounts of Tinuvin 326 in chloroform.
Another technique uses the fluorescence of these
compounds. Uvitex OB can be detected in a chloroform
22
solution (0.8% w/v of polymer) of polystyrene by
excitation at 370 nm and recording the fluorescence at
435 nm. Standard solutions at the 0.8 w/v level of virgin
polystyrene and known amounts of Uvitex OB are used
as calibrants.
It is also possible to use gas chromatography (e.g.,
Tinuvin P, Tinuvin 326, Tinuvin 327 and Cyasorb
UV531 in toluene extracts of polyethylenes), thin layer
chromatography (e.g., benzophenone and salicylic acid
types in polyethylenes) and HPLC. This latter method
has been used extensively for the determination of
antioxidants but has not received as much attention in
the literature for UV stabilisers.
It is also the case that the white pigment titanium
dioxide provides protection against UV light and so
this can be added at reasonable high loadings (e.g., 10%
or greater) to products such as window frames. The
amount of titanium dioxide in a plastic can be
determined after acid digestion of the matrix by the
use of an elemental technique such as AAS/ICP.
6.2 Antioxidants
HPLC based techniques have been widely used by
analysts for the determination of antioxidants in plastics
and a review has been provided by Sidwell (400).
The chromatogram obtained for the determination of
Irganox 1076 in an HDPE compound is shown in
Figure 12. An extract of the polymer was analysed
using a C
18
reverse phase column with UV detection at
230 nm and a mobile phase of 70:30 methanol/water
changing to 100% methanol.
There is a useful HPLC method which can be used on
plastics for the detection and quantification of a wide
range (20 species) of antidegradants. The sample is
dissolved up using a suitable solvent at an elevated
temperature if necessary. A non-solvent (e.g., methanol)
is then added and the extract analysed by HPLC using
the following conditions:
Injection volume 25 l
HPLC column Aqua 5 C
18
ODS reverse phase
column 150 mm x 3.0 mm
(or similar)
Mobile phase A= 75:25 Methanol/Water
B= 50:50 Ethyl Acetate/Acetonitrile
Gradient Time %A %B
Initial 90 10
After 25 min 0 100
Flow rate 2.0 ml/min
Figure 12
HPLC chromatogram of HDPE for determining Irganox 1076
23
Detection UV detector set at 270 nm
Temperature 40 C
The following antioxidants are examples of those that
can be determined using this technique:
(1) Irganox 1010
(2) Irganox 1098
(3) Irganox 1076
(4) Irganox 1330
(5) Butylated hydroxytoluene
(6) Irgafos 168
(7) Triclosan
The chromatogram obtained using this method to
separate a complex cocktail of antidegradants is shown
in Figure 13.
The wide applicability of this method is due to the
mobile phase mixture.
The capability of HPLC has been greatly extended by
the commercialisation of affordable liquid
chromatography-mass spectroscopy (LC-MS)
instruments. The mass selective detector enables
unknown samples to be analysed and the antioxidants
present to be identified. The LC-MS technique
therefore compliments GC-MS and, with it, enables
the complete molecular weight/volatility/polarity range
to be covered.
TLC is comparatively easy and cheap to use and it is
both quick and accurate for the identification of
Figure 13
HPLC chromatogram of a complex mixture of antidegradants
24
antioxidants in plastic extracts. Irrespective of the
complexity of the extract composition and the amount
used, this method can be used to give a sharp separation
for identification purposes. Distinctive Rf values and
colours can be seen for each antioxidant depending on
the stationary phase, the developing solvent used and
the detection agent.
TLC, in addition to being used for identification
purposes, can be used in a semi quantitative way;
the logarithm of the spot area being proportional to
the quantity of the analyte in the spot, and this value
being compared to spots containing standard
amounts of the analyte.
Gas chromatography has been used for the analysis of
phenolic and amine type antioxidants. Antioxidants
which have high boiling points cannot be directly by
GC but they can be analysed as derivatives such as
acetates, trifluoroacetates, trimethyl silyl-ethers, methyl
ethers, etc. Trimethyl silane based antioxidants, for
example, give good separations on standard silicone
based columns (a.10).
Benchtop LC-MS instruments are proving to be
excellent tools in the analysis of plastics of unknown
composition to identify and, once this is achieved,
quantify the antioxidant present. Prior to the advent
of LC-MS it was very difficult to use conventional
HPLC for this task because of the large range of
possible compounds.
Using the general analysis conditions shown below a
number of antioxidants can be detected in toluene or
chloroform extracts of plastics:
Sample preparation: Around 5 mg of extract is diluted
1/20 with 80% acetonitrile/water
Instrument: Agilant 1100 series LC-MS
Column: Zorbac SB-C
18
, 5 um,
2.1 mm x 150 mm
Mobile phase: A=water, B=acetonitrile
Gradient Time A B
Initially 15% 85%
after 10 min 1% 99%
or Initially 35% 65%
after 10 min 10% 90%
Flow rate: 0.7 ml/min
Injection volume: 5 l
MS conditions: Atmospheric Pressure Chemical
Ionisation (APCI)
Ion mode: Positive or negative
Vapouriser: 300 C
Scan range: 200-1600 amu
Fragmentor: 70 or 120 volts (The fragmentor
voltage is chosen to modify the
degree of fragmentation and
hence sensitivity)
Antioxidants which have been identified in polyolefins
using the above conditions include:
Irgafos 168
Irganox 1076
Irganox B225 (50:50 mixture of Irganox 1010
and Irgafos 168)
7 Determination of Functional
Additives
7.1 Process Aids and Lubricants
In PVC technology certain polymeric additives can be
considered as process aids. These polymers have a
similar composition to those used as impact modifiers
in PVC formulations but are more compatible and so
are primarily included to ensure more uniform flow
and hence improve surface finish. Such process aids
include ABS, chlorinated polyethylene, MBS, EVA-
PVC graft polymers and acrylate-methacrylate
copolymers. As these are usually found in unplasticised
PVC, direct analysis of the product by IR will usually
indicate the presence of those that have a distinctive
spectrum as no masking by plasticiser will take place.
However, even rigid PVC can contain a small amount
of phthalate and so it is advisable to carry out a solvent
extraction to clean up the matrix first. Where the
process aid (e.g., chlorinated polyethylene) has a
relatively bland spectrum, a technique such as NMR
will be required to both detect and quantify it. NMR
will usually be required to quantify the other types as
well, unless the spectrum is very distinctive and
standards of known composition are available.
25
In the case where a relatively large quantity of filler
(talc) has to be incorporated into a polymer (e.g.,
polypropylene) it is often necessary to use a process
aid/lubricant such as a zinc or calcium stearate. A
quantification of the process aid can be achieved by
the analysis of the sample for the metal by acid
digestion-AAS. The stearate can be qualitatively
detected by solvent extraction GC-MS.
7.2 Slip Additives
It is common for aliphatic amides to be incorporated
into plastics, particularly polyethylenes, to act as slip
additives.
It is possible to use LC-MS to detect these types of
slip additives in plastic samples. Using the LC-MS
conditions described in Section 6.2, it is possible to
detect Behenamide (mixture of two aliphatic amides
of molecular weight 331 and 339) and erucamide
(molecular weight 337) in solvent extracts of
polyethylene and polypropylene.
It is also possible to use GC and GC-MS to analyse
these and another common slip additive oleamide in
extracts from plastics as they have sufficient volatility
to elute from the GC column.
7.3 Pigments
Pigments are used extensively in plastic compounds
and can be of one of four main types:
(1) Inorganic compounds
(2) Organo-metallic compounds
(3) Organic compounds
(4) Carbon black
Pigments such as titanium dioxide and iron oxide
belong to the first group and the analysis of these is
relatively easy as they are thermally stable (so can be
determined in both the sample ash or in the sample in
the as received state) and have a diagnostic metal atom
together with a simple chemical structure. Analysis
techniques used are therefore elemental methods such
as AAS and ICP.
Groups 2 and 3 present the analyst with a greater
challenge as there is a very wide number commercially
available, they have relatively high molecular weights
and so cannot be easily removed from the matrix by
solvent extraction and can be thermally labile.
One technique which has been used to identify both these
types of pigment and inorganic ones is vapour phase
ultraviolet absorption spectrometry at 200 nm (a.11). In
this method the samples are powdered and then directly
vapourised in the heated graphite atomiser. Thermal
ultraviolet profiles of organic pigments show absorption
bands between 300 C and 900 C, while profiles of
inorganic pigments are characterised by absorption bands
at temperatures above 900 C. Specific assignments are
made with respect to temperature, relative intensity and
width of the absorption bands.
A relatively unknown technique (laser desorption fourier
transform ion cyclotron resonance mass spectroscopy)
has been used (397) to identify dyes in plastics such as
polymethylmethacrylate. A detection limit of 0.1% was
obtained, which compared with a limit of 1-2% using
an ATR infrared spectroscopy technique.
Infrared spectroscopy techniques can be useful,
particularly if the plastic matrix itself (e.g., polyethylene)
has a relatively simple infrared spectrum and if standard
infrared spectra of a wide range of pigments is available.
Carbon black is used extensively as a black pigment in
products such as cable sheaths. The amount present is
usually less than 2% and so its quantification by TGA
can be difficult due to the small sample size (10 mg)
used. The standard method to quantify the amount of
carbon black in such a product is therefore the tube
furnace as much larger sample sizes can be used (e.g.,
2 g) and hence more accurate quantifications obtained.
7.4 Antistatic Agents
Antistatic agents are usually hygroscopic compounds
which readily attract moisture and so inhibit the build
up of a static charge on the surface of a plastic product.
They are used in many applications from the body of
the humble plastic pen to numerous packaging
applications.
The selection of an antistatic agent depends greatly on
the polymer matrix since a degree of incompatibility
is vital to ensure that migration to the surface of the
product occurs at a fast rate after manufacture. Exact
chemical composition information can be difficult to
obtain from suppliers and so analysis for these additives
can be difficult.
26
In the case of polystyrene, quaternary ammonium
compounds are widely used and for polyethylene,
polyethylene glycol alkyl esters can be used.
In the case of the glycol esters, these can of sufficiently
low molecular weight to be extractable by solvents such
as diethyl ether and then identified by a chromatographic
technique such as GC-MS. As in a number of cases it is
to be expected that LC-MS will play a role in the analysis
of these additives in the future.
7.5 Crosslinking Agents and Co-Agents
For some plastic products (e.g., cable sheathing) it
can be necessary to impart a degree of crosslinking
into the product to achieve the requisite physical
properties. This can be achieved by irradiation using
gamma rays. However, some polymers degrade when
subjected to high energy radiation as illustrated in
Table 6. Chemical agents such as peroxides are also
used. These species produce diagnostic breakdown
products the identification of which will reveal the
type of peroxide used.
The most useful technique for this type of work is GC-
MS. There are two possible modes of sample
introduction: solution injection and dynamic
headspace. In the case of the former a useful method
of sample preparation involves cryogenic grinding of
0.3 g of the sample, followed by extraction using 2 ml
of diethyl ether in an ultrasonic bath for 30 minutes.
The resulting extract is then analysed under the
following conditions:
Instrument: Hewlett Packard 6890/5973 GC-MSD
Carrier: Helium @ 2.0 ml/min constant flow
Injection mode: 1 l splitless (0.75 min; 50 ml/min)
Injection temperature: 320 C
Column type: RTX5-MS 30 m x 0.25 mm,
0.25 m film thickness
Column temperature: 40 C for 5 min, 20 C/min
up to 300 C held for 12 min
MS settings: 20 to 620 Daltons scanned
every 0.33 s
In the case of the dynamic headspace approach a
relatively small amount of sample (e.g., 3 mg) is heated
in the oven of a dynamic desorption unit and the
volatiles produced collected in a cryogenically cooled
Tenax filled trap. The experimental conditions are as
follows:
Dynamic Headspace
Instrument: Perkin Elmer ATD 400
Desorption temperature: 150 C for 10 min
Desorption flow: Helium @ 20 ml/min
Trap collection temperature: 30 C
Trap injection temperature: 250 C
Trap outlet split flow: 9 ml/min
Trap inlet split flow: off
Split: 10:1
GC-MS
The conditions used are the same as for the diethyl
ether method with the exception of the following:
GC Column temperature: 30 C to 50 C at 5 C/min,
following by 20 C/min to
300 C and then held at
300 C for 12 min
Carrier Helium @ 0.07 MPa
n o i t a i d a r y g r e n e h g i h o t d e t c e j b u s s r e m y l o p f o r u o i v a h e B 6 e l b a T
k n i l s s o r c t a h t s r e m y l o P e d a r g e d t a h t s r e m y l o P
e n e l y h t e y l o P
d i c a c i l y r c a y l o P
e t a l y r c a l y h t e m y l o P
e d i m a l y r c a y l o P
s r e m y l o p o c e l i r t i n o l y r c a - e n e r y t S
( y l o P ) e n e r y t s l y h t e m -
e t a l y r c a h t e m l y h t e m y l o P
d i c a c i l y c a h t e m y l o P
e d i r o l h c e n e d i l y n i v y l o P
E F T C P
E F T P
e n e l y p o r p y l o P
27
For either analytical approach, identification of the
diagnostic cure system breakdown species is by
reference to mass spectral libraries such as those
produced by the National Institute of Standards and
Technology (USA) (NIST), the Royal Society of
Chemistry, Wiley/NBS (a.12) and the US
Environmental Protection Agency (EPA)/National
Institute of Health (NIH). The mass spectra of the
majority of species of interest are in these libraries and
so, providing the knowledge to reconstruct cure systems
is available, successful attempts can be made.
One problem associated with this task is that a number
of peroxide curing agents breakdown to give more that
one product and a number of these are common to more
than one peroxide species. This is demonstrated in
Table 7.
In addition to identifying the type of peroxide used,
these GC-MS techniques will also identify the type of
co-agent (e.g., triallyl cyanurate (TAC) or triallyl
isocyanurate (TAIC)) used.
7.6 Blowing Agents
There are two main types of blowing agent used with
polymer systems in general:
(1) Chemical Chemical compounds (principally
organic) that undergo chemical
decomposition at the processing
temperature to form a gaseous species
(e.g., nitrogen) which will create the
cellular structure.
Examples include azo compounds,
nitroso compounds, sulfonyl hydrazide
compounds and sodium bicarbonate.
(2) Physical Low boiling point organic compounds
(e.g., dichloromethane or pentane)
which volatilise at the processing
temperature to create a cellular
structure.
With plastics, the most widely used type are the
physical blowing agents.
Where it is suspected that a physical type blowing
agent has been used to produce a foam, is it possible
to use headspace GC-MS to identify it. Even in the
blown state, the high sensitivity of the technique
enables an assignment to be made from the small
amount of residual blowing agent that will be present.
It is usual to use this type of blowing agent in
amorphous plastics that have glass transition
temperatures around 100 C, e.g., styrenics. This
enable the expansion of the plastic to be well
controlled.
The reactivity of the chemical blowing agent type can
make analysis difficult (e.g., they will decompose in
the injection port of a GC-MS instrument), and the
approach that is used is to indirectly identify them by
the determination of breakdown fragments. The GC-
MS instrument is the best choice for this and a library
of typical breakdown fragments is required.
Quantification of the chemical blowing agent in an
unblown product is very difficult as the polarity and
reactivity (e.g., hydrogen bonding reactions and
thermal instability) can cause problems during isolation
from the compound and subsequent analysis. In terms
of reverse engineering, this is unlikely to be required
since the product will invariably be already blown. For
laboratories that are carrying out quality control work,
other properties such density and expansion ration can
be used to determine compound loadings.
s m e t s y s e r u c t n e r e f f i d h t i w d e t a i c o s s a s e i c e p s c i t s o n g a i D 7 e l b a T
e v i t a r u c e d i x o r e P s e i c e p s c i t s o n g a i D
0 4 / 4 1 x o d a k r e P y r a i t r e T l o n a t u b
) l o n a h t e m e n e z n e b ) l o n a h t e m l y h t e m i D - 1 , 1 ( - i D 3 , 1
t r e T e d i x o r e p l y m u c l y t u b - l o n a h t e m e n e z n e b l y h t e m i D - 1 , 1
e n o n e h p o t e c A
y r a i t r e T l o n a t u b
e d i x o r e p l y m u c i D l o n a h t e m e n e z n e b l y h t e m i D - 1 , 1
e n o n e h p o t e c A
28
7.7 Flame Retardants
As with blowing agents, there are two main categories
of flame retardant: organic and inorganic.
The amount and type of organic flame retardant present
in a plastic compound can be determined in an
analogous way to the plasticiser, since this type of flame
retardant is usually similar in molecular weight and
polarity and, hence, extractability. Once the type of
organic flame retardant has been determined by IR, an
accurate quantification can be obtained by carrying out
an elemental analysis for the halogen (or other relevant
element, e.g., phosphorus) on the unextracted sample.
The extract value itself will rarely provide a meaningful
quantification as other species, particularly any process
aid/plasticiser, will contribute to it as well. In some
instances (e.g., organophosphates) it may be possible
to use an HPLC analysis of the extract to quantify the
flame retardant. GC based techniques can also be used
in some cases, but bromide types present problems for
these techniques because of their relatively high
molecular weights (> 900).
Care must be taken over the quantification of inorganic
flame retardants, since some of them (e.g., antimony
trioxide) can react with the organic flame retardant
present, or break down to produce volatile products,
under quantitative ashing conditions, and during
analysis by thermal techniques such as TGA. A good
initial approach is a semi-quantitative elemental
analysis by XRF, to see which types are present.
Accurate quantifications can then be obtained by
precise elemental determinations.
If it is known that hydrated alumina is present in the
sample, it is possible to quantify this reasonably well
using TGA, by making use of the water loss data.
Hydrated alumina loses close to 35% of its weight when
it is heated to 550 C in a TGA experiment.
7.8 Impact Modifiers
The most commonly encountered impact modified
plastic is high impact polystyrene (HIPS). The impact
modification is achieved by incorporating discreet
domains of a rubber (butadiene) within the polystyrene
matrix. The level of butadiene can be varied according
to the requirements of the end use. A high level can
convert a glassy brittle material into a ductile, tough
product. The efficiency of the butadiene to improve
impact resistance alone is not solely related to
concentration, but is also dependent on the size and
distribution within the matrix of the domains that
contain it. Actual impact performance is determined
by physical tests such as the Charpy and Izod impact
tests, and the size and distribution of domains is
investigated by transmission electron microscopy
(TEM), but there are a number of chemical tests that
can be carried out to determine the level of modifier.
(1) IR analysis - this is performed on a pressed film
and the relative size of the absorption bands due to
styrene (700 cm) and butadiene (966 cm) are taken
and compared to standards of known styrene-
butadiene levels.
(2) NMR - the plastic is dissolved and the level of the
two polymers determined by specific shift areas.
(3) Classical wet chemistry - the butadiene level is
determined in solution by reaction of a reagent with
the double bonds.
There are some instances (e.g., rubber impact
modification of nylon) where the chemical properties
of the two polymers are so dissimilar that solubility
differences can be used to isolate and, in this case,
quantify the rubber modifier. The test is carried out by
taking an accurately weighed sample and refluxing it
in formic acid until the plastic is digested and only the
rubber phase remains. The rubber is then washed, dried
and weighed.
Other plastics which can contain rubber modifiers (or
at least modifiers that have lower glass transition
temperatures than the plastic phase) include PET and
PVC. In the case of PVC, acrylates and methacrylates
are common and the normal approach is to use IR to
detect the modifier and then NMR to quantify it.
8 Analysis of Plastics for Food
Contact Use
For more than 30 years work has been going on
involving food contact plastics and the effect that
migrants from plastics products have on food. The first
European Directive (78/142/EEC), which was on the
vinyl chloride monomer content of food contact PVC,
was published in the late 1970s and this was followed
ultimately by the more comprehensive Plastics
Directive (90/128/EEC) in 1990. Since 1990, there has
been a gradual harmonisation of European testing
requirements through amendments to 90/128/EEC. The
seventh amendment (2002/17/EC) has recently been
29
published and the initial requirements for testing overall
and specific monomer migration have now grown to
include additive (e.g., antioxidant) migration.
In general, there are two types of analytical test that
are carried out on food contact plastics:
(1) Global migration tests - In these, the plastic is put
into contact with an appropriate food simulant
under representative end use conditions and the
total amount of material that has migrated into the
simulant determined gravimetrically or, in the case
of involatile food simulants such as olive oil, by
gas chromatography.
(2) Specific migration tests - Again, the plastic is
contacted with a food simulant but any analytical
work in targeted on a specific additive and its
concentration determined using an appropriate
chromatographic technique.
In the case of certain plastics materials, e.g., ABS,
grades that are intended for food use have to meet
certain residual monomer targets. Direct analysis of
these polymers is undertaken to determine the
concentration of these monomers.
8.1 Global Migration Tests
The following food simulants are used for food contact
plastics:
Distilled water - Aqueous food use
Distilled water 95%:Ethanol 5% - Alcoholic
beverages such as beers and lagers
Distilled water 85%:Ethanol 15% - Wines
Distilled water 60%:Ethanol 40% - Spirits
A solution of 3% w/v acetic acid in distilled water -
Acidic aqueous foods
Olive oil
*
- Fatty foods (also isopropanol or hexane)
(
*
Isopropanol and Hexane have been introduced
as fatty food simulants to circumvent the analytical
problems that can occur with olive oil due to its
potential variability as a natural product and
involatility.)
As mentioned, the global migration figure for a particular
plastics material is determined gravimetrically. One
g n i t s e t t c a t n o c d o o f r o f e r u t a r e p m e t d n a e m i t t c a t n o C 8 e l b a T
) C E / 1 1 7 / 2 8 e v i t c e r i D C E (
e s u l a u t c a n i t c a t n o c f o s n o i t i d n o C s n o i t i d n o c t s e T
s r u o h 4 2 > e m i t t c a t n o C . 1
5 < T C 5 t a s y a d 0 1 C
5 0 4 < T < C C 0 4 t a s y a d 0 1 C
s r u o h 4 2 d n a s r u o h 2 n e e w t e b e m i t t c a t n o C . 2
5 < T C 5 t a s r u o h 4 2 C
5 0 4 < T < C C 0 4 t a s r u o h 4 2 C
0 4 > T C s w a L l a n o i t a N h t i w e c n a d r o c c a n I
s r u o h 2 n a h t s s e l e m i t t c a t n o C . 3
5 < T 5 t a s r u o h 2 C
5 0 4 < T < C C 0 4 t a s r u o h 2 C
0 4 0 7 < T < C C 0 7 t a s r u o h 2 C
0 7 0 0 1 < T < C C 0 0 1 t a r u o h 1 C
0 0 1 1 2 1 < T < C C 1 2 1 t a n i m 0 3 C
1 2 1 > T C s w a L l a n o i t a N h t i w e c n a d r o c c a n I
30
approach is to use conditioned glass crucibles and to
dry off the simulant on a hot plate after the contact
experiment has been performed under the appropriate
conditions (time and temperature).
Once the appropriate simulant has been chosen the
contact time and temperature to use are given in EC
Directive 82/711/EEC (Table 8).
In addition, for plastics in contact with food for which
a preservation temperature of less than 20 C is required
the test condition will be 10 days at 20 C.
The overall global migration limit for plastics is stated
in the EC Directive 90/128/EEC as being 10 mg/dm
2
(surface area of plastic). This limit can be expressed as
60 mg/kg of foodstuff in certain situations. To be used
for food contact a plastics product must meet this
requirement.
In a number of packaging types, only one side of a
plastic film or laminate may contact the food. Specific
single side migration cells have been developed (e.g.,
by PIRA) to enable the migration from a material under
these conditions to be investigated.
8.2 Specific migration and residual monomer tests
In addition to the global migration limit 90/128/EEC
also provides a number of specific migration limits
(SMLs) for plastic monomers (Table 9).
There are also SMLs for plastic additives, some
examples are shown in Table 10.
In the case of some monomers, 90/128/EEC gives limits
(called quantification limit-monomer (Qm)) relating to
the plastic material itself. For example, vinylidene
chloride has a QM of 5 mg/kg of plastic.
Over the years, the detection of species migrating from
food contact materials has advanced hand in hand with
the gradual lowering of analytical detection limits
brought about by the refinement of the techniques. For
example, the SML for acrylonitrile is set at not
detectable above 0.02 mg/kg (i.e., 20 parts per billion)
and this would not be obtainable on a routine basis
without the benefits of modern instrumentation.
The development of suitable methods for the detection
of the wide range of monomers and additives used in
) C E E / 8 2 1 / 0 9 ( s r e m o n o m c i t s a l p r o f s L M S 9 e l b a T
r e m o n o M L M S
e t a t e c a l y n i V f f u t s d o o f g k / g m 2 1
e l i r t i n o l y r c A f f u t s d o o f g k / g m 2 0 . 0 e v o b a e l b a t c e t e d t o N
m a t c a l o r p a C f f u t s d o o f g k / g m 5 1
e d y h e d l a m r o F f f u t s d o o f g k / g m 5 1
d i c a c i l a h t h p e r e T f f u t s d o o f g k / g m 5 . 7
e d i r o l h c e n e d i l y n i V f f u t s d o o f g k / g m 5 0 . 0 e v o b a e l b a t c e t e d t o N
) C E E / 8 2 1 / 0 9 ( s e v i t i d d a c i t s a l p e m o s r o f s L M S 0 1 e l b a T
e v i t i d d A L M S
s r e t s e e t a l a h t h p d n a e t a p i d A f f u t s d o o f g k / g m 5 . 1
e d i x o i r t y n o m i t n A f f u t s d o o f g k / g m 1 0 . 0
T H B f f u t s d o o f g k / g m 0 . 3
s n o b r a c o r d y h d e t a n e g o r d y H f f u t s d o o f g k / g m 0 . 3
s n o b r a c o r d y h l a n o i t n e v n o C f f u t s d o o f g k / g m 3 . 0
e d i m a r a e t s / e d i m a e l O e s u d o o f y t t a f r o f d e s u e b t o n n a C
31
food contact materials requires the application of state
of the art analytical techniques. Normally, headspace
methods are preferred for volatile monomers as such
methods overcome a lot of the problems of sample matrix
clean-up. In principle the food contact simulant, foodstuff
or plastic material is heated in a sealed vial fitted with
an inert septum (usually PTFE coated rubber). The vial
is heated to an accurate set temperature normally in the
range 80-100 C, for an equilibrium time of at least one
hour. The headspace above the sample is then analysed
for the presence of the analyte. The quantity of analyte
in the headspace will always be in equilibrium with the
amount present in the sample. Standard addition methods
are used to obtain calibration curves, with the calibrant
vials being analysed under the same conditions (i.e., time,
temperature and ratio of headspace to bulk material
(polymer if necessary)) as the samples. To acquire
sufficiently low detection limits it is sometimes
necessary to use specific detectors (e.g., a nitrogen/
phosphorus detector (NPD)) or, in the case of mass
selective detectors, a single ion monitoring approach.
For species that are too involatile for headspace based
methods, other chromatographic and spectroscopic
methods are employed.
A summary of the analytical techniques used in food
migration work is shown in Table 11.
In the cases where HPLC has been assigned, LC-MS
would also be applicable.
9 Determination of Stabilisers in PVC
Although it is one of the bulk thermoplastics, PVC
suffers from relatively poor stability to ageing agencies
such as heat and UV light. In order to achieve its status
as an important plastic it was therefore necessary to
develop a specific additive group: PVC stabilisers.
These technological developments have resulted in a
range of stabilisers being available that are appropriate
for different grades of PVC, products and end uses.
Some of the main types are:
(a) Lead stabilisers (e.g., lead carbonate, lead stearate,
lead phthalate)
(b) Metallic soaps (e.g., stearates, palmitates,
ricinoleates and octoates of cadmium, barium,
calcium and zinc)
(c) Organo-tin compounds (e.g., dibutyltin di-iso-
octylthioglycollate)
(d) Epoxide stabilisers (e.g., epoxidised oils and
bisphenol A epoxide resins).
The analyst has to bear in mind that it is common for a
number of different stabilisers to be used in a PVC
compound in order achieve the optimum ageing resistance.
g n i t s e t n o i t a r g i m n i d e s u s e u q i n h c e t l a c i t y l a n A 1 1 e l b a T
e t y l a n A e u q i n h c e T
e d i r o l h c l y n i V C G e c a p s d a e H
e n e r y t S C L P H d n a C G e c a p s d a e H
d i c a c i l a h t h p e r e T C L P H
l o c y l g e n e l y h t E C G e c a p s d a e H
e l i r t i n o l y r c A D P N h t i w C G e c a p s d a e H
e n e i d a t u B ) D S M ( r o t c e t e d e v i t c e l e s s s a m h t i w C G e c a p s d a e H
s e t a n a y c o s I C L P H n o i t a s i t a v i r e D
e d y h e d l a m r o F y r t e m i r o l o c n o i t a s i t a v i r e D
s d i c a c i n a g r O C I r o C L P H r i a p n o I
s r e s i c i t s a l P C L P H
s t n a d i x o i t n A C F S r o C G , C L P H
s c i n a g r o n I P C I r o S A A
s c i n a g r o r a l o P s i s e r o h p o r t c e l e y r a l l i p a c d n a C L P H
32
It is obvious that a large number of these stabilisers
contain metal atoms and so a cost effective way of
achieving an initial evaluation of the type of stabiliser
present is to use a semi-quantitative XRF technique
on the sample in the as received state. Care should be
taken with this as some inorganic pigments/fillers
(e.g., titanium dioxide) can mask certain key elements
(e.g., cadmium).
If it is a case of quantifying a known stabiliser, then
AAS or ICP can be used to quantify the metal and, with
knowledge of the compound formula, the result obtained.
The organo-tin compounds are widely used and for
analytical considerations it is convenient to divide them
into those that contain sulfur and those that do not. To
the first group belong compounds like dialkyltin
mercaptides, mercaptoesters and mercapto
carboxylates, to the second, dialkyltin carboxylates and
their esters. The identification of acids and alcohols
present in tin stabilisers containing no sulfur and the
identification of alcohols from stabilisers containing
mercaptoesters presents little or no difficulty. However,
the identification of the thioacid and of the alkyl groups
attached directly to tin can prove more difficult,
especially if long chain acids form part of the compound
or if the stabiliser is not pure, e.g., if it contains
plasticiser. The thioacid may also tend to decompose
during hydrolysis procedures. The application of a
number of analytical methods (e.g., NMR, IR and GC)
to determine these types of stabiliser in PVC extracts
have been described by Udris (a.13).
Some classic methods based on titration and TLC to
determine organo-tin compounds in solvent extracts
of PVC include:
Potentiometric titration of organo-tin in the extract
with standard sodium methoxide in pyridine using
antimony and calomel electrodes (a.14).
Titration of dialkyltin thiol compounds in benzene/
methanol extract with standard silver nitrate (in IPA
medium) using sulfide coated wire electrode (a.13).
TLC of organo-tin thioacids and thiols using
Kielselgel G plates with development with
glacial acetic acid and detection with catechol
violet (a.15).
TLC of organo-tins using Kieselgel GF 254 with
development using butanol/glacial acetic acid
and detection with catechol violet and UV
irradiation (a.16).
Of the other types of organo-metallic stabilisers,
Malkova and co-workers (a.17) have described an
alternating current polarographic method for the
determination of cadmium, zinc and barium stearates
or laurates in PVC. Other techniques used on PVC
extracts include, column chromatography for barium,
cadmium and zinc salts of fatty acids, paper
chromatography for cadmium, lead and zinc salts of
fatty acids (a.18) and polarography for cadmium, lead
and zinc salts (a.19).
The advent of bench top LC-MS instruments has
enabled the analysis of stabilisers such as the organo-
tin type to be re-examined and laboratories such as
the Analysis Division at Rapra Technology Limited
are investigating the capability of this technique in
this area. This could be another area of plastics
analysis where LC-MS replaces the more traditional
techniques.
10 Analysis of Plastic Laminates and
Fibres
Plastic laminates are used extensively from the ordinary
crisp packet to high specification products for medical
and pharmaceutical use. In all these cases, laminates
are used since the application demands a number of
properties which no single polymer exhibits.
Taking the example of the crisp packet, the innermost
layer must be inert to the product and provide a barrier
to air, the outside layer has to be capable of being
printed onto and the middle layer (or tie layer) has to
be able to stick both of the other two together.
One of the principle analytical techniques for the
analysis of laminates is the infrared microscope. This
instrument is capable of recording transmission infrared
spectra from sample down to 10 square microns in size.
The approach is usually to prepare a section of the
laminate by microtoming a section and then recording
a spectrum of each layer aided by the masking off of
the other layers. The sectioning is often undertaken
obliquely in order to maximise the apparent layer
thickness. The microscope also allows the thickness
of each layer to be determined.
It is also possible to use an ATR technique to record
infrared spectra of the outside layers and reserve the
IR microscope for the central layers. This is possible
because the ATR technique only penetrates a few
microns into the surface of the layers. It is also possible
by choosing the appropriate crystal (e.g., germanium,
33
zinc selenide, etc) to control the depth of penetration.
This can be useful if the layers are particularly thin.
Using the knowledge gained by infrared spectroscopy
of the generic polymer types present, the assignments
can be refined by the use of DSC. Due to the fact that
laminates by their nature are often constructed of
completely different plastic types, the complete
structure can be analysed in one operation and the
melting endotherm transitions obtained used to
differentiate between various grades. For example in
the case of a laminate which had been shown to be
comprised of a polyethylene and a nylon, it would be
possible to differentiate between LLDPE, LDPE and
HDPE, and nylon 6 from nylon 6,6.
It is also possible to use a Raman microscope to analyse
the different layers that are present within a laminate.
As with the IR microscope, it has the ability to isolate
individual layers and, given a satisfactory database, the
spectra obtained can be used for identification purposes.
The Raman spectra for four common polymer types
are shown in Figure 14.
Examination of the cross section of laminate samples
under an optical microscope enables the individual
layers to be viewed. Phase contrast microscopes can
aid the differentiation of layers of similar refractive
index. The use of a polarising microscope can also assist
in characterising individual layers and is particularly
useful when heating laminates under a microscope on
a hot stage to recognize the characteristic melting
temperature of the individual layers.
There are a number of synthetic fibres that can be used
to produce both woven and non-woven fabrics. The
most popular include polyamide, polyester and acrylics
and they can be used in products as varied as clothing
and life rafts.
Once again, the infrared microscope is ideal at
recording generic polymer identification spectra from
individual fibres. Once the generic type has been
established, further refinement of the assignment can
be obtained by DSC (e.g., specific polyamide type)
and, where a number of fibres are available GPC
(molecular weight).
Other microscopic techniques, such as optical (aspect
ratio), SEM (surface morphology) and EDAX
(elemental analysis), Raman microscopy and atomic
force microscopy can be used to further characterise
the product.
Figure 14
Raman spectra of (a) polyethylene, (b) PVC, (c)
polystyrene and (d) polyethylene terephthalate
34
11 Surface Analysis of Plastics
There are a number of analytical techniques that can
be used to obtain data on the surface of plastics
materials or products. Three of the techniques, IR and
Raman microscopy and Edax are covered in Sections
2.2.1, 2.2.6 and 2.6. It can be argued that these
techniques have come into being as the logical
development of the original, general purpose
techniques.
There are however a number of analytical instruments
that have been developed with the specific intention of
analysing surfaces. Three of the principal ones will be
mentioned in this section.
11.1 X-Ray Photoelectron Spectroscopy (XPS)
In this case the surface of the sample is irradiated with
soft X-rays. These X-rays are sufficiently energetic to
cause photoemission of electrons from the core levels
of atoms present on the sample surface. The
photoelectrons generated are collected and passed to
an electron energy analyser and detector. The measured
kinetic energy (KE) of an electron is given by :
KE = hv - BE - sigma
where: hv = energy of the X-ray photon
BE = Binding energy
sigma = work function of the spectrometer
The binding energy of a given core electron is
characteristic of the element and it is this which
enables the elements on the surface of a sample to be
identified. It is also possible to carry out quantitative
work by measuring the relative intensities of the
photoemission from each of the elements present. The
binding energy of a core level depends principally on
the charge on the nucleus of the atom concerned and
smaller changes are induced as a result of chemical
bonding. Although small, such charges are measurable
and provide a means of studying the chemistry of the
sample surface (a.20, a.21).
Because only electrons from the top few atomic layers
will have sufficient energy to escape, the technique is
very surface specific and results are normally obtained
from between 5 and 10 nm depth at a detection limit of
around 0.1 atom percent. The analysis area is typically
3-10 mm
2
and all the elements with the only exception
of hydrogen can be detected.
Because of its ability to determine surface chemistry,
XPS can be particularly useful in the analysis of
polymer surfaces to see if oxidation has taken place
and, if so, what functional groups (e.g., ester, acid,
aldehyde) the oxygen is present in.
This ability of XPS to detect oxygen containing
functional groups is shown in the narrow and broad
scan spectra of PET presented in Figure 15.
Another application is the analysis of polymers to
determine if certain surface treatments (e.g., corona
discharge) have been carried out satisfactorily.
In common with the other surface analysis techniques,
it can also be used to investigate surface
contamination problems and to determine the
composition of the fracture surfaces in adhesion
failures.
11.2 Laser Induced Mass Analysis (LIMA)
In the LIMA technique, the surface of the sample is
subjected to a pulsed UV laser which is sufficiently
energetic to volatilise a small volume (about 1 m
cube) of material. The ionised fragments in this
volume are then separated and identified by means of
a time of flight mass spectrometer. Both negative and
positive fragment data can be obtained.
The analysis area in a LIMA experiment is typically
1-2 m, the analysis depth 0.25-0.5 m and the
detection limit 10-100 ppm. The technique has the
ability to detect all of the elements in a qualitative way.
The technique is very useful for determining
compounds on the surface by means of these elements
and molecule fragments, but it is very sensitive, and
care must be taken to ensure that the surface is not
contaminated (e.g., by handling without gloves) and
that the representative control samples are available
to assist in the interpretation of the data.
Its sensitivity and surface specificity make it ideal in
the detection of very low levels of contamination/
modification. For example, the detection of a
monolayer of silicone contamination of a plastic part
that was hampering the wetting of a paint. It can also
be used to analyse particulate impurities, fibres and
defects in surface coatings.
LIMA is also referred to as laser microprobe mass
spectroscopy (LAMMS).
35
Figure 15
XPS spectra of PET (a) narrow spectrum (b) broad spectrum
(a)
(b)
36
11.3 Secondary Ion Mass Spectroscopy (SIMS)
In this technique the sample surface is bombarded by a
primary ion beam (positive ions of argon, caesium,
oxygen or gallium). These primary ions impart energy
to the surface and, as a consequence of the collisions
produced, ions, atoms and molecular fragments (called
sputtered particles) are ejected. The primary ions may
penetrate several atom layers into the surface, but the
sputtered particles only come from the outer 2-3 atom
layers. In common with the other two techniques,
therefore, SIMS is very surface specific and it is possible
to restrict it to a single monolayer. The analysis area is
typically 150 m, the detection limit is 1 ppm and all
the elements are detectable.
Two types of SIMS experiment can be carried out: static
SIMS and dynamic SIMS. In the former case, the surface
is bombarded with low energy ions and molecular and
atomic fragments are produced without the experiment
changing the nature of the surface appreciably; the
surface chemistry can therefore be investigated.
Dynamic SIMS uses high energy ions to obtain highly
sensitive elemental data down to ppb levels, but the
structural information is lost.
In the case of static SIMS, dedicated libraries are required
to enable the mass spectra of the fragments to be
identified (a.22).
Another application of SIMS is in the study of the
migration of additives (e.g., slip additives and antistats)
onto the surface of plastics.
It is often the case that complementary surface analysis
techniques such as SIMS and XPS can be used together
in order to successfully solve a failure or characterisation
problem. In such cases, XPS would be used to generate
quantitative information, whilst SIMS would provide
qualitative clues with respect to the chemistry. An
example of this is where XPS has successfully detected
and quantified silicon on a surface which is not
responding well to bonding with an adhesive, but the
chemical form that the silicon is in is not readily apparent,
i.e., it could be silica, silicate or silicone. Analysis of the
same surface by static SIMS enables the mass spectrum
of the sputtered top layer fragments to be determined
and the presence of m/e ions at 43, 73 and 147 confirm
that a polydimethyl siloxane is present.
12 Failure Diagnosis
It is an unfortunate fact that plastic products fail in
service. One of the major reasons for this is an incorrect
formulation of the product initially, which is a
technological failing, the other is where the formulation
is correct for the application, but where there has been
a problem in the mixing/processing side, leading to a
product that does not meet the specification. Analysing
the plastic component can be useful in failure diagnosis.
12.1 Common Compositional Problems
If it is suspected that the composition of the product is
not correct, for example that the antioxidant or correct
cure system has not been incorporated into the
compound, then the appropriate species specific tests
that have been discussed earlier can be carried out. If
possible, it is advisable to conduct the analysis
alongside that of a sample known to be of the correct
composition. This ensures that no product specific
matrix effects/interference reactions affect the data
obtained and hence the conclusions reached.
A surprisingly large number of failure problems can be
solved by carrying out a simple series of tests including a
polymer identification check by IR, a bulk compositional
analysis by TGA and a molecular weight determination.
Molecular weight determination is very important in the
case of plastics because of the wide use (sometimes
unauthorised) of regrind material. Unfortunately, the
quality of regrind plastic can vary greatly due to the
degradation, and hence reduction in molecular weight
and associated physical properties, that a plastic
undergoes when it is reground. This depends greatly on
the conditions (e.g., heat and time of heating) that it is
subjected to during the regrinding process. Also, if a
material already contains a proportion of reground
material the onset of degradation can be accelerated by
structural anomalies already present in the polymer. The
widespread applicability of GPC to determine the
molecular weight distribution of the majority of common
plastics makes it the perfect technique to investigate if
regrind is in a sample. Although small amounts (e.g.,
5%) of reasonably high quality regrind can be hard to
spot, any significant amount will reveal itself by a shift
in the distribution towards the low molecular weight end.
As usual with GPC, the availability of reference samples
is important as the technique is mainly comparative.
Most of the failures that are associated with the use of
either some or too much regrind are related to a reduction
in the strength properties of the plastic, but another
reasonably common type of failure is odour, especially
in packaging applications. This odour is invariably due
to oxygenated degradation products of the plastic and
can be detected and analysed by headspace GC-MS.
37
12.2 Environmental Stress Cracking
Environmental stress cracking (ESC) is the premature
initiation of cracking and embrittlement of a plastic
due to the simultaneous action of stress and strain and
contact with specific fluids. It is estimated that 15% of
all plastic component failures are due to ESC. The
source of stress is often that which is unavoidably
processed in during moulding and so an applied stress
is not a pre-requisite. The fluid is sometimes that for
which the component was designed to contain or
conduct, but it is often supplied by such agencies as
adhesives, paints, cleaning agents and inks.
Because this type of failure is associated with relatively
mobile (i.e., low molecular weight) liquids which are
normally present in small concentrations the technique
of GC-MS is very well suitable to its investigation. A
particularly effective approach is dynamic headspace
GC where any stress cracking fluid can be removed
from the plastic matrix without the use of another
solvent and long heating times enable it to be
concentrated up to aid detection. An area of plastic that
has not stress cracked can be used as a control.
There are cases where stress cracking can occur due to
the migration of a less volatile liquid (e.g., a plasticiser).
An example of such a case is the stress cracking of
ABS due to the migration of plasticiser from PVC, and
this can be approached by the detection of phthalate in
the ABS matrix by solvent extraction and then analysis
of the extract using HPLC.
Where the liquid is relatively non-volatile and complex
in composition (such as silicone oil which causes
cracking of polyethylene) again a solvent extraction
technique has to be performed with either infrared
microscopy analysis of a cast micro-film or a liquid
chromatography method (i.e., LC-MS or HPLC) as the
analysis technique.
A review of the environmental stress cracking of
plastics has been produced by Wright (315).
12.3 Contamination Problems
Plastic products can fail, both aesthetically and
physically, because of contaminants. Chemical
resistance and electrical failure are less likely causes
of failure as this type of contaminant is not usually
present at a high enough concentration.
Contamination can enter the product stream either in
the ingredients used in the production, or during the
manufacturing stage (e.g., mixing, extruding or
moulding).
More often than not this contamination is in the form
of solid, discreet entities which makes their removal
from the product relatively easy. Once removed the
microscopic techniques IR and Edax are excellent at
obtaining assignment data in a cost effective way.
Where enough of the contaminant is obtainable (e.g.,
1 mg), and if a mixture of chemicals is suspected, a
bulk composition by TGA can be obtained. If
identification problems are still occurring, more
sophisticated techniques such as GC-MS, SIMS and
LIMA can be employed. Where the contamination is
in a liquid form, a similar analytical regime can be used.
A number of plastic products can suffer from solid
inclusions, but it is probably most common in extruded
products such as car door seals.
It is also possible to use a Raman microscope system
for the analysis of contaminants in plastic materials
(293). One situation where the technique is particularly
useful is in the identification of very small (e.g., a few
micrometers in diameter) polymer gel inclusions within
the same polymer matrix. Often these gels have a higher
degree of crystallinity and Raman spectroscopy with
its high spatial resolution and ability to differentiate
between difference degrees of crystallinity is the ideal
technique to differentiate between these and
contamination by a foreign material.
Contamination of plastics products by a species at a
low level (i.e., less than 1% or at ppm levels) can
sometimes be important, for example if a product is to
be used in the pharmaceutical industry. If it is suspected
that the contaminant is, or contains, a metal, then AAS
can be employed. If the presence of an organic molecule
is suspected, then headspace GC-MS can be used to
identify and quantify the species. The high sensitivity
of this technique normally makes the use of a control
sample extremely important for a quick interpretation
of the output, which is often complex.
12.4 Odour and Emissions Problems
The continuing drive to improve customer care and the
high profile of health and safety issues, has led to
pressure on the suppliers of plastics components to
certain industries to minimise odours, and volatiles in
general, from their products. This is particular true of
the automotive industry.
There are a number of specific tests that automotive
companies insist that plastics components manufactured
38
by suppliers have to pass. An example of such a test is
the VW emissions test which involves placing the
component in a cell of given dimensions and heating
the cell for a given time and a specified temperature.
Rather than carry out a detailed analysis of the
components liberated from the component, the result is
expressed in terms of ppm of total organic compounds
as determined by an organic vapour analyser (OVA).
Limits are given as to the permissible concentrations.
For quality control purposes it is the case at present
that human smell panels will be used in preference to
instrumental analytical techniques which do not yet
adequately mimic the human response. There are
practical drawbacks to this approach, leading to a lot
of research going into electronic noses utilising a
number (e.g., 32) of sensors based on organic
conducting polymers. These devices enable fingerprints
of satisfactory products to be recorded which are used
as references for quality checks.
Work has been carried out to determine the additives
which contribute the most to the overall odour of plastic
products. One of the most useful techniques is
headspace GC-MS. It is advisable to use the dynamic
form of headspace sampling as this enables the volatiles
from the sample to be concentrated. This benefit is
important as some chemical species can cause an odour
problem at very low levels due to the specific sensitivity
of the human nose.
For this type of work the dynamic headspace sampler
(e.g., the Perkin Elmer ATD 400) is operated in a
diffusion mode where the sample is heated at a
relatively low temperature (e.g., 50 C), which helps
to ensure that additional volatile species are not
generated due to degradation of the sample, for a
relatively long period of time (e.g., in excess of 30
minutes). The odour species collected in the trap of
the dynamic headspace sampler can then be analysed
under the following conditions:
Headspace trap injection temperature: 200 C
GC column type: SGE RTX5 MS 30 m x
0.25 mm, 0.25 m film
GC column temperature 30 C to 50 C at 5 C/
min and then 20 C/min
(cryogenic cooling) to 320 C.
MS conditions 20 to 450 atomic mass units
scanned every 0.33 s
13 Conclusion
This review describes the analysis of plastics, plastic
compounds and plastic products in as comprehensive
a way as is possible within the format of a Rapra
Review Report. The abstracts from the Rapra
Pol ymer Li brary and t he addi t i onal readi ng
references provided should greatly assist the analyst
who requi res more i nformat i on on recent
developments.
For the future, the reduction in cost of LC-MS
systems will increase their accessibility and, in
combination with GC-MS, will greatly improve the
efficiency and accuracy with which the analysis of
antidegradants, cure systems, plasticisers and other
additives can be carried out. The combination of
these two instruments will enable the full spectrum
of polarity and molecular weight to be covered and
enable a quantum leap in capability to be achievable
by all analytical laboratories. Experiments which for
years have had to be carried out by TLC because of
the limitations of conventional HPLC instruments
will now be carried out by LC-MS.
The specific analysis techniques SIMS, XPS and
LIMA are becoming increasing routine and, as a
result, cost effective for consultants to use in
characterisation and failure diagnosis work and
therefore an expansion of their use is guaranteed.
In t he t hermal anal ysi s fi el d, a number of
developments have occurred in recent years, with
modulated temperature forms of TGA, DSC and
TMA bei ng brought out by manufact urers.
Modulating the temperature enables these techniques
to deliver better, more informative data on samples.
Another development within the thermal analysis
group is the micro-thermal analysis (micro-TA)
i nst rument . Thi s t echni que combi nes t he
topographical mapping capabilities of a scanning
probe microscope with the ability to perform
localised thermal analysis (DTA and TMA) on a
micron scale. The instrument is also capable of being
connected to a GC-MS via a heated interface for the
chemical identification of specific features.
It is clear that, even with the development of new
and more advanced techniques, the analysis of plastic
compounds and products will continue to present the
pol ymer anal yst wi t h compl ex and di ffi cul t
challenges.
39
Additional References
a.1 Surface Characterisation of Advanced
Polymers, Eds., L. Sabbatini and P.G.
Zambonin, Wiley-VCH, 1993.
a.2 G. Lawson and J. Sidwell, Plastics and Rubber
International, 1983, 8, 6, 15.
a.3 J.L. Koenig, Spectroscopy of Polymers,
Elsevier, 1999.
a.4 T.R Crompton, Manual of Plastics Analysis,
Plenum, 1998.
a.5 T.R. Crompton, Practical Polymer Analysis,
Plenum Press, 1993.
a.6 Polymer Spectroscopy, Ed., A.H. Fawcett,
Wiley, 1996.
a.7 J. Haslam, H.A. Willis and D.C.M. Squirrell,
Identification and Analysis of Plastics, 2
nd
Edition, Butterworth, 1972.
a.8 P.J. Wyatt, Analytica Chimica Acta, 1992,
272, 1.
a.9 D.O. Hummel, Atlas of Polymer and Plastics
Analysis, Volume 2, Carl Hanser Verlag, 1984.
a.10 H.B.S Conacher and B.D. Page, Journal of
Chromatographic Science, 1979, 17, 188.
a.11 P. Tittareli, T. Zerlia, A. Colli and G. Ferrari,
Analytical Chemistry, 1983, 55, 220.
a.12 F. Lafferty and D.B. Stauffer, Wiley/NBS
Registry of Mass Spectral Data, John Wiley &
Sons, 1989.
a.13 J. Udris, Analyst, 1971, 96, 130.
a.14 A. Groagova and M.A. Pribyl, Analytical
Chemistry, 1968, 234, 423.
a.15 F. Belpaire, Revue Belge des Matieres
Plastiques, 1965, 6, 201.
a.16 D. Simpson and B.R. Currell, Analyst, 1971,
96, 515.
a.17 L.N. Malkova, A.I. Kalanin and E.M.
Derepletchikova, Zhurnal Analiticheskoi
Khimii, 1972, 27, 1924.
a.18 E. Schroeder and K. Thinius, Deutsche Farben
Zeitschrift, 1960, 14, 146.
a.19 E. Schroeder and S. Malz, Deutsche Farben
Zeitschrift, 1958, 5, 417.
a.20 Practical Surface Analysis, Eds., D. Briggs and
M.P. Seah, John Wiley and Sons, 1988.
a.21 Handbook of X-Ray Photoelectron
Spectroscopy, Ed., G.E. Muilenberg, Perkin
Elmer Corporation, Eden Prarie, MN, 1979
(update 1992-95).
a.22 D. Brigg, A. Brown and J.C. Vickerman, A
Library of Standard Static SIMS Spectra,
Wiley, 1989.
40
41
Appendix 1
Solubility Parameters of Plastics, Plasticisers and Typical Solvents
s c i t s a l p f o s r e t e m a r a p y t i l i b u l o S
e p y T c i t s a l P r e t e m a r a P y t i l i b u l o S
E F T P 2 . 6
E F T C P 2 . 7
e n e l y h t e y l o P 0 . 8
e n e l y p o r p y l o P 0 . 8
y l o P t e t a l y r c a h t e m l y t u b - 3 . 8
y l o P n e t a l y r c a h t e m l y x e h - 6 . 8
y l o P n e t a l y r c a h t e m l y t u b - 7 . 8
e t a l y r c a l y t u b y l o P 8 . 8
e t a l y r c a h t e m l y h t e y l o P 0 . 9
e n e r y t s y l o P 2 . 9
e t a l y r c a h t e m l y h t e m y l o P 2 . 9
C V P 5 . 9
e t a n o b r a c y l o p A l o n e h p s i B 5 . 9
e d i r o l h c e n e d i l y n i v y l o P 2 . 2 1 - 8 . 9
e s o l u l l e c l y h t E 3 . 0 1 - 5 . 8
e t a r t i n - i d e s o l u l l e C 5 5 . 0 1
T E P 7 . 0 1
s r e m y l o p l a t e c A 1 . 1 1
e t a t e c a - i d e s o l u l l e C 5 3 . 1 1
6 , 6 n o l y N 6 . 3 1
l y h t e m y l o P e t a l y r c a o n a y c - 1 . 4 1
e l i r t i n o l y r c a y l o P 1 . 4 1
s r e s i c i t s a l p f o s r e t e m a r a p y t i l i b u l o S
r e s i c i t s a l P r e t e m a r a P y t i l i b u l o S
s l i o c i n i f f a r a P 5 . 7
s l i o c i t a m o r A 0 . 8
e t a p i d a l y t c o i D 7 . 8
e t a c a b e s l y t c o i D 7 . 8
e t a l a h t h p l y c e d i D 8 . 8
e t a c a b e s l y t u b i D 9 . 8
e t a l a h t h p l y t c o i D 9 . 8
e t a l a h t h p l y h t e y x o t u b - 2 i D 3 . 9
e t a l a h t h p l y t u b i D 4 . 9
e t a h p s o h p l y n e h p i r T 8 . 9
e t a h p s o h p l y l o t i r T 8 . 9
e t a h p s o h p l y l y x i r T 9 . 9
r e h t e l y z n e b i D 0 . 0 1
e t a l a h t h p l y h t e m i D 5 . 0 1
42
s t n e v l o s f o s r e t e m a r a p y t i l i b u l o S
t n e v l o S r e t e m a r a P y t i l i b u l o S
e n a t n e p - o e N 3 . 6
n e n a x e H - 6 . 6
r e h t e l y h t e i D 4 . 7
e n o t e k l y p o r p o s i - i D 0 . 8
e n a x e h o c y C 2 . 8
c e s e t a t e c a l y m A - 3 . 8
e d i r o l h c a r t e t n o b r a C 6 . 8
e n i d i r e p i P 7 . 8
e n e l y X 8 . 8
r e h t e l y h t e m i D 8 . 8
e n e u l o T 9 . 8
e n a p o r p o r o l h c i D - 2 , 1 0 . 9
F H T 1 . 9
e t a t e c a l y h t E 1 . 9
e n e z n e B 2 . 9
m r o f o r o l h C 3 . 9
) K E M ( e n o t e k l y h t e l y h t e M 3 . 9
e n e l y h t e o r o l h c i r T 3 . 9
e n e l y h t e o r o l h c a r t e T 4 . 9
e n a h t e o r o l h c i r T 6 . 9
) M C D ( e n a h t e m o r o l h c i D 7 . 9
e n o n a x e h o l c y C 7 . 9
e d i r o l h c i d e n e l y h t E 8 . 9
N , N e d i m a t e c a l y h t e i D - 9 . 9
e n o t e c A 9 . 9
o e n e z n e b o r o l h c i D - 0 . 0 1
e d i f l u s i d n o b r a C 0 . 0 1
N , N e d i m a m r o f l y h t e i D - 6 . 0 1
n l o n a t u B - 4 . 1 1
l o n a x e h o c y C 4 . 1 1
e l i r t i n o t e c A 9 . 1 1
N , N e d i m a m r o f l y h t e m i D - 1 . 2 1
d i c a c i t e c A 6 . 2 1
l o n a h t E 7 . 2 1
e d i x o f l u s l y h t e m i D 9 . 2 1
d i c a c i m r o F 5 . 3 1
l o n a h t e M 5 . 4 1
l o n e h P 5 . 4 1
l o c y l g e n e l y h t E 6 . 4 1
l o r e c y l G 5 . 6 1
r e t a W 4 . 3 2
43
Appendix 2
Specific Gravities of Plastics and Compound Ingredients
s r e m y l o p f o s e i t i v a r g c i f i c e p S
r e m y l o P y t i v a r G c i f i c e p S
e n e l y h t e y l o p y t i s n e d w o L 2 9 . 0
e n e l y h t e y l o p y t i s n e d h g i H 6 9 . 0
e n e l y p o r p y l o P 0 9 . 0
e d i r o l h c l y n i v y l o P 1 4 . 1
E F T P 2 . 2
E F T C P 1 . 2
e d i r o u l f e n e d i l y n i v y l o P 5 . 1
e d i r o l h c e n e d i l y n i v y l o P 7 . 1
e n e r y t s y l o p l a t s y r C 5 0 . 1
e n e r y t s y l o p t c a p m i m u i d e M 5 0 . 1
e n e r y t s y l o p t c a p m i h g i h y r e V 2 0 . 1
N A S 6 0 . 1
S B A t c a p m i m u i d e M 7 0 . 1 - 4 0 . 1
S B A t c a p m i h g i H 4 0 . 1 - 1 0 . 1
S B M 0 1 . 1 - 7 0 . 1
e t a l a h t h p e r e t e n e l y t u b y l o P 1 3 . 1
e t a l a h t h p e r e t e n e l y h t e y l o P 7 3 . 1
n i s e r c i l o n e h p e s o p r u p l a r e n e G 5 3 . 1
n i s e r c i l o n e h p - e n i m a l e M 6 . 1 - 5 . 1
e d y h e d l a m r o f - a e r U 6 . 1 - 5 . 1
e n o f l u s y l o P 4 2 . 1
e t a n o b r a c y l o P 2 . 1
e d i x o e n e l y n e h p y l o P 6 0 . 1
r e m y l o p o m o h l a t e c A 3 4 . 1
r e m y l o p o c l a t e c A 1 4 . 1
e d i m i y l o P 2 4 . 1
6 , 4 n o l y N 8 1 . 1
6 , 6 n o l y N 4 1 . 1
6 n o l y N 3 1 . 1
0 1 , 6 n o l y N 9 0 . 1
2 1 , 6 n o l y N 7 0 . 1
1 1 n o l y N 4 0 . 1
2 1 n o l y N 2 0 . 1
44
s t n e i d e r g n i g n i d n u o p m o c c i t s a l p f o s e i t i v a r g c i f i c e p S
t n e i d e r g n I y t i v a r G c i f i c e p S
e t a c i l i s m u i n i m u l A 0 1 . 2
e d i x o i r t y n o m i t n A 0 4 . 5
n e m u t i B 4 0 . 1
e t a f l u s m u i r a B 0 3 . 4
e t a c i l i s m u i c l a C 0 1 . 2
k c a l b n o b r a C 0 8 . 1
x a w a b u a n r a C 9 9 . 0
y a l c a n i h c d e n i c l a C 0 5 . 2
) n i l o a k ( y a l c a n i h C 0 6 . 2
e r b i f n o t t o C 5 0 . 1
l o c y l g e n e l y h t e i D 2 1 . 1
e t i h p a r G 4 0 . 2
e d i x o n o r I 1 . 5 - 5 . 4
n i l o n a L 8 0 . 1
) e m i l ( e d i x o m u i c l a C 9 1 . 2
e g r a h t i L 0 3 . 9
e d i x o m u i s e n g a M 0 6 . 3
e t a n o b r a c m u i s e n g a M 1 2 . 2
a c i M 0 8 . 2
l i o l a r e n i M 1 9 . 0
d i c a c i e l O 0 9 . 0
l i o n i f f a r a P 0 8 . 0
x a w n i f f a r a P 0 9 . 0
n i s o R 7 0 . 1
a c i l i S 5 9 . 1
d i c a c i r a e t S 5 8 . 0
r u f l u S 5 0 . 2
) e t a c i l i s m u i s e n g a m ( c l a T 0 8 . 2
) e s a t a n a ( e d i x o i d m u i n a t i T 0 9 . 3
) e l i t u r ( e d i x o i d m u i n a t i T 0 2 . 4
e t a n o b r a c m u i c l a C 5 6 . 2
e d i x o c n i Z 5 5 . 5
e t a r a e t s c n i Z 0 1 . 1
45
Abbreviations and Acronyms
AAS atomic absorption spectroscopy
ABS acrylonitrile-butadiene-styrene
amu atomic mass units
APCI atmospheric pressure chemical ionisation
API atmospheric pressure ionisation
ATR attenuated total reflectance
BS British standard
DCM dichloromethane
DMTA dynamic mechanical thermal analysis
DOP dioctyl phthalate
DSC differential scanning calorimetry
Edax energy dispersive analysis
EI electron ionisation
ELS evaporative light scattering
EPA Environmental Protection Agency (US)
ESC environmental stress cracking
ESI electrospray ionisation
EVA ethylene-vinyl acetate copolymer
FID flame ionisation detector
FT Fourier transform
FTIR Fourier transform infrared spectroscopy
GC gas chromatography
GC-MS gas chromatography-mass spectrometry
GPC gel permeation chromatography
HDPE high density polyethylene
HIPS high impact polystyrene
HPLC high performance liquid chromatography
ICP inductively coupled plasma
IR infrared spectroscopy
ISO International Standards Organisation
KE kinetic energy
LALLS low angle laser light scattering
LAMMS laser microprobe mass spectroscopy
LC-MS liquid chromatography-mass spectroscopy
LDPE low density polyethylene
LIMA laser induced mass analysis
LLDPE linear low density polyethylene
MALLS multi-angle laser light scattering
MBS methylmethacrylate-butadiene-styrene
46
MEK methyl ethyl ketone
micro-TA micro-thermal analysis
Mn number average molecular weight
MSD mass selective detector
Mw weight average molecular weight
Mz Z average molecular weight
NIH National Institute of Health (US)
NIST National Institute of Standards and Technology (US)
NMR nuclear magnetic resonance
NPD nitrogen/phosphorus detector
OVA organic vapour analyser
PE polyethylene
PET polyethylene terephthalate
PMMA polymethylmethacrylate
PP polypropylene
PTFE polytetrafluoroethylene
PVC polyvinyl chloride
Rf Rf value is defined as the distance from the start line on the plate to the analyte spot after
development, divided by the distance from the start line to the solvent front and is reasonably
constant for a given TLC plate type and developing solvent
RI refractive index
SAN styrene-acrylonitrile copolymer
SEM scanning electron microscope
SFC supercritical-fluid chromatography
SIMS secondary ion mass spectrometry
SML specific migration limits
TAC triallyl cyanurate
TAIC triallyl isocyanurate
TEM transmission electron microscopy
T
g
glass transition temperature
TGA thermogravimetric analysis
THF tetrahydrofuran
TLC thin layer chromatography
T
m
melting temperature
TMA thermomechanical analysis
UV ultraviolet
VA vinyl acetate
Vis visible light
XPS X-ray photoelectron spectroscopy
XRD X-ray diffraction
XRF X-ray fluorescence
References and Abstracts
Copyright 2002 Rapra Technology Limited 47
Abstracts from the Polymer Library Database
Item 1
Polymer Testing
21, No.5, 2002, p.591-5
SPECTROSCOPIC BEHAVIOUR OF POLYVINYL
ALCOHOL FILMS WITH DIFFERENT
MOLECULAR WEIGHTS
Abd El-Kader K M; Orabi A S
Suez Canal,University
Details are given of the preparation of PVAL films by a
casting technique. Optical absorption and transmission
measurements were performed. The identification of
molecular structures and assignments of energy bands
were also studied using FTIR and NMR. Correlations
between refractive index and molecular weight were
investigated. 17 refs.
EGYPT
Accession no.856878
Item 2
International Journal of Polymeric Materials
51, No.4, 2002, p.315-23
EFFECTS OF CURING TEMPERATURE ON
POLY(ETHYLENE TEREPHTHALATE)
Al-Raheil I A
Mutah,University
The effect of cure temperature over the range from 280
to 350C on PETP was investigated and changes in polymer
structure analysed by various techniques, including DSC,
TGA, scanning electron microscopy and hot-stage
microscopy. Changes in the crystallisation behaviour of
PETP at the different cure temperatures and the
morphology of the PETP spherulites are discussed and
melting data of the melt crystallised PETP at 215C are
presented. 16 refs.
JORDAN
Accession no.856733
Item 3
Journal of Applied Polymer Science
84, No.8, 23rd May 2002, p.1524-32
KINETIC STUDY OF HINDERED AMINE LIGHT
STABILIZER UNDER NATURAL WEATHERING
CONDITIONS
Kaci M; Hebal G; Benhamida A; Boukerrou A;
Djidjelli H; Sadoun T
Bejaia,University
The photografting kinetics of a hindered amine light
stabiliser (HALS) containing a polymerisable double bond
in low density polyethylene (LDPE) films was studied
under natural weathering conditions. The HALS (PBH-
3, chemical structure shown) was added to the polymer
at a concentration of 0.3 wt.%. The photografting kinetics
were determined by spectroscopic measurement of the
absorption band area of the stabiliser around 308 nm in
the UV spectra and 1605 cm -1 in the FTIR spectra,
corresponding to benzylidene malonate and benzylidene
malonic groups respectively. Parallel measurements on
the free PBH-3 content after chloroform extraction of the
photostabiliser from the polymer matrix by UV and gas
chromatography showed that in natural weathering
grafting took place in the LDPE film after very short
exposure times of 127 and 168 hours as indicated by UV
and FTIR respectively. The curves for the photografting
and the free HALS kinetics were similar. The
photografting mechanism was thought to involve a quick
photoreaction between the methylene double bond of the
stabiliser and the polymer macroalkyl radicals, with
consequent formation of polymer-bonded aminyl
stabiliser derivatives. 24 refs.
ALGERIA
Accession no.853710
Item 4
Polymer Bulletin
48, No.1, March 2002, p.43-51
PYROLYSIS OF GAMMA-IRRADIATED
BISPHENOL-A POLYCARBONATE
Navarro-Gonzalez R; Coll P; Aliev R
CNRS; Mexico,Universidad Nacional Autonoma
This work shows the application of quantitative pyrolysis-
gas chromatography coupled with infrared spectroscopy
and electron impact mass spectrometry in the study of
radiation-induced scission of bisphenol-A polycarbonate
(PC). PC under vacuum was gamma-irradiated using a
60Co source in the dose range from 0.125 to 1.0 MGy.
This was followed by flash pyrolysis under an inert
atmosphere observed by GC-FTIR-MS. Pyrolysis of the
irradiated PC gave different products depending on the
dose. Yields of carbon dioxide and methane decreased
with dose whereas those of phenol and 4-methylphenol
increased. The yields of benzene and toluene were
unaffected by irradiation. Analysis of the products in this
study helped to infer two main pathways for the radiation-
induced scission of PC that involve carbonate bond
rupture or aliphatic-aromatic bond rupture. 30 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
MEXICO; WESTERN EUROPE
Accession no.853698
Item 5
Journal of Polymers and the Environment
8, No.4, Oct. 2000, p.167-74
SENSITIVE ELECTROCHEMICAL IMPEDANCE
SPECTROSCOPY METHOD FOR DETECTION
OF POLYIMIDE DEGRADATION BY
48 Copyright 2002 Rapra Technology Limited
MICROORGANISMS
Gu J-G; Cheng S-P; Liu J; Gu J-D
Shenyang,Agricultural University; Nanjing,University;
Beijing,University of Aeronautics & Astronautics;
Hong Kong,University
An electrochemical impedance spectroscopy method was
evaluated for monitoring the microbial degradation of
polyimides for electronic packaging. A mixed culture of
fungi isolated from degraded polyimides was used as the
microbial inoculum and scanning electron microscopy
was employed to examine fungi growing on the surface
of the inoculated polyimides. The data from the
microscopic analysis was utilised to further support the
relationship between changes in the impedance spectra
and microbial degradation of the polyimide. 30 refs.
CHINA; HONG KONG
Accession no.853552
Item 6
PVC 2002: Towards a Sustainable Future. Proceedings
of a conference held Brighton, 23rd-25th April 2002.
London, IOM Communications Ltd., 2002. Paper 14,
p.157-65, 21cm, 012
PLATE-OUT IN PVC EXTRUSION
Gilbert M; Varshney N; Van Soom K; Schiller M
Loughborough,University; Honeywell; Chemson
(Institute of Materials)
The results are reported of a study of plate-out in PVC
extrusion carried out using several analytical techniques,
including DSC, SEM-EDX, FTIR spectroscopy and laser
ionisation mass spectrometry. A special die and calibrator
unit developed to investigate plate-out are illustrated and
the reproducibility of the method evaluated. The effects
of water content and anti-plate-out additives, such as
alumina and silica, on plate-out are discussed and
mechanisms explaining the formation of plate-out are
proposed. 11 refs.
AUSTRIA; BELGIUM; EUROPEAN COMMUNITY; EUROPEAN
UNION; UK; WESTERN EUROPE
Accession no.852750
Item 7
PVC 2002: Towards a Sustainable Future. Proceedings
of a conference held Brighton, 23rd-25th April 2002.
London, IOM Communications Ltd., 2002. Paper 9,
p.116-23, 21cm, 012
DETERMINING THE LEVEL OF GELATION BY
ODSC ON PVC WINDOW PROFILES
Klingenfuss H; Zahn A
Sueddeutsches Kunststoff-Zentrum
(Institute of Materials)
The degree of gelation of PVC window profiles and of
weld beads was investigated using oscillating differential
calorimetry (ODSC). Tests carried out on a PVC dry blend
revealed that this analytical technique was capable of
determining the degree of gelation of very small samples
and permitted the determination of gelation at every point
of the profile and weld without the need for calibration
samples. 7 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
UK; WESTERN EUROPE
Accession no.852745
Item 8
Polymer International
51, No.5, May 2002, p.379-85
STUDIES OF CURE KINETICS OF
POLYISOIMIDE BY DIFFERENTIAL SCANNING
CALORIMETRY IN THE SOLID STATE
Kim Y J; Son G I; Kim J-H
Sung Kyun Kwan,University
Detailed kinetic studies of the thermal imidisation of
polyisoimide by DSC are described. Both isothermal and
dynamic methods were used to obtain kinetic parameters
and a phenomenological rate equation for estimating the
degree of imidisation as a function of time. 15 refs.
KOREA
Accession no.851649
Item 9
Journal of Adhesion
76, No.1, 2001, p.55-74
EVALUATING CURE OF A PMDI-WOOD
BONDLINE USING SPECTROSCOPIC,
CALORIMETRIC AND MECHANICAL
METHODS
Harper D P; Wolcott M P; Rials T G
Washington State,University; US,Dept.of
Agriculture,Forest Service
The cure of polymeric diphenylmethane diiso-
cyanate(pMDI)/wood bondline in a controlled saturated
steam environment was monitored using micro-dielectric
analysis(micro-DEA). Saturated steam environments were
produced between 110 and 140C. The degree of cure
calculated from micro-DEA was a basis for further
spectroscopic, calorimetric and mechanical evaluation.
Interpretation of calorimetric and spectroscopic analysis
revealed a high consumption of isocyanate early in cure.
Mechanical strength, however, as revealed by lap shear
tests, did not develop until late in cure. Low lap shear
strengths and a plateau in conversion rates were detected
for samples pressed at 110 and 120C. Several components
of the analysis suggested that low temperature cure could
result in crystal formation, leading to diffusion controlled
cure. 24 refs.
USA
Accession no.851472
Item 10
Journal of Advanced Materials
34, No.2, April 2002, p.33-7
DEGREE OF CURE, HEAT OF REACTION AND
VISCOSITY OF 8552 AND 977-3 HM EPOXY
RESINS
Ng S J; Boswell R; Claus S J; Arnold F; Vizzini A
US,Naval Air Warfare Center; Maryland,University
The heat of cure, degree of cure and viscosity of two epoxy
resins (Hexcel 8552 and Cytec Fiberite 977-3 HM) were
investigated using a modulated differential scanning
calorimeter and a rheometric digital analyser.
Mathematical models were developed to correlate the rate
of the degree of cure and the viscosity with the degree of
cure and used to predict the kinetic behaviour of the epoxy
resins, which was then compared with that of Hercules
3501-6. A comparison was also made of cure models
developed based on neat and prepreg forms of the
viscosity data. 6 refs.
USA
Accession no.850900
Item 11
Polymers & Polymer Composites
10, No.3, 2002, p.237-48
CURE BEHAVIOUR AND STRUCTURE OF
DICYANATE-EPOXY NOVOLAC BLENDS
Guo B; Fu W; Jia D; Qiu Q; Wang L
South China,University of Technology
The objectives of this work are to investigate the cure
behaviour and structure of bisphenol A dicyanate-novolac
epoxy blends. The cure characteristics were investigated
by gel time determination and dynamic DSC. To disclose
the structural differences between cured cyanate-novolac
epoxy blends and more traditional cyanate-diglycidyl
ether systems, FTIR investigations were performed on
the two kinds of blends, and in situ FTIR was used to
examine the Bauer mechanism. The effects of epoxy
concentration in the blend on the cure kinetics was
investigated using two blends with different molar ratios,
and in situ FTIR. 33 refs.
CHINA
Accession no.850546
Item 12
Macromolecular Chemistry & Physics
203, No.4, 15th March 2002, p.653-62
MISCIBILITY AND CRYSTALLIZATION
BEHAVIOUR OF POLYETHYLENE
TEREPHTHALATE/POLYVINYLIDENE
FLUORIDE BLENDS
Rahman M H; Nandi A K
Indian Association for the Cultivation of Science
The miscibility of PETP and PVDF was studied. The Tg,
melting point, the crystallisation temperature and the
crystallinity values of the blends of different
compositions, prepared at different conditions were
measured. The polymer-polymer interaction parameter
was measured from equilibrium melting point depression
data. 50 refs.
INDIA
Accession no.850061
Item 13
Chichester, John Wiley & Sons, 1999, pp.xiv,409.
23cm. 911
MICROSTRUCTURAL CHARACTERISATION
OF MATERIALS
Brandon D; Kaplan W D
Haifa,Technion Institute
This unreferenced book describes the technical and
theoretical aspects of a wide range of techniques for studying
the microstructure of materials, including X-ray and electron
diffraction; optical microscopy, including polarised optical
microscopy and interference microscopy; transmission and
scanning electron microscopy; X-ray microanalysis; electron
energy loss spectroscopy; and surface analysis by
photoelectron spectroscopy, Auger electron spectroscopy,
and secondary ion mass spectrometry. The techniques are
described from sample preparation through information
acquisition to interpretation of results. A final chapter
describes the derivation of quantitative structural data from
the results of these techniques. Examples used in the
book mainly involve highly ordered materials such as
metals and inorganic crystalline materials, but many of
the techniques used are applicable to polymers. Problems
for the reader are included.
ISRAEL
Accession no.849739
Item 14
Polimeros: Ciencia e Tecnologia
11, No.4, Oct./Dec.2001, p.213-21
Portuguese
NEAR-INFRARED SPECTRA OF
POLYSTYRENE, POLY(METHYL
METHACRYLATE) AND POLYCARBONATE
De Araujo S C; Kawano Y
Sao Paulo,Instituto de Quimica
The near-infrared (NIR) spectra of amorphous polymers
PS, PMMA and polycarbonate (PC) are studied. The
tentative assignment of the overtone and combination
frequencies is made using the curve fitting calculations and
the local mode theory. Anharmonicity correction and
mechanical frequency are determined from a Birge-Sponer
plot. A tentative assignment of stretch overtone frequency
of CH2 and CH functional groups of PS; CH3 and CO
functional groups of PMMA; and CH, CH3 and CO
functional groups of PC is made. An anharmonicity
correction of 57 and 58 cm-1 is obtained for CH2 and CH
stretch modes of PS; 59 and 9 cm-1 for CH3 and CO stretch
modes of PMMA; and 53, 59 and 10 cm-1 for CH, CH3
and CO stretch modes of PC, respectively. 21 refs.
BRAZIL
Accession no.849333
Item 15
Macromolecules
35, No.7, 26th March 2002, p.2667-75
THERMAL PROPERTIES OF CROSS-LINKED
POLYISOPROPYLACRYLAMIDE,
POLYMETHACRYLIC ACID, THEIR RANDOM
COPOLYMERS, AND SEQUENTIAL
INTERPENETRATING POLYMER NETWORKS
Diez-Pena E; Quijada-Garrido I; Frutos P; Barrales-
Rienda J M
CSIC
The thermal properties of polyisopropyl acrylamide,
polymethacrylic acid, isopropyl acrylamide-methacrylic
acid copolymers and their blends were investigated by
DSC and TGA. The state of the water was studied on the
basis of DSC traces of swollen samples. The Tg of the
same series of materials was also measured. 64 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;
WESTERN EUROPE
Accession no.849122
Item 16
Applied Spectroscopy
56, No.2, Feb.2002, p.187-91
RAMAN MICROSCOPY AND MAPPING AS A
PROBE FOR PHOTODEGRADATION IN
SURFACE RELIEF GRATINGS RECORDED ON
LAYER-BY-LAYER FILMS OF CONGO RED/
POLYELECTROLYTE
Constantino C J L; Aroco R F; He J A; Zucolotto Z; Li
L; Olveira O N; Kumar J; Tripathy S K
Windsor,University; Lowell,Massachusetts University
Raman microscopy, mapping and surface-enhanced
Raman scattering techniques are applied to investigate
the degradation of Congo Red (CR) in a surface relief
grating (SRG) recorded on electrostatically assembled
layer-by-layer film of CR alternated with polydimethyl
diallylammonium chloride (PDAC). Photoinduced
degradation is suggested by a decrease in the Raman bands
assigned to CR with a concomitant increase in the
background signal. More degradation is observed in the
valleys of the SRG, which correspond to the most
illuminated areas. In a line mapping across the SRG, the
Raman intensity of CR bands follows the modulation of
the grating, which indicates that photodegradation of CR
contributes at least partially to the SRG formation.
Surface-enhanced resonance Raman scattering (SERRS)
indicates that the phenyl ring groups are located at the
film surface. Mapping of the Raman signal over many
periods of SRG shows that, within the limits of detection,
the chromophores appear to be oriented in much the same
way throughout the film. They have no preferred
orientation in the peaks and valleys of the SRG after the
recording process is completed. 23 refs.
CANADA; USA
Accession no.848921
Item 17
Injection Molding
10, No.1, Jan. 2002, p.40-4
THE MATERIALS ANALYST: PART 50. THE
CASE OF THE DISAPPEARING CONTAMINANT
Sepe M
Dickten & Masch Mfg.
A report is presented on the diagnosis of the failure of a
component made from a 33% glass-reinforced nylon 66
on the assembly line with the aid of DSC, thermal
gravimetric analysis, which was utilised to determine filler
content and type, X-ray fluorescence and IR spectroscopy.
The analytical procedures employed indicated that failure
of the component could be attributed to the presence of
chlorine probably arising from contamination of the
process by PVC.
USA
Accession no.848744
Item 18
Journal of Polymer Science: Polymer Physics Edition
40, No.5, 1st March 2002, p.434-53
FREE VOLUME, GLASS TRANSITION, AND
DEGREE OF BRANCHING IN METALLOCENE-
BASED PROPYLENE/ALPHA-OLEFIN
COPOLYMERS: POSITRON LIFETIME,
DENSITY, AND DIFFERENTIAL SCANNING
CALORIMETRIC STUDIES
Dlubek G; Bamford D; Rodriguez-Gonzalez A;
Bornemann S; Stejny J; Schade B; Alam M A; Arnold M
Bristol,University; ITA Institut fuer Innovative
Technologien GmbH; Martin-Luther-Universitat Halle
Results of the above studies are presented and are
discussed with particular reference to Tg and degree of
branching, local free volume and degree of branching,
local free volume and Tg, specific volume and degree of
branching, and number density of holes and degree of
branching. 56 refs.
UK; WESTERN EUROPE
Accession no.848572
Item 19
Polymer Preprints. Volume 42. Number 2. Fall 2001.
Proceedings of a conference held Chicago, Il., 7th-11th
April 2002.
Washington, D.C., ACS,Div.of Polymer Chemistry,
2001, p.13-4
POSITRON ANNIHILATION SPECTROSCOPY
AS A NOVEL SURFACE PROBE OF POLYMERS
Jean Y C; Zhang R; Mallon P; Chen H; Huang C-M; Li
Y; Zhang J; Huang Y Y; Sandreczki T C; Wu Y
Missouri-Kansas City,University
(ACS,Div.of Polymer Chemistry)
Positron annihilation spectroscopy (PAS) is a special non-
destructive evaluation (NDE) technique for materials
characterisation, which uses the positron (anti-electron).
Positron-electron annihilation gamma-rays reveal useful
information about the electronic and defect properties of
materials under study. The unique repulsive force between
the positron and the ion cores of materials makes the
positron ideal for probing defects at the atomic and
molecular levels. In recent years, PAS was developed as a
useful tool to probe the microscopic properties of polymeric
materials. One of the great successes in this line of research
is the direct determination of polymer free volume and hole
properties at an atomic scale (0.2-2 nm). Most existing PAS
studies emphasise the bulk of polymers in measuring
positron annihilation lifetime. Recently, another method
of positron annihilation radiation, Doppler broadening of
energy spectra, coupled with a slow positron beam, has
been developed to examine the defect profile near the
surface. The results of experiments on the photodegradation
of polymer-based coatings induced by 313 nm UV
irradiation as studied by slow positron annihilation
spectroscopy are reported and correlated with gloss
measurements. The sub-nanometer defect S parameter is
found to decrease with exposure time. Current results
suggest that the slow positron technique is a sensitive tool
for detecting degradation of polymers in a time much earlier
than for any existing testing methods. It is particularly
sensitive to the surface defect properties. Applications of
PAS to systems of polymers and fillers appear to be
interesting to investigate in the near future. 6 refs.
USA
Accession no.847946
Item 20
Adhesives & Sealants Industry
9, No.1, Feb. 2002, p.38-40
ENHANCED DSC INSTRUMENTATION
IMPROVES DESIGN AND
CHARACTERIZATION OF ADHESIVES
Cassel R B
TA Instruments
The use of differential scanning calorimetry (DSC) for the
characterisation and development of adhesive products is
discussed. The Q Series DSC with Advanced Tzero
Technology from TA Instruments is described, with
reference to the advantages it affords as a new and enhanced
tool for improved design and characterisation of adhesives.
The development incorporates a new measurement
principle with an additional sensor that together provide
compensation for intrinsic instrument distortion of the DSC
signal. With distortion virtually eliminated, it is possible
to measure specific-heat capacity directly in a single scan,
and to achieve greater sensitivity and accuracy. Analysis
time is also reduced, especially for modulated temperature
differential scanning calorimetry. Its use in curing analysis
of a two-part epoxy, and of pressure-sensitive adhesives is
demonstrated. 3 refs.
USA
Accession no.847415
Item 21
Macromolecules
35, No.5, 26th Feb. 2002, p.1797-804
LIQUID CHROMATOGRAPHY OF SYNTHETIC
POLYMERS UNDER CRITICAL CONDITIONS.
THE CASE OF SINGLE ELUENTS AND THE
ROLE OF THETA CONDITIONS
Macko T; Hunkeler D; Berek D
Swiss Federal Institute of Technology; Slovak
Academy of Sciences
PMMA, polybutyl methacrylates and polystyrenes in
various solvents were investigated with bare silica gel
and silica C18 bonded phases. The effect of variations in
eluent nature on polymer retention is discussed. Critical
conditions were identified in some single eluents which
are thermodynamically poor solvents for the polymers.
37 refs.
SLOVAK REPUBLIC; SLOVAKIA; SWITZERLAND; WESTERN
EUROPE
Accession no.847047
Item 22
Macromolecules
35, No.5, 26th Feb. 2002, p.1677-84
LOW-TEMPERATURE CRYSTALLIZATION OF
ETHYLENE-RAN-PROPYLENE COPOLYMERS.
CONFORMATIONAL REARRANGEMENT OF
SEQUENCES DURING THE FORMATION OF
THE AGGREGATES
Bracco S; Comotti A; Simionutti R; Camurati I;
Sozzani P
Milan,University; Basell Spa
Low-temperature crystallisation of ethylene-propylene
copolymers was followed by DSC and solid-state NMR.
The trans conformation fraction identifying the aggregates
was detected for all temperatures independent of thermal
history. 41 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;
WESTERN EUROPE
Accession no.847031
Item 23
Macromolecular Materials and Engineering
286, No.7, 27th July 2001, p421-8
THERMOGRAVIMETRY OF THERMOPLASTIC
POLYIMIDE POWDERS UNDER FOUR
DIFFERENT ATMOSPHERES
Xin-Gui Li; Mei-Rong Huang; He Bai; Yu-Liang Yang
Tongji,University; Tianjin Customs Central Laboratory;
Fudan,University
The high resolution thermogravimetry technique uses a
variable heating rate response to changes in the weight
loss rate to both reduce test times and improve definition.
The thermal degradation of a thermoplastic polyimide
polymer in nitrogen, helium, argon and air was analysed
using both conventional and high resolution
thermogravimetric analysis techniques. It was concluded
that the thermal degradation results varied with both
atmosphere and test technique with the high resolution
technique providing more precise data in the inert
atmosphere tests but less resolution in air.
Thermogravimetric analysis data for a number of
polyimide polymers is tabulated. The thermoplastic
polyimide polymer evaluated was more thermally stable
than many other polyimides. Complete details of the test
techniques are given with full discussion of the results.
40 refs.
CHINA
Accession no.846773
Item 24
83, No.12, 2002, p.2522-7
CRYSTALLIZATION AND CROSSLINKING OF
POLYAMIDE-1010 UNDER ELEVATED
PRESSURE
Jun Yang; Wenfei Dong; Yucheng Luan; Jingjiang Liu;
Shue Liu; Xingguan Guo; Xudong Zhao; Wenhui Su
Changchun,Institute of Applied Chemistry;
Jilin,University
This study looked at the structural changes to polyamide-
1010 (PA1010) when it was treated at 250 degC for 30
min at a pressure of 0.7-2.5 GPa. Crystals grew when the
pressure was below 1.0 GPa or above 1.2 GPa.
Crosslinking occurred in the pressure range 1.0-1.2 GPa.
DSC and wide angle x-ray diffraction showed that PA1010
lost its crystallisation ability after treatment at pressures
of 1.0-1.2 GPa. Crystallised PA1010 had a greater thermal
stability than crosslinked PA1010 at 400 degC. 20 refs.
CHINA
Accession no.846587
Item 25
Kautchuk und Gummi Kunststoffe
55, No.1-2, 2002, p.9-14
German
ANALYSIS OF TECHNICAL POLYMER BLENDS
WITH COUPLING OF LIQUID
CHROMATOGRAPHY WITH FTIR
SPECTROSCOPY
Pasch H; Rode K; Kloninger C; Esser E
Deutsches Kunststoff-Institut
The coupling of liquid chromatography with FTIR
spectroscopy provides a new and interesting method for
the detailed analysis of complex polymer systems. The
application of this hyphenated technique to the analysis
of polymer blends shows that it is possible to identify the
different blend components by their spectral
characteristics. Components of different chemical
compositions are determined selectively and their
chemical structure is analysed through well-resolved
FTIR spectra. For structure elucidation, all facilities of
state-of-the-art FTIR spectroscopy can be used. From the
chromatographic and spectroscopic data, contour
diagrams are generated that present the molecular
heterogeneity of the sample in the coordinates molar mass
and chemical composition. 17 refs.
WESTERN EUROPE
Accession no.846265
Item 26
Polymer
43,No.6,2002,p.1835-47
THERMAL DEGRADATION OF PET AND
ANALOGOUS POLYESTERS MEASURED BY
THERMAL ANALYSIS-FOURIER TRANSFORM
INFRARED SPECTROSCOPY
Holland B J; Hay J N
Birmingham,University
The thermal degradation of two commercial PET samples
and two laboratory prepared polyesters, poly(ethylene
isophthalate) and poly(diethylene glycol terephthalate),
was studied using thermogravimetry and thermal analysis-
FTIR. The commercial PET samples were copolymerised
with diethylene glycol and isophthalic acid groups in
different proportions, and their thermal stabilities were
found to differ. Through a study of the thermal degradation
of poly(diethylene glycol terephthalate) and poly(ethylene
isophthalate), it was found that diethylene glycol and
isophthalate units promoted thermal degradation through
increased chain flexibility and more favourable bond
angles, respectively. The thermal degradation of all the
polyesters tested led to the formation of non-volatile
residue. IR spectroscopic analysis indicated that the
residue consisted almost exclusively of interconnected
aromatic rings. 21 refs.
EU; EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
WESTERN EUROPE; WESTERN EUROPE-GENERAL
Accession no.846155
Item 27
Progress in Organic Coatings
43, No.4, Dec.2001, p.226-32
SIMPLE RAMAN TECHNIQUE TO MEASURE
THE DEGREE OF CURE IN UV CURABLE
COATINGS
Nichols M E; Seubert C M; Weber W H; Gerlock J L
Ford Research Laboratory
The curing of four UV-curable clearcoats was studied by
confocal Raman microscopy. The disappearance of the
C:C line near 1636/cm provided the signature for the
curing of the samples, but quantification of the degree of
cure by standard peak fitting and baseline subtraction
methods did not work well because of sample
fluorescence, baseline shifts and overlapping peaks. A
smoothed second-derivative processing approach
overcame all of these difficulties and provided a simple,
rapid and objective quantification procedure. Steep cure
gradients through the thickness of the clearcoat, due to
screening of the bottom of the clearcoat by both the UVA
and photoinitiator, were observed. Cure gradients at the
top of the clearcoat due to oxygen inhibition were also
observed. The most complete cure throughout the film
thickness was obtained with a mixture of standard and
red-shifted photoinitiators. 9 refs.
USA
Accession no.846135
Item 28
Polymer
43, No.5, 2002, p.1587-97
FULL COPOLYMER CHARACTERIZATION BY
SEC-NMR COMBINED WITH SEC-MALDI
Montaudo M S
CNR
Random copolymers with units of methyl methacrylate,
butyl acrylate, styrene and maleic anhydride were studied
by fractionating the copolymer by size exclusion
chromatography(SEC), collecting 30 to 40 fractions and
then recording both the NMR and MALDI spectra of the
fractions. In a successive step, bivariate distribution of
chain sizes and composition maps were derived from
knowledge of the molar mass, weight and composition
of the copolymer fractions. The compositional distribution
was obtained by summation of the sections of the bivariate
distribution which belonged to a narrow compositional
range. A model for SEC fractionation of copolymers was
developed which allowed prediction of the composition
and D(x) of the SEC fraction, D(x) being the ratio between
the number-average and the weight-average molar mass,
with x being the fraction number. Off-line SEC-MALDI
measurements were performed in order to measure D(x)
experimentally for the random copolymers. 31 refs.
WESTERN EUROPE
Accession no.846119
Item 29
Polymer Testing
21, No.2, 2002, p.155-61
BISPHENOL A-BASED POLYCARBONATES:
CHARACTERIZATION OF COMMERCIAL
SAMPLES
Delpech M C; Coutinho F M B; Habibe M E S
Rio de Janeiro,Universidade Federal; Rio de
Janeiro,Universidade Estadual; Polialden Petroquimica SA
Samples of bisphenol A polycarbonate were characterised
by DSC, TGA, FTIR spectroscopy, size exclusion
chromatography(SEC), vapour pressure osmometry
(VPO) and viscometry. The samples exhibited the same
FTIR spectrum profile and almost the same values of Tg
and initial temp. of degradation. Slight differences were,
however, observed in differential TGA curves, which
could be due to the presence of additives. The number-
average molec.wts. of the samples, as received and
purified, were determined by VPO in two different
solvents, trichloromethane and THF. Viscometric average
molec.wts. were obtained in trichloromethane at 25C. Five
different equations were used to calculate intrinsic
viscosities and viscometric constant values. Relative
molec.wts. and polydispersities were determined by SEC,
in THF at 35C and in trichlorobenzene at 135C. It was
confirmed that the results obtained in the latter solvent
were in better agreement with those obtained by the other
techniques. 25 refs.
BRAZIL
Accession no.845967
Item 30
Plastics Engineering
58, No.2, Feb. 2002, p.40/55
PLASTICS ANALYSIS - THE ENGINEERS
RESOURCE FOR TROUBLESHOOTING
PRODUCT AND PROCESS PROBLEMS AND
FOR COMPETITIVE ANALYSIS
Ezrin M
Connecticut,University
Methods for competitive analysis, troubleshooting process
and product problems, plastics analysis, analysis of failed
products and analysis of polymeric formulations are
discussed. Procedures covered include FTIR spectroscopy,
Raman spectroscopy, NMR spectroscopy, surface analysis
by spectroscopy, gas chromatography/mass spectrometry,
atomic force microscopy and techniques for analysing
unidentified formulations. 47 refs.
USA
Accession no.845139
Item 31
Journal of Applied Medical Polymers
5, No.2, Autumn 2001, p.77-9
NOVEL TECHNIQUE FOR THE DETECTION OF
A HINDERED AMINE LIGHT STABILIZER,
BASED ON SILICON TECHNOLOGY
Narayan S; Lee R E; Hallberg D; Malatesta V
Great Lakes Chemical Corp.; Great Lakes Chemical
Italia
Details are given of the development of a novel method
to detect the presence of a hindered amine light stabiliser
in PP, based on silicon technology. The method consisted
of extracting the stabiliser from the PP matrix followed
by detection and quantification using proton NMR. 3 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; USA;
WESTERN EUROPE
Accession no.844622
Item 32
Adhasion Kleben & Dichten
45, No.12, 2001, p.34-8
German
NON-DESTRUCTIVE NUCLEAR MAGNETIC
RESONANCE CONTACT TECHNIQUE -
EXAMPLES AND POSSIBILITIES
Hartwig A; Wolter B
Fraunhofer-Institut fuer Ang.Materialforschung;
Bundesministerium fuer Wirtschaft; DECHEMA
On page 25 of the November 2001 issue of Adhaesion,
Kleben & Dichten, the nuclear magnetic resonance
contact technique was introduced as a new sort of method
for non-destructive characterisation of polymers. This
article uses examples from the area of epoxy resins and
thick-layer bondings to give an impression of typical,
potential applications for this new non-destructive testing
method. 2 refs.
WESTERN EUROPE
Accession no.844288
Item 33
55, No.12, Dec.2001, p.1729-32
FORENSIC ANALYSIS OF SINGLE FIBRES BY
RAMAN SPECTROSCOPY
Miller J V; Bartick E G
Washington G.,University; US,FBI
Microscopical analysis by FT-IR spectroscopy has been
the preferred method for obtaining additional information
on the polymeric composition of a fibre. It allows
unequivocal determination of the generic class and
frequently permits sub-classification. FT-IR analysis
cannot be conducted while the fibre is mounted due to
the strong absorption of IR radiation by glass. The fibre
must be removed from the slide and rinsed to clean off
the mounting medium before preparing the fibre. This
increases sample preparation time and the chance for
sample loss. Glass produces little response to Raman
spectroscopy. Therefore, Raman analysis of fibres can be
conducted while the fibre remains mounted on a glass
slide under coverslips. The theoretical beam width of the
laser is 0.8 mu m; thus, Raman will potentially permit
measurement of microfibres used in some fabrics in the
current market. The samples do not need to be thinned or
flattened, as with IR, because the photons are scattered
from the surface and not transmitted through the sample.
The current literature contains limited reports and citations
on the use of Raman microprobe spectroscopy for forensic
analysis of fibres. It has previously been shown that it is
possible to scan fibres while they are taped onto a glass
slide. By the same sample preparation method, it has been
demonstrated that it is possible to differentiate between
several generic and sub-generic classes of fibres. It is
illustrated that it is possible to scan through a glass
coverslip and mounting medium to obtain polymeric
identification of non-dyed fibres. 14 refs.
USA
Accession no.843701
Item 34
83, No.5, 31st Jan.2002, p.956-66
SAFETY ASSESSMENT OF POLYMERIC
ADDITIVES FOR FOOD PACKAGING:
HYDROLYSIS OF POLYMERIC PLASTICISERS
BY DIGESTIVE FLUIDS
Hamdani M; Thil L; Gans G; Feigenbaum A E
Institut National de la Recherche Agronomique; BASF AG
The safety of polymeric plasticisers capable of migrating
into food was assessed by an in vitro study of the hydrolysis
of poly(1,2-propylene adipate) (PPA) by digestive fluid
liquids. Freshly prepared simulated intestinal fluid solutions
produced a high degree of hydrolysis. As indicated by high
performance size exclusion chromatography, the bulk
plasticiser disappeared completely, and low molecular
weight oligomers were produced within 4 hours. Gas-phase
chromatography indicated no significant conversion to free
monomers after hydrolysis, and NMR tests showed that
the cleavage selectivity occurred selectively at primary ester
linkages. Silica gel fractionation of the hydrolysate gave
six oligomeric fractions, which were recovered and
analysed. Proton NMR was used to evaluate the absolute
molecular weight of the plasticisers and the hydrolysis
products. Under simulated gastric and saliva conditions the
degree of hydrolysis was less than 2%. 3 refs.
GERMANY; WESTERN EUROPE
Accession no.842741
Item 35
81, No.7, 15th Aug.2001, p.1588-94
CHARACTERIZATION OF BRANCHED
POLYMERS BY SIZE EXCLUSION
CHROMATOGRAPHY COUPLED WITH
MULTIANGLE LIGHT SCATTERING
DETECTOR. I. SIZE EXCLUSION
CHROMATOGRAPHY ELUTION BEHAVIOR OF
BRANCHED POLYMERS
Podzimek S; Vlcek T; Johann C
Wyatt Technology Corp.; Pardubice,University; Wyatt
Technology Deutschland GmbH
The elution behaviour of randomly branched PS and star-
branched poly(benzyl methacrylate) with different levels
of branching was studied by size exclusion
chromatography (SEC) coupled with a multiangle light
scattering detector. The highly branched polymers showed
abnormal SEC elution behaviour. After normal elution at
small elution volumes, the molar mass and root mean
square radius of the eluting molecules increased with
increasing elution volume. Reasons for this were explored
and discussed. SEC separation was compared with
separation by thermal field flow fractionation. 8 refs.
CZECH REPUBLIC; EUROPEAN COMMUNITY; EUROPEAN
UNION; GERMANY; USA; WESTERN EUROPE
Accession no.842695
Item 36
Revista de Plasticos Modernos
81, No.538, April 2001, p.461-6
Spanish
APPLICATION OF INFRARED SPECTROSCOPY
AND THERMAL ANALYSIS IN MONITORING
THE CURE OF THERMOSETTING RESINS
USED IN THE AIRCRAFT INDUSTRY
Sanchez-Blazquez A
CASA
The amine cure of Hexcel 8552 epoxy resin, for use as
the matrix in carbon fibre-reinforced composites for
application in aircraft construction, was monitored by
near-infrared spectroscopy. This technique was validated
by comparison of the results with those obtained by
modulated DSC. 18 refs.
HEXCEL COMPOSITES
WESTERN EUROPE
Accession no.842573
Item 37
Progress in Colloid & Polymer Science
Vol.117, 2001, p.167-71
SURFACE CHARACTERISATION OF
POLYLACTIDE/POLYGLYCOLIDE
COPOLYMERS
Kiss E; Lam C N C; Due T M; Vargha-Butler E I
Budapest,Eotvos Lorand University;
Toronto,University; Biophy Research
The wettability and the surface composition of
biodegradable polymers used as drug delivery particles
are determined and compared. Films of polylactic acid,
polyglycolic acid and their copolymers with four different
lactide, glycolide ratios of 85/15, 75/25, 65/35 and 50;
50 are formed by solvent-casting on polar (silicone wafer
glass and silica) substrates. Advancing and receding water
contact angles are measured goniometrically and also by
using the automated axisymmetric drop shape analysis
method. Both the advancing and the receding water
contact angles of the copolymers are higher than expected
from the values obtained for the two homopolymers
considering the increasing glycolide content of the
copolymers. Surface analysis of the polyester films is
performed by X-ray photoelectron spectroscopy at various
take-off angles to get information on the depth distribution
of the components. Surface enrichment of the nonpolar
(lactide) component in the outermost layer of the
copolymer films is detected. The wettability behaviour is
in accordance with the surface composition, results
suggesting a surface activity effect resulting in the
orientation of the nonpolar segments of the copolymer
chains towards the surface of the film and hence producing
more hydrophobic character for the copolymer films than
should be due to their bulk composition. 20 refs.
Accession no.842190
Item 38
Synthetic Metals
124, No.2-3, 22nd Oct.2001, p.407-14
STUDY OF THE SURFACE POTENTIAL AND
PHOTOVOLTAGE OF CONDUCTING
POLYMERS USING ELECTRIC FORCE
MICROSCOPY
Barisci J N; Stella R; Spinks G M; Wallace G G
Wollongong,University
The effect of the polymer composition, preparation
method and nature of the substrate on the surface potential
(SP) of conducting polymer films is investigated. Both
the average value and the distribution of SP across the
polymer surface are influenced by these factors.
Polythiophenes, potentially useful for solar energy
conversion, are used to examine the generation of light-
induced changes in SP. Results suggest the possibility of
determining the local variations of the surface
photovoltage and the photovoltaic properties of polymer
films intended for use in photovoltaic devices. 16 refs.
AUSTRALIA
Accession no.842093
Item 39
Polymer Degradation and Stability
75, No.1, 2002, p.185-91
STUDY ON METHANOLYTIC
DEPOLYMERIZATION OF PET WITH
SUPERCRITICAL METHANOL FOR
CHEMICAL RECYCLING
Yong Yang; Yijun Lu; Hongwei Xiang; Yuanyuan Xu;
Yongwang Li
Chinese Academy of Sciences
Polyethylene terephthalate (PET) was subjected to
methanolytic depolymerisation with supercritical
methanol in a stirred stainless steel autoclave at
temperatures of 523-543 deg.C, pressure 8.5-14.0 MPa,
and a 3-8 methanol to PET weight ratio. The solid products
obtained, consisting mainly of dimethyl terephthalate and
small amounts of methyl-(2-hydroxyethyl) terephthalate,
bis(hydroxyethyl) terephthalate, dimers, and oligomers,
were analysed by high performance liquid
chromatography (HPLC), and the liquid products, mainly
ethylene glycol and methanol were analysed by gas
chromatography (GC). The temperature, weight ratio of
methanol to PET, and the reaction time had a very marked
effect on dimethyl terephthalate yield and the degree of
PET depolymerisation, but the effect of pressure was
insignificant above the methanol critical point. The
optimum PET depolymerisation conditions were:
temperature 533-543 K, pressure 9.0-11.0 MPa, and a
methanol to PET weight ratio of 6-8. The
depolymerisation of several PET wastes from the Chinese
market was studied under the optimum conditions. 28 refs.
CHINA
Accession no.841527
Item 40
75, No.1, 2002, p.153-9
THE EFFECT OF ULTRAVIOLET STABILISERS
ON THE PHOTODEGRADATION OF
Fechine G J M; Rabello M S; Souto-Maior R M
Pernambuco,Federal University; Paraiba,Universidad
Federal
The weathering behaviour of polyethylene terephthalate
(PET) samples obtained by bi-axial tension in the
laboratory over a period of up to about 1100 hours was
studied. The mechanical properties of films obtained from
the samples having different types of UV stabilisers, e.g.
a triazine ultraviolet absorber (Tinivin 1577), carbon
black, or a TiO2/BaSO4 mixture, were tested, and the
films were examined by UV-VIS spectroscopy, titration,
size exclusion chromatography, and FTIR. The results
showed that the unstabilised films were easily degraded,
resulting in considerable deterioration in mechanical
properties and a molecular weight decrease. The triazine
was the most effective stabiliser. 38 refs.
BRAZIL
Accession no.841524
Item 41
75,No.1, 2002, p.123-9
INITIAL STEPS AND EMBRITTLEMENT IN
THE THERMAL OXIDATION OF STABILISED
POLYPROPYLENE FILMS
Fayolle B; Audouin L; Verdu J
Ecole Nationale Superieure des Arts et Metiers
Physicochemical and mechanical characterisation
methods were used to study the oxidation of 100 micron
stabilised polypropylene films at 130 deg.C in air.
Stabiliser consumption (UV spectrophotometry) and
molecular weight decrease (steric exclusion
chromatography) could be observed during the induction
period, when no carbonyl build-up could be detected by
IR spectroscopy. These structural modifications had an
effect on the fracture properties, as indicated by the
essential work of fracture (EWF) method, whereas the
ultimate tensile elongation showed no significant changes.
The results show that the EWF method is useful for
characterising the degradation induced embrittlement of
initially ductile polymers. The experimental data reported
suggest that the problem of the spatial heterogeneity of
the oxidation process requires further discussion. 21 refs.
WESTERN EUROPE
Accession no.841521
Item 42
Biomaterials
23, No.6, March 2002, p.1439-46
EFFECTS OF THE STERILISATION METHOD
ON THE WEAR OF UHMWPE ACETABULAR
CUPS TESTED IN A HIP JOINT SIMULATOR
Affatato S; Bordini B; Fagnano C; Taddei P; Tinti A;
Toni A
Bologna,Istituti Ortopedici Rizzoli; Bologna,Universita
Details are given of the effects of sterilisation methods
on the wear and changes in physical properties of ultra-
high molecular weight PE acetabular cups. The
crystallinity of the cups was evaluated by micro-Raman
spectroscopy as a function of the inner surface position.
The partial least square calibration was used to correlate
the Raman spectra with the crystallinity of the polymer
measured by DSC. 52 refs.
WESTERN EUROPE
Accession no.840964
Item 43
Polymer Preprints. Volume 41. Number 2. Conference
proceedings.
Washington, D.C., 20th-24th Aug.2000, p.1792-3
CHARACTERISATION OF PLANT FIBRES BY
INFRA-RED SPECTROSCOPY
Garside P; Wyeth P
Southampton,University
The application of IR spectroscopy with respect to the
characterisation of cellulosic (plant) fibres is
demonstrated. The ability to characterise fibres is of
importance to textile conservators, as this information aids
in the determination of the age and origin of the artefact
from which they are taken, and may influence the choice
of treatment. The fibres under examination are taken
largely from the bast group (flax, hemp, jute and ramie);
in addition, sisal and cotton are compared. FT-IR
microspectroscopy and ATR techniques are employed. To
complement the conventional use of these methods, the
inherent polarisation effects of the equipment are
exploited to record polarised IR spectra. Jute, sisal and
cotton are readily differentiated, but flax, hemp and ramie
prove more difficult to distinguish. Peak ratio techniques
are applied in the latter case. 2 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
WESTERN EUROPE
Accession no.840045
Item 44
Journal of Coatings Technology
73, No.923, Dec. 2001, p.43-50
ON THE USE OF THE ATOMIC FORCE
MICROSCOPE TO MONITOR PHYSICAL
DEGRADATION OF POLYMERIC COATING
SURFACES
VanLandingham M R; Nguyen T; Byrd W E; Martin J W
US,National Inst.of Standards & Technology
Changes in the surface properties of a model thermosetting
acrylic melamine polymeric coating system similar to
systems widely used as automotive clearcoats were
followed using atomic force microscopy (AFM). The
samples were exposed to a range of relative humidities,
different temperatures and various UV wavelengths and
a full factorial experimental design was utilised. A
mechanism for the formation of pits in the surface of the
coatings, as observed by AFM, was developed and the
relationship between the chemical and physical
degradation of the coatings discussed. 21 refs.
USA
Accession no.839365
Item 45
Polymer Plastics Technology and Engineering
40, No.5, 2001, p.767-81
STABILISATION OF FREE RADICALS IN
FILLED OLIGOESTER ACRYLATES
Kadossov E B; Kovarski A L; Kasparov V V;
Zapadinski B I; Tikhonov A P
Russia,Academy of Science; Mendeleev University of
Chemical Technology
The results are reported of a study of the formation and
decay of free radicals during the photocrosslinking of an
oligocarbonate methacrylate filled with two types of silica
differing in particle size or hydroxyapatite using ESR
spectroscopy. The data are correlated with those obtained
for molecular mobility using a spin probe and the kinetics
of radical accumulation during photocrosslinking are
discussed along with the kinetics of termination of
radicals. 17 refs.
RUSSIA
Accession no.839176
Item 46
81, No.537, March 2001, p.345-52
Spanish
ANALYSIS OF SYNTHETIC POLYMERS BY
CAPILLARY ELECTROPHORESIS
Simo C; Barbas C; Cifuentes A
Instituto de Fermentaciones Industriales; San Pablo-
CEU,Universidad
The principles of the various modes of capillary
electrophoresis are examined, and applications of these
techniques in the molecular weight characterisation of
polymers are discussed. 40 refs.
WESTERN EUROPE
Accession no.839085
Item 47
55, No.11, Nov. 2001, p.1514-22
RAMAN SPECTROSCOPY DETERMINATION
OF THE THERMOPLASTIC CONTENT WITHIN
EPOXY RESIN-COPOLYETHERSULFONE
BLENDS
van Overbeke E; Devaux J; Legras R; Carter J T;
McGrail P T; Carlier V
Louvain,Universite Catholique; ICI
Details are given of the possibility of using Raman
spectroscopy to determine the local thermoplastic content
within an epoxy resin/copolyethersulphone blend. The
required calibration of the Raman data is presented. The
applicability of the calibrations to blends containing
chlorine-ended copolyethersulphone is discussed. Results
obtained with small or large Raman confocal holes were
also compared. 40 refs.
BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION;
UK; WESTERN EUROPE
Accession no.838755
Item 48
74, No.2, 2001, p.321-6
XPS CHARACTERIZATION OF FRIEDEL-
CRAFTS CROSS-LINKED POLYSTYRENE
Jianqi Wang; Jianxin Du; Hongyang Yao; Wilkie C A
Beijing,Institute of Technology; Marquette,University
The combination of a difunctional alkylating agent, either
hydroxymethylbenzyl chloride or alpha,alpha-
dichloroxylene, with PS or high-impact PS together with
a Friedel-Crafts catalyst, 2-ethylhexyldiphenylphosphate,
and an amine for reaction with hydrogen chloride was
studied by X-ray photoelectron spectroscopy. The results
confirmed the theories proposed from previous
investigations using TGA, i.e. crosslinking of the polymer
occurred as the temp. was raised and the alcohol-
containing alkylating agent gave a greater amount of
crosslinking than did the dichloro compound. 13 refs.
CHINA; USA
Accession no.838285
Item 49
202, No.16, 7th Nov. 2001, p.3228-33
CHARACTERIZATION OF THE
CROSSLINKING KINETICS OF A THIN
POLYMERIC LAYER BY REAL-TIME
DIELECTRIC RELAXATION SPECTROSCOPY
Schonhals A; Fritz A; Pfeiffer K
Berlin,University; Micro Resist Technology GmbH
The crosslinking kinetics of a thin polymeric layer on a
prepolymer of a phthalic acid diallyl ester was studied by
real-time dielectric spectroscopy. Activation energies were
estimated for the reaction using the temperature
dependence of the time constant. The change of the
relaxation rate of the dynamic Tg with the reaction time
was obtained from dielectric loss data. 20 refs.
WESTERN EUROPE
Accession no.838158
Item 50
LCGC Europe
14, No.12, Suppl., Dec.2001, p.8/21
CONSIDERATIONS ON COLUMN SELECTION
AND OPERATING CONDITIONS FOR LC-MS
Sandra P; Vanhoenacker G; Lynen F; Li L; Schelfaut M
Kortrijk,Research Institute for Chromatography;
Ghent,University
Mass spectrometry is slowly, but surely becoming the
detection system of choice for liquid chromatography
analysis in many areas. An overview is presented of
column and mobile phase selection for LC-MS. Relatively
simple guidelines are advanced to successfully optimise
LC-MS for several applications. This article discusses the
fundamentals of LC related to MS hyphenation, adapting
LC to LC-MS methods, normal-phase liquid
chromatography, supercritical fluid chromatography,
reversed-phase liquid chromatography, size exclusion
chromatography, ion-exchange chromatography, affinity
chromatography and capillary electrophoresis. 25 refs.
WESTERN EUROPE
Accession no.837996
Item 51
Polymer
42, No.20, 2001, p.8461-7
STATES OF WATER IN DIFFERENT
HYDROPHILIC POLYMERS - DSC AND FTIR
STUDIES
Ping Z H; Nguyen Q T; Chen S M; Zhou J Q; Ding Y D
Fudan,University; Rouen,University
Differential scanning calorimetry and Fourier transform
infrared spectroscopy techniques were used to study the
structure of water molecules in polyvinyl alcohol and
polyethylene grafted acrylate hydrophilic polymers.
Varying amounts of water were added to test samples and
the samples conditioned to the sorption equilibrium state
in sealed containers for 24 hours prior to evaluation. It was
concluded that below a threshold water content, depending
on the polymers physical and chemical structure, water
molecules absorbed in hydrophilic polymer cannot form
ice crystals in the polymer matrix. Above this threshold
content, the water crystallises but below zero. It was also
demonstrated that the absorbed water in hydrophilic
polymers develops differing hydrogen bonds in the first
and second hydration layers. It was concluded that the
potential influence of these intermolecular interactions
should therefore be taken into account whenever a polymer
is used with a solvent. 25 refs.
CHINA; EUROPEAN COMMUNITY; EUROPEAN UNION;
FRANCE; WESTERN EUROPE
Accession no.837027
Item 52
Polymer
42, No.20, 2001, p.8425-34
PHYSICAL AND MECHANICAL PROPERTIES
OF POLYETHYLENE FOR PIPES IN RELATION
TO MOLECULAR ARCHITECTURE. PART I.
MICROSTRUCTURE AND CRYSTALLISATION
KINETICS
Hubert L; David L; Seguela R; Vigier G; Degoulet C;
Germain Y
Institute Nationale des Sciences Appliquees; Atofina
Five high density polyethylene bimodal copolymers with
varying molecular architectures designed for pipe
applications were tested to evaluate the relationships
between structure properties contributing towards
improved end use properties. Crystallisation kinetics were
studied in relation to molecular architecture using
chromatography, density columns, differential scanning
calorimetry, X-ray scattering, rising temperature elution
fractionation and infrared spectroscopy. From the test
results, it was concluded that the normal correlation
between kinetics, molecular structure and molecular
topology found with unimodal copolymers does not apply
with bimodal copolymers as the crystal surface free energy
was sensitive to topological changes resulting from
architectural molecular changes. Complete details of the
experimental procedures and test results are given with
extensive discussion of the background theory and results.
60 refs.
FRANCE; WESTERN EUROPE
Accession no.837023
Item 53
LCGC Europe
14, No.9, Sept. 2001, p.564/9
INVESTIGATION OF A NOVEL SOL-GEL
DERIVED STATIONARY PHASE FOR GAS
CHROMATOGRAPHY
Cervini R; Day G; Hibberd A; Sharp G; Froud A
SGE International Pty Ltd.; SGE Europe Ltd.
The effectiveness of using a novel, sol-gel material
incorporating PEG or wax as a capillary column stationary
phase is described. Chromatograms demonstrating
inertness, partitioning capability and robustness for a
range of applications are presented. 10 refs.
AUSTRALIA; EUROPEAN COMMUNITY; EUROPEAN UNION;
UK; WESTERN EUROPE
Accession no.836916
Item 54
Polymer Engineering and Science
41, No.10, Oct.2001, p.1714-30
TEMPERATURE MODULATED DSC STUDIES
OF MELTING AND RECRYSTALLIZATION IN
POLY(OXY-1,4-PHENYLENEOXY-1,4-
PHENYLENECARBONYL-1,4-
PHENYLENE)(PEEK)
Kampert W G; Sauer B B
DuPont Central Research & Development
The thermal and crystal morphological properties of
amorphous and melt-crystallised PEEK were investigated.
Two different molec.wts. were studied by temp.-
modulated DSC(TMDSC) over a broad range of annealing
times and temps. The lower molec.wt. PEEK under all
crystallisation conditions was found to exhibit secondary
crystal melting in the low endotherm region, followed by
melting of primary crystals superimposed with a large
recrystallisation contribution. Primary crystal melting
broadly overlapped with melting of the recrystallised
species and contributed to the broad highest endotherm.
Recrystallisation contributions and the interpretation of
TMDSC were partially confirmed by independent rapid
heating rate m.p. determinations and variable heating rate
DSC. The higher molec.wt. PEEK showed many
similarities but generally had smaller levels of
reorganisation above the annealing temp. under most
higher temp. crystallisation conditions. TMDSC provided
good resolution of recrystallisation and related events
compared with standard DSC. The broad and substantial
exothermic recrystallisation in amorphous samples was
also examined, showing that recrystallisation continued
through the final melting region. 42 refs.
USA
Accession no.836355
Item 55
Macromolecular Symposia
Vol.174, Aug.2001, p.413-34
STRATEGIES IN TWO-DIMENSIONAL LIQUID
CHROMATOGRAPHIC SEPARATION OF
COMPLEX POLYMER SYSTEMS
Berek D
Slovak,Academy of Sciences
The separation of complex polymer systems by two-
dimensional liquid chromatography is discussed. Methods
are reviewed in which the effect of polymer molec.wt. on
polymer retention is suppressed. The resulting one
parameter separation systems can be on-line or off-line
connected to another separation system such as size
exclusion chromatography in order to provide more detailed
characterisation of complex polymers. Selected procedures
for the re-concentration of diluted polymer solutions are
also considered. These could be used for increasing the
concentration of sample(s) leaving the first dimension
separation column. Some arrangements for controlled
sample re-introduction into the second dimension
separation column are outlined. 48 refs. (World Polymer
Congress, IUPAC MACRO 2000, 38th Macromolecular
IUPAC Symposium, Warsaw, Poland, July 2000)
SLOVAK REPUBLIC; SLOVAKIA
Accession no.836231
Item 56
81, No.536, Feb.2001, p.244-8
Spanish
PERMEABILITY OF METHANOL, TOLUENE,
FUELS AND OXYGENATED FUELS IN AN
ETHYLENE-VINYL ALCOHOL COPOLYMER
USED AS A BARRIER COMPONENT TO GASES,
AROMAS AND HYDROCARBONS
Lagaron J M; Powell A K
Jaume I,Universitat; BP Chemicals Ltd.
Measurements were made of the permeation rates of
methanol, toluene, a 50/50 toluene/isooctane fuel (fuel
C) and fuel C with 10% ethanol or 15% methanol through
EVOH films. Large scale methanol and water induced
plasticisation was suggested by large solvent uptakes and
confirmed by the observation of considerable decreases
in Tg. The permeability of fuel C increased significantly
when methanol was present, while the high barrier
properties of EVOH to hydrocarbons was maintained for
fuel C containing ethanol. 9 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; UK;
WESTERN EUROPE
Accession no.835449
Item 57
81, No.536, Feb.2001, p.236-43
Spanish
ETHYLENE-VINYL ALCOHOL COPOLYMERS
AND THEIR APPLICATIONS IN FOOD
PACKAGING
Cerrada M L
Instituto de Ciencia y Tecnologia de Polimeros
The gas barrier properties of ethylene-vinyl alcohol
copolymers are examined as a function of ethylene and
vinyl alcohol content, and their use in combination with
other plastics in films, bottles and other containers for
food packaging is discussed. Results are presented of a
study of the crystal structure of three copolymers having
different compositions. 11 refs.
WESTERN EUROPE
Accession no.835448
Item 58
proceedings.
MAPPING CHEMICALLY HETEROGENEOUS
POLYMER SYSTEM USING CHEMICAL
MODIFICATION AND ATOMIC FORCE
MICROSCOPY
Raghavan D; Gu X; VanLandingham M; Nguyen T
Washington,Howard University; US,National Inst.of
Standards & Technology
Interactions between a film and its external environment
are strongly influenced by the surface chemistry and
morphology of the film. Extensive research has been
conducted to provide in-depth microstructural information
of thin polymer films using analytical techniques such as
small-angle X-ray scattering, X-ray photoelectron
spectroscopy, neutron scattering and secondary ion-mass
spec trometry. However, these techniques lack the lateral
resolution to detect and map the heterogeneity in polymer
films. With the advent of atomic force microscopy (AFM),
it is possible to provide direct spatial mapping of surface
topography and surface heterogeneity at nanometer
resolution. A combination of tapping mode and force
mode AFM techniques has been effective in mapping
mechanically heterogeneous regions in multi-component
polymer systems. Recent developments in chemically
functionalised AFM tips have allowed mapping of
chemically heterogeneous lithographically patterned
surfaces by AFM at the molecular scale. This technique
is known as chemical force microscopy. However,
mapping chemical heterogeneity in a polymer system by
chemical force microscopy pose difficulties because of
chain length variation and irregular packing of chains at
the probe surface. The objective is to chemically degrade
one component of a model blend and then identify the
degraded component by AFM. A model blend consisting
of polyethylene acrylate (PEA) and PS is selected due to
the difference in the hydrolysis characteristics of PEA
and PS. Acid is selected as the aggressive chemical
medium so as to accelerate the hydrolysis of one
component in the model blend film. 9 refs.
USA
Accession no.835296
Item 59
proceedings.
OVERVIEW OF STATE-OF-THE-ART SPM OF
CRYSTALLINE POLYMERS
Miles M J; Hobbs J K; McMaster T J; Baker A A;
James P J; Blakely S T; Aissaoui M-N
Bristol,University
Scanning probe microscopy is a family of a dozen or more
microscopies essentially based on the concept and
technology of the founding member, scanning tunnelling
microscopy. The most appropriate and widely-used of
these microscopies in the study of polymer systems is
atomic force microscopy (AFM), which in many of its
modes of operation is suitable for imaging relatively soft
solids such as polymers and biological materials. In the
simplest AFM modes of operation (contact and tapping),
topographic images representing the surface of the
polymer specimen can be obtained. At the lamellar crystal
level, such images have generally confirmed morphology
and crystalline structures deduced from transmission
electron microscopy (TEM) or X-ray studies. However,
the resolution of the AFM can go beyond that easily
achievable with TEM imaging of polymers. At higher
resolution, AFM has, in some cases, revealed unpredicted
surface structures. 26 refs.
WESTERN EUROPE
Accession no.835289
Item 60
Polymer
43, No.1, 2002, p.159-70
QUANTIFYING SHORT CHAIN BRANCHING
MICROSTRUCTURES IN ETHYLENE 1-OLEFIN
COPOLYMERS USING SIZE EXCLUSION
CHROMATOGRAPHY AND FOURIER
TRANSFORM INFRARED SPECTROSCOPY
(SEC-FTIR)
Deslauriers P J; Rohlfing D C; Hsieh E T
Chevron Phillips Chemical Co.
Ethylene-1-olefin copolymers are used to demonstrate an
SEC-FTIR method for the analysis of short chain
branching distribution (SCBD) across the molecular
weight distribution (MWD). The chromatograms were
obtained using the root mean square absorbance in the
3000-2700 cm power -1 spectral range (with FTIR serving
as a concentration detector). The spectra from individual
time sections of the chromatogram were then analysed
for comonomer branch levels using a chemometric
method, and the error in the reported SCB content of each
section was estimated. By using the appropriate training
sets, chemometric models for giving SCB versus
chemometric models were constructed for obtaining SCB
versus MWD profiles of enough accuracy for detecting
trends resulting from catalysis and process changes in low-
and high-density polyethylene samples. The model was
used for accurate quantification of branching levels in
polyolefins within plus or minus 0.5/1000 total carbons
(i.e. about 0.1 mol percentage) in samples having
relatively low SCB levels, i.e. less than 10 SCB/total
carbons and mixed branch types. 20 refs.
USA
Accession no.835164
Item 61
82, No.7, 14th Nov.2001, p.1677-90
SURFACE MODIFICATION OF LOW DENSITY
POLYETHYLENE (LDPE) FILM AND
IMPROVEMENT OF ADHESION BETWEEN
EVAPORATED COPPER METAL FILM AND
LDPE
Ju-Shik Kong; Dong-Jin Lee; Han-Do Kim
Pusan,National University
The effects of chromic acid treatment for periods of time
between 1 and 60 minutes and oxygen plasma treatment
for periods of time between 30 and 90 seconds on the
surface of low density polyethylene films were examined
by attenuated total reflectance fourier transform infrared
spectroscopy, electron spectroscopy for chemical analysis
(ESCA), scanning electron microscopy and water contact
angle. The effect of chromic acid treatment on the tensile
strength of the samples was evaluated and tensile strength
reduced with increasing treatment time. Adhesion of
copper film to the treated surface was evaluated by a
scratch test. It was found that both surface roughness and
number of polar groups on the surface increased with
increasing treatment times of both chromic acid and
oxygen plasma, resulting in lowered water contact angle.
Blackening of a film sample occurred after 30 minutes
treatment in chromic acid. Adhesion of copper film
initially increased with increasing treatment times, but
optimum adhesion properties consistent with tensile
strength retention were established with 30 minutes
chromic acid treatment followed by 30 seconds oxygen
plasma treatment. 14 refs.
KOREA
Accession no.834851
Item 62
Advanced Materials & Processes
159, No.10, Oct.2001, p.66-7
SURFACE ENGINEERING TECHNOLOGIES
Sudarshan T S
Materials Modification Inc.
The 15th International Conference on Surface
Modification Technologies will be held in November in
Indianapolis. This article presents a few paper abstracts
and lists the titles of the sessions. Papers include: structure
and properties of HVOF sprayed amorphous polymer
matrix nanocomposite coatings; field experience with
advanced soft-metal surfaces on carbon steel bolting
materials used in gall-prone gasketed joints that operate
at elevated temperatures; characterisation of industrial
coatings with atomic force microscopy; characterising
aluminium pretreatments for structural adhesive bonding;
the Air Force manufacturing technology laser peening
initiative; and iron aluminide based coating deposited by
high energy density processes.
USA
Accession no.834668
Item 63
82, No.6, 7th Nov.2001, p.1382-90
PROPERTIES AND MORPHOLOGY OF
POLY(ETHYLENE TEREPHTHALATE) AND
HIGH-DENSITY POLYETHYLENE BLEND
Guerrero C; Lozano T; Gonzalez V; Arroyo E
Nuevo Leon,Universidad Autonoma
Blends of polyethylene terephthalate (PET) and high
density polyethylene (HDPE), widely used in the soft
drinks industry, were studied with and without a
compatibiliser. The compatibilising agent was a surlyn
copolymer of ethylene and methacrylic acid partially
neutralized with zinc, the olefinic segment of which is
compatible with HDPE, whereas the carboxylic acid
groups form hydrogen bonds with the PET carbonyl
groups. Infrared spectroscopy, differential scanning
calorimetry, scanning electron microscopy, and the
mechanical properties were used to assess the
effectiveness of the compatibiliser. 29 refs.
MEXICO
Accession no.832040
Item 64
73, No.3, 2001, p.467-70
CORRELATION BETWEEN THERMAL
PROPERTIES AND CONFORMATIONAL
CHANGES IN POLY(ETHYLENE
TEREPHTHALATE)/POLY(ETHER IMIDE)
BLENDS
Ruvolo-Filho A; de Fatima Barros A
Sao Carlos,Universidade Federal
Virgin and recycled polyethylene terephthalate (PET) was
blended with polyether-imide (PEI) in proportions
between 0 and 50 percent PEI content and samples were
examined by differential scanning calorimetry and Fourier
transform infrared spectroscopy. All blends were
completely miscible, as indicated by a single glass
transition temperature which is dependent on blend
composition. Crystallisation rates of PET were retarded
strongly at 20 percent PEI content and above, but degree
of crystallinity was easily determined from a linear
correlation between a structural parameter measured
spectroscopically and enthalpy of fusion. Trans conformer
activation energy measurement confirmed the effects of
PEI content on crystallisation of PET. 9 refs.
BRAZIL
Accession no.831829
Item 65
73, No.3, 2001, p.463-6
EFFECT OF INTERFACE MODIFICATION ON
THE PHOTO-STABILITY OF PIGMENTED
POLYETHYLENE FILMS
Anna P; Bertalan G; Marosi G; Ravadits I; Maatoug M
A
Budapest,University of Technology & Economics
Examination of the ageing characteristics of high density
polyethylene films containing phthalocyanine green and
titanium white and other pigments with those of lightly
stabilised polymer film without pigments was carried out
using tensile analysis, differential scanning calorimetry
and ultraviolet spectroscopy. The early failure of the
phthalocyanine pigmented sample, and subsequent UV
spectroscopic examination showed that the cause was
adsorption of stabilisers onto the pigment surface.
Reactive surfactant coating of pigments was shown to
considerably extend the film stability by reducing their
adsorbency. 9 refs.
EASTERN EUROPE; HUNGARY
Accession no.831828
Item 66
73, No.3, 2001, p.387-92
MECHANISM OF PHOTOSTABILIZATION OF
PERFLUOROPOLYETHER COATINGS BY
HINDERED AMINE STABILISERS
Luda M P; Camino G; Laurenti E; Novelli S;
Temtchenko T; Turri S
Torino,Universita; Centro Ricerche Ausimont
The mechanism of operation of hindered amine stabilisers
(HAS) against photodegradation in perfluoro polyethers
incorporated into a coating material of polyurethane has
been studied by infrared spectroscopy, gas
chromatography-mass spectrometry and electron spin
resonance spectroscopy. Under curing conditions
normally utilised for coil coating (280 degrees Centigrade
for 1 minute in air), the HAS was found to increase the
number of urea bridges in the polyurethane network, and
reduce the amount of unreacted isocyanate, giving a
structure which is more resistant to photooxidation.
Byproducts of the high temperature cure process, caused
by partial transformation of the HAS into -NH derivatives
act as antioxidants. The unreacted HAS was found to
slowly evaporate from the test film, but whilst present
acted as a radical scavenger. 8 refs.
WESTERN EUROPE
Accession no.831816
Item 67
Plast 21
No.101, April 2001, p.77-9
Spanish
INFRARED THERMOGRAPHY: THE COLOURS
OF HEAT
ASCAMM
The use of IR thermography in the study of injection
moulds and injection moulded plastics parts is discussed,
and details are given of research and development projects
being undertaken by ASCAMM of Spain using this
technique.
WESTERN EUROPE
Accession no.831329
Item 68
Polymers for Advanced Technologies
12, No.9, Sept, 2001, p.515-23
HIGH RESOLUTION SOLID-STATE CARBON 13
NMR STUDY OF AS-CURED AND IRRADIATED
EPOXY RESINS
Ngono-Ravache Y; Foray M-F; Bardet M
Grenoble,University
Details are given of the effects of strong ionising
radiations on the physico-chemical modifications of
epoxy resins. The sensitivity of the epoxy resins to
radiation was determined using carbon 13 NMR. 20 refs.
WESTERN EUROPE
Accession no.831124
Item 69
55, No.8, Aug. 2001, p.984-91
RAMAN AND INFRARED
MICROSPECTROSCOPIC MAPPING OF
PLASMA-TREATED AND GRAFTED POLYMER
SURFACES
Keen I; Rintoul L; Fredericks P M
Queensland,University of Technology
A section of the surface of a predominantly PP substrate
containing a small amount of PE copolymer and a small
amount of blended EPM was characterised before and
after plasma treatment and after graft copolymerisation
with PS by means of Raman and ATR/IR mapping. The
maps constructed indicated variations in crystallinity
across the surface, the distribution of EPM and the
distribution of hydroxy groups introduced onto the surface
by plasma treatment. 24 refs.
AUSTRALIA
Accession no.830453
Item 70
POLYMER PROCESSING ENGINEERING. 01.
Proceedings of a conference held June 2001.
London, IOM Communications Ltd., 2001, Paper 5,
p.46-58, 012
AT-PROCESS RAMAN SPECTROMETRY OF
POLYMER MELTS
Dhamdhere M; Li J; Deshpande B; Patil P; Hansen M G
Tennessee,University
(Institute of Materials; Interdisciplinary Research
Centre)
In-line monitoring of EVA extrusion was carried out using
in-line fibre optic Raman spectroscopy. Vinyl acetate
content in the random copolymer and melt indices of
various grades of the EVA were determined and vinyl
acetate content in the samples correlated using linear least
squares and PLS analysis. Hierarchical Cluster analysis was
employed as a pattern recognition technique to follow the
natural clustering tendencies of the EVA samples. 10 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; UK; USA;
WESTERN EUROPE
Accession no.830358
Item 71
Polymer Testing
20, No.7, 2001, p.729-40
DIRECT SOLID SAMPLING METHODS FOR
GAS CHROMATOGRAPHIC ANALYSIS OF
POLYMER/ADDITIVE FORMULATIONS
Bart J C J
Messina,University
The present state of the art in direct solid sampling
methods for gas chromatographic analysis of additives
encapsulated in polymers is reviewed. Techniques
considered are static and dynamic headspace methods,
thermal desorption and solid phase microextraction.
Applications for each method are discussed. 54 refs.
WESTERN EUROPE
Accession no.830211
Item 72
Antec 2001.Conference proceedings.
Dallas, Texas, 6th-10th May, 2001, paper 620
DETERMINATION OF CONDENSABLE
VOLATILES DURING POLYMER PROCESSING
USING AN ANALYTICAL EXTRUDER
Buzanowski W C; Gunderson J; Froelicher S
Dow Chemical Co.
(SPE)
A method of collecting and analysing the volatiles created
during extrusion is described, in which the extruder is part
of the analytical instrumentation. A non-vented 19 mm (3/
4 in) single screw extruder was fitted with a right angle 3.2
mm single strand die, which in turn carried a glass tube
with a bulb near the die exit to allow for polymer swell,
and a side arm for attachment of the sampling system. The
polymer extruded into the glass tube, the less volatile
materials condensing in the tube, and the more volatile
materials being withdrawn by the side arm and trapped in
a set of three impingers containing an appropriate chilled
trapping solution. The volatiles from the glass tube were
removed by rinsing and analysed by Fourier transform
infrared spectroscopy and gas chromatography-mass
spectrometry. The trapping solutions were analysed directly.
The equipment was used to determine the influence of
extrusion time on volatile emissions from polycarbonate,
the influence of melt temperature on volatile loss from a
polycarbonate/styrene-acrylonitrile copolymer blend, and
the influence of additives on volatile loss from a glass-
filled polymer. 6 refs.
USA
Accession no.830052
Item 73
81, No.8, 22nd August 2001, p.1902-13
DYNAMIC MECHANICAL ANALYSIS STUDY
OF THE CURING OF PHENOL-
FORMALDEHYDE NOVOLAC RESINS
Markovic S; Dunjic B; Zlatanic A; Djonlagic J
Belgrade,University
Using dynamic mechanical analysis the curing reactions
of typical phenol-formaldehyde novolac resins were
followed. The evolution of various rheological parameters
was recorded for samples of the resins on cloth. A third-
order phenomenological equation described the curing
reaction. The influences of the structure, composition and
physical treatment on the curing kinetics were evaluated.
20 refs.
EASTERN EUROPE; YUGOSLAVIA
Accession no.829458
Item 74
81, No.11, 12th Sept.2001, p.2779-85
RIGID AMORPHOUS PHASE AND LOW
TEMPERATURE MELTING ENDOTHERM OF
STUDIED BY MODULATED DIFFERENTIAL
SCANNING CALORIMETRY
Song M
Loughborough,University
Three similar samples of polyethylene terephthalate (PET)
prepared by isothermal cold crystallisation in the
differential scanning calorimetry (DSC) cell (PET1), melt
crystallisation at a steady cooling rate and annealing for
various times in the DSC cell (PET2), and quenching from
300 degrees centigrade to -20 degrees over a period of 5
minutes (PET3) were used to study the glass transition
effects in the rigid amorphous phase and the low
temperature melting endotherm using modulated DSC.
As annealing time increased in PET2 the increment of
heat capacity (IHC) at annealing temperature increased
and the IHC at the glass transition temperature decreased.
It was deduced that the low temperature melting
endotherm originated with transitions in the rigid
amorphous fraction, and it was noted that the glasslike
transition of this fraction occurred between glass transition
and melting temperatures. 23 refs.
WESTERN EUROPE
Accession no.829381
Item 75
81, No.10, 6th Sept.2001, p.2387-98
COMPARISON OF THERMAL DEGRADATION
CHARACTERISTICS OF POLY(ARYLENE
SULFONE)S USING THERMOGRAVIMETRIC
ANALYSIS/MASS SPECTROMETRY
Li-Hsiang Perng
Ta Hwa,Institute of Technology
Thermogravimetric analysis with gas chromatography and
mass spectrometry were used in the analysis of the thermal
degradation of polyether sulphone (PES) and
polysulphone (PSF). Evolution of sulphur dioxide and
phenol from random chain scission in a one stage
pyrolysis was observed in both cases with apparent initial
thermal stability of the PES being lower than PSF, but
fire retardation of PES was better due to reduction of the
sulphone group by hydrogen radicals. More pyrolysis
products were identified from the PSF than from the PES.
Thermal stability of ether and sulphone groups appeared
similar in PES but in PSF the sulphone groups proved
the more stable. A simple kinetic model was developed
which showed good agreement between theoretical and
experimental pyrolysis curves for both polymers. 20 refs.
TAIWAN
Accession no.829337
Item 76
81, No.12, 19th Sept.2001, p.3064-8
TEMPERATURE AND ATMOSPHERE
INFLUENCES ON SMOKE COMPOSITION
DURING THERMAL DEGRADATION OF
Malgorzata Dzieciol; Jerzy Trzeszczynski
Szczecin,Technical University
The less volatile compounds formed during the thermal
degradation of polyethylene terephthalate (PET) under
different conditions at 200-700 deg.C in nitrogen and air
atmospheres were studied. The compounds were trapped
on a glass fibre filter and analysed by capillary gas
chromatography using a mass spectrometer (GC-MS), and
high performance liquid chromatography. The results
were tabulated, and plots were drawn of the degradation
temperatures in nitrogen and air atmospheres versus the
weight changes of terephthalic acid and monovinyl
terephthalate evolved from PET. The effects of the
atmosphere and temperature on smoke emission and
composition during PET thermal degradation were
considered. 28 refs.
EASTERN EUROPE; POLAND
Accession no.826911
Item 77
Macromolecules
34, No.15, 17th July 2001, p.5224-8
STUDIES OF MISCIBILITY BEHAVIOUR AND
HYDROGEN BONDING IN BLENDS OF
POLYVINYLPHENOL AND
POLYVINYLPYRROLIDONE
Kuo S W; Chang F C
Taiwan,National Chiao Tung University
Blends of polyvinyl phenol with polyvinyl pyrrolidone
were prepared by solution casting from DMF solutions.
DSC, FTIR, and NMR were used to investigate the
hydrogen bonding and miscibility of the blend. The Tg
of the blend was determined. 22 refs.
CHINA
Accession no.825682
Item 78
Journal of Thermal Analysis and Calorimetry
64, No.2, 2001, p.549-55
CRYSTALLIZATION AND MELTING OF
POLYCARBONATE STUDIED BY
TEMPERATURE-MODULATED DSC (TMDSC)
Schick C; Wurm A; Merzlyakov M; Minakov A;
Marand H
Rostock,University; Moscow,General Physics Institute;
Virginia,Polytechnic Institute & State University
TMDSC measurements conducted at reasonably high
frequencies for bisphenol-A polycarbonate(PC, Lexan)
allowed for the determination of base-line heat capacity.
Vitrification and devitrification of the rigid amorphous
fraction(RAF) could be directly observed. 0.01 Hz
appeared to be a reasonably high frequency for PC. The
RAF of PC was established during isothermal
crystallisation. Devitrification of the RAF seemed to be
related to the lowest endotherm. For PC, the melting of
small crystals between the lamellae was expected to yield
the lowest endotherm. 27 refs.
GENERAL ELECTRIC CO.
RUSSIA; USA; WESTERN EUROPE
Accession no.825045
Item 79
Shawbury, Rapra Technology Ltd., 2001, p.iv, 174,
25cm, 91T
EASY IDENTIFICATION OF PLASTICS AND
RUBBERS
VERLAYE G A L; ROEGES N P G; DE MOOR MO
KaHo Sint-Lieven
This book presents an identification scheme developed
over the last thirty years for thermoplastics, common
thermosets, a few copolymers and elastomers. The
techniques used are based on simple tests such as the
behaviour of polymers in liquids and in a flame. The book
also covers Infrared spectroscopy. Main headings are:
Simple tests (melting, solubility, burning characteristics,
odour recognition, dripping, flotation, halogen test,
nitrogen- and sulphur-test); Recording an IR spectrum;
Identification flow charts; Thermoplastics; Cellulose and
starch; Thermosets; Elastomers. (15 Refs)
UK; WESTERN EUROPE
Accession no.824868
Item 80
UTECH 2000. Proceedings of a conference held The
Hague, Netherlands, 28th-30th March 2000.
London, 2000, Other Rigid Foam Developments
Session, Paper 1, pp.4, 012
LONG-TERM ENERGY EFFICIENCY OF PU-
INSULATION FOR REFRIGERATION
Seifert H; Biedermann A
Elastogran GmbH
(Crain Communications Ltd.; European Isocyanate
Producers Association)
The ageing behaviour of rigid PU foams was investigated
using gas chromatographic quantitative evaluation of the
cell gas composition in the foams. The change in thermal
conductivity of the foams during ageing was also
examined as was the dimensional stability of the foams
under diffusion open conditions and the results obtained
correlated with the K x A-values from refrigerator cabinets
via the change in cell gas composition. The data obtained
revealed that the ageing process of appliances could be
simulated in a tenth of the time by measuring diffusion
opened PU foams. 2 refs.
NETHERLANDS; WESTERN EUROPE
Accession no.824859
Item 81
International Polymer Science and Technology
28, No.5, 2001, p.T/79-80
STUDY OF POLYMER-FILLER INTERACTION
BY INVERSE GAS CHROMATOGRAPHY
Gukasyan S Z
The surface modification of fillers with polymeric
substances is discussed with reference to improvement
of the properties of filled polymers. When the fillers are
modified with polymers, the boundary layer contains not
only the matrix filler, but also the modifying polymer,
and when the modifying polymer interacts with the surface
filler, the properties of both the mineral component and
the modifier are altered. One characteristic which reflects
the result of polymer-filler interaction is the glass
transition temperature of the modifier. To determine this
parameter for a very low content of polymer, the method
of inverse gas chromatography was used using the
modified filler as the stationery phase. The study
investigated the use of travertine and tuff, the surfaces of
which were modified with latices of a copolymer of
styrene and methacrylic acid. 3 refs. (Article translated
from Plasticheskie Massy, No.8, 2000, p.36)
RUSSIA
Accession no.824324
Item 82
Molecular Crystals & Liquid Crystals
Vol.353, 2000, p.95-108
COMPOSITES MADE FROM
LIGNOCELLULOSICS AND THERMOSET
POLYMERS
Aramguren M I; Marcovich N E; Reboredo M M
INTEMA
Preparation and testing of composites from a styrene/
unsaturated polyester thermoset matrix and wood flours
from different wood species was carried out. Studies were
carried out on Pine (Pino Eliottis), eucaliptus (Eucaliptus
Saligna) and marmelero (Ruprechia Laviflora), a
softwood and two semi-hard woods, respectively. The
particles were used untreated and chemically modified
with maleic anhydride. For the characterisation of
untreated and treated flours, thermogravimetric analysis
and analytical techniques were utilised. Dispersion of the
fibrous particles, in addition to maximum fibre
concentration (accompanied by complete wetting of the
wood fibres) was dependent on the treatment and on the
wood species utilised. Bending and compression tests
suggested some improvement in the performance of the
composites, if the wood flour was previously esterified.
Changes in the fracture surfaces due to maleic anhydride
treatment of the fibres were observed using scanning
electron microscopy. 12 refs.
ARGENTINA
Accession no.824162
Item 83
73, No.2, 2001, p.251-7
THERMAL CHARACTERISTICS OF ADDITION-
CURED PHENOLIC RESINS
Reghunadhan C P; Bindu R L; Ninan K N
Vikram Sarabhai Space Centre
The thermal cure characteristics, kinetics of thermal
degradation and pyrolysis of four different addition cured
phenolic resins were investigated using various
techniques, including DSC, DMA, FTIR spectroscopy,
TGA and X-ray diffraction. Resins investigated were
propargyl ether resins and phenyl azo-, phenyl ethynyl-
and maleimide-functional resins. A comparison of the data
obtained for all the phenolic resins was made as a function
of molecular structure. 12 refs.
INDIA
Accession no.824043
Item 84
UTECH 2000. Proceedings of a conference held The
Hague, Netherlands, 28th-30th March 2000.
London, 2000, Innovations: Flexible Foam
Developments Session, Paper 5, pp.4, 012
VOC DETECTION IN POLYURETHANE
FLEXIBLE FOAMS
Occhiello E; Tavan M; Pannocchia P; Fava F
EniChem
(Crain Communications Ltd.; European Isocyanate
Producers Association)
The detection of volatile organic compounds in polyols
and PU foams using SPME, gas chromatography and gas
chromatography-mass spectroscopy is demonstrated.
Accession no.823982
Item 85
73, No.1, 2001, p.163-7
THERMAL, PHYSICAL AND CHEMICAL
STABILITY OF POROUS POLYSTYRENE-TYPE
BEADS WITH DIFFERENT DEGREES OF
CROSSLINKING
Yanhong Li; Yunge Fan; Jianbiao Ma
Nankai,University
The thermal decomposition of porous polystyrene beads
with differing crosslinking degrees using divinyl benzene
were evaluated using thermogravimetry and differential
scanning calorimetry techniques. The test results showed
that the thermal stability of the beads increased with higher
degrees of crosslinking. DSC analysis revealed that the
glass transition temperatures gradually increased with
crosslinking levels up to 30% crosslinking by weight, but
above this level beads were thermally stable as the glass
transition temperature was replaced by an exothermic
peak. Complete details of the testing procedures and
results are given 15 refs.
CHINA
Accession no.823950
Item 86
73, No.1, 2001, p.69-74
EXAMINATION OF A LOW DENSITY
POLYETHYLENE (LDPE) FILM AFTER 15
YEARS OF SERVICE AS AN AIR AND WATER
BARRIER
Moller K; Gervert T; Holmstrom A
Sweden,National Testing & Research Institute
Comparisons between accelerated ageing tests and tests
on polymeric materials aged in actual service conditions
to identify possible degradation mechanisms appear to
be the only reliable method of predicting long term service
lifetimes. A low density polyethylene film used as an air
and water barrier for 15 years in an exterior wall
construction was characterised using tensile testing,
spectroscopy and chromatography techniques. Although
the mechanical properties of the film were unaffected by
ageing, its antioxidant stabilisers were severely degraded.
Full details of the ageing conditions, test methods and
results are given. 16 refs.
EUROPEAN UNION; SCANDINAVIA; SWEDEN; WESTERN
EUROPE
Accession no.823940
Item 87
73, No.1, 2001, p.47-67
VACUUM PYROLYSIS OF COMMINGLED
PLASTICS CONTAINING PVC. PART II.
PRODUCT ANALYSIS
Miranda R; Pakdel H; Roy C; Vasile C
Quebec,Universite Laval; Pyrovac Institute Inc.; Petru
Poni,Institute of Macromolecular Chemistry
Vacuum pyrolysis was performed on HDPE, LDPE, PP,
PS and PVC materials individually, and also on a mixed
plastics sample containing the five polymers. The main
gaseous and liquid products, including chlorinated
hydrocarbons, were identified by chromatography, and
the yields and pyrolysis products were compared for the
individual and mixed runs. The results suggested that the
pyrolysis yields of the plastics mixtures were similar to
those calculated from the pyrolysis of the individual
polymers. However, the chlorine content was lower than
expected indicating limited interaction during pyrolysis.
Full details of the experimental procedures are given
including a detailed tabulation of all the pyrolysis
products. 54 refs.
CANADA; EASTERN EUROPE; RUMANIA
Accession no.823939
Item 88
73, No.1, 2001, p.15-22
THERMO-OXIDATIVE STABILITY OF PP
WASTE FILMS STUDIED BY IMAGING
CHEMILUMINESCENCE
The spread of oxidation in artificially recycled PP
materials, with and without stabilisation, was monitored
using imaging chemiluminescence techniques. The results
were compared with estimates made using Fourier
transform infrared spectroscopy and differential scanning
calorimetry techniques. It was concluded that although
the conventional techniques gave residual lifetimes of five
cycles, imaging chemiluminescence showed that a
significant reduction in oxidative stability had occurred
after only two cycles. Full details of the imaging
chemiluminescence technique used are given with
detailed results. 12 refs.
Accession no.823934
Item 89
DEVELOPMENTS IN POLYMER ANALYSIS AND
CHARACTERISATION Proceedings of a conference
held Shawbury, UK, 10th May 1999.
Shawbury, 1999, Paper 4, p.1-15, 012
CHEMICAL CHARACTERISATION OF
POLYURETHANES
Forrest M J
(Rapra Technology Ltd.)
Polyurethane chemistry is briefly outlined, additives
generally used in polyurethanes are indicated and the
analytical techniques used to characterise the structure,
composition and properties of PUs and PU-based products
are discussed in a comprehensive manner. Techniques
covered include spectroscopic, chromatographic techniques
and miscellaneous techniques, such as wet chemistry
techniques. Sections are included dealing with the
characterisation of polymer structure and starting materials,
molecular weight determinations, characterisation of
additives and cure reaction studies. 14 refs.
WESTERN EUROPE
Accession no.822952
Item 90
Vol. 169, May 2001, p.45-55
CHARACTERIZATION OF THE
INTERACTIONS IN POLYMER/SILICA
SYSTEMS BY INVERSE GAS
CHROMATOGRAPHY
Voelkel A; Milczewsk K; Jeczalik J
Poznan,University of Technology
The inverse gas chromatography technique, (IGC) is
presented as a method of characterisation of the
interactions in polymer-modified silica systems. The
authors propose to express the magnitude of modified
filler/polymer interactions by means of the Flory-Huggins
parameter. Polyether-urethane/modified silica systems
containing different amounts of filler were investigated,
and information relating to the physicochemical properties
of oligomer and modified silicas were presented by means
of the solubility factor to describe the properties of the
polymer layer, and the Flory-Huggins parameter which
describes the polymer-solute or mixture polymer/silica-
solute interactions. These parameters are obtained from
inverse gas chromatography experiments. The influence
of the IGC experiment temperature, the content of
modified silica, and the nature of test solute on the
evaluated parameters are presented and discussed. 7 refs.
Accession no.822644
Item 91
80, No.8, 23rd May 2001, p.1305-11
EFFECT OF RECYCLED POLYPROPYLENE ON
POLYPROPYLENE/HIGH DENSITY
POLYETHYLENE BLENDS
Bonelli C M C; Martins A F; Mano E B; Beatty C I
Rio de Janeiro,Universidade Federal;
Florida,University
A study was made of the effects of addition of recycled
polypropylene on the incompatible blends of virgin
polypropylene with high-density polyethylene. The
characteristics of the recycled polypropylene were
determined by spectrographic and thermal analysis means.
The mechanical properties of the blends were determined.
The 50/50 blend of the two virgin polymers benefited most
from the addition of the recycled polypropylene. 9 refs.
BRAZIL; USA
Accession no.821546
Item 92
72, No.1, 2001, p.175-86
CHEMICAL AND MORPHOLOGICAL
MODIFICATIONS OF IRRADIATED LINEAR
LOW DENSITY POLYETHYLENE (LLDPE)
Guadagno L; Naddeo C; Vittoria V; Camino G;
Cagnani C
Salerno,University; Turin,University; Montell Italia
SpA
Spherilene technology produced films of linear low
density polyethylene which were exposed to UV
irradiation to simulate accelerated weathering.
Comparison was made with a set of films annealed at
60C and no irradiation. The resulting chemical structures
were examined using FTIR. The findings were that the
degradation is dominated by the formation of carbonyl
and vinyl species. 22 refs.
WESTERN EUROPE
Accession no.820850
Item 93
72, No.1, 2001, p.31-45
FACTORS AFFECTING THE ADSORPTION OF
STABILISERS ON TO CARBON BLACK (FLOW
MICRO-CALORIMETRY STUDIES). IV.
SECONDARY ANTIOXIDANTS
Pena J M; Allen N S; Edge M; Liauw C M; Valange B
Manchester,Metropolitan University; Cabot Corp.
Using flow micro-calorimetry, X-ray photoelectron
spectroscopy and Fourier transform infra-red
spectroscopy techniques the surface activity of different
types of carbon black with secondary antioxidants (aryl
phosphites and phosphonites) have been examined. Both
in the overall adsorption activity and the levels of probe
adsorption significant differences were observed. Two
factors were reported which were found to influence the
behaviour of phosphite stabilisers. 29 refs.
UK; WESTERN EUROPE
Accession no.820835
Item 94
50, No.6, June 2001, p.635-42
DEGRADATION OF HIGH BARRIER
ETHYLENE-VINYL ALCOHOL COPOLYMER
UNDER MILD THERMAL-OXIDATIVE
CONDITIONS STUDIED BY THERMAL
ANALYSIS AND INFRARED SPECTROSCOPY
Lagaron J M; Gimenez E; Suara J J
Jaume I,Universitat
The thermooxidative degradation of a solution cast
ethylene-vinyl alcohol copolymer (containing 32
mol.percent ethylene) used in barrier applications was
studied at three temperatures immediately above the
melting point using thermogravimetric analysis, DSC and
FTIR spectroscopy. The weight loss measured by
thermogravimetric analysis was fast at short times and
slowed down progressively. The weight loss of about 3.6
percent measured by thermogravimetric analysis resulted
from chemical alterations in the polymer. DSC showed
small changes in crystallinity, melting point and glass
transition and broadening of the melting endotherms in
samples exposed to the more severe thermooxidative
treatments. FTIR showed a transformation of the vinyl
alcohol hydroxyl groups into carbonyl groups and the
creation of double bonds. Changes in degradation kinetics,
and possibly mechanisms, were thought to occur with
increasing time. FTIR measurements indicated that
transformation of the hydroxyl groups led to a weakening
of the overall hydrogen bonding strength in the degraded
samples so a reduction in the intermolecular cohesion,
and hence the barrier properties of the copolymer, could
be anticipated. 19 refs.
WESTERN EUROPE
Accession no.819207
Item 95
Polymer Science Series B
43, Nos. 3-4,March/April 2001, p.105-8
TRANSFORMATIONS OF ANTIMONY-
HALOGEN- AND NITROGEN-PHOSPHORUS-
BASED FLAME RETARDANTS IN
POLYOLEFINS AND THEIR PERFORMANCE
Bogdanova V V
Belorussian,State University
Degradation products from both antimony-halogen based
and nitrogen-phosphorus based flame retardants were
studied using X-ray diffraction and atomic emission
analysis. Evidence of the retardation mechanisms in use
against combustion was obtained for each system and in
each case emission of volatile combustion inhibitors at
the degradation temperature of the polymer matrix was
the critical factor. 11 refs
BELARUS; BELORUSSIA
Accession no.818458
Item 96
Polimery
45, Nos.11-12, 2000, p.51-8
Polish
PYROLYSIS GAS CHROMATOGRAPHY AND
NEW POSSIBILITIES OF ITS USE IN THE
ANALYSIS OF POLYMERS
Hetper J
Major conditions are formulated to ensure that pyrolysis
gas chromatography yields reliable and repeatable results,
particularly when non-volatile substances such as
polymers are analysed. The authors own modification
of PGC is presented, involving the use of a pyrolysis
attachment with the mobile reaction zone. Resulting data
are compared with those obtained by conventional
pyrolysis gas chromatography. 34 refs.
Accession no.816530
Item 97
New York, John Wiley & Sons, Inc., 1999, pp.xv,752
CHEMICAL SEPARATIONS- PRINCIPLES,
TECHNIQUES, AND EXPERIMENTS
MELOAN, C E
KANSAS STATE UNIVERSITY
This combination laboratory manual and reference source
provides a working knowledge of an array of separation
methods. In forty-two chapters, it explores all major
categories of separation. With an emphasis upon everyday
practice rather that theory, this book explains the
principles and parameters of these methods and provides
59 specific experiments to demonstrate proper procedures.
These experiments feature step-by-step protocols for each
separation scheme, precise instructions on setting up the
apparatus, and checklists for essential chemicals and
supplies. Main Headings include Separations involving
phase changes; Separations involving extraction;
Separations involving chromatography; Separations
involving ion exchange resins; Separations involving
electric fields; Separations involving flotation;
Separations involving membranes; Separations involving
miscellaneous techniques.
USA
Accession no.816497
Item 98
Polymer Bulletin
46, No.2-3, April 2001, p.191-6
MISCIBILITY OF POLYETHERIMIDE AND
POLYBUTYLENE NAPHTHALATE BLENDS
Lin C H; Wang C S
Taiwan,Kung Shan Institute of Technology;
Taiwan,National Cheng Kung University
DSC, optical microscopy, and SEM were performed to
characterise the miscibility of a blend of polybutylene
naphthalate and polyetherimide. Data were compared with
theoretical predictions. 6 refs.
CHINA
Accession no.816205
Item 99
Journal of the National Institute of Materials and
Chemical Research
8, No.4, 2000, p.149-59
Japanese
POSITRONIUM FORMATION AND DIFFUSION
IN POLYMERS
Hirata K; Kobayashi Y
High-energy positrons injected into condensed matter
quickly lose their energy, become thermalised and
annihilate with one of the electrons of the medium into
gamma rays. In polymers, some of the positrons form a
hydrogen-like bound state between a positron and an
electron prior to the annihilation. This bound state is called
positronium (Ps). Ps is formed by recombination of a
positron and one of the electrons released from the
molecules in terminal positron spur. Positron-electron
recombination in the positron spur competes with other
reactions, so that the Ps formation probability depends
on various factors. The influence of additives, polar
groups and external field on Ps formation in polymers is
discussed. A possibility of using Ps as a radiation chemical
probe for polymers is described. Ps formed as a result of
positron-electron recombination interacts with a
subnanometer-size free volume hole, and diffuses over a
certain distance before annihilation. The diffusion
coefficient of Ps is determined using a chemical reaction
between Ps and an additive, and its diffusion length in
amorphous polymers is estimated to be ca.1 nm. This
result is of fundamental importance to apply Ps as a probe
for studying free volume in polymers. 68 refs.
JAPAN
Accession no.815833
Item 100
80, No.11, 13th June 2001, p.2120-2
SOLID-STATE NMR AND XPS STUDIES OF PVA/
SUGARCANE COMPOSITES
Tavares M I B; Stael G C; Gorelova M M; de Menezes
S M C
Rio de Janeiro,Cidade Universitaria
Bagasse, taken directly from the sugarcane mills, was
dried, cut to lengths of 5 mm, and blended with
poly(ethylene-co-vinyl acetate) in proportions up to 60
wt%. The composites were characterised by solid-state
nuclear magnetic resonance spectroscopy and X-ray
photoelectron spectroscopy. A homogeneous copolymer
covering on the surface of the fibres was achieved, the
samples exhibiting homogeneity at the molecular level.
The best physical interaction between the fibres and the
matrix was achieved with the sample containing 60 wt%
fibre. 10 refs.
BRAZIL
Accession no.814366
Item 101
39, No.3, 1st Feb.2001, p.337-41
PHYSICAL AGING OF POLYCARBONATE
INVESTIGATED BY DYNAMIC
VISCOELASTICITY
Apaki O; Horie M; Masuda T
Kyoto,University
Dynamic viscosity measurements were used to determine
the physical ageing at 110C of polycarbonate using
samples quenched from the molten state. The test results
showed that there was a memory effect in the
polycarbonate of the quenching processes, but as
equilibrium is reached then the memory becomes lost.
Evidence is shown that the structure of the polymeric
chain in the glassy state relaxes over larger segment scale
lengths because the scale of the movable segments is
related to temperature. 29 refs.
JAPAN
Accession no.814126
Item 102
Polymer
42, No.13, 2001, p.5523-9
SEC-FTIR CHARACTERIZATION OF SEMI-
CRYSTALLINE HDPE AND PP
Verdumen-Noel L; Baldo L; Bremmers S
DSM Research
A pressure transducer in combination with the size
exclusion chromatography-FTIR technique was used to
characterise semi-crystalline materials such as HDPE and
random PP copolymers. The comonomer content (butene
for HDPE and ethylene for PP) decreased with increasing
molar mass. For two HDPE samples produced by the dual
reactor process, this decrease occurred stepwise with a
constant comonomer amount on either side of the step.
For all the HDPE samples, the amount of end
unsaturations decreased with molar mass. The
concentration of side and trans unsaturations was too low
to be determined. 8 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION;
Accession no.813974
Item 103
286, No.3, 30th March 2001, p.161-7
MATRIX-ASSISTED LASER DESORPTION/
IONIZATION MASS SPECTROMETRY OF
SYNTHETIC POLYMERS, 5A. ANALYSIS OF
POLY(PROPYLENE OXIDE)S BY COUPLED
LIQUID CHROMATOGRAPHY AT THE
CRITICAL POINT OF ADSORPTION AND
MALDI-TOF MASS SPECTROMETRY
Keil C; Esser E; Pasch H
Darmstadt,Deutsches Kunststoff-Institut
Poly(propylene oxide)s were analysed efficiently by
coupled liquid chromatography and MALDI-TOF mass
spectrometry. The techniques were coupled via a robotic
interface where the matrix was coaxially added to the
eluate and spotted dropwise onto the MALDI target. Size
exclusion chromatography and liquid chromatography at
critical conditions of adsorption coupled to MALDI-TOF
gave useful structural information on oligomer masses
and chemical composition; The technique showed the
presence of diols and monools in addition to the triols in
poly(propylene oxide) triols. The oligomer distributions
of all functionality fractions were determined. 23 refs.
WESTERN EUROPE
Accession no.813967
Item 104
Polimery
45, No.10, 2000, p.701-6
Polish
OXIDATION AND DESORPTION OF OXYGEN
FROM THE UPPER LAYER OF ACTIVATED
POLYPROPYLENE FILM
Zenkiewicz M
Photoelectron spectroscopy was used to study oxidation
of biaxially oriented polypropylene film. X-rays and
ultrahigh vacuum associated with the method of study
were found to promote oxygen desorption from the upper
layer. 6 refs. Articles from this journal can be requested
for translation by subscribers to the Rapra produced
International Polymer Science and Technology.
Accession no.813667
Item 105
Macromolecules
34, No.8, 10th April 2001, p.2667-72
SELF-FOCUSING IN GRADIENT LIQUID
ADSORPTION CHROMATOGRAPHY OF
POLYMERS
Degoulet C; Perrinaud R; Ajdari A; Prost J; Benoit H;
Bourrel M
TotalFinaElf; Atofina; Elf Atochem North America
Inc.; ESPCI; Institut Curie; Institut Charles Sadron
The separation process occurring during liquid
chromatography of polymers in a gradient of composition
of the eluent was examined. The main feature was that,
after a transient regime, the concentration profile tended
to move as a front, i.e. without diffusive spreading in time.
This results in relatively sharp peaks and the observation
that long columns were useless. A simple analytical model
was proposed for this self-focussing process that allowed
optimal conditions of operation to be determined. This
analysis was supported by experimental tests. 13 refs.
USA; WESTERN EUROPE
Accession no.813456
Item 106
Macromolecules
34, No.8, 10th April 2001, p.2395-7
NONDESTRUCTIVE MEASUREMENT OF A
GLASS TRANSITION TEMPERATURE AT SPIN-
CAST SEMICRYSTALLINE POLYMER SURFACES
Hyun J; Aspnes D E; Cuomo J J
North Carolina,State University
A non-destructive technique for characterisation of the
surface Tg in PETP is described which involves analysis
of the variation of the ellipsometrically measured
refractive index with temp., using the spectral dependence
of the penetration depth of light to discriminate between
surface and bulk transitions. The surface Tg is shown to
be lower than that of the bulk for spin-cast semicrystalline
PETP films because of density variation and Tg is found
to be lowered further by plasma processing. 18 refs.
USA
Accession no.813421
Item 107
Vol.165, March 2001, p.91-8
RECENT DEVELOPMENTS IN POLYOLEFIN
CHARACTERISATION
Pasch H
A brief review is presented on techniques for the analysis
of polyolefins and additives in polyolefins. Techniques
considered include high-temperature GPC combined with
FTIR spectroscopy for the analysis of chemical
composition as a function of molar mass, crystallisation
fractionation for the analysis of short-chain branching in
LLDPE and of polyolefin blends and pyrolysis-gas
chromatography-mass spectrometry for the determination
of additives, such as antioxidants, in polyolefins. 13 refs.
(3rd Annual UNESCO School & IUPAC Conference on
Macromolecules and Materials Science, Stellenbosch,
South Africa, 2000)
WESTERN EUROPE
Accession no.813085
Item 108
Vinyltec 2000. Conference proceedings.
Philadelphia, Pa., 11th-12th Oct.2000, p.198-202
USE OF ADVANCED ANALYTICAL METHODS
TO ENHANCE THE PERFORMANCE OF VINYL
MATERIALS
Isner J D; Eiden R W
Polymer Diagnostics Inc.
(SPE,Vinyl Div.; SPE,Philadelphia Section)
Analytical laboratories are asked to perform a variety of
test methods in order to solve problems relating to the
performance or otherwise of vinyl materials, and whilst
there are many individual problems that need to be solved,
they can be categorised, it is argued, by a relatively small
number of questions. Five of these questions are
addressed, and ways in which a laboratory may answer
them are discussed. Suggestions are made for techniques
that may be used for each question, and examples of
problems are given. Recent advances in analytical
techniques can be used to address topics such as lifetime
prediction and failure analysis. Questions related to
identification, commercialisation, competitiveness, failure
and performance.
USA
Accession no.811310
Item 109
Journal of Materials Science Letters
20, No.3, 1st Feb.2001, p.257-8
COMMENTS ON A NEW RAMAN PEAK IN A
HIGH-DENSITY POLYETHYLENE
Rodriguez A B; Young R J
Navarra,Universidad Publica; Manchester,University;
UMIST
Raman spectroscopy yields information about the
molecular structure of materials based on the observation
of scattered light spectra, and has been used extensively
in the investigations of polymer structure and
composition: chemical structure and interactions,
morphology, crystalline and amorphous structure,
processing effects and orientation, etc. As an analytical
technique, however, it is not free from artefacts, i.e.
apparent experimental results that are not actually real
but are due to the experimental methods or conditions.
One factor that may be responsible for the presence of
artefacts in Raman spectroscopy is external background
light. There are numerous potential sources of external
background light that lead to sharp spectral peaks. If they
are not excluded from the collection optics of the Raman
instrument, they can lead to noise, or artefacts,
superimposed on the Raman spectrum from the sample.
This background light can come from either the sample
or from the environment around the sample. A study of
the latter is reported. 14 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; UK;
WESTERN EUROPE
Accession no.811165
Item 110
80, No.7, 16th May 2001, p.1071-84
PHASE BEHAVIOUR AND MOLECULAR
MOBILITY IN POLYURETHANE/STYRENE-
ACRYLONITRILE BLENDS
Vatalis A S; Kanapitsas A; Delides C G; Viras K; Pissis P
Kozani,Technological Education Institute;
Athens,University; Athens,Kapodistrian University
The molecular mobility and microphase separation in
blends of crosslinked polyurethane (PUR) and styrene-
acrylonitrile (SAN) copolymer were investigated. The
PUR and SAN copolymer were prepared by reactive
blending with polymer polyols. DSC, thermally
stimulated depolarisation currents (TSDC) techniques,
dielectric relaxation spectroscopy (DRS) and dynamic
mechanical thermal analysis over a wide range of
temperatures and frequencies were used in the
investigation. Results by each technique indicated that
the degree of microphase separation of PUR into hard-
segment (HS) microdomains and soft-segment (SS)
microphase increases on addition of SAN. The various
techniques used were initially compared with each other.
Results showed that for the dynamic glass transition of
the PUR SS microphase the characteristic time scales at
the same temperature are similar for DSC, TSDC and
DMTA and shorter for DRS. The PUR/SAN blends are
classified as fragile systems. 40 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; GREECE;
WESTERN EUROPE
Accession no.810314
Item 111
Macromolecular Rapid Communications
22, No.2, 8th Feb.2001, p.51-67
EVANESCENT WAVE LIGHT SCATTERING.
FUSION OF THE EVANESCENT WAVE AND
LIGHT SCATTERING TECHNIQUES TO THE
STUDY OF COLLOIDS AND POLYMERS NEAR
THE INTERFACE
Matsuoka H
Kyoto,University
The evanescent wave light scattering technique, which is
produced by a fusion of the evanescent wave technique
and light scattering technique, is a very powerful an useful
tool for investigation of colloidal particles and polymers
near the surface and interfaces. Two kinds of evanescent
wave light scattering apparatuses are developed. One is
the evanescent wave dynamic light scattering (EVDLS)
technique and the other is the evanescent wave light
scattering microscope (EVLSM). By EVDLS, the diffusion
behaviour of a colloidal particle near the interface can be
extracted quantitatively as a function of the distance from
the interface. The diffusion coefficient is smaller than those
for particles in bulk, reflecting electrostatic and
hydrodynamic interactions. By EVLSM, the interaction
potential profile between a colloidal particle and the surface
in dispersion can be directly evaluated. EVLSM will play
an import role in colloidal interaction studies, especially at
a low ionic strength. It is also shown that a particle dynamics
study is possible by the EVLSM technique. A new field
will be developed in colloid science and polymer science
by application of the evanescent wave light scattering
technique, i.e. fusion of the evanescent light and a scattering
JAPAN
Accession no.809623
Item 112
79, No.6, 7th Feb.2001, p.1101-12
ULTRASONICATION AND MICROWAVE
ASSISTED EXTRACTION OF DEGRADATION
PRODUCTS FROM DEGRADABLE
POLYOLEFIN BLENDS AGED IN SOIL
Contat-Rodrigo L; Haider N; Ribes-Greus A; Karlsson
S
Stockholm,Royal Institute of Technology;
Valencia,Polytechnical University
Degradation in soil of samples of a polyolefin blend
treated with two different biodegradable additives (a
starch/iron mixture and a commercial product (Mater-Bi
AF05H)) was studied using two non-conventional
extraction techniques. The period studied was from 0 to
21 months, and extracted products were analysed by gas
chromatography mass spectroscopy. Molecular weight
changes were monitored using high-temperature size
exclusion chromatography. Extraction techniques were
ultrasonication and microwave assisted extraction (MAE).
Reproducibility of ultrasonification was found better with
improved extraction of carboxylic acids and other
products than MAE methods, but both were found faster
than conventional (soxhlet) extraction techniques. Tables
indicate the relative amounts of different extraction
products and molecular weight changes in the polymer
blend found over the 21-month period for both
biodegradable additive types. 17 refs
SCANDINAVIA; SPAIN; SWEDEN; WESTERN EUROPE
Accession no.808785
Item 113
10, No.4, Oct./Dec.2000, p.202-8
Portuguese
ETHYLENE COPOLYMERS ANALYSIS BY
FRACTIONATION TECHNIQUES
Escher F F N; Silva L P; Galland G B; Benetti A
Rio Grande do Sul,Universidade Federal; Ipiranga
Petroquimica SA
Ethylene-butene copolymers were fractionated according
to molecular size by direct extraction by different solvents
and at different temperatures. Samples were also
fractionated by differences in crystallinity using DSC.
Fractions were characterised using carbon 13 NMR, FTIR,
GPC and DSC. 9 refs.
BRAZIL
Accession no.808128
Item 114
Journal of Polymer Science: Polymer Chemistry
Edition
39, No.5, 1st March 2001, p.630-9
NEW SEGMENTED POLYESTER-URETHANES
FROM RENEWABLE RESOURCES
Liu Y; Lindblad M S; Ranucci E; Albertsson A-C
Sweden,Royal Institute of Technology
The physical and mechanical properties of aliphatic
polyesters from propanediol and succinic acid were
improved by their combination with aromatic urethane
segments capable of establishing strong intermolecular
hydrogen bonds. Characterisation was carried out using
proton NMR, size exclusion chromatography, DSC, and
dynamic mechanical analysis. The influence of the ratio
of hard and soft segments on degree of crystallinity, Tg,
melting point, tensile strength, elongation and Youngs
modulus was examined. 24 refs.
EUROPE
Accession no.808057
Item 115
80, No.1, 4th April 2001, p.1-9
CROSSLINKING AND ITS EFFECTS ON
POLYANILINE FILMS
Tan H H; Neoh K G; Liu F T; Kocherginsky N; Kang E T
Singapore,National University
Polyaniline base films with varying degrees of
crosslinking were cast from methylpyrrolidone solutions
at different processing temperatures. The effects of
crosslinking on solubility, morphology, tensile strength,
doping characteristics and transport of ions across the
films were investigated. Characterisation was undertaken
using UV visible spectroscopy, atomic force microscopy,
and elemental analysis. 18 refs.
SINGAPORE
Accession no.807643
Item 116
Vol.162, Dec.2000, p.227-33
STUDY OF POLYMER COMPLEXES BY
EXCLUSION CHROMATOGRAPHY COUPLED
WITH LIGHT SCATTERING IN COMBINATION
WITH FLUORESCENCE SPECTROSCOPY
Mrkvickova L; Pokorna V; Pecka J
Czech Republic,Academy of Sciences
PMMA stereocomplexes prepared at different
concentration in dilute tetrahydrofuran solutions are studied
by size exclusion chromatography coupled with refractive
and light scattering detectors in combination with
fluorescence spectroscopy. A considerable increase in
segment density due to complexation compared with free
PMMA chain is only slightly affected by the polymer
concentration in solution where stereocomplexes are
formed. At polymer concentrations up to 3 x 10-3 g cm-3,
an increase in non-uniformity of polymer complex
molecular weight and size and a shift to higher values of
both are observed. In semidilute solutions stereocomplexes
virtually do not become heavier and larger. 6 refs.
CZECH REPUBLIC
Accession no.806260
Item 117
Polymer
42, No.8, 2001, p.3859-66
STRUCTURE FORMATION DURING THE
ISOTHERMAL CRYSTALLISATION OF
ORIENTED AMORPHOUS POLY(ETHYLENE
TEREPHTHALATE) FILMS
Radhakrishnan J; Kaito A
Japan,National Institute of Materials & Chemical
Research
A study was made of structure formation during the
isothermal crystallisation of oriented, amorphous PETP
film from the glassy state using in situ FTIR spectroscopy,
in situ wide-angle X-ray diffraction and small angle X-
ray scattering. The PETP films were prepared by rolling
melt quenched films to a draw ratio of 2 and an evaluation
made of the changes in the conformation and orientation
order of the PETP chains during crystallisation along with
the development of crystalline structure. Structure
organisation before and during isothermal crystallisation
is discussed and a comparison made of the crystallisation
behaviour of oriented with that of isotropic PETP. 27 refs.
JAPAN
Accession no.806185
Item 118
Orlando, Fl., 7th-11th May, 2000, paper 678
USE OF CONTACT-ATOMIC FORCE
MICROSCOPY IN PLASTIC MATERIAL
SURFACES
Reyes E; Guerrero C
Nuevo Leon,Universidad Autonoma
(SPE)
Using thin films of isotactic polypropylene, poly(ethylene
terephthalate) and polystyrene, the range of atomic force
microscopy contact forces and the scanning frequencies
required to obtain sharp and clear 3-D images of polymer
surfaces was determined, by systematically varying these
parameters, starting with typical values used for rigid
surfaces. The optimum values were determined to be a
contact force of 88-150 nN, and a scanning frequency of
1.0-1.5 Hz. 12 refs.
MEXICO
Accession no.805686
Item 119
79, No.3, 18th Jan.2001, p.473-8
PYROLYSIS GAS CHROMATOGRAPHIC
ANALYSIS OF POLYACRYLONITRILE
Minagawa M; Onuma H; Ogita T; Uchida H
Yamagata,University
In the pyrolytic gas chromatographic analysis (PGCA) of
acrylonitrile polymer under an inert atmosphere at 500-900
deg.C, lower nitriles, including methyl cyanide, HCN, and
acrylonitrile were the main degradation products, but lower
hydrocarbons, e.g. methane and ethylene, resulting from
secondary decomposition, were also detected. Thermo-
analytical data, including data on the relation between
retention time and nitrile polarity, and the limiting yield on
pyrolysis as a function of temperature were obtained. On
the basis of these results, specific applications of PGCA and
the usefulness of this method for studying the thermal
degradation of acrylonitrile polymer are indicated. 20 refs.
JAPAN
Accession no.804442
Item 120
West Conshohocken, Pa., 2000, pp.3. NALOAN
ASTM D 3465-. TEST METHOD FOR PURITY OF
MONOMERIC PLASTICISERS BY GAS
CHROMATOGRAPHY
American Society for Testing & Materials
ASTM D 3465-
Version 2000. Photocopies and loans of this document
are not available from Rapra.
USA
Accession no.801052
Item 121
Polymer News
25, No.10, Oct.2000, p.359-60
ANALYSIS OF AIRCRAFT COATING BY
SECONDARY ION MASS SPECTROSCOPY
Usmani A M; Donley M
UDC; Wright-Patterson Air Force Base
An analysis was made of a flat aircraft coating using
secondary ion mass spectroscopy, which revealed that the
coating was a polyurethane C type based on isophorone
diisocyanate, diethylene glycol and adipic acid. X-ray
photoelectron spectroscopy was employed to determine
pigments and extenders. 10 refs.
USA
Accession no.800157
Item 122
THERMODYNAMIC AND KINETIC ANALYSIS
OF SEMICRYSTALLINE RECYCLATES BY DSC
Cassel R B; Li L
Perkin-Elmer Inc.
(SPE)
Developments in differential scanning calorimetry (DSC)
for the characterisation of semicrystalline thermoplastics,
including mixed recyclates are discussed. The techniques
include stepwise DSC for the accurate determination of
specific heat capacity, rapid determination of crystallinity
using the Gray-Mathot total enthalpy technique, and
analysis of crystallisation kinetics. The techniques show
the influence of impurities on the glass transition
temperature, crystallinity and crystallisation. 6 refs.
USA
Accession no.799956
Item 123
NOVEL TECHNIQUE FOR THE DETECTION OF
A HINDERED AMINE LIGHT STABILIZER
(HALS), BASED ON SILICON TECHNOLOGY
Narayan S; Lee R E; Hallberg D; Malatesta V
Great Lakes Chemical Corp.; Great Lakes Chemical
Italia
(SPE)
A technique for the determination of HALS in
polypropylene was developed. The HALS, based on a
polysiloxane backbone with tetramethyl piperidine side
chains, was melt blended with the polypropylene which
was then spun into fibres. The chopped fibres were
dissolved in toluene, the polymer precipitated using
methanol, and the filtrate dried. A solution of the filtrate
was then prepared and analysed by proton nuclear
magnetic resonance spectroscopy. The peak at 0.1 ppm
was attributed to the methyl group on the silicon atom of
the HALS, and was used for quantitative purposes.
Polypropylene pellets were also prepared containing a
lower concentration of HALS, which was subsequently
subjected to direct extraction to prevent the loss which
may occur during polymer reprecipitation. 3 refs.
USA
Accession no.799954
Item 124
ANALYTICAL METHODOLOGIES EMPLOYED
IN A COMPREHENSIVE FDA FOOD CONTACT
COMPLIANCE INVESTIGATION: ANALYSIS
FOR RESIDUAL MONOMERS, RESIN
OLIGOMERS, ADDITIVES AND MODIFIERS IN
SEVERAL FOOD SIMULATING SOLVENTS
Eberhard J S; McCort-Tipton M M
Covance Laboratories
(SPE)
The FDA considers that materials which come into contact
with food, such as processing machinery and packaging,
to be indirect food additives, and the potential migration
of materials into the food requires determination. Ethanol/
water solutions and food oils are commonly used as food
simulating solvents when determining migration. The
subsequent determination of the migrating species (which
may include residual monomers, oligomers, additives and
modifiers) may be by liquid and gas chromatography, and
mass spectroscopy.
USA
Accession no.799953
Item 125
Polymer
42, No.4, 2001, p.1449-59
PHASE SEPARATION IN MISCIBLE POLYMER
BLENDS AS DETECTED BY MODULATED
TEMPERATURE DIFFERENTIAL SCANNING
CALORIMETRY
Dreezen G; Groeninckx G; Swier S; Van Mele B
Leuven,Catholic University; Brussels,Free University
The phase separation of two partially miscible polymer
blends was studied using modulated temp.
DSC(MTDSC). The lower critical solution temp.
demixing behaviour of PEO blended with polyether
sulphone(PES) and with poly(3,4'-diphenylene ether
isophthaloyl amide), as determined by cloud point temps.
with optical microscopy, was in good agreement with
results obtained from non-isothermal MTDSC
measurements. The non-isothermal MTDSC apparent
heat capacity evolution was time-dependent. It was
influenced by the endothermic demixing enthalpy and,
in the case of PEO/PES blends, by the vitrification of a
high-Tg phase formed. Quasi-isothermal MTDSC
measurements contained information on the kinetics of
demixing and remixing, emphasising the added value
of MTDSC to follow in situ the diffusion-controlled
phase separation processes of partially miscible polymer
blends. 32 refs.
WESTERN EUROPE
Accession no.798922
Item 126
Vol.283, Nov.2000 p.153-62
CHARACTERIZATION OF FLAME-SPRAYED
PEEK COATINGS BY FTIR-ATR, DSC AND
ACOUSTIC MICROSCOPY
Simonin L; Liao H
CREST; Belfort-Montbeliard,Universite de
Technologie
Poly (aryl ether ether ketone) (PEEK) was utilised as a
name-sprayed coating because of its good mechanical
properties, low friction coefficient and high thermal
stability. Fine polymeric powders were warmed up in
oxyacetylene flame and sprayed onto a previously heated
aluminium substrate. Investigation of the degree of
crystallinity of PEEK coatings was carried out using
differential scanning calorimetry (DSC), according to
the rate of cooling after the spraying process. Structural
modifications were revealed by FTIR-ATR, attributed
to interactions between the flame and the polymeric
powders. Ultrasonic methods were developed, especially
acoustic microscopy, to study the variations of
mechanical properties at the surface and the defects
inside the material. In general terms, flame-sprayed
coatings contain a large amount of porosity. Particularly
suited to the observation of large defects (exceeding 50
microns) inside the polymeric materials is low-frequency
microechography, a non-destructive technique. 19 refs.
Accession no.798668
Item 127
Polymer Preprints, Volume 40, Number 2, August
1999, Conference proceedings.
New Orleans, La., August 1999, p.1043-4
MALDI/TOF/MS STUDY OF HOMOPOLYMERS
AND AMPHIPHILIC DIBLOCK COPOLYMERS
BASED ON SULPHONATED POLYSTYRENE
Yang A; Nonidez W K; Mays J W
Birmingham,University of Alabama
Matrix-assisted laser desorption ionisation time of flight
mass spectroscopy (MALDI/TOF/MS) provides a new
way to probe polymers; it can provide information on
molecular weight, molecular weight distribution, mass
of end groups and mass of repeating units. Further
information, such as reactivity ratios, individual block
chain length and its distribution, etc., can be obtained
based on mass information. Polystyrene sulphonic acid
and its sodium salt form have been successfully
characterised by MALDI/TOF/MS, but no MALDI/TOF/
MS study of diblock copolymers containing a polystyrene
sulphonic acid block appears to be evident. The results
of such a study of amphiphilic diblock copolymers,
NaPSS-b-PtBS, and their precursors, PSb-PtBS, are
reported. Number-average and weight-average molecular
weights (Mn and Mw), polydispersity indices and extents
of sulphonation are obtained. 13 refs.
USA
Accession no.798428
Item 128
71, No.1, 2001, p.123-34
QUALITY-DETERMINATION OF RECYCLED
PLASTIC PACKAGING WASTE BY
IDENTIFICATION OF CONTAMINANTS BY GC-
MS AFTER MICROWAVE ASSISTED
EXTRACTION (MAE)
Camacho W; Karlsson S
Sweden,Royal Institute of Technology
The resulted are reported of an investigation into the
quality of recycled HDPE and PP separated from mixed
municipal solid waste carried out using gas
chromatography-mass spectrometry. The development of
a simple and rapid microwave assisted extraction method
for the systematic analysis of low molec.wt. compounds,
such as decomposition products and additives, in
polymers is also reported and successfully applied to the
analysis of contaminants in the above recycled plastics.
15 refs.
EUROPE
Accession no.796627
Item 129
70, No.2, Nov.2000, p.269-75
RAMAN SPECTRAL MAPPING OF
PHOTOOXIDISED POLYPROPYLENE
Blakey I; George G A
Queensland,University of Technology
The photooxidation of unstabilised, isotactic PP was
investigated using Raman spectral mapping in
combination with SEM/energy dispersive X-ray analysis,
which permitted the determination of Ziegler-Natta
catalyst residue distribution throughout the PP. It was
found that oxidation was heterogeneous at a microscopic
scale and that a high local concentration of catalyst
residues resulted in the stabilisation of the polymer in the
immediate vicinity and the formation of mobile reactive
species, which initiated oxidation at sites away from the
catalyst. 30 refs.
AUSTRALIA
Accession no.795269
Item 130
Macromolecules
33, No.19, 19th Sept.2000, p.7088-92
SOLUTION CARBON-13 NMR
CHARACTERIZATION OF NYLON 66:
QUANTITATION OF CIS AMINE
CONFORMERS, ACID AND AMINE GROUPS,
AND CYCLIC UNIMERS
Southern Mississippi,University
Edited by: Davis R D; Steadman S J; Jatterr W L;
Mathias L J
Using a mixed 2,2,2-trifluoroethanol/deuteriochloroform
solvent system, well-resolved solution carbon-13 NMR
spectra of nylon-66 samples were obtained which showed
several low intensity peaks which were not seen in more
acidic solvents. The low intensity peaks were correlated
with the methylene carbons near cis amide conformers,
acid and amine end groups and within cyclic oligomers.
The quantitative contents of these components for a
typical nylon-66 sample were 1.1 mol% cis amide
conformers, 1.0 mol% acid end groups and 0.5 mol%
amine end groups. From end group concentrations, the
number-average molecular weight of the nylon-66 was
calculated to be 30 177 g/mol. The chemical shift values
of methylene carbons in the end groups and in cyclic
oligomers was pH sensitive and thus depended on the
relative concentrations of acid and amine groups in each
sample. 12 refs.
USA
Accession no.794402
Item 131
40, No.11, Nov.2000, p.2442-55
EVALUATION OF THREE METHODS FOR THE
MEASUREMENT OF CRYSTALLINITY OF PET
RESINS, PREFORMS, AND BOTTLES
Bashir Z; Al-Aloush I; Al-Raqibah I; Ibrahim M
SABIC R & D
The crystallinity of PETP resins, preforms and bottles was
investigated using DSC, modulated DSC and density
measurements. The PETP employed was a bottle-grade
PETP copolymer containing 1.5% isophthalic acid. The
accuracy, precision and validity of the techniques
employed were evaluated and problems encountered in
interpreting the results assessed. 47 refs.
SAUDI ARABIA
Accession no.793608
Item 132
Kautchuk und Gummi Kunststoffe
53, No.10, Oct.2000, p.574/81
German
DIRECT ANALYSIS OF ADDITIVES IN
POLYMERIC MATERIALS BY PYROLYSIS-GAS
CHROMATOGRAPHY-MASS SPECTROMETRY
Meyer-Dulheuer T; Pasch H; Geissler M
This article describes the direct analysis of additives by
pyrolysis-gas chromatography-mass spectrometry. Using
this method it is possible to identify additives quickly
and reliably without separation of the polymer matrix. A
small specimen of the sample is pyrolysed, i.e. degraded
under inert gas atmosphere. The pyrolysis products are
separated by gas chromatography and ionised in the mass
spectrometer by electron-impact ionisation. By comparing
the results with library data it is possible to identify
unknown additives unambiguously and with high
accuracy. 10 refs.
WESTERN EUROPE
Accession no.792613
Item 133
61, No.2, 2000, p.589-96
CALORIMETRIC ANALYSIS OF AN ISOTACTIC
POLYPROPYLENE GAMMA-IRRADIATED IN
VACUUM
Spadaro G; Valenza A
Palermo,University
The molecular modifications induced in an isotactic PP
gamma-irradiated in vacuum under a complete set of
experimental conditions are studied by means of calorimetric
analysis. The influence of the irradiation parameters, the total
absorbed dose, D, and the dose rate, I, has previously been
analysed and a simple kinetic model based on the rates of
the main reactions occurring during irradiation, i.e. beta-
scission, addition to double bonds and termination, was also
discussed. It is shown how thermal analysis confirms the
model forecasts and in particular the existence of the
inversion conditions: below them the main effect is
molecular degradation, while above them the main effects
are chain-branching and crosslinking. 12 refs.
WESTERN EUROPE
Accession no.792350
Item 134
ICAC 99. Conference proceedings.
Bristol, UK, 23rd-24th Sept.1999, p.133-43
IDENTIFICATION OF KEY CURE STAGES IN
LIQUID MOULDING PROCESSES BY
PARALLEL PLATE DIELECTRIC ANALYSIS
McIlhagger A T; Matthews S T; Brown D; Hill B
Ulster,University
(IOM Communications Ltd.; Ulster,University;
IMechE)
The aerospace industry has recognised the major benefits
associated with fibre reinforced composite materials. The
more popular techniques available for composite
production are the traditional wet lay-up or autoclave and
resin transfer moulding (RTM). Efforts to further reduce
processing time and improve part quality have focused
on improved process control. To date this has been based
on off-line techniques. The need for on-line cure
monitoring is widely recognised and this will require the
development of suitable in-mould sensors. The
Engineering Composites Research Centre (ECKE) has
investigated and concentrated on the specific problems
encountered in the aerospace industry. Of the available
cure monitoring methods, parallel plate dielectric analysis
(DEA) appears to offer the greatest potential for
determining the through-thickness cure state of the resin
during cure. A laboratory dielectric instrument is utilised
to simulate RTM and autoclave cure cycles for composite
structures containing non-conductive and conductive
fibres and for different resin systems used in the aerospace
industry. Key resin cure stages are identified by an
appropriate dielectric signal and correlated with data from
other thermal and mechanical techniques. Insulated
parallel plate dielectric sensors are being developed for
use in the laboratory instrument with the potential for
incorporation into composite production tooling. 26 refs.
WESTERN EUROPE
Accession no.790059
Item 135
Polymer Journal (Japan)
32, No.7, 2000, p.610-5
INFRARED SPECTROSCOPIC AND
MODULATED DIFFERENTIAL SCANNING
CALORIMETRY STUDY OF PHYSICAL AGING
IN BISPHENOL A POLYCARBONATE
Jin Lu; Yong Wang; Deyan Shen
Academia Sinica
FTIR spectroscopy was used to study the conformational
changes in quenched bisphenol A polycarbonate films
during physical ageing. The conformation changed
gradually from the high energy trans-cis conformation to
the low energy trans-trans conformation on sub-glass
transition temperature annealing. In-situ FTIR studies on
the conformational changes of films quenched from the
rubbery and sub-glass transition temperature annealed for
different times were carried out while increasing the
temperature through the glass transition region. The
results indicated that incremental changes in the
population of trans-cis conformers in the quenched sample
were gradual, whereas rather abrupt changes occurred in
the sub-glass transition temperature annealed samples.
The energy absorbed during the abrupt conformational
change represented only part of the endothermic peak
observed by modulated DSC. The authors concluded that
some new cohesional entanglements may be formed
during physical ageing. 28 refs.
CHINA
Accession no.789734
Item 136
32, No.7, 2000, p.560-6
CALORIMETRIC AND INFRARED
SPECTROSCOPIC ANALYSIS OF MULTIPLE
MELTING ENDOTHERMS OF
Yong Wang; Jin Liu; Deyan Shen
The multiple melting behaviour of PETP was studied
using DSC, FTIR spectroscopy and temperature
modulated DSC by examining PETP samples subjected
to special schemes of crystallisation and annealing
treatment at different temperatures. On one-step and two-
step annealing, a series of multiple endothermic minor
peaks was observed, resulting from the melting of
imperfect crystals during crystallisation. Both dual
morphology and melting-recrystallisation-remelting
mechanisms were probably responsible for the observed
multiple melting behaviour which was dependent on the
thermal history of the PETP samples. 34 refs.
CHINA
Accession no.789727
Item 137
Analytical Chemistry
72, No.19, 1st Oct.2000, p.4550-4
GPC SEPARATION OF POLYMER SAMPLES
FOR MALDI ANALYSIS
Hanton S D; Liu X M
Air Products & Chemicals Inc.; Lab Connections Inc.
MALDI mass spectrometry was combined with GPC
analysis for broad polydispersity polymers with the use
of liquid chromatography interface. Results for PMMA
were compared with a blend of five narrow PMMA
standards that mimic the broad dispersed material. 24 refs.
USA
Accession no.789529
Item 138
Polymers Paint Colour Journal
190, No.4432, Sept.2000, p.25-6
WATCHING PAINT DRY
Middleton J
The development of nuclear magnetic resonance imaging,
a technique previously only used in medicine, to provide
various information, including the drying rate, position
of water and curing in waterborne coatings, is discussed.
The principles of magnetic resonance imaging are outlined
and work conducted at Surrey University in conjunction
with Resonance Instruments to design equipment for
coatings analysis is described.
SURREY,UNIVERSITY; RESONANCE
INSTRUMENTS
WESTERN EUROPE
Accession no.789465
Item 139
78, No.5, 31st Oct.2000 p.1009-16
CRYSTALLIZATION OF LOW-DENSITY
POLYETHYLENE- AND LINEAR LOW-DENSITY
POLYETHYLENE-RICH BLENDS
Drummond K M; Hopewell J L; Shanks R A
RMIT University
Using differential scanning calorimetry (DSC) the
crystallisation of a series of low-density polyethylene
(LDPE)- and linear low-density polyethylene (LLDPE)-
rich blends was examined. After continuous slow cooling
DSC analysis showed a broadening of the LLDPE melt
peak and subsequent increase in the area of a second
lower-temperature peak with increasing concentration of
LDPE. Melt endotherms following stepwise
crystallisation (thermal fractionation) detailed the effect
of the addition of LDPE to LLDPE, showing a nonlinear
broadening in the melting distribution of lamellae, across
the temperature range 80-140 degrees Celsius, with
increasing concentration of LDPE. A rise in the population
of crystallites melting in the region between 110 and 120
degrees Celsius, a region was observed where as a pure
component LDPE does not melt. A decrease in the
crystallite population over the temperature range where
LDPE exhibits its primary melting peaks (90-110 degrees
Celsius) was noted, indicating that a proportion of the
lamellae in this temperature range (attributed to either
LDPE or LLDPE) were shifted to a higher melt
temperature. 30 refs.
Accession no.789066
Item 140
49, No.9, Sept.2000, p.1007-13
USING SPECTROSCOPY WITH
CHEMOMETRICS TO MEASURE POLYMER
MOLAR MASS
Shenton M J; Herman H; Stevens G C
Surrey,University
The ability to determine the molar mass of a polymer is
of fundamental importance to describe polymer molecular
characteristics. Conventional methods for measuring
molar mass include viscometry, osmometry, light
scattering and analytical gel permeation chromatography.
Although high quality data can be obtained by these
methods, the results can be significantly affected by
sample preparation, and they are often time consuming
and unsuitable for real-time on-line processing. The
potential of determining polymer molar mass using optical
spectroscopy combined with chemometric analysis is
demonstrated. This is technically attractive because
optical spectroscopy is routinely used to collect process
data on-line and some refineries routinely monitor and
control blending using near-infrared spectroscopy. A
comparable development to monitor polymer molar
masses on-line from systems already being used to
measure density and melt index, would be of potential
value to many sectors of the polymer production and
processing industry. Chemometrics is a multivariate
methodology that allows the information from entire
spectra to be used; it can be considered as a maximal
compression technique. Extracted factors can then be
regressed against property data by using a well-
characterised set of training samples to produce
predictive regression models. It is shown that simple
spectroscopic methods, such as the Raman technique
discussed, when coupled with chemometrics, are capable
of providing molar mass and distribution information.
This is illustrated with reference to polydimethylsiloxanes
in the liquid phase. 18 refs.
WESTERN EUROPE
Accession no.787562
Item 141
Composite Interfaces
7, No.2, 2000, p.81-92
INVESTIGATING INTERPHASE
DEVELOPMENT IN WOOD-POLYMER
COMPOSITES BY INVERSE GAS
CHROMATOGRAPHY
Rials T G; Simonsen J
USDA; Oregon,State University
The influence of secondary interactions on the
development of interfacial structure in composites of
wood and amorphous thermoplastic polymers is not well
understood. Inverse gas chromatography is used to
investigate the effect of different polymers on the surface
energy of partially or fully coated white pine wood meal.
In this way, the development of the interphase is
monitored as a function of polymer depth on the wood
surface. The polymers are selected to provide a range of
functional groups and include PS, PMMA, PVC,
polymethacrylic acid and polymethacrylonitrile. The
overall variation of the dispersive component of the
surface energy and the ratio of acceptor to donor
coefficients appear to group themselves into two
categories based upon the polarity of the polymers
functional groups. In addition, the high loadings required
for stabilisation of the less polar polymers suggest that a
relatively large volume of the matrix phase isaffected by
the wood filler. 20 refs.
USA
Accession no.786897
Item 142
Polymer Science Series B
42, Nos.5-6, May-June 2000, p.169-74
IR SPECTROSCOPY STUDY OF POLYMER
POROSITY
Pakhomov P M; Kruglova E V; Khizhnyak S D
Tver,State University
IR spectroscopic method is developed for evaluating the
porosity (concentration and size of pores) in polymers.
PE and PAN films of various porosity are prepared from
the solutions in liquid and solid paraffins. The
concentration and maximum pore size in the bulk and in
a surface layer of the samples are determined by IR
spectroscopy in the transmission and reflection modes,
respectively. The results obtained are in agreement with
the data of optical and atomic force microscopy. 12 refs.
RUSSIA
Accession no.786845
Item 143
Iranian Polymer Journal
9, No.2, April 2000, p.117-24
STUDY OF CRYSTALLINITY OF HIGH-
DENSITY POLYETHYLENE BY INVERSE GAS
CHROMATOGRAPHY
Ghaemy M; Hadjmohammadi M R; Tabaraki R
Mazandaran,University
The crystallinity of HDPE (Poliran-HD0035 and Irapol-
5620) was investigated using inverse gas chromatography.
The effects of flow rate of carrier gas and sample size on
peak retention volume and of the amount of injection on
retention volume were evaluated. Retention diagrams and
degrees of crystallinity of the HDPEs were determined
and compared with those of LDPE. 15 refs.
IRAN
Accession no.786383
Item 144
77, No.7, 15th Aug.2000, p.1419-31
CURE MODELING AND MONITORING OF
EPOXY/AMINE RESIN SYSTEMS. 1. CURE
KINETICS MODELING
Karkanas P I; Partridge I K
Cranfield,University
An investigation using differential scanning calorimetry
was carried out under both isothermal and dynamic curing
conditions to determine the cure kinetics of four epoxy/
amine resins. Various cure kinetic models were used to
compare them with the results of the DSC results. Good
fits were found, in good agreement with the experimental
results for the resin systems. 22 refs.
WESTERN EUROPE
Accession no.786048
Item 145
International Polymer Science and Technology
27, No.6, 2000, p.T/7-T/9. (Translation of Muanyag es
Gumi, No.3, 2000, p.89)
APPLICATION OF STATE-OF-THE-ART
METHODS IN ADHESION TECHNOLOGY. 1
Vabrik R; Czajlik I; Bertoti I; Keresztes Z; Ille A;
Rusnak I; Vig A; Kalman E
The use is demonstrated of microscopic analysis
techniques for the investigation of adhesive failure. PVC
sheet was bonded to glass using a M35R hybrid UV
curable adhesive based on epoxy resin. Atomic force
microscopy and X-ray induction photoelectron
spectroscopy were used for the chemical characterisation
of of failure surfaces. 11 refs.
Accession no.785593
Item 146
78, No.1, 3rd Oct. 2000, p.166-72
EFFECT OF POLY(VINYL CHLORIDE)/
CHLORINATED POLYETHYLENE BLEND
COMPOSITION ON THERMAL STABILITY
Klaric I; Vrandecic N S; Roje U
Split,University
The miscibility of PVC and chlorinated PE and the effect
of the blend composition on the heat stability of the PVC
were investigated using several techniques, including
TGA and DSC. The apparent activation energy of PVC
dehydrochlorination in the blends was calculated and
experimental TGA curves compared with those predicted
using the additivity rule. It was found that the blends were
heterogeneous and that addition of chlorinated PE in a
specific temperature range resulted in an improvement
in the heat stability of the PVC. 22 refs.
CROATIA
Accession no.784861
Item 147
Polymer
41, No.22, Oct.2000, p.8161-5
APPLICATION OF MODULATED-
TEMPERATURE DIFFERENTIAL SCANNING
CALORIMETRY TO THE STUDY OF
CRYSTALLISATION KINETICS IN POLY(E-
CAPROLACTONE)-POLY(STYRENE-CO
ACRYLONITRILE) BLENDS
Song M; Hourston D J
Loughborough,University
In order to evaluate the application of modulated-
temperature differential scanning calorimetry (M-TDSC)
to the study of the crystallisation kinetics of semi-
crystalline polymers, isothermal crystallisation kinetics
in poly(e-caprolactone)-SAN blends are investigated. The
temperature dependence of d ln G/dT (G =crystal growth
rate), determined by M-TDSC agrees approximately with
previous experimental data and theoretical values. These
were obtained from direct measurements of spherulite
growth rate by optical microscopy. Here, theoretical and
M-TDSC experimental results show that the d ln G/dT
versus temperature plots are not sensitive to the non-
crystalline component in the poly(e-caprolactone)-SAN
blends. 15 refs.
WESTERN EUROPE
Accession no.784242
Item 148
Polymer
41, No.22, Oct.2000, p.8151-4
PORE DIMENSION OF WATER TREES IN PE:
NMR STUDIES
Judeinstein P; Carmo Lanca M; Marat-Mendes J; Rault J
Paris-Sud,Universite; Portugal,Universidade Nova de
Lisboa
In PE films aged under electric field the crystallisation of
water (and melting of ice) is studied by quadrupolar NMR,
this technique allows determination of water concentration
as low as 10 -4. It is shown that the pore dimensions of
the tracks forming the water trees of the order of 2.5 nm
are independent of the ageing time. The mobility of water
in these water trees and in porous glass, of similar pore
dimensions, are compared. 17 refs.
PORTUGAL; WESTERN EUROPE
Accession no.784240
Item 149
77, No.10, 6th Sept.2000, p.2178-8
CURE MODELLING AND MONITORING OF
EPOXY/AMINE RESIN SYSTEMS. II.
NETWORK FORMATION AND
CHEMOVISCOSITY MODELLING
Karkanas P I; Partridge I K
Cranfield,University
The glass transition temperature (Tg) advancement and
the chemoviscosity development under isothermal
conditions are investigated for four epoxy/amine systems,
including commercial RTM6 and F934 resins. Differential
scanning calorimetry is the thermoanalytical technique
used to determine the Tg advancement, and rheometry
for determination of the chemoviscosity profiles of these
resin systems. The complex cure kinetics are correlated
to the Tg advancement via a one-to-one relationship using
Di Benedettos formula. It is revealed that the three-
dimensional network formation follows a single activated
mechanism independent of whether the cure kinetics
follow a single or several activation mechanisms. The
viscosity profiles show the typical characteristics of
epoxy/amine cure. A modified version of the Williams-
Landel-Ferry equation (WLF) is adequate to model the
viscosity profiles of all the resin systems, in the
temperature range 130 to 170 deg.C, with a very good
degree of accuracy. The parameters of the WLF equation
are found to vary in a systematic manner with cure
temperature. Further correlation between Tg and viscosity
shows that gelation, defined as the point where viscosity
reaches 10 4 Pas, occurs at a unique Tg value for each
resin system, which is independent of the cure conditions.
16 refs.
WESTERN EUROPE
Accession no.784172
Item 150
Fire & Materials
24, No.2, March/April 2000, p.101-12
SMOKE GAS ANALYSIS BY FOURIER
TRANSFORM INFRARED SPECTROSCOPY -
SUMMARY OF THE SAFIR PROJECT RESULTS
Hakkarainen T; Mikkola E; Laperre J; Gensous F;
Fardell P; Le Tallec Y; Bajocchi C; Paul K; Simonson
M; Deleu C; Metcalfe E
VTT Building Technology; Centexbel; Elf Atochem
SA; UK,Building Research Establishment; CEMATE;
LSF SUD srl; Rapra Technology Ltd.; Sweden,National
Testing & Research Institute; Ghent,University;
Greenwich,University
The determination of toxic components from fire gases
is difficult because the environment is hot, reactions are
often temperature dependent, and a lot of soot may be
produced. Due to the different properties of the gas
components, a different time-consuming procedure for
each species has traditionally been used. The use of FTIR
(Fourier transform infrared) spectrometers as a continuous
monitoring technique overcomes many of the problems
in smoke gas analyses. FTIR offers an opportunity to set
up a calibration and prediction method for each gas
showing a characteristic spectral band in the infrared
region of the spectrum. The objective of the SAFIR project
was to further develop the FTIR gas analysis of smoke
gases to be an applicable and reliable method for the
determination of toxic components in combustion gases
related to fire test conditions. The optimum probe design,
filter parameters and the most suitable sampling lines in
terms of flow rate, diameter, construction material and
operating temperature have been specified. In the large
scale, special concern was given to the probe design and
the effects of the probe location as well as practical
considerations of the sampling line length. Quantitative
calibration and prediction methods have been constructed
for different components present in smoke gases.
Recommendations on how to deal with interferents, non-
linearities and outliers have been provided and a
verification method for the spectrometer for unexpected
variations and for the different models have been
described. FTIR measurement procedures in different fire
test scenarios are studied using the recommendations of
this project for measurement techniques and analysis and
an interlaboratory trial of the FTIR technique in smoke
gas analysis is carried out to define the repeatability and
reproducibility of the method in connection with a small
scale fire test method, the cone calorimeter. 9 refs.
FINLAND; FRANCE; ITALY; SCANDINAVIA; SWEDEN; UK;
WESTERN EUROPE
Accession no.784096
Item 151
Polymer
41, No.23, Nov.2000, p.8241-5
USE OF RAMAN SPECTROSCOPY TO STUDY
THE REACTION BETWEEN AN AMINE-
TERMINATED THERMOPLASTIC AND EPOXY
RESINS
van Overbeke E; Carlier V; Devaux J; Carter J T;
McGrail P T; Legras R
Louvain,Universite Catholique; ICI Plc
Reactive thermoplastics are often used as toughening
modifiers for epoxy resins. Raman spectroscopy was used
to follow the reaction of aromatic amines with epoxide
monomers through the evolution of an amine-substituted
aromatic vibration. A double shift of this peak was correlated
with the formation of secondary and tertiary amines. Band
assignment was confirmed by the study of model
compounds. Using this method, qualitative observation of
the reaction between an amine-terminated copolyether-
sulphone thermoplastic and epoxide was performed.
Unfortunately, in the blend studied containing the curing
agent, a band appearing upon curing overlapped with the
band characterising the end group reaction. 17 refs.
UK; WESTERN EUROPE
Accession no.783075
Item 152
68, No.3, 2000, p.437-43
SEMI-QUANTITATIVE ANALYSIS OF
THERMAL DEGRADATION IN
POLYPHENYLENE ETHER
Kinoshita M; Nemoto T; Souda T; Takeda K
Koito Mfg.Co.Ltd.; Shibaura,Institute of Technology
The use of simple computer simulation and analysis of
the thermal degradation products of differently thermally
aged samples of melt processed polyphenylene ether film
gave information on possible degradation routes for this
polymer. An increase in dimeric products was noted with
increased thermal ageing, but not in monomeric products.
To explain the distribution of scission products found
experimentally, the simple computer model was arranged
to simulate cleavage rates of methylene bridge, ether and
sidechain links. Although results were not totally
conclusive, it was noted that both ether bridge and side
chain cleavage rates were similar, and approximately nine
times lower than cleavage rates of the methylene bridge.
It is suggested that quantitative results determined will
give detailed information on flame retardance due to the
understanding of rates of volatile product generation at
the polymer surface. 28 refs.
JAPAN
Accession no.782776
Item 153
68, No.3, 2000, p.321-6
COMPARATIVE ANALYSIS OF THE PHOTO-
OXIDATION OF POLYSTYRENE AND
POLY(ALPHA-METHYLSTYRENE)
Mailhot B; Jarroux N; Gardette J-L
Ensemble Universitaire des Cezeaux
Fourier transform infrared spectroscopy (FTIR) and mass
spectroscopy were used to study the photo-oxidation of
both poly(alpha-methylstyrene) (PMS) and polystyrene
(PS) films which had been irradiated at different
temperatures and with different radiation sources under
an oxygen atmosphere. The oxidised films were treated
with ammonia or sulphur tetrafluoride and photolysis
carried out under vacuum. Photoproducts from both
polymers were broadly similar, but aromatic ketone
concentration was higher from the PMS and a new ketone
was also identified from this source. Routes for formation
of identified photoproducts are proposed. 13 refs.
WESTERN EUROPE
Accession no.782763
Item 154
ACS, Polymeric Materials Science & Engineering Fall
Meeting 1999. Volume 81. Conference proceedings.
New Orleans, La., 22nd-26th Aug.1999, p.242-3
ANALYSIS OF THE NANOPHASE STRUCTURE
OF SEMICRYSTALLINE POLYMERS WITH
ATOMIC FORCE MICROSCOPY (AFM),
MICROCALORIMETRY (MC) AND
TEMPERATURE-MODULATED
CALORIMETRY (TMC)
Wunderlich B
Tennessee,University; Oak Ridge National Laboratory
(ACS,Div.of Polymeric Materials Science & Engng.)
Semicrystalline, polymeric materials consist usually of
metastable aggregates of strongly coupled microphases or
nanophases with their constituent, micrometre-long, flexible
molecules traversing multiple phase domains. Some 40 years
ago it was established that well-formed crystals are often
lamellar with a thickness of only about 10 nm. Between these
lamellae one can find the remaining amorphous phase with
even smaller dimensions. Less perfect crystallisation can
decrease the crystal dimensions to as little as 1-2 nm in all
dimensions. An operational definition of the microphase is
its having at least one dimension smaller than a micrometre,
while nanophases are approached when the small dimension
approaches 10 nm. Characteristic of the microphases is the
need to consider the surface properties for their description,
i.e. the melting temperature depends on the surface free
energy. Nanophases, in turn, show an interaction between
opposing surfaces, i.e. they may show no bulk properties. If
the dimensions decrease below 1 nm, the macroscopic phase
description has reached its limit. Many macromolecules can,
however consist of alternating sequences of nanometer-
length chain segments that are immiscible, so that in all their
phase structures there is a strong tendency of nanophase
separation. It is shown that special tools must be developed
to probe the nanophase structures and properties of polymers.
Some new information available by using three rather new
techniques their combinations are described. 10 refs.
USA
Accession no.780666
Item 155
CRYSTALLISATION AND MELTING OF
POLYMER CRYSTALS REVEALED BY T-M DSC
Toda A; Oda T; Tomita C; Hikosaka M; Arita T;
Saruyama Y
Hiroshima,University; Kyoto,Institute of Technology
Temperature-modulated differential scanning calorimetry
(T-MDSC) applies a thermal modulation in temperature
to a conventional DSC run and determines a dynamic heat
capacity from the relationship between the modulation
components of temperature and of heat flow. Primary
application of this technique has been the measurement
of specific heat capacity and the examination of the
anomaly in a relaxation process such as alpha process
related to the glass transition. An application to the first-
order phase transitions of crystallisation and melting of
polymer crystals has recently been suggested. The method
and typical results are described. 13 refs.
JAPAN
Accession no.780663
Item 156
FILM FORMATION IN POLYMER LATEX
BLENDS: MICROSPECTROSCOPIC 3D STUDIES
Zhao Y; Urban M W
North Dakota State University
A series of previous studies on latex films indicates that
mobility of low molecular weight species in particular
surfactant molecules, may be affected by latex glass
transition temperature, and subsequently, by free volume
of a polymer matrix, surface tension at the film/air and
film/substrate interfaces, compatibility and coalescence
times, to name just a few. It appears that there are other
factors that not only influence distribution of individual
components including distribution of surfactants, but also
may significantly affect film formation. In an effort to
enhance understanding of these multi-phase latex blends
and their coalescence, a series of experiments on latexes
containing PS and poly-n-butyl acrylate (p-nBA) blends
is presented. An attempt is made to identify factors
affecting film formation of PS/p-nBA latex blends using
multi-dimensional vibrational spectroscopic methods, and
these findings are compared with respective copolymers.
The effects of SDOSS exudation by latex composition,
particle and annealing temperatures are also addressed in
terms of phase separation and dynamics of
macromolecular segments. 21 refs.
USA
Accession no.780632
Item 157
FAILURE STUDIES OF ADHESION BY UV
REFLECTION AND FLUORESCENCE
TECHNIQUES
Kim N-J; Jeong C N; Sung C S P; Sung N-H
Connecticut,University; Tufts University
Various techniques such as optical and electron microscopy,
IR-ATR ESCA and SIMS have been used for failure mode
analysis in polymeric adhesive joints. However, these
techniques are not amenable for in situ, non-destructive
examination of the failure surfaces as failure occurs. In
order to develop in situ techniques, UV reflection and
fluorescence methods are evaluated, as they can be applied
via optical fibres to the actual failure surface. Failure
surfaces of two types of adhesive joints are examined by
UV reflection and fluorescence, complemented by FT-IR
ATR studies. The first joint studied is PU on epoxy-coated
steel. The second is PETP/PE/PETP. 8 refs.
USA
Accession no.780560
Item 158
72, No.11, 1st June 2000, p.2490-8
CHARACTERISATION OF POLYETHER AND
POLYESTER POLYURETHANE SOFT BLOCKS
USING MALDI MASS SPECTROMETRY
Mehl J T; Murgasova R; Dong X; Hercules D M;
Nefzger H
Vanderbilt University; Bayer Corp.
Selective degradation reactions combined with MALDI
analysis were applied for molecular weight determination
of polyether and polyester polyurethane soft blocks. Size
exclusion chromatography was combined with MALDI to
provide accurate molecular weight determination. 44 refs.
USA
Accession no.778970
Item 159
Vol.152, March 2000, p.267-78
ANALYSIS OF COMPLEX POLYMERS BY
MALDI-TOF MASS SPECTROMETRY
Pasch H; Ghahary R
German Plastics Institute
The results are reported of an analysis of the functionality,
molar mass and chemical composition of complex
polymers, using MALDI-TOF mass spectrometry and a
combination of MALDI-TOF mass spectrometry and
liquid chromatography. Polymers investigated included
polyamide-12, bisphenol A polycarbonate, methoxylated
melamine-formaldehyde resin, carboxy-terminated PS
and PMMA. 33 refs.
WESTERN EUROPE
Accession no.778702
Item 160
Journal of Injection Molding Technology
4, No.2, June 2000, p.84-91
ANALYSIS OF STYRENE PLASTIC RESIDUES
ON INJECTION MOULDING TOOLS
Makinen M; Astola J; Poutanen J; Alen R; Paakkonen E
Tampere,University of Technology;
Jyvaskyla,University
The contaminating substances formed during the injection
moulding of ABS and PS parts were removed from the
mould surface. The residues were characterised using
FTIR, gas chromatography, pyrolysis gas
chromatography, elemental analysis, detection reaction
test of bromine, and different dissolving tests. The
chemical composition of the contamination was clarified
and suitable solvents for dissolving these products were
selected. 6 refs.
EUROPEAN UNION; FINLAND; SCANDINAVIA; WESTERN
EUROPE
Accession no.776471
Item 161
Polymer
41, No.15, 2000, p.5949-55
UNDERSTANDING VITRIFICATION DURING
CURE OF EPOXY RESINS USING DYNAMIC
SCANNING CALORIMETRY AND
RHEOLOGICAL TECHNIQUES
Lange J; Altmann N; Kelly C T; Halley P J
Queensland,University
The gelation and vitrification transitions during cure of
an epoxy resin-amine system were examined using
rheological, modulated DSC and FTIR techniques. The
results of DMA showed that gelation was observed before
vitrification at all temps. where it could be rheologically
defined. By comparing different rheological criteria for
vitrification, it was seen that the vitrification transition
was a gradual process that extended over a large part of
cure at all temps. where it occurred. Results from
modulated DSC measurements showed that the
calorimetric vitrification times were longer than the
vitrification times obtained from rheological
measurements at cure temps. above 100C, but that at lower
temps. calorimetric vitrification occurred before, or at the
same time as, rheological vitrification. Theoretical
gelation times, estimated from FTIR conversion data,
were found to be consistently shorter than the observed
gelation times. Theoretical vitrification times agreed well
with the observed times. The magnitude of the vitrification
transition, expressed either as amount of change in heat
capacity or as maximum value of loss tangent, was found
to decrease approximately linearly with increasing cure
temp. 34 refs.
AUSTRALIA
Accession no.776348
Item 162
Macromolecules
33, No.8, 18th April 2000, p.3180-3
COMPLETE ASSIGNMENT OF PROTON AND
CARBON 13 NMR SPECTRA OF
POLYVINYLCARBAZOLE
Karali A; Froudakis G E; Dais P; Heatley F
Crete,University; Manchester,University
Details are given of the assignment of the proton and
carbon 13 spectra of polyvinylcarbazole by using a
number of modern gradient two-dimensional NMR
experiments. The relationship between the assignments
and the conformational and dynamic properties of the
polymer is discussed. 13 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; GREECE; UK;
WESTERN EUROPE
Accession no.776167
Item 163
59, Nos.1-2, 2000, p.409-24
CHARACTERISATION OF POLYURETHANE
COATINGS USING THERMOANALYTICAL
TECHNIQUES
Ginic-Markovic M; Choudhury N R; Matisons J G;
Williams D R G
South Australia,University; Adelaide,University
A two-pack PU coating was analysed using
thermoanalytical techniques. The curing reaction was
monitored using pressure differential calorimetry,
rheometry and dynamic mechanical analysis. The
decomposition behaviour was examined using TGA. 13
refs.
AUSTRALIA
Accession no.776090
Item 164
Injection Molding
8, No.6, June 2000, p.42/50
MATERIALS ANALYST: PART 33 -
DETERMINING COMPOSITION
Sepe M
This article focuses on the problems associated with
identifying a polymer. There are three major techniques
that are particularly helpful in identifying the type of
polymer used in a compound. These are DSC, TGA and
IR spectroscopy. Each of these techniques has its
strengths, and in determining the composition of the
polymer, the task is to highlight properties and behaviour
that are distinctive.
USA
Accession no.775805
Item 165
Polymer
41, No.11, 2000, p.4361-5
RAPID MICROWAVE INDUCED
DEPOLYMERISATION OF POLYAMIDE 6
Klun U; Krzan A
Ljubljana,National Institute of Chemistry
Polyamide 6 depolymerisation was performed using
microwaves as the energy source for the acid catalysed
hydrolysis, with phosphoric acid as the catalyst. The
product mixture was analysed by chromatographic and
spectroscopic methods. 19 refs.
SLOVENIA
Accession no.774158
Item 166
Polymer
41, No.11, 2000, p.4039-46
MATRIX-ASSISTED LASER DESORPTION/
IONISATION MASS SPECTROMETRY OF
SYNTHETIC POLYMERS. IV. COUPLING OF
SIZE EXCLUSION CHROMATOGRAPHY AND
MALDI-TOF USING A SPRAY-DEPOSITION
INTERFACE
Esser E; Keil C; Braun D; Montag P; Pasch H
Darmstadt,Deutsches Kunststoff-Institut
Size exclusion chromatography and MALDI-TOF mass
spectrometry was coupled via a robotic interface. For
polydisperse synthetic polymers a continuous track of
matter was deposited onto the matrix surface. Spectra
were taken from different positions of the polymer track.
Data are presented for PS, PMMA and butyl methacrylate-
methyl methacrylate copolymers. 20 refs.
WESTERN EUROPE
Accession no.774127
Item 167
Muanyag es Gumi
37, No.3, 2000, p.89-91
Hungarian
APPLICATION OF STATE-OF-THE-ART
METHODS IN ADHESION TECHNOLOGY. I.
Vabrik R; Czajlik I; Bertoti I; Keresztes Zs; Ille A;
Rusznak I; Vig A; Kalman E
Atomic force microscopy (AFM) and X-ray photoelectron
spectroscopy (XPS) were used to study the nature of the
failure interface and the failure mechanism in a PVC film/
adhesive/glass system. The failure mode was found to be
mostly interfacial, occurring at the glass/adhesive interface,
and also partially cohesive, located in the adhesive layer
very close to the interface. The results are discussed in
relation to the chemical nature of the interface and the
failure mechanism. 11 refs. Articles from this journal can
be requested for translation by subscribers to the Rapra
produced International Polymer Science and Technology.
Accession no.773793
Item 168
78, No.521, Nov.1999, p.541-6
Spanish
STRUCTURAL CHARACTERISATION OF
MULTILAYER POLYMERIC MATERIALS BY
MICRORAMAN SPECTROSCOPY
Sanz R; Martin B; Merino J C; Pastor J M
Valladolid,Universidad
Results are presented of a study in which confocal
microRaman spectroscopy was used to determine the
structure of the individual polymers present in a series of
multilayer food packaging films. 8 refs.
AMCOR FLEXIBLES ESPANA SA
WESTERN EUROPE
Accession no.773260
Item 169
Iranian Journal of Polymer Science & Technology
12, No.2, Summer 1999, p.1-8
Persian
KINETIC STUDY OF THE AUTO-OXIDATION
OF POLYURETHANE
Semsarzadeh M A; Salehi H
Tarbiat Modarres University
Gel permeation chromatography was used to study the
kinetics of the auto-oxidation of polyurethane. The
stationary state rate and the induction time were
determined at various temperatures. FTIR and H NMR
were used to determine the alcohol, acetate and formate
compounds in the auto-oxidation products.
IRAN
Accession no.773140
Item 170
Journal of Macromolecular Science B
B39, No.2, 2000, p.279-96
TIME-RESOLVED FTIR STUDY OF
CRYSTALLISATION BEHAVIOUR OF MELT-
CRYSTALLISED POLYPHENYLENE SULPHIDE
Yu J; Asai S; Sumita M
Tokyo,Institute of Technology; China,Textile
University
The crystallisation behaviour of polyphenylene sulphide
was studied using time-resolved FTIR spectroscopy and
the results obtained correlated with DSC measurements.
The 1073 cm/1 amorphous band was selected for the time-
resolved measurements. The procedure provided details
on the microstructure of the PPS, including heterogeneity
of the amorphous phase above and below Tg. A method
is proposed for calculating the rigid, amorphous fraction
in terms of the increase in the slope of the absorbance
variation with temperature at the glass transition. 43 refs.
CHINA; JAPAN
Accession no.772147
Item 171
76, No.6, 9th May 2000, p.938-46
OPTIMIZATION OF EXPERIMENTAL
PARAMETERS FOR THE QUANTIFICATION OF
POLYMER ADDITIVES USING SFE/HPLC
Thilen M; Shishoo R
Swedish Institute for Fibre & Polymer Research
A study was conducted with the aim of extracting the
antioxidants Irganox 1010 and Irgafos 168 from a PP
matrix by using the supercritical fluid extraction(SFE)
technique and by subsequent analysis using high-
performance liquid chromatography(HPLC). The
experimental parameters of temp., pressure and modifiers
were varied to find the best extraction conditions. The
optimum temp. and pressure for extraction of these
polymer additives were found to be 120 and 384 bar, with
methanol as the modifier. The quantitative extractions
were significantly faster than those reported previously
in the literature. The results showed that the SFE/HPLC
technique used in these experiments was a reliable and
environmentally-friendly alternative to the commonly-
used liquid extraction and analytical methods. 22 refs.
EUROPE
Accession no.770687
Item 172
Vol.148, Dec.1999, p.463-81
CHARACTERIZATION OF ACRYLIC DENTAL
POLYMERS
Vera-Graziano R; Martinez-Richa A; Palacios-Alquisira
J; Barcelo-Santana F; Castano-Meneses V
Mexico,Universidad Nacional Autonoma;
Guanajuato,Universidad
The chemical composition, dimensions and the molecular
parameters of four dental acrylic polymer materials and
two polyacrylic acids of different molec.wt. used as model
compounds were studied by NMR and IR spectroscopies,
GPC, intrinsic viscosity and light scattering
measurements. Two of the dental polymers were shown
to be mainly polyacrylic acid, while one showed the peak
pattern for an acrylic acid/methyl acrylate copolymer of
about 2:1 composition and one was an oligomer derived
from 2-hydroxyethyl methacrylate. The steric hindrance
parameter, molecular stiffness and second virial
coefficient were calculated using different thermodynamic
models. The Flory-Fox-Shafgagen and the Stockmayer-
Fixman models fitted the experimental data reasonably
well and could be use to describe the molecular parameters
of the acrylic polymers. 18 refs. (7th International
Conference on Polymer Characterization (POLYCHAR-
7), Denton, Texas, USA, Jan.1999)
MEXICO
Accession no.770356
Item 173
Flame Retardants 2000. Conference proceedings.
London, 8th-9th Feb.2000, p.185-92
PRACTICE OF FTIR ANALYSIS FOR FIRE
GASES (SAFIR)
Mikkola E
VTT Building Technology
(BPF; Interscience Communications Ltd.; APME;
European Flame Retardant Assn.; Fire Retardant
Chemicals Assn.)
The use of FTIR (Fourier transform infrared)
spectrometers as a continuous monitoring technique
overcomes many of the problems associated in analyses
of hot fire gases. FTIR offers an opportunity to set up a
calibration and prediction method for each gas showing
a characteristic spectral band in the infrared region of the
spectrum. A European project, SAFIR, aims to further
develop the FTIR gas analysis of smoke gases to be an
applicable and reliable method for the determination of
toxic components in combustion gases related to fire test
conditions. Within this project, optimal working
conditions including sampling, calibration and analysis
for FTIR fire gas method are defined and verified under
a variety of fire test scenarios. The FTIR method are
shown to be a repeatable and reproducible method for
the determination of the most important toxic gas
components of real fires. Moreover, the findings of this
project concerning sampling techniques are most relevant
for other methods used for defining fire gases. 5 refs.
EUROPEAN UNION; FINLAND; SCANDINAVIA; WESTERN
EUROPE
Accession no.768669
Item 174
Surface Coatings International
83, No.3, March 2000, p.111-8
DETERMINATION OF VOC EMISSIONS FROM
LATEX PAINTS DURING AND AFTER
APPLICATION; METHODS, PERFORMANCE
AND PRECISION
Zeh H
Wacker Polymer Systems GmbH
VOC emissions from indoor latex paints during and after
application is determined by four different test methods:
a chamber method in which an emission chamber is
combined with gas chromatography, two practical
methods in which VOC emitted in a room is measured
either by the determination of the total organic carbon or
by infrared spectroscopy, and an in-can-individual-VOC
method which determines the VOC of a liquid paint by
the quantitative analysis of each volatile component. VOC
emission data gathered by these methods are compared
with calculations from a dynamic computer model
describing the time-dependence of the VOC emission in
the room atmosphere. This comparison indicates that the
in-can-individual-VOC method with computer
calculation allows variations in the size of the room, the
application rate, VOC content of the paint and the rate of
air change, without the necessity of additional
experiments, and therefor, offers an approach with a
reduction in costs. 10 refs.
WESTERN EUROPE
Accession no.768107
Item 175
72, No.902, March 2000, p.53-61
ACID ETCH OF AUTOMOTIVE CLEARCOATS.
II. COMPARISON OF DEGRADATION
CHEMISTRY IN LABORATORY AND FIELD
TESTING
Schmitz P J; Holubka J W; Xu L-F
Ford Motor Co.
X-ray photoelectron spectroscopy was used to determine
whether exposure conditions used in the laboratory
gravimetric etch testing of acrylic melamine clearcoats
simulated field degradation pathways. The surface
chemistry of the field exposed panels was examined and
the results compared with those for laboratory treated
powders having identical technologies. Consistency in the
formation of a melamine salt and ammonium sulphate
upon field exposure and laboratory acid treatment
indicated that the laboratory treatment conditions
simulated the field exposure conditions. 7 refs.
USA
Accession no.767768
Item 176
Journal of Adhesion Science and Technology
14, No.5, 2000, p.745-64
XPS ANALYSIS OF THE COVERAGE AND
COMPOSITION OF COATINGS ON GLASS
FIBRES
Thomason J L; Dwight D W
Owens-Corning Science & Technology Center
The use of X-ray photoelectron spectroscopy as a method
for characterising different sizings on glass fibres was
evaluated. A model, based on a patchy sizing overlay
hypothesis, was developed to aid in the reduction of data
obtained from the X-ray photoelectron spectroscopic
analysis. It is shown that the spectroscopic results, when
combined with the weight fraction of the sizing, provide
a quantitative value for the coverage of the fibre surface
by the sizing. 25 refs.
USA
Accession no.767755
Item 177
Polymer News
25, No.2, Feb.2000, p.56-8
POLYMER ANALYSIS AND
CHARACTERISATION
Garbassi F
EniChem SpA
Analytical techniques, such as mass spectroscopy, atomic
absorption spectroscopy and atomic emission
spectroscopy, for the detection of trace elements, mainly
metal trace elements, in polymers, used particularly in
food, are briefly considered. The disadvantages and
suitability of such techniques are summarised. 10 refs.
WESTERN EUROPE
Accession no.766702
Item 178
Adhesion 99. Conference Proceedings.
Cambridge, UK, 15th-17th Sept.1999, p.369-73
INTERPHASE CHEMISTRY OF CARBON FIBRE
COMPOSITE MATERIALS
Prickett A C; Vickers P E; Smith P A; Watts J F
Surrey,University
(IOM Communications Ltd.)
The fibre-matrix interface in carbon fibre-reinforced
epoxy resin composites was studied by time of flight
secondary ion mass spectrometry (ToF-SIMS) using novel
preparation techniques. The initial adsorption between
uncured resin or amine curing agent and the fibre was
investigated by the use of adsorption isotherms obtained
by the analysis of fibre surfaces following immersion in
liquid solutions of the resin. The intact interphase of a
composite could be examined by ToF-SIMS following
mode I or mode II failure within the spectrometer by the
use of carefully designed in-situ fracture stages. 11 refs.
WESTERN EUROPE
Accession no.765326
Item 179
Adhesion 99. Conference Proceedings.
Cambridge, UK, 15th-17th Sept.1999, p.347-50
MICRO THERMAL ANALYSIS AT
INTERPHASES
Hassler R; zur Muhlen E
Dresden,Institut fuer Polymerforschung; TA
Instruments GmbH
(IOM Communications Ltd.)
Details are given of a thermal analysis technique, referred
to as micro thermal analysis, which combines the high
resolution positioning of scanning probe microscopy with
some of the quantitative analysis capabilities of conventional
thermal analysis. The application of this technique in
characterising the thermal properties of interfaces in
aluminium/epoxy resin adhesive joints and in glass fibre-
reinforced epoxy resin composites is described. 7 refs.
UK; WESTERN EUROPE
Accession no.765322
Item 180
Macromolecules
33, No.1, 11th Jan.2000, p.120-4
BRANCHING AND CROSSLINKING IN
RADIATION-MODIFIED PTFE. A SOLID-STATE
NMR INVESTIGATION
Fuchs B; Scheler U
Dresden,Institute of Polymer Research
High-resolution fluorine 19 NMR was used to investigate
the structural changes resulting from PTFE electron
irradiation under vacuum. A quantitative analysis of the
data was used to establish the density of side groups and
branches. 20 refs.
WESTERN EUROPE
Accession no.764731
Item 181
Color and Appearance Retec 1999. Conference
proceedings.
Nashville, Tn., 27th-29th Sept.1999, p. 178-87
USING MICROSCOPY AS A PROBLEM
SOLVING TOOL IN PLASTICS
Compton C
Sun Chemical Corp.
(SPE,Color & Appearance Div.)
Microscopy is a valuable tool for pigment evaluation and
problem solving in plastics and other applications. The
organic pigments used in plastic applications are typically
sub-micron in size. Pigment performance is greatly affected
by how well the pigment particles are incorporated in the
polymer medium. Various microscopic evaluation
techniques that can be used to investigate dispersion quality,
strength development and thermal stability are reviewed.
In addition, various microscopic techniques for identifying
contaminants are discussed. 7 refs.
USA
Accession no.764247
Item 182
Composites Part A: Applied Science and
Manufacturing
31A, No.2, 2000, p.165-71
FAILURE PHENOMENA IN TWO-
DIMENSIONAL MULTI-FIBRE
MICROCOMPOSITES. PART IV: A RAMAN
SPECTRASCOPIC STUDY ON THE INFLUENCE
OF THE MATRIX YIELD STRESS ON STRESS
CONCENTRATIONS
van den Heuval P W J; Peijs T; Young R J
Eindhoven,University of Technology; UMIST; Queen
Mary & Westfield College
Raman spectroscopy is used to study the influence of shear
yield stress of the matrix on stress situations in carbon
fibre/epoxy resin composites containing a planar fibre
array. A mixture of two curing agents, with different
functionality and molecular weights, are used to cure the
epoxy resin in order to obtain a matrix with varying cross-
linked density. The carbon fibres are surface treated to
give good fibre-matrix adhesion. Three matrix systems
are investigated in the study, each with a different yield
stress. The mechanical properties of each material are
measured under tension and shear conditions. 35 refs.
NETHERLANDS; UK; WESTERN EUROPE
Accession no.763633
Item 183
Journal of Macromolecular Science A
A36, No.11, 1999, p.1751-8
POLYPROPYLENE PIPES FOR DRINKING
WATER SUPPLY
Hametner C
Austrian Plastics Institute
The migration of phenolic antioxidants (which are
typically used for the stabilisation of PP pipes) into
drinking water in contact with PP pipes was studied.
Austrian, German and International Standard methods
were used for water at 23C and 60C. The low molecular
degradation product 2,4-di-tert-butylphenol, rather than
the high molecular antioxidants, was detected in the
aqueous extracts. In warm water extracts, the
concentration of phenols, the total organic carbon content
and the effect on odour and flavour were considerably
higher than in cold. Alkaline water extracted higher
amounts of phenols but acidic drinking water showed no
effect. Thermal loading of PP during the extrusion process
significantly increased the extractable phenols, total
organic carbon content and flavour number/threshold
odour. 7 refs.
AUSTRIA; EUROPEAN UNION; WESTERN EUROPE
Accession no.763574
Item 184
West Conshohocken, PA, 1999, pp.6. NALOAN.
ASTM D 2124-. METHOD FOR ANALYSIS OF
COMPONENTS IN POLY (VINYL CHLORIDE)
COMPOUNDS USING AN INFRARED
SPECTROPHOTOMETRIC TECHNIQUE
American Society for Testing & Materials
ASTM D 2124-
Version 99. Photocopies and loans of this document are
not available from Rapra.
USA
Accession no.760789
Item 185
72, No.900, Jan.2000, p.69-74
ANALYSIS OF EXEMPT PAINT SOLVENTS BY
GAS CHROMATOGRAPHY USING SOLID-
PHASE MICROEXTRACTION
Bodrian R R
California,Polytechnic University
Acetone, methyl acetate and parachlorobenzotrifluoride
have been exempted as VOC solvents by the EPA. In
measuring coating VOC content, separate methods for
determining exempt solvents are required. One such
method utilises solid-phase microextraction to sample the
headspace of solvent-based coatings to which the
surrogates acetone-d6, methyl acetate-d3 and/or
metachlorbenzotrifluoride have been added. The sampled
exempt coating solvents are thermally desorbed and
analysed using gas chromatography with flame ionisation
or mass spectral detection. This paper presents the results
obtained for acetone and toluene in a large number of
aerosol paints. Additionally, the results from a round-robin
study for acetone, methyl acetate and
parachlorobenzotrifluoride in commercial solvent-based
coatings are reported. 17 refs.
USA
Accession no.760572
Item 186
57, No.3, 1999, p.847-51
IDENTIFICATION OF POLYETHYLENE BY
DIFFERENTIAL SCANNING CALORIMETRY
Tsukame T; Kutsuzawa M; Sekine H; Saitoh H;
Shibasaki T
Saitama,Criminal Investigation Laboratory;
Saitama,University
A forensic sample consisting of melt-recrystallised
polymers recovered from the scene of a fire in a factory
is identified by differential scanning calorimetry. The
factory commonly used two kinds of film sheets, A and
B, made by different manufacturers. It is necessary to
decide whether the forensic sample related to material A
or B. The forensic sample and reference samples of
materials A and B are subjected to IR spectroscopy and
pyrolysis gas chromatograph mass spectrometry
measurements, which reveal their PE nature. The thermal
behaviour of the samples is examined by differential
scanning calorimetry (DSC) and they are found to be
blends of two kinds of PEs, LDPE and LLDPE. The
samples can be identified and distinguished from each
other via the DSC measurements. 6 refs.
JAPAN
Accession no.760331
Item 187
58, No.1, 1999, p.13-8
THERMAL CHARACTERISATION OF
POLYURETHANE ACRYLATE RESINS
Ledru J; Saiter J M; Grenet J; Yuossef B; Burel F;
Bunel C
Rouen,University; Rouen,Institut National des Sciences
Appliquees
Polyurethane acrylate resins cured by two different
methods, thermally and photochemically, are investigated
by means of differential scanning calorimetry and
thermally stimulated depolarisation currents. Even if both
curing methods lead to the same material from a chemical
point of view, important differences exist between the
thermocured resin and the photocured resin in terms of
molecular relaxation behaviour. 8 refs.
WESTERN EUROPE
Accession no.760327
Item 188
53, No.11, Nov.1999, p.1412-8
IN-LINE NEAR-INFRARED MONITORING OF
POLYMER PROCESSING. I. PROCESS/
MONITOR INTERFACE DEVELOPMENT
Reshadat R; Desa S; Joseph S; Mehra M; Stoev N;
Balke S T
Toronto,University
Near-infrared inline monitoring of polymer processing
means using an optical fibre-assisted spectrometer to
obtain spectra of the polymer melt flowing through
commonly used processing equipment (an extruder).
Conditions in the extruder are typically 200 deg.C and
20 MPa. The design of interfaces between the
spectrometer and the molten polymer is shown. Three
designs are shown, each permitting monitoring at a
different location in the process: a melt-at-die interface,
a melt-in-barrel interface and a strand interface. These
designs are for monitoring just before the extruder exit,
in the main barrel of the extruder and after the product
exits from the extruder as a strand, respectively. All these
interfaces protect the inserted optical fibre probe from
the harsh environment within the extruder while
permitting easy replacement or a probe without
interrupting the process. This latter characteristic is very
important because it permits easy probe repair as well as
the use of other types of probes (for monitoring colour or
particles, for example) to be used during a run. Examples
of near-infrared spectra obtained with each of the
interfaces used with an immiscible blend of PE and PP
are shown. Large differences in the spectra demonstrate
that the design of the interface will affect multivariate
analysis directed at composition prediction. Subsequent
papers are directed at using the melt-at-die interface for
composition prediction and accounting for nonlinear
relationships between absorbance and concentration. 6
refs.
CANADA
Accession no.760231
Item 189
53, No.11, Nov.1999, p.1403-11
THERMAL VOLATILISATION ANALYSIS: A
VERSATILE PLATFORM FOR
SPECTROSCOPIC INVESTIGATION OF
POLYMER DEGRADATION PROCESSES
Guo X; Huang B; Dyakonov T; Chen Y; Padron L;
Vickstrom T; Kuhn J; Hodkiewicz J; Stevenson W T K
Wichita,State University; Harrick Scientific Co.;
Oklahoma State University; Koch Industries Inc.; ATI
Instruments
Thermal volatilisation analysis (TVA) and sub-ambient
thermal volatilisation analysis (SATVA) techniques are
described. In addition to rate profiling of the volatile
product flux of thermal degradation under high-vacuum
conditions through measurement of pressure in the
vacuum line as a function of sample temperature, the TVA
technique is shown to afford a convenient method for an
on the basis of volatility under high-vacuum conditions,
of product fractions of thermal degradation for subsequent
spectroscopic analysis. The capacity and flexibility of
TVA as a platform for these analyses are illustrated in a
case study format by degrading poly(bisphenol A, 2-
hydroxy propylether). The overall degradation process is
quantified, and most significant pathways of thermolysis
are identified through subsequent spectroscopic analysis
of products of decomposition. The design and construction
of a modified vacuum-tight long-path gas IR cell, as an
interface allowing for the application of Fourier transform
infrared spectroscopy (FT-IR) for the online analysis of
volatile products of polymer degradation, is described.
Proof of concept and application of this new analytical
technique, subsequently referred to as TVA/FT-IR, is
illustrated through the examination of appropriate aspects
of the thermal degradation of PMMA polymers. 49 refs.
USA
Accession no.760230
Item 190
71, No.21, 1st Nov.1999, p.4793-9
GEL PERMEATION CHROMATOGRAPHY
COUPLED TO FOURIER TRANSFORM MASS
SPECTROMETRY FOR POLYMER
CHARACTERIZATION
Aaserud D J; Prokai L; Simonsick W J
Florida,University
On-line coupling of GPC to Fourier transform(FT) mass
spectrometry(MS) using a modified commercial
electrospray ionisation(ESI) interface was studied.
Selected oligomer profiles for the sodiated oligomer ions
of a narrow molec.wt. PMMA were generated and used
for obtaining a calibration curve. Using the MS-generated
calibration curve and the refractive index response for
quantification, an accurate MWD was calculated and
shown to be in good agreement with the value specified
by the supplier. GPC/ESI/FT-MS also allowed for an
unequivocal end group determination and characterisation
of a secondary distribution due to the formation of cyclic
reaction products. A glycidyl methacrylate/butyl
methacrylate copolymer with a broad MWD was
analysed, fractionation and high resolving power being
required for adequate characterisation. MWD data showed
the advantages of coupling high-resolution MS and GPC
to overcome the difficulty of analysing polydisperse
polymers with MS alone. 34 refs.
USA
Accession no.759794
Item 191
Polymer
40, No.26, 1999, p.7341-50
SURFACE STRUCTURE OF KEVLAR FIBRE
STUDIED BY ATOMIC FORCE MICROSCOPY
AND INVERSE GAS CHROMATOGRAPHY
Rebouillat S; Peng J C M; Donnet J-B
Du Pont de Nemours International SA; Haute-
Alsace,Universite
Kevlar fibre surface structure is primarily and directly
observed in the filament configuration by the tapping
mode at omi c force mi croscopy (AFM). The
microfibrils feature is observed with an average width
of 500 nm, composed of various types of periodical
units of an average size 50 nm in a pleating appearance.
At the less crystalline spot on the Kevlar fibre surface,
the periodical organisations exhibit the skin core-like
differentiation. In contrast, at the highly crystalline
spot, the periodicity is more uniformly arranged by a
rect angul ar net work manner. Inverse gas
chromatography (IGC) is used as a tool to investigate
the surface structure heterogeneity by calculating the
surface energy of different types of probes adsorbed
on t he Kevl ar fi bre surface. The energy si t es
distribution plot of n-hexylamine adsorption at finite
dilution exhibits a two-adsorbing-peaks curve. At the
higher energy site, a possible hydrogen bonding
interaction is proposed between n-hexylamine and
oxygen-containing groups formed at the less crystalline
surface. According to the AFM and IGC results, a
Kevlar fibre surface organisations model at the
nanometer scale is proposed. 19 refs.
SWITZERLAND; WESTERN EUROPE
Accession no.758987
Item 192
200, No.10, Oct.1999, p.2345-55
THERMAL DEGRADATION MECHANISMS OF
POLYETHERIMIDE INVESTIGATED BY
DIRECT PYROLYSIS MASS SPECTROMETRY
Carroccio S; Puglisi C; Montaudo G
Istituto per la Chimica e la Tecnol.dei Mat.Pol.;
Catania,University
The thermal degradation of poly(2,2' -bis(3,4-
dicarboxyphenoxy)phenylpropane-2-phenylenediimide)
was investigated by TGA and direct pyrolysis mass
spectrometry and the pyrolysis of this polyimide
compared with that of an aromatic polyamide (NOMEX).
The structure of preformed oligomers from the purified
polyetherimide and the structure of high temperature
pyrolysis products obtained at 620C were examined and
the thermal degradation pathways involved in the
degradation elucidated. 32 refs.
WESTERN EUROPE
Accession no.757742
Item 193
200, No.10, Oct.1999, p.2205-7
COLLECTION OF SOLID-STATE CARBON-13
CP/MAS NMR SPECTRA OF COMMON
POLYMERS
Wilhelm M; Neidhoefer M; Spiegel S; Spiess H W
Max-Planck-Institut fuer Polymerforschung; Wiley-
VCH Verlag GmbH
A collection of high resolution solid-state Carbon-13
NMR spectra of a wide range of polymers is presented. It
is useful for reference purposes in case of unknown or
partly unknown samples, such as polymer blends, block
copolymers or polymeric latices. 16 refs.
WESTERN EUROPE
Accession no.757725
Item 194
66, No.1, 1999, p.107-25
VACUUM PYROLYSIS OF PVC. II: PRODUCT
ANALYSIS
Miranda R; Pakdel H; Roy C; Darmstadt H; Vasile C
Quebec,Universite Laval; Institut Pyrovac Inc.; Petru
Poni,Institute of Macromolecular Chemistry
Vacuum pyrolysis of pure PVC was carried out at various
temperatures between 220 and 520C and under a total
pressure of 2 kPa. The main gaseous and liquid pyrolysis
products obtained during the different stages of thermal
degradation were identified and quantified by
chromatographic methods. Global mass balance and
chlorine mass balance were determined and different
methods of capturing hydrogen chloride under vacuum
conditions were tested. The elemental composition,
surface properties and calorific value of the solid residue
were determined. 43 refs.
CANADA; EASTERN EUROPE; RUMANIA
Accession no.757340
Item 195
Polymer Recycling
4, No.1, 1999, p.13-25
COMPOSITIONAL ANALYSIS AND
FEASIBILITY STUDY OF RECYCLED HDPE
FOR DIRECT FOOD CONTACT APPLICATIONS
Salafranca J; Cacho J; Nerin C
Zaragoza,University
Five HDPE samples, consisting of a virgin HDPE for
food-contact applications, three samples of this polymer
taken after each of the three sequential recycling cycles
and a real post-consumer sample were analysed. Two
different extraction methods were applied: a combination
of maceration and sonication; and the total dissolution of
the polymer. In order to evaluate both the feasibility of
using these polymers in food-contact applications and the
evolution of HDPE composition through the recycling
process, samples were analysed by both qualitative and
quantitative GC-MS. Furthermore, GC-FID was applied
to the determination of alpha-alkenes, the most
representative compounds as indicators of polymer matrix
degradation. Finally, antioxidants were analysed by
reversed phase HPLC. 34 refs.
WESTERN EUROPE
Accession no.756660
Item 196
48, No.10, Oct.1999, p.1042-5
EFFECTS OF UV RADIATION ON SEVERAL
HIGH-PERFORMANCE POLYIMIDE
COMPOSITES
Kiefer R L; Herring K; Wylie B J; Orwoll R A;
Thibeault S A
Williamsburg,College of William & Mary; NASA
Langley Research Center
Three carbon fibre-reinforced polyimides were exposed
to UV radiation at 177C, at three different intensities for
three different times, so that the product of intensity and
time was a constant. Intensities of 1, 2 and 3 suns, where
one sun is the power in space at one earth-sun distance,
were used, for a time periods of 500, 250 and 167 h. The
samples were characterised by X-ray photoelectron
spectroscopy (XPS), thermogravimetric analysis,
thermomechanical analysis and dynamic mechanical
analysis. Measurement of bulk properties showed no
difference between samples exposed to heat and UV
radiation, and control samples. Surface analysis by XPS
showed an apparent decrease in carbonyl concentration
on the surface of some exposed samples. This was
correlated to surface contamination by a silicone-
containing material. 3 refs.
USA
Accession no.756185
Item 197
Composites Part A: Applied Science and
Manufacturing
30A, No.12, 1999, p.1401-13
USE OF XPS FOR CHARACTERISATION OF
GLASS FIBRE COATINGS
Thomason J L; Dwight D W
X-ray photoelectron spectroscopy was applied to a study
of commercial and experimental glass fibres using three
different instruments. A protocol for plotting ratios of
appropriate atom concentrations was developed and the
plots used to estimate the surface coverage of the coating
on the glass fibres and provide data on the chemical
composition of the coating. The relationships between
the spectroscopic data and coated glass fibre parameters
are demonstrated using an overlay model and data from
the three instruments are compared. 22 refs.
USA
Accession no.755993
Item 198
71, No.20, 15th Oct.1999, p.4776-80
COMPOSITION AND MICROSTRUCTURE
DETERMINATION OF A LATEX SYSTEM BY
PYROLYSIS GAS CHROMATOGRAPHY
Frank Cheng-Yu Wang
Dow Chemical Co.
The composition and microstructure of polymers in a
l at ex syst em were st udi ed by pyrol ysi s gas
chromatography. The composition and microstructure
of a polymer in the emulsion phase were identified by
direct pyrolysis of the latex system, followed by
comparing the trimer peak pattern with appropriate
microstructure standards. The polymer in the aqueous
phase was pre-pyrol ysi s deri vat i sed wi t h
tetrabutylammonium hydroxide to convert the acid to
its butyl ester. Similar procedures were then used to
explore the composition and microstructure of the
polymer in the aqueous phase. Polymers analysed
included SCX-2660 (probably a styrene-methyl
methacrylate-butyl acrylate terpolymer), styrene-butyl
acrylate copolymer and styrene-alpha-methylstyrene-
butyl acrylate terpolymer. 17 refs.
JOHNSON S.C.,& SON INC.
USA
Accession no.755899
Item 199
Oxford, Butterworth-Heinemann Ltd., 1999,
pp.xxvii,920. 24cms. 12/1/00. 011
PLASTICS MATERIALS. 7TH EDN.
Brydson J A
The latest edition, now the seventh, of this reputable text
book, provides an overview of the scientific, technological
and economic aspects of currently available plastics and
related materials, and also focuses on new materials -
many based on metallocene catalyst technology.
Developments with condensation polymers, including
several new polyester-type materials of interest for bottle
blowing and/or degradable plastics, are also covered. This
edition also attempts to explain the basis of metallocene
polymerisation. The commercial importance of the
materials discussed is also noted.
Accession no.755818
Item 200
74, No.10, 5th Dec.1999, p.2432-8
CHARACTERIZATION OF BISPHENOL A-
BASED EPOXY RESINS BY HPLC, GPC, GPC-
MALLS, VPO, VISCOMETRY, AND END GROUP
ANALYSIS: ON THE IDENTIFICATION OF 2,3-
DIHYDROXYPROPYL-CONTAINING
COMPOUNDS, DETERMINATION OF MOLAR
MASS DISTRIBUTION, AND BRANCHING
Podzimek S; Kastanek A
SYNPO
Results of the above characterisation are presented and
discussed with particular reference to determination of
alpha-glycol-containing compounds, determination of
molar mass and molar mass distribution, determination
of branching and determination of refractive index
increment. 19 refs.
CZECH REPUBLIC
Accession no.755647
Item 201
Journal of Vinyl and Additive Technology
5, No.3, Sept.1999, p.148-58
NMR SPECTRA OF LEAD STABILISERS
Grossman R F
Halstab Corp.
High resolution proton and 13C NMR spectra of lead-
based heat stabilisers and their reaction products, obtained
using the magic angle spinning technique, support
structural assignments inferred from IR spectra. These
demonstrate that lead stabilisers are unique compounds,
rather than the double salts of lead oxide found in
textbooks. 8 refs.
USA
Accession no.755491
Item 202
Polymers for Advanced Technologies
10, No.4, April 1999, p.237-43
CHARACTERISATION OF THE SURFACE OF
BULK-MOULDED COMPOUNDS
Vallat M F; Schultz J; Mauzac C; Jacquin M
Institut de Chimie des Surfaces et Interfaces; PSA
Etudes et Recherches Centre Technique de Belchamp
The surface characterisation of bulk moulding compound
(BMC) automotive parts using complementary techniques
of surface analysis, i.e. SEM, X-ray photoelectron
spectroscopy, time of flight secondary ion mass
spectroscopy, glow discharge spectroscopy and contact
angle is described. Similarities and differences between
BMC surfaces and sheet moulding compound (SMC)
surfaces are pointed out. Particular emphasis is placed on
mould release agents (polymeric and stearate) on the surface
which can influence future bonding behaviour. 14 refs.
WESTERN EUROPE
Accession no.754736
Item 203
200, No.9, 1999, p.2074-9
INVESTIGATION OF MOLECULAR
DIMENSIONS OF POLYSTYRENE AS A
FUNCTION OF SOLVENT COMPOSITION:
APPLICATION TO LIQUID
CHROMATOGRAPHY AT THE EXCLUSION-
ADSORPTION TRANSITION POINT
Baran K; Laugier S; Cramail H
ENSCPB
Liquid chromatography was used to study PS standards at
the exclusion-adsorption transition point using silica
adsorbents having differing porosities in various eluents. The
behaviour of model PS chains in solvent mixtures
corresponding to the critical adsorption conditions was
evaluated using viscometry and light scattering. It was found
that critical adsorption conditions could be achieved if the
polymer chains entered the pores of the stationary phase and
that the characteristics of the elution mode could be defined
with the aid of the polarity index of the eluent. 20 refs.
WESTERN EUROPE
Accession no.752269
Item 204
Vol.141, 1999, p.95-101
RECENT ADVANCES IN THE ANALYSIS OF
POLYMERS AND COPOLYMERS BY MASS
SPECTROMETRY
Montaudo M S
Istituto per la Chimica e la Tecnol.dei Mat.Pol.
Progress which has been made in the use of MALDI mass
spectroscopy to provide reliable molec.wt. and MWD
values is reported. Molec.wt. averages and MWD of
polydisperse samples (PMMA, siloxanes, polyesters and
copolyesters) were obtained by off-line coupling of SEC
equipment with the MALDI mass spectrometer. SEC
traces of the samples were recorded, selected fractions
were analysed by MALDI-TOF and the average
molec.wts. of the fractions were determined from the mass
spectrum. A method for analysing unknown copolymers,
which involves the use of Markoffian statistics, is also
presented. 26 refs.
WESTERN EUROPE
Accession no.752091
Item 205
Polimery
44, No.4, 1999, p.246-54
Polish
USE OF PHOTOELECTRON SPECTROSCOPY
IN STUDIES OF THE DEPTH PROFILE OF
POLYPROPYLENE FILM
Zenkiewicz M; Golebiewski J
Metalchem Plastics Processing Institute
The physical fundamentals of photoelectron spectroscopy
are reviewed and the range of applications is given. Three
PP films were examined and the depth of oxidation was
found to be in the nanometer range. The oxidation level
of the external layer increases as the specific energy of
corona discharges is increased. 27 refs. Articles from this
journal can be requested for translation by subscribers to
the Rapra produced International Polymer Science and
Technology.
Accession no.747688
Item 206
LCGC International
12, No.9, Sept.1999, p.577/87
LC-MS ANALYSIS OF POLYMER ADDITIVES
BY EL AND API: IDENTIFICATION AND
QUANTIFICATION
Yu K; Block E; Balogh M
Waters Corp.
Mass spectrometry can be the ideal detector for liquid
chromatography because it offers both universality and the
required selectivity for complex analytical problems. The
two most popular types of interface for the benchtop single
quadrupole LC-mass spectrometer are the particle beam
interface and the atmospheric pressure ionisation interface.
The particle beam interface is used to generate electron
ionisation spectra and the API interface is used to generate
either electrospray or atmospheric pressure chemical
ionisation. This comprehensive article supplies a detailed
analysis of a study in which organic extractable from
polypropylene was used as the model analyte to
demonstrate how the information obtained separately from
EI and API can be complementary. Seven compounds were
separated and detected by both MS detectors. 35 refs.
USA
Accession no.747567
Item 207
Macplas International
No.10, Aug.1999, p.64-70
DIFFERENTIAL SCANNING COLORIMETRY
AND INFRARED SPECTROSCOPY IN
POLYMER ANALYSIS
Panarotto A; Bertucci M
Cesap
Differential scanning calorimetry is one of the most
commonly used methods for characterising the thermal
properties of polymers. This method, particularly if
complemented by IR spectroscopic analysis, also allows
the nature of the materials under test to be determined.
The principles involved in DSC and IR spectroscopy are
discussed.
WESTERN EUROPE
Accession no.745360
Item 208
Polimery Tworzywa Wielkoczasteczkowe
44, No.3, 1999, p.218-21
Polish
DETERMINATION OF MIGRATION OF
DIMETHYL TEREPHTHALATE AND
DIMETHYL ISOPHTHALATE FROM PLASTICS
Stareczek T; Kaminska G; Ermel J; Kortylewska
Edited by: Gliwice,Institute of Plastics & Paint Industry
A gas chromatographic method is described for
determining dimethyl terephthalate and dimethyl
isophthalate in food simulants. The method consists in
extracting DMT and DMIP from the food simulants with
chloroform and analysing of the compounds by GC with
the use of calibration curves and diethyl terephthalate as
an internal standard. 3 refs. Articles from this journal can
be requested for translation by subscribers to the Rapra
produced International Polymer Science and Technology.
Accession no.745025
Item 209
73, No.2, 11th July 1999, p.221-6
EVALUATION OF EVA-PVAC BLEND
BEHAVIOUR BY 1-D AND 2-D SOLID-STATE
NMR
De Souza C M G; Pacheco C R; Tavares M I B
Rio de Janeiro,Universidade Federal; PETROBRAS
Ethylene-co-vinyl acetate and poly(vinyl acetate) blends
were prepared in different proportions by melting in a
HAAKE Rheomix mixer. The blends were prepared at a
fixed temperature, rotation rate, and processing time.
High-resolution solid state NMR was used to characterise
the blends with respect to structure-mobility-compatibility
using magic angle spinning with cross-polarisation and
high power hydrogen decoupling and measurements of
the proton spin-lattice relaxation time in the rotating
frame. Miscibility between polymer chains was also
studied by two-dimensional hydrogen ion/carbon-13 shift
correlation (HETCOR). 21 refs.
BRAZIL
Accession no.743489
Item 210
Macromolecules
32, No.11, 1st June 1999, p.3671-3
LIQUID ADSORPTION CHROMATOGRAPHY
OF COPOLYMERS: MOLAR MASS
(IN)DEPENDENT RETENTION
Berek D
Slovak Academy of Sciences
Liquid adsorption chromatography with a continuous
solvent gradient elution was shown by several previous
authors to be capable of separating random and graft
copolymers according to their chemical composition, with
their molar masses not playing an important role. A
tentative explanation of this finding is presented. It is
assumed that the copolymer species travel along the
column with a velocity which exactly corresponds to that
of the eluent composition, exhibiting a displacing power
just necessary to prevent a fast progress of the
macromolecules due to their exclusion. Under specific
conditions, retention of macromolecules at this adsorption
promoting barrier depends almost exclusively on the
copolymer composition and not on its molar mass. This
hypothesis is based on the mechanism of the recently-
proposed and tested liquid chromatographic elution of
homopolymers under limiting conditions of desorption
and takes into account the simultaneous effect of
adsorption and exclusion of macromolecules onto/from
the column packing. 17 refs.
Accession no.743327
Item 211
Polymer Recycling
3, No.4, 1997/1998, p.263-7
PROCEDURES FOR THE COMPOSITIONAL
ANALYSIS OF REINFORCED POLYESTER
RECYCLATE
Bream C E; Hornsby P R
Brunel University
In order to consider effective strategies for the recovery
and reuse of plastics recyclates, a quantitative method is
described for the characterisation of polyester-based
moulding compounds. Analytical procedures are
described for the quantification of fibre, filler and fire
retardant contents in polyester moulding compounds
containing calcium carbonate filler, glass fibre
reinforcement, and aluminium hydroxide flame retardant.
3 refs.
WESTERN EUROPE
Accession no.742796
Item 212
High Performance Plastics
Aug.1999, p.10
IDENTIFICATION OF PLASTICS IN WASTE
A review is presented of the methods used in the
identification of plastics waste prior to recycling
operations, which was published in International Polymer
Science and Technology, and translated from a Polish
source. Rapid spectroscopic methods are indicated, and
their use in packaging and automotive recycling are
discussed.
Accession no.742675
Item 213
37, No.13, 1st July 1999, p.1485-94
GLASS TRANSITION AND MISCIBILITY IN
BLENDS OF TWO SEMI-CRYSTALLINE
POLYMERS: POLYARYL ETHER KETONE AND
POLYETHER ETHER KETONE
Woo E M; Tseng Y C
Taiwan,National Cheng Kung University
A study was made of the miscibility in the amorphous
region of melt mixed blends composed of a novel polyaryl
ether ketone (PK99) and PEEK using various methods,
including optical microscopy, DSC, SEM, FTIR
spectroscopy and wide-angle X-ray diffraction. Samples
were physically aged in order to resolve any possible
overlapping Tgs but only one single Tg was detected over
the entire composition range. No evidence for
isomorphism was found and the crystal forms of the
respective polymers remained distinct and unchanged by
miscibility in the amorphous region. 14 refs.
TAIWAN
Accession no.742306
Item 214
53, No.6, June 1999, p.672-81
POST-CONSUMER PLASTIC IDENTIFICATION
USING RAMAN SPECTROSCOPY
Allen V; Kalivas J H; Rodriguez R G
Idaho,State University
The suitability of Raman spectroscopy, when used with
K-nearest neighbours, library searching or cyclic subspace
regression, for computerised classification of post-
consumer plastics was evaluated. Plastics investigated
were PETP, PP, PS, PVC, HDPE AND LDPE.
Modifications were made to the original cyclic subspace
regression algorithm for modelling multiple sample
properties and the adapted algorithm employed to directly
compare the mechanisms of principal component
regression and the PLS2 form of partial least-squares. It
was found that Raman spectroscopy could be used to
identify both HDPE and LDPE. 33 refs.
USA
Accession no.741260
Item 215
53, No.5, May 1999, p.557-64
COMPARISON OF NEAR-INFRARED AND
RAMAN SPECTROSCOPY FOR THE
DETERMINATION OF CHEMICAL AND
PHYSICAL PROPERTIES OF NAPHTHA
Min-Sik Ku; Hoeil Chung
SK Corp.
Near-infrared and FTIR Raman spectroscopy were
compared and evaluated for the quantitative analysis of
naphtha using partial least-squares regression. 19 refs.
SOUTH KOREA
Accession no.740339
Item 216
53, No.5, May 1999, p.551-6
FOURIER TRANSFORM RAMAN SPECTRA OF
LINEAR LOW-DENSITY POLYETHYLENE AND
PREDICTION OF THEIR DENSITY BY
MULTIVARIATE DATA ANALYSIS
Sano K; Shimoyama M; Ohgane M; Higashiyama H;
Watari M; Tomo M; Ninomiya T; Ozaki Y
Kwansei-Gakuin,University; Hyogo,Prefectural Police
Headquarters; Yokogawa Electric Co.
FTIR spectra were measured for pellets of sixteen kinds
of LLDPE with short branches and one kind of PE without
any branch to explore the effects of the branches on the
physical properties and the Raman spectrum. Partial least
squares analysis regression was applied to the Raman
spectra after multiplicative scatter correction to propose
a calibration model that predicts the density of LLDPE.
38 refs.
JAPAN
Accession no.740338
Item 217
71, No.893, June 1999, p.53-60
INVERSE GAS CHROMATOGRAPHY, SURFACE
PROPERTIES, AND INTERACTIONS AMONG
COMPONENTS OF PAINT FORMULATIONS
Ziani A; Xu R; Schreiber H P; Kobayashi T
Ecole Polytechnique de Montreal; Nippon Paint Co.
Inverse gas chromatography analysis at very high dilution
and at finite concentrations of probe injection was carried
out on a series of polymers and pigments used in paint
formulations. Values of dispersion surface energies, and
of acid-base interaction parameters were obtained for the
materials, and pair interaction parameters were calculated
from the results. The dispersion stability of each pigment/
polymer combination was measured and correlated with
the acid-base interaction parameters of the materials, and
is shown to justify the availability of fundamental
thermodynamic interaction data to optimise performance
aspects of protective coatings. 23 refs.
CANADA; JAPAN
Accession no.739845
Item 218
71, No.10. 15th May 1999, p.2037-45
ANALYSIS OF POLYMERIC FLAME
RETARDANTS IN ENGINEERING
THERMOPLASTICS BY PYROLYSIS GAS
CHROMATOGRAPHY WITH AN ATOMIC
EMISSION DETECTOR
Wang F C Y
Dow Chemical Co.
Halogen-containing polymeric flame retardants in
engineering thermoplastics were analysed by pyrolysis
gas chromatography(Py-GC) with an atomic emission
detector(AED) and a mass selective detector(MSD). The
AED was very effective in monitoring halogen-containing
pyrolysates after Py-GC. The type of polymeric flame
retardant used in thermoplastics could be identified by
peak pattern recognition through an AED halogen element
trace. A set of thermoplastic resins containing different
brominated polymeric flame retardants was studied. After
generation of the pyrogram by Py-GC/AED, those
pyrolysates produced from polymeric flame retardants
were identified by MSD analysis of a complex total ion
chromatogram generated by the thermoplastic resins. The
results demonstrated the effectiveness of the AED in the
tasks of specific element monitoring and component
pattern recognition. The advantages and disadvantages
of using the AED are also discussed. 11 refs.
USA
Accession no.738049
Item 219
ACS, Polymeric Materials Science and Engineering.
Vol.76. Conference proceedings.
San Francisco, Ca., Spring 1997, p.128-9. 012
ATOMIC FORCE MICROSCOPY STUDY OF
INTRAOCULAR LENS IMPLANTS -
TOPOGRAPHY AND SURFACE PROPERTIES
Kowalewski T; Ravi V N
Washington,University; St.Louis,Veterans Affairs
Medical Center
Cataracts are one of the most common causes of
worldwide blindness. They are presently corrected by
surgery in which the natural cataractous lens is replaced
by a synthetic intraocular lens. Successful visual
rehabilitation is not only a function of patients health
and the surgical technique, but it also depends on the
optical, mechanical and bioperformance of the intraocular
lens. Visual deterioration after surgery has been attributed
to cellular debris deposited on the lens surface and
capsular opacification resulting from inflammation.
Although the exact sequence of events that take place
when an implant is exposed to the ocular environment in
vivo is not known, protein adsorption, complement
activation and cellular adhesion have been implicated and
believed to be influenced by the surface properties of the
implants. The surface characteristics (surface topography
and viscoelasticity) of intraocular lenses are investigated
using tapping-mode atomic force microscopy. 9 refs.
USA
Accession no.737604
Item 220
Polymer
40, No.17, 1999, p.4763-7
CALORIMETRY: 14. EFFECT OF MOLECULAR
INTERACTIONS ON GLASS TRANSITION
BEHAVIOUR AND INCREMENT OF HEAT
CAPACITY IN MISCIBLE POLYMER BLENDS
Song M; Hourston D J; Pollock H M; Hammiche A
Loughborough,University; Lancaster,University
Modulated differential scanning calorimetry was used
to study miscible polymer blends. The blends studied
were poly(vinyl acetate)/poly(methyl acrylate),
poly(phenylene oxide)/PS and two poly(styrene-co-
acrylonitrile)/PMMA blends, the last two containing
different acrylonitrile contents. Specific molecular
interactions determined whether the glass transition
temperature and the increment of heat capacity versus
composition showed positive or negative deviations
from linearity for the blend systems. In the non-
interacting system (poly(vinyl acetate)/poly(methyl
acrylate)), the glass transition temperature and increment
of heat capacity showed linear behaviour with
composition. Thermodynamic theories for the observed
results were discussed. 17 refs.
WESTERN EUROPE
Accession no.737361
Item 221
LCGC International
12, No.7, July 1999, p.432/6
QUANTITATIVE ANALYSIS OF
POLY(METHYLMETHACRYLATE) IN DRUGS
BY CURIE-POINT PYROLYSIS GAS
CHROMATOGRAPHY
Muguruma S; Uchino S; Oguri N; Kiji J
Japan Analytical Industry Co.Ltd.; Tottori,University
Curie-point pyrolysis gas chromatography was used for
the quantitative analysis of residual synthetic adsorbent
crosslinked PMMA used in drug purification. Levels of
PMMA adsorbent below 0.15% in drug substances were
successfully measured quantitatively by Py-GC using
characteristic peaks that reflect the structure of the
adsorbent, demonstrating that this analytical technique
can be used to monitor compliance with the limit of 0.1%
organic impurity in drug substances stipulated by ICH
guidelines. 12 refs.
JAPAN
Accession no.736647
Item 222
72, No.7, 16th May 1999, p.913-25
HIGH-PERFORMANCE LIQUID
CHROMATOGRAPHY-MASS SPECTROMETRY
OF EPOXY RESINS
Fuchslueger U; Rissler K; Stephan H; Grether H J;
Grasserbauer M
Ciba Specialty Chemicals Inc.; Vienna,Technical
University
The application of liquid chromatography coupled to
mass spectrometry for the analysis of epoxy resins was
shown in two examples. Electrospray (ESI) and
atmospheric pressure chemical ionisation (APCI) were
compared with respect to the ionisation of diglycidyl
ether of bisphenol A (DGEBA)-based epoxy resins. By-
products in a typical modified solid DGEBA-based
epoxy resin and in a new weatherable crosslinker for
powder coating applications were characterised and
discussed. 26 refs.
AUSTRIA; SWITZERLAND; WESTERN EUROPE
Accession no.734831
Item 223
13, No.5, 1999, p.629-45
ADHESION CHARACTERISATION OF
PROTECTIVE ORGANIC COATINGS BY
ELECTROCHEMICAL IMPEDANCE
SPECTROSCOPY
Deflorian F; Fedrizzi L
Trento,University
This review describes in detail the influences on adhesion
of different pretreatments or organic coatings, considering
aluminium, galvanised steel, and stainless steel substrates,
and it was shown that the information obtained using an
electrochemical approach can be used for adhesion
evaluation, with particular attention to monitoring of
adhesion in an aqueous environment, which is the most
detrimental for protective organic coatings. 40 refs.
WESTERN EUROPE
Accession no.733531
Item 224
200, No.5, May 1999, p.1134-42
POSSIBILITIES AND LIMITS OF PHOTON
CORRELATION SPECTROSCOPY IN
DETERMINING POLYMER MOLECULAR
WEIGHT DISTRIBUTIONS
Faraone A; Magazu S; Maisano G; Villari V; Maschio G
Messina,University
The effect of concentration and polydispersity on the
collective diffusion coefficient(Dc) evaluated using
photon correlation spectroscopy was investigated on
PMMA in acetone solutions. The concentration
dependence of the Dc followed a linear regression law,
the slope being fairly independent of polydispersity,
molec.wt. and temp. The diffusion coefficient at infinite
dilution obeyed a given scaling law. The inversion of the
scattered intensity autocorrelation data by the
regularisation method CONTIN permitted the evaluation
of the MWD function of the polymeric samples. Although
this algorithm gave valuable information on average
amounts or on the widths of the distribution, it had limited
resolution power. A comparison with the results obtained
by size exclusion chromatography was therefore carried
out for a set of samples having monomodal and bimodal
distribution functions. 22 refs.
WESTERN EUROPE
Accession no.733222
Item 225
Coloring Technology for Plastics.
New York, N.Y., Plastics Design Library, 1999, p.197-
207. 52
MEASURING STABILISERS IN PIGMENTED
PLASTICS WITH NEAR-INFRARED
SPECTROSCOPY
Solera P; Nirsberger M; Castillo N
Ciba Specialty Chemicals Corp.
Edited by: Harris R M
Near-infrared (NIR) spectroscopy has become a
commonplace analytical tool in the plastics industry. NIR
techniques have made quantification of many organic
components in polymer processing easy and quick. The
work presented outlines the methodology for using NIR
to measure stabiliser levels in colour concentrates and
natural polymer formulations. Advantages and limitations
are considered as well as particle size and product form.
4 refs.
USA
Accession no.732217
Item 226
Coloring Technology for Plastics.
New York, N.Y., Plastics Design Library, 1999, p.191-
5. 52
PRACTICAL ANALYSIS TECHNIQUES OF
POLYMER FILLERS BY FOURIER
(FTIR)
Coles B J; Hall C J
Hauser Inc.
Edited by: Harris R M
The identification of polymers by FTIR is often
complicated by the presence of fillers. However, for kaolin
clay, FTIR analysis should be able to identify the filler
and predict its concentration using a standard curve. The
resulting percentage is more reliable than a simple ash,
which may change the chemical composition of the filler.
2 refs.
USA
Accession no.732216
Item 227
Pitture e Vernici
75, No.5, March 1999, p.7-8
English; Italian
E.I.S. EVALUATION OF ATTACHED AND FREE
POLYMER FILMS
Castela A S; Simoes A M P
Evaluation of the volume fraction of water in organic
coatings in immersion is often made by electrochemical
impedance spectroscopy, EIS, and based upon the
evolution of the coating capacitance. Among the several
models and equations proposed for this determination,
the most frequently used is the Brasher equation. Most
frequently these determinations are made with applied
coatings, although studies can be found in the literature
using free films. The behaviour of a commercial coating
- PVC plastisol - is studied, both applied on a metallic
substrate and as a free film.
WESTERN EUROPE
Accession no.731759
Item 228
55, No.2, 1999, p.559-63
TG/FT-IR STUDIED OF POLY(VINYL
CHLORIDE) BLENDS
Pielichowski K
Krakow,Technical University
Thermogravimetry coupled with FTIR was used to
investigate the stabilising action of 3-(2,4-
dibromophenylazo)-9-(2,3-epoxypropane)carbazole on
the degradation of PVC. This secondary stabiliser
increased the initial temperature of hydrogen chloride
evolution (the main process responsible for PVC
decomposition), thereby allowing its application for novel
PVC systems with enhanced thermal stability. 10 refs.
Accession no.731454
Item 229
71, No.9, 1st May 1999, p.1809-14
POLYMER ANALYSIS BY LIQUID
CHROMATOGRAPHY/ELECTROSPRAY
IONISATION TIME-OF-FLIGHT MASS
SPECTROMETRY
Nielen M W F; Buijtenhuijs F A
Akzo Nobel Central Research
Different liquid chromatography modes in polymer
analysis were successfully interfaced with electrospray
ionisation time-of-flight mass spectrometry in a single
experimental set-up: the mass spectrometry data from size
exclusion chromatography/mass spectrometry of PMMA
were used as absolute calibration points in the size
exclusion chromatography/refractive index
chromatogram, and monomer mass and end groups were
inferred from the isotopically resolved mass spectra. 44
refs.
Accession no.731446
Item 230
Polymer Preprints. Volume 40. Number 1. March 1999.
Conference proceedings.
Boston, Ma., March 1999, p.226-7. 012
SURFACE MODIFICATION OF POLYSTYRENE
STUDIED BY IR-VISIBLE SUM FREQUENCY
GENERATION SPECTROSCOPY
Zhang D; Dougal S; Yeganeh M S
Exxon Research & Engineering Co.
The effects of UV light and oxygen plasma on PS surfaces
is investigated using SFG spectroscopy. The observed
spectral changes provide strong support for the
photooxidation of the aromatic ring at the PS surface, as
observed by the dramatic decrease in the aromatic C-H
vibration during photo irradiation and plasma treatment.
It is also found that the kinetics of the photooxidation of
the PS surface, monitored by SFG, is much faster than
similar process observed by other techniques, such as
FTIR or SIMS. 13 refs.
USA
Accession no.730043
Item 231
Polymer Composites
20, No.2, April 1999, p.314-20
CHARACTERISATION OF MIXED FIBRE
NYLON COMPOSITES INCORPORATING
COMPOSITE SCRAP
Licea-Claverie A; Carrillo F J U; Alvarez-Castillo A;
Castano V M
Tijuana,Instituto Tecnologico; Zacatepec,Instituto
Tecnologico; UNAM
Recycling of engineering thermoplastics and their
composites is discussed. A study on nylon-6,6 based
composites with mixed glass fibre and carbon fibre
reinforcement, including nylon composite scrap in their
formulation, were reported. Several formulations were
prepared by injection moulding and were characterised
by stress-strain measurements, impact testing,
simultaneous DTA and TGA, density measurements and
SEM. Mechanical and thermal properties of the resulting
composites are presented, discussed, and compared with
a virgin standard composite. 26 refs.
MEXICO
Accession no.729302
Item 232
71, No.7, 1st April 1999, p.1316-22
CHARACTERIZATION OF NATURAL RESIN
SHELLAC BY REACTIVE PYROLYSIS-GAS
CHROMATOGRAPHY IN THE PRESENCE OF
ORGANIC ALKALI
Wang L; Ishida Y; Ohtami H; Tsuge S; Nakayama T
Nagoya,University; Gifu Shellac Manufacturing
Co.Ltd.
A method for determining the chemical composition of
natural resin shellac was developed based on reactive
pyrolysis-gas chromatography(Py-GC) in the presence of
an organic alkali, tetramethylammonium
hydroxide(TMAH). Py-GC using 25% TMAH aqueous
solution permitted the highly sensitive determination of
terpenic acids, aleuritic acid, several minor fatty acids and
the wax components of shellac as their methyl derivatives
on the resulting pyrograms with less than 2.0 % relative
standard deviations without using any cumbersome
pretreatment. The observed average distributions of each
resin acid component determined by reactive Py-GC for
shellac samples from India and Thailand showed that the
average ratios among terpenic acids, aleuritic acid and the
other fatty acids were about 53:24:14 for Indian shellac
and 51:35:14 for Thailand shellac, respectively, suggesting
a slightly significant difference. Clearer discrimination of
the shellac samples from the two different countries was,
however, achievable by applying principal component
analysis for the mole percent distributions of all the acidic
components determined by reactive Py-GC. 24 refs.
INDIA; JAPAN; THAILAND
Accession no.727139
Item 233
ACS Polymeric Materials Science and Engineering.
Fall Meeting 1997. Volume 77. Conference
proceedings.
Washington, D.C., 1997, p.594-5 .012
EFFECT OF SECOND DIMENSION SAMPLING
RATE AND PARTICLE SIZE ON RESOLUTION
AND RUN TIME IN TWO DIMENSIONAL
LIQUID CHROMATOGRAPHY FOR THE
ANALYSIS OF POLYMERS
Murphy R E; Schure M R; Foley J P
Rohm & Haas Co.; Villanova,University
The optimisation of a two dimensional high performance
liquid chromatography (HPLC) (reverse phase liquid
chromatography/gel permeation chromatography (GPC))
system for the analysis of low molecular weight polymers
is described. A test mixture of polyethylene glycols and a
commercial surfactant was used. The analysis time of the
second dimension, GPC, was varied by using different
columns. The columns had different particle sizes and
lengths, and the two dimensional resolution was compared
by varying the run time in the second dimension.
Following the optimisation, it was possible to complete a
two dimensional analysis in the time normally taken for
a normal gradient HPLC run. It was established that
conventional columns could be run with higher flow rates
without a significant loss of resolution. The combination
of shorter and smaller particle GPC columns resulted in
lower sampling periods at lower flow rates than
conventional columns. The highest sampling rate into the
second dimension gave the best resolution. 7 refs.
USA
Accession no.726180
Item 234
Shawbury, Rapra Technology Ltd., 1997, pp.315.
220.00. 30cms. 9922
RAPRA COLLECTION OF INFRARED SPECTRA
OF RUBBERS, PLASTICS AND
THERMOPLASTIC ELASTOMERS. SECOND
EDITION
Sidwell J A
This book provides a set of transmission and pyrolysate
spectra of a comprehensive range of technically important
rubber and plastics materials including copolymers and
blends which are in current use. Materials are indexed
under both polymer and trade name.
Accession no.725345
Item 235
Polymer
40, No.12, 1999, p.3479-85
INVERSE GAS CHROMATOGRAPHIC
CHARACTERIZATION OF POLY(ETHYLENE
OXIDE)
Al-Saigh Z Y
Columbus,State University
The inverse gas chromatography method was used to
obtain the thermodynamic properties and the surface
energy of a semicrystalline polymer, PEO. PEO was used
as a stationary phase in the chromatographic column and
16 solutes with a different chemical nature were used as
eluents. Alkanes showed endothermic interaction
parameters and the molar heat of mixing in a temp. range
of 70-130C. Acetates and alcohols showed better
interactions with the PEO layer and butanol was found to
be the best solvent for PEO among all solutes used. The
variation in molec.wt. of PEO above 400 g/mol showed
no apparent effect on the interaction coefficients. The
dispersive contribution of the surface energy of PEO was
measured as a function of temp., which ranged from 8.00
and 13.00 mJ/sq m, indicating a poor surface energy of
PEO. 43 refs.
USA
Accession no.721885
Item 236
Journal of Adhesion
68, Nos.1-2, 1998, p.117-42
QUANTIFICATION OF COATING ADHESION
USING LASER INDUCED DECOHESION
SPECTROSCOPY
Meth J S; Sanderson D; Mutchler C; Bennison S J
DuPont Co.
A new technique, laser induced decohesion spectroscopy,
is presented, which is capable of measuring the practical
work of adhesion between a transparent polymer coating
or substrate. A laser pulse directed onto the sample creates
a blister at the transparent/opaque interface. The blisters
internal pressure depends on the laser pulse energy, and
at a critical pressure the sample fractures, creating an
annular debond similar to that obtained in the standard
blister test. By measuring physical variables such as the
curvature of the blister, and its radius and thickness, it is
possible to deduce the practical work of adhesion. 19 refs.
USA
Accession no.721348
Item 237
13, No.3, 1999, p.379-91
DETERMINATION OF THE ADHESION
PROPERTIES OF AN ALKYD PIGMENTED
COATING BY ELECTROCHEMICAL
IMPEDANCE SPECTROSCOPY
Gonzalez J E G; Rosca J C M
Gran Canaria,University
Impedance measurements were performed in different
frequency ranges at open circuit potential for an alkyd
coating with titanium dioxide as a mineral pigment in
3% sodium chloride. The most probable impedance
equivalent circuit method was considered for data
analysis. The interpretation of the impedance spectra
permitted the determination of water permeation, the
formation of blisters, swelling of the coating, and the loss
of adhesion. 17 refs.
WESTERN EUROPE
Accession no.721335
Item 238
ACS Polymeric Materials Science and Engineering.Fall
Meeting 1997.Volume 77.Conference proceedings.
Washington, D.C., 1997, p.48-9 012
QUANTITATION IN THE ANALYSIS OF
OLIGOMERS BY HPLC WITH ELSD
Trathnigg B; Kollroser M; Maier B; Berek D; Janco M
Graz,Karl-Franzens-Universitat; Slovak Academy of
Sciences
The influence of the operating parameters used when
operating evaporative light scattering detectors in
conjunction with high performance liquid
chromatography for the characterisation of oligomers was
investigated, using polyether samples. It was concluded
that the instrument was useful because it provided gradient
elution, however, very careful calibration was required
to obtain reliable quantitative data. 16 refs.
AUSTRIA; WESTERN EUROPE
Accession no.720839
Item 239
Washington, D.C., 1997, p.46-7 012
APPLICATION OF SEC AND HPLC TO THE
CHARACTERIZATION OF POLYMERS,
OLIGOMERS, AND SMALL MOLECULES USED
IN COATINGS AND INKS
Kuo C; Grieser M D; Robinson D
Henkel Corp.
Applications are given of the use of size exclusion
chromatography and high performance liquid
chromatography for the characterisation of coatings
systems which either use water as the major solvent or
utilise low molecular weight polymers, oligomers, and
reactive additives which are then reacted to produce high
molecular weight and crosslinked films. 6 refs.
USA
Accession no.720838
Item 240
Washington, D.C., 1997, p.35-6 012
LIQUID CHROMATOGRAPHY OF
MACROMOLECULES UNDER LIMITING
CONDITIONS OF SOLUBILITY: FIRST
EXPERIMENTAL OBSERVATIONS
Bartkowiak A; Hunkeler D; Murgasova R; Berek D
Szczecin,Technical University; Swiss Federal Institute
of Technology; Slovak Academy of Sciences
Liquid chromatography at the critical adsorption point
(LC LCS) was investigated. The solubility of
macromolecules, the sensitivity of LC LCS to such
variables as the injection volume, concentration injected,
mobile phase flow rate and mixing between the injection
zone, were investigated, using polymethyl methacrylate
(PMMA) and polyacrylamide standards. It is proposed
that using tetrahydrofuran and n-hexane as eluents for
PMMA, at the LC LCS, limited polymer insolubility or
even local precipitation is combined with the size
exclusion of macromolecules. 12 refs.
EASTERN EUROPE; POLAND; SLOVAK REPUBLIC;
SLOVAKIA; SWITZERLAND; WESTERN EUROPE
Accession no.720833
Item 241
Washington, D.C., 1997, p.31-2 012
MACROMOLECULES AT THE CRITICAL
ADSORPTION POINT: PROBLEMS AND
PITFALLS
Berek D; Janco M
The role of column packing pore size in liquid
chromatography at the critical adsorption point was
investigating using three silica gels and a series of
polymethyl methacrylates (PMMA), using toluene,
tetrahydrofuran (THF) or their mixtures as eluents.
Toluene strongly promotes adsorption of PMMAs on the
silica surface, whereas THF suppresses adsorption. It was
established that the pore size of the column packings
played an important role in liquid chromatography at the
critical adsorption point. The column with the smallest
pores largely determined the behaviour of the whole set.
The feasibility of using silica gel as column packings for
liquid chromatography at the critical adsorption point is
questioned. 14 refs.
Accession no.720831
Item 242
Washington, D.C., 1997, p.22-3 012
2D-LC OF FUNCTIONAL POLYETHERS
Trathnigg B; Kollroser M; Parth M
Graz,Karl-Franzens-Universitat
A combination of liquid chromatography under critical
conditions using coupled density and RI detection in one
dimension, and gradient high performance liquid
chromatography in the second dimension, was used in
the two-dimensional chromatographic analysis of the
oligomers present in fatty alcohol ethoxylates. Full
resolution was achieved. 6 refs.
Accession no.720827
Item 243
Washington, D.C., 1997, p.20-1 012
MOLECULAR CHARACTERIZATION OF
COMPLEX POLYMERS BY COUPLED LIQUID
CHROMATOGRAPHIC PROCEDURES
Berek D
Size exclusion chromatography alone cannot characterise
the constituents of complex polymer systems. Separation
selectivity and characterisation of complex systems may
be enhanced with liquid chromatographic (LC) methods
utilising combinations of different separation
mechanisms. These are termed coupled LC procedures.
The applications of a variety of coupled LC procedures
are discussed. 16 refs.
Accession no.720826
Item 244
ACS Polymeric Materials Science & Engineering,
Spring Meeting 1998. Volume 78. Conference
proceedings.
Dallas, Tx., Spring 1998, p.102-3. 012
COUPLED PROGRAMMED PYROPROBE-MASS
SPECTROMETRY AND
THERMOGRAVIMETRIC-MASS
SPECTROMETRY
Carraher C E; Molloy H M; Louda J W; Baker E
Florida,Atlantic University; Florida,Center for
Environmental Studies; Midwest Research Institute
In 1977, a thermogravimetric analysis unit was
successfully coupled with a mass spectrophotometer, TG-
MS. More recently, a coupled programmed pyroprobe-
mass spectrophotometry system, also utilising IR
spectroscopy, was employed as a means of describing
degradation sequences as a function of temperature. The
application of these tools as a means to define polymer
structure and degradation products is described. 9 refs.
USA
Accession no.719193
Item 245
ACS Polymeric Materials Science & Engineering,
Spring Meeting 1998. Volume 78. Conference
proceedings.
Dallas, Tx., Spring 1998, p.219-20. 012
SECONDARY TRANSITIONS IN POLYMERS
PROBED BY DIFFERENTIAL SCANNING
CALORIMETRY
Bertolucci P R H; Harmon J P
South Florida,University
The use of differential scanning calorimetry to identify
secondary transitions in thermoplastics is studied. The
temperature and breadth of the secondary transition are
related to the those of the alpha transition in a variety of
methacrylate, acrylate and styrene polymers, as well as
polycarbonate. The effect of thermal history and the
position and sharpness of these endothermic transitions
is discussed. Some comparisons are made between this
technique and results obtained via dielectric analysis and
dynamic mechanical analysis obtained in the laboratory.
7 refs.
USA
Accession no.718740
Item 246
200, No.2, Feb.1999, p.413-21
THERMAL PROPERTIES AND
CRYSTALLISATION BEHAVIOUR OF
POLYHYDROXYBUTYRIC ACID IN BLENDS
WITH CHITIN AND CHITOSAN
Ikejima T; Yagi K; Inoue Y
Tokyo,Institute of Technology
Films of blends of polyhydroxybutyric acid with chitin
and chitosan were prepared as completely biodegradable
polyester-polysaccharide composites. Crystallisation was
examined using DSC. Data are given from FTIR and
carbon 13 NMR. 31 refs.
JAPAN
Accession no.716972
Item 247
Journal of Biomedical Materials Research (Applied
Biomaterials)
48, No.1, 1999, p.5-8
EXTRACTABLE FREE MONOMERS FROM
SELF-CURED DENTAL SEALANTS RESULTING
FROM DISPENSING ERRORS
Vaubert V M; Moon P C; Love B J
Virginia,Polytechnic Institute
HPLC experiments were performed on a series of self-
curing polybisglycidyl methacrylate dental sealants that
were deliberately mismixed. The amount of extractable
sealant under conditions of nonideal processing was
measured. 13 refs.
USA
Accession no.716163
Item 248
Macromolecular Rapid Communications
20, No.2, Feb. 1999, p.95-7
CURING OF MONOMER COMPOSITES. II. USE
OF NMR TO MONITOR REAL TIME CURING
DYNAMICS
Martin S J; McBrierty V J; Dowling J; Douglass D C
Dublin,Trinity College; Bausch & Lomb Inc.
Details are given of a method for monitoring the real-
time curing dynamics of composite monomers, exploiting
site specific information provided by high resolution
NMR. Data using polyvinylpyrrolidone, polyhydroxy-
ethyl methacrylate and polybutylhydroxycyclohexyl
methacrylate are compared with results from a computer
simulation based on a multicomponent kinetic model.
7 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; IRELAND;
WESTERN EUROPE
Accession no.716161
Item 249
13, No.1, 1999, p.19-34
RHEO-PHOTOACOUSTIC (RPA) FTIR
SPECTROSCOPIC STUDIES OF THE
ADHESION OF THERMOSETS TO
POLYOLEFINS
Pennington B D; Urban M W
Rheophotoacoustic FTIR analysis and previously
developed theory were utilised in an attempt to correlate
the molecular level interactions in polymer bilayer
systems under elongational interactions in polymer bilayer
systems under elongational deformations and changes in
potential energy, leading to determination of the work of
adhesion. This research expands the scope of previous
findings and provides a relationship between the C-H
stretching vibrational energy changes for acrylic/PE,
epoxy/PE, acrylic/PP, and epoxy/PP bilayer systems and
the interfacial forces responsible for adhesion. 39 refs.
USA
Accession no.715972
Item 250
71, No.2, 15th Jan.1999, p.468-75
IDENTIFICATION AND DETERMINATION OF
CROSSLINKERS IN CROSSLINKED
POLYVINYLPYRROLIDONE(PVP) BY
PYROLYSIS-GAS CHROMATOGRAPHY(GC)/
MASS SPECTROMETRY(MS)
Cheng T M H; Malawer E G
International Specialty Products
Pyrolysis-GC and pyrolysis-GC/MS were used to identify
and quantify specific nitrogen-containing crosslinker
compounds incorporated into the structures of crosslinked
PVP polymers which appeared to be identical by FTIR
spectroscopy. The pyrolyser regenerated and volatilised
specific crosslinkers which could be distinguished from
other pyrolysate compounds by either peak retention time
or mass spectral release. Individual compounds studied
included 3-ethylidene-1-vinyl-2-pyrrolidone, 3,3'-
ethylidenebis(1-vinyl-2-pyrrolidone) and N,N-
divinylimidazolidone. In general, the level of specific
crosslinkers in various commercial products ranged from
1.8 to 2.5% w/w. The effect of pyrolysis temp. on this
level varied with the crosslinkers studied. The crosslinker
content obtained by this technique correlated with the
swell volume data for a specific series of crosslinked PVP
samples made with a single crosslinker and having similar
particle size distributions. The pyrolysis methodology
could not distinguish the level of crosslinker which was
incorporated as a pendant functionality from that portion
which was incorporated through both vinyl groups. 26
refs.
USA
Accession no.715578
Item 251
Polymer Testing
17, No.8, Dec.1998, p.533-41
NMR STUDY OF COMMERCIAL
POLYETHYLENE-CO-VINYL ACETATE
de Souza C M G; Tavares M I B
Rio de Janeiro,Cidade Universitaria
Two EVA materials with distinct vinyl acetate ratios are
studied by nuclear magnetic resonance using solution and
solid techniques. These studies are made in order to obtain a
relation between the structure-properties-mobility and this
response can be utilised in order to have precise information
for new applications as well as better understanding of the
material behaviour. The results show that these polymers
present characteristic mobilities as a function of vinyl acetate
in the copolymer. Thus, as the quantity of vinyl acetate
increases the dyads and tryads distribution and the molecular
mobility in the copolymer change, as a consequence of the
different commercial applications. 13 refs.
BRAZIL
Accession no.714141
Item 252
54, No.2, 1998, p.565-76
METHOD FOR ANALYSIS OF THE MEASURED
CURVES OF TEMPERATURE-MODULATED
DIFFERENTIAL SCANNING
CALORIMETRY(TMDSC) INVESTIGATION IN
THE MELTING REGION OF POLYMERS
Schawe J E K; Bergmann E; Winter W
Ulm,University; IFA GmbH
The measured signal of the TMDSC was examined for the
case of polymer melting. Fourier transform analysis was
used to evaluate the data, the resulting information being
the amplitude and the phase shift of the first harmonic of
the periodic heat flow component. It was shown that this
procedure was not sufficient for quantitative discussions if
deviations from the symmetric curve shape occurred in the
measured heat flow curves. For polymer melting, it was
shown that asymmetric curves would be measured if the
experimental temp. amplitude was too large. 15 refs.
WESTERN EUROPE
Accession no.713454
Item 253
54, No.2, 1998, p.477-99
APPLICABILITY OF TEMPERATURE-
CALORIMETRY(TMDSC) TO POLYMERIC
SYSTEMS. GENERAL THEORETICAL
DESCRIPTION BASED ON THE FULL HEAT
CAPACITY FORMULATION
Scherrenberg R; Mathot V; Steeman P
DSM Research
An overview is presented of the different aspects of
TMDSC, using a general theoretical description based
on the full heat capacity formulation. It is demonstrated
that processes studied with the aid of TMDSC can be
simply classified into three distinct regimes, depending
on the time scale and the susceptibility of the process to
the temp. modulation. 47 refs.
Accession no.713453
Item 254
Muanyag es Gumi
34, No.12, 1997, p.A12-4
Hungarian
ASSESSMENT OF THE THERMAL HISTORY OF
EXTRUDED UPVC
Marossy K
BorsodChem Rt.
The paper deals with the investigation by differential
scanning calorimetry of extruded rigid PVC formulations.
The DSC traces of processed UPVC depend on the
thermal history of the melt. The DSC tests can be used to
estimate extrusion conditions e.g. of failed products. 16
refs. Articles from this journal can be requested for
translation by subscribers to the Rapra produced
International Polymer Science and Technology.
Accession no.713264
Item 255
Surface Coatings International
82, No.1, Jan.1999, p.26-30
USE OF ELECTROCHEMICAL IMPEDANCE
SPECTROSCOPY FOR THE DETERMINATION
OF THE PROTECTIVE PROPERTIES OF
SOLVENT- AND WATER-BASED PAINT
SYSTEMS
Al-Hashem A; Carew J A; Hasan A
Kuwait,Institute for Scientific Research
In this work, electrochemical impedance spectroscopy
was used to evaluate the corrosion protection properties
of the solvent-based coatings and water-based coating
systems currently being proposed for use in the industrial
installations in the Arabian Gulf region. Evaluation of
corrosion damage levels for three coating systems after
90 day immersion in 0.5M NaCl was performed using
the EIS and visual observations. 22 refs.
KUWAIT
Accession no.713236
Item 256
Journal of Materials Science
33, No.19, 1st Oct.1998, p.4721-5
RAMAN SPECTRA OF HIGH MODULUS
POLYETHYLENE FIBRES BY RAMAN
MICROSCOPY
Lu S; Russell A E; Hendra P J
Southampton,University
Raman microscopy was used to analyse a series of high
modulus PE fibres, relating the Raman scattering
anisotropy to the mechanical performance of the
filaments. Measurements of the band intensity ratio of
the fibres were made and related to their Youngs modulus.
This relationship is useful in morphological studies of
PE fibres. 10 refs.
WESTERN EUROPE
Accession no.711133
Item 257
52, No.12, Dec.1998, p.1498-504
MEASUREMENT OF ORIENTATION AND
CRYSTALLINITY IN UNIAXIALLY DRAWN
POLY(ETHYLENE TEREPHTHALATE) USING
POLARISED CONFOCAL RAMAN
MICROSCOPY
Everall N J
ICI Wilton Research Centre
Polarised confocal Raman microscopy was used to
measure molecular orientation in uniaxially drawn PETP
films, prepared with draw ratios from 1 to 3.5. The
orientation of both polarised Raman microscopy and
polarised attenuated total reflection IR spectroscopy.
Crystallinity profiles were measured through the thickness
of the film samples and compared with the orientation
gradients existing in the films. This procedure was to
determine whether the intuitive assumption that
orientation and crystallinity would be positively correlated
actually holds true on the microscopic scale for these
samples. 18 refs.
WESTERN EUROPE
Accession no.711041
Item 258
Plasticheskie Massy (USSR)
No.3, 1997, p.30-3
Russian
BREAKDOWN OF AMMONIUM SALTS WITH
REFERENCE TO THEIR INTRODUCTION INTO
WOOD-BASED COMPOSITES
Vigdorovich A I; Efremov V N
The possibility was studied of using ammonium salts as
plasticisers for wood-based composites, and the
breakdown of the ammonium salts during heating was
studied by differential thermal gravimetry. 15 refs. Articles
from this journal can be requested for translation by
subscribers to the Rapra produced International Polymer
Science and Technology.
RUSSIA
Accession no.710456
Item 259
38, No.11, Nov.1998, p.1873-81
PHYSICAL AND RELAXATION PROPERTIES
OF FLAME-SPRAYED ETHYLENE-
METHACRYLIC ACID COPOLYMER
Brogan J A; Berndt C C; Simon G P; Hewitt D
Stony Brook,University; Monash,University
Details are given of the range of physical and chemical
properties of flame-sprayed ethylene-methacrylic acid
copolymer following different processing conditions.
Coatings were produced at a range of specific
temperatures by varying the propane flow rate and gun
traverse rate. Coatings were scanned using dielectric
relaxation spectroscopy. 24 refs.
AUSTRALIA; USA
Accession no.709520
Item 260
30, No.10, 1998, p.771-4
CRYSTALLITE SIZES AND LATTICE
DISTORTIONS OF GEL-SPUN ULTRA-HIGH
MOLECULAR WEIGHT POLYETHYLENE
FIBRES
Xiao-Ping Hu; You-Lo Hsieh
California,University
A detailed method is reported for deriving the lattice
distortions and crystallite sizes of UHMWPE fibres using
a full wide angle X-ray diffraction patterns. The
instrumental broadening and the background scattering
is represented by a binomial. A discussion is included
about the diffraction trace, peak assignments, and unit
cell dimensions. 26 refs.
USA
Accession no.709342
Item 261
Chinese Journal of Polymer Science
16, No.4, 1998, p.332-8
DETECTION OF TG BY MODULATED
Rui Song; Jing Chen; Jingui Gao; Xin Lin; Qingrong Fan
The glass transition of PETP samples which were
subjected to solvent induced crystallisation (SINC) was
investigated by modulated differential scanning
calorimetry (MDSC) and density measurements. The
differential heat capacity signal from MDSC was used to
monitor the SINC process. 16 refs.
CHINA
Accession no.709335
Item 262
71, No.1, 3rd Jan.1999, p.1-6
MICROWAVE PLASMA REACTIONS OF
IMIDAZOLE ON POLY(VINYL CHLORIDE)
SURFACES: A SPECTROSCOPIC STUDY
Schmitt B R; Heung Kim; Urban M W
A closed-system microwave plasma reactor was used to react
imidazole molecules to PVC surfaces. Newly created
surfaces were analysed using ATR FTIR spectroscopy.
Surface reactions on PVC were heavily dependent on a prior
thermal history of the PVC substrate. A mechanism for the
PVC-imidazole reactions was also presented. The PVC was
useful as an implant for biomedical applications. 10 refs.
USA
Accession no.709309
Item 263
52, No.11, Nov.1998, p.1483-7
SAMPLING CONSIDERATIONS FOR FT-
RAMAN SPECTROSCOPY OF POLYMERS AND
SOLUTIONS
Barrerra B A; Sommer A J
Miami,University
Details are given of the determination of apparent
absorption coefficients and optimal sample thickness of
PE, PETP, cellulose, and cyclohexane by FT-Raman
analysis. A relationship was developed that permits the
optimal sample thickness for FT-Raman measurements
to be determined by measuring the absorbance spectrum
of a sample whose thickness is known. Results are
discussed in the context of scattering theory, sampling
considerations, and spectral artifacts. 9 refs.
USA
Accession no.709038
Item 264
71, No.3, 18th Jan.1998, p.371-5
PROPYLENE OLIGOMERS: EXTRACTION
METHODS AND CHARACTERISATION BY
FTIR, HPLC, AND SEC
El Mansouri H; Yagoubi N; Scholler D; Feigenbaum A;
Ferrier D
INRA
Details are given of the isolation of propylene oligomers
from polymer matrix by dissolution precipitation and
Soxhlet methods. Characterisation was undertaken by
FTIR, UV spectroscopy, HPLC, and GPC. Data were used
to explain their behaviour toward packaged food products
in PP packaging. 18 refs.
WESTERN EUROPE
Accession no.708984
Item 265
European Polymer Journal
34, No.12, Dec.1998, p.1817-28
CURING OF POLYMER COMPOSITES. I. NMR
CHARACTERIZATION OF COMPONENT
MONOMERS
Martin S J; OBrien J E; Dowling J; McBrierty V J
Dublin,Trinity College; Bausch & Lomb Inc.
The use of NMR to probe the in-situ curing of monomer
mixtures commonly encountered in the manufacture of
contact lenses was studied. Spectral lines were identified
which monitored curing with time of individual
components in the monomer mix. This information can
aid in gaining an understanding of the overall curing
dynamics and provide important guidance in establishing
suitable protocols in the manufacturing process. As a
precursor to this goal, several commonly-used component
materials were characterised by high resolution proton
and carbon-13 NMR spectroscopies. The efficacy of the
overall procedure is demonstrated. 20 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; IRELAND;
WESTERN EUROPE
Accession no.706520
Item 266
8, No.1, Jan./March 1998, p.46-53
Portuguese
THERMAL STABILITY OF POLYETHYLENE
TEREPHTHALATE PACKAGING:
DETERMINATION OF OLIGOMERS
Freire M T de A; Reyes F G R; Castle L
Campinas,Universidade Estadual; UK,Min.of
Agriculture,Fisheries & Food
PETP food packaging materials were subjected to
different heating conditions (50 minutes at 120-230C),
and oligomers were identified by HPLC coupled with
mass spectrometry and used as a parameter for evaluating
the thermal stability of PETP. Small changes in oligomer
distribution were observed only for samples heated at
230C, suggesting that PETP was thermally stable under
the heating conditions employed. The results also
suggested the suitability of PETP as a food packaging
material for use in conventional and microwave ovens,
and for secondary recycling under controlled conditions.
28 refs.
BRAZIL; EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
WESTERN EUROPE
Accession no.706082
Item 267
52, No.2, 1998, p.261-74
THERMAL ANALYSIS OF SOME
ENVIRONMENTALLY DEGRADABLE
POLYMERS
Day M; Cooney J D; Shaw K; Watts J
Canada,National Research Council
The thermal characteristics of a series of degradable
polymers for use in commercial composting facilities was
investigated using TGA and DSC. Phase changes
associated with some of the polymers investigated may
cause problems in the interpretation of data from
composting degradation studies. Several biodegradable
polymers were observed to have melt transitions at
temperatures similar to those found in a composting
environment. 19 refs.
CANADA
Accession no.705674
Item 268
70, No.12, 19th Dec.1998, p.2457-61
NUCLEAR MAGNETIC RESONANCE STUDY
OF COMMERCIAL POLY(VINYL ACETATE)
De Souza C M G; Tavares M I B
Rio de Janeiro,Universidade Federal
The commercial poly(vinyl acetate) bulk was studied by
NMR at solution and solid state to understand the
behaviour of this polymer to obtain information on
structure, sample molecular mobility, and heterogeneity.
To analyse the behaviour of this polymer, NMR
techniques were chosen, such as carbon-13 solution,
magic angle spinning, cross-polarisation/magic angle
spinning, proton spin-relaxation time in the rotating frame
parameter and dipolar dephasing experiment. 13 refs.
BRAZIL
Accession no.705529
Item 269
52, No.1, 1998, p.145-55
German
THERMOANALYTICAL CHARACTERISING
UV-CURED POLYMER FILMS
Hosselbarth B; Friese K; Geyer W
Institut fuer Oberflaechenmodifizierung eV; Leipzig-
Halle Ltd.; Umweltforschungzentrum
Thermooxidative and thermomechanical stabilities of
radiation-cured acrylates and epoxides were examined by
TGA, DMA and DSC. The polymeric trifunctional
acrylates PETIA, TMPTA and THEIC displayed the
highest temperatures of onset of degradation. The high
crosslinking density of the films resulted in an almost
temperature-independent complex E-modulus, as
measured by DMA. With increasing degree of
ethoxylation or propoxylation of the monomers, decreases
in thermal stability and strength were found. For
difunctional polymeric acrylates and epoxides, the TG
temperature was measured. The average degree of curing
of UV-cured epoxy films could be determined from the
temperature of the maximum in the loss modulus. 13 refs.
WESTERN EUROPE
Accession no.705282
Item 270
52, No.1, 1998, p.131-43
German
DETERMINATION OF VINYL ACETATE
CONTENT IN EVA COPOLYMERS. FACILITIES
AND LIMITS OF APPLICATIONS OF MASS
SPECTROMETRY ANALYSIS METHODS
Haussler L; Pompe G; Albrecht V; Voigt D
Dresden,Institut fuer Polymerforschung
Ethylene-vinyl acetate copolymers were investigated by
simultaneous thermal analysis and pyrolysis gas
chromatography. Both devices were coupled to a mass
spectrometer. Calibration with polyvinyl acetate led to
sufficient accuracy in relation to the vinyl acetate content,
because of the linear calibration plot. Quantitative
determination of vinyl acetate was carried out at both 500
and 700 C. The calibration plot was linear provided that
the mass of vinyl acetate did not exceed a critical value.
18 refs.
WESTERN EUROPE
Accession no.705281
Item 271
Composites Science & Technology
58, No.10, 1998, p.1641-7
CHEMICAL ANALYSIS OF A FIELD-FAILED
COMPOSITE SUSPENSION INSULATOR
Chughtai A R; Smith D M; Kumosa M S
Denver,University
The type of corrosive environment responsible for brittle
fracture of suspension composite insulators was
established. A series of FTIR experiments was performed
to identify chemical functionalities formed during the
degradation process of composite insulators affected by
brittle fracture. It was shown that the brittle fracture
process was caused by the formation of nitric acid either
outside or inside an insulator leading to stress corrosion
cracking of the glass/polymer composite rod material.
Nitrate was detected on the composite fracture surfaces
inside a 115 kV suspension composite insulator which
failed in service by brittle fracture. 17 refs.
USA
Accession no.705241
Item 272
International Journal of Adhesion & Adhesives
18, No.5, 1998, p.319-31
LOW RESOLUTION PULSED NMR AND
ULTRASOUND STUDY TO MONITOR THE
CURE OF AN EPOXY RESIN ADHESIVE
Cocker R P; Chadwick D L; Dare D J; Challis R E
Keele,University; Manchester,Metropolitan University
The cure of an epichlorohydrin-bisphenol A resin and
curing agent containing a primary diamine and an amido-
polyamine was studied using two complementary
techniques, low resolution pulsed NMR spectroscopy and
measurement of pulsed broad bandwidth ultrasound
propagation velocity and absorption changes. The two
techniques independently gave a similar picture of the
cure process, predicting cure events at the same times.
The results obtained indicated that the cure followed
distinct phases, i.e. an initial liquid stage where short
polymer chains were formed, followed by a second stage
where longer molecules developed, a third stage where
crosslinking between chains occurred and the adhesive
began to solidify, and a final stage when solidification
was completed. 19 refs.
WESTERN EUROPE
Accession no.704884
Item 273
62, No. 1, Oct. 1998, p.41-8
MECHANISMS OF THERMAL DEGRADATION
OF A POLYESTER FLAME-RETARDED WITH
ANTIMONY OXIDE/BROMINATED
POLYCARBONATE STUDIED BY
TEMPERATURE-PROGRAMMED ANALYTICAL
PYROLYSIS
Sato H; Kondo K; Tsuge S; Ohtani H; Sato N
Nagoya,University; Toray Research Center Inc.
Thermal degradation of a flame-retarded PBTP consisting
of PBTP and a synergistic flame-retardant system based
on brominated polycarbonate (copolycarbonate
containing units from bisphenol A and tetrabrominated
bisphenol A plus tribromophenoxy end groups) and
antimony trioxide was studied by means of various
temperature-programmed analytical pyrolysis techniques
such as temperature-programmed pyrolysis-mass
spectrometry, temperature-programmed pyrolysis-atomic
emission detection and temperature-programmed
pyrolysis-gas chromatography. During the degradation of
the flame-retarded PBTP, brominated phenols were first
observed to evolve at temperatures slightly lower than
those for the flammable product evolution from the
substrate polymer PBTP, followed by the evolution of
hydrogen bromide over the whole range of degradation
temperatures for the substrate polymer. These degradation
processes were closely related to the synergistic effects
of antimony trioxide on the decomposition of brominated
polycarbonate in the flame-retardant system to promote
the thermal degradation of brominated polycarbonate at
lower temperatures than those for pure brominated
polycarbonate. Furthermore, the evolution of the flame
poisoning antimony tribromide formed through the
reaction between brominated polycarbonate and antimony
trioxide could also be monitored directly by temperature-
programmed pyrolysis techniques. On the basis of the
data obtained by these temperature-programmed pyrolysis
techniques, the thermal degradation of the flame-retarded
PBTP and synergistic flame-retarding mechanisms are
discussed. 10 refs.
JAPAN
Accession no.704607
Item 274
74, No.495, Sept.1997, p.255-61
Spanish
FTIR SPECTROPHOTOMETRY FOR THE
DETECTION OF MICROSTRUCTURAL
CHANGES IN A POLYPROPYLENE/
POLYETHYLENE COPOLYMER CAUSED BY
ARTIFICIAL AGEING
Romeu J; Pages P; Carrasco F
Cataluna,Universidad Politecnica; Girona,Universidad
A study was made of microstructural changes occurring
in blue and red samples of an ethylene-propylene
copolymer exposed to artificial ageing in a Xenotest
chamber for up to 5000 hours. The effects of ageing
were quant i fi ed by Fouri er t ransform IR
spectrophotometry. By calculating the reduced
absorption in selected spectral bands, it was possible
to detect oxidation and chain scission reactions and
variations in isotacticity which differed in the
differently coloured specimens. 8 refs.
WESTERN EUROPE
Accession no.702522
Item 275
70, No.7, 14th Nov.1998, p.1307-10
MULTIDIMENSIONAL SPECTROMETRY AND
MAPPING
Fateley W G; Deverse R A; Hammaker R M
Kansas State University
A new inexpensive approach is described for mapping
molecular structure in polymeric materials which includes
the combination of interferometers and Hadamard
transform techniques to perform multidimensional
spectometry and mapping. 17 refs.
USA
Accession no.702159
Item 276
Journal of Materials Science.Materials in Medicine
9, No.9, Sept.1998, p.529-33
INVESTIGATION OF GLASS-IONOMER
CEMENTS USING DIFFERENTIAL SCANNING
CALORIMETRY
Khalil S K H; Atkins E D T
Bristol,University
Six commercial glass-ionomer cements commonly used
for various dental applications were investigated using
DSC. Heat flow behaviour and heat capacity of the
cements were measured during isothermal (at 37 C) setting
reactions. All materials underwent an exothermic setting
process, but with different enthalpies of reactions and
different heat capacities; there were no remaining endo-
or exothermic reactions after the setting of the cement.
All materials examined were effective thermal insulators.
18 refs.
WESTERN EUROPE
Accession no.702142
Item 277
33, No.14, 15th July 1998, p.3511-7
MOLECULAR ORGANISATION IN
STRUCTURAL PVDF
Glennon D; Cox P A; Nevell R T; Nevell T G; Smith J
R; Tsibouklis J; Ewen R J
Portsmouth,University; West of England,University
Poly(vinylidene fluoride) containing 10% dibutyl sebacate
plasticiser, as used in the construction of flexible oil and
gas pipelines, was exposed to raised temperatures for
prolonged periods of time, to acid etching and to various
tensile deformation regimes. The effects of these
treatments on crystallinity and surface properties of this
material were examined in the light of analytical data
obtained by FTIR, DSC, X-ray diffraction, X-ray
photoelectron spectroscopy, goniometry and a variety of
microscopy techniques. 36 refs.
WESTERN EUROPE
Accession no.701984
Item 278
Food Additives and Contaminants
15, No.3, 1st April 1998, p.346-54
PARTS-PER-TRILLION DETERMINATION OF
STYRENE IN YOGHURT BY PURGE-AND-TRAP
GAS CHROMATOGRAPHY WITH MASS
SPECTROMETRY DETECTION
Nerin C; Rubio C; Cacho J; Salafranca J
Zaragoza,University
Headspace sampling methods prior to capillary gas
chromatography are widely used for the determination
of volatile compounds present in very different types of
samples. An automated and rapid system for
determination of volatiles from yoghurt was developed.
Thirty-five volatile organic compounds(VOCs) were
identified in PS cups used for yoghurt packaging and 42
VOCs from yoghurt samples. Quantitative analysis of
styrene in several samples from the Spanish retail market
was carried out. 16 refs.
WESTERN EUROPE
Accession no.700270
Item 279
70, No.6, 7th Nov.1998, p.1201-7
PHOTODEGRADATION OF TEFLON AF1600
DURING XPS ANALYSIS
Popovici D; Sacher E; Meunier M
Montreal,Ecole Polytechnique
Teflon, type AF1600, which contains perfluorinated
dioxole rings, was found to suffer significant degradation
when exposed to X-rays whilst undergoing investigation
by X-ray photoelectron spectroscopy. The degradation
mechanism was significantly different to that of
fluoropolymers which contain only carbon and fluorine.
It was established that oxygen was at least as twice as
susceptible as fluorine, and that the amounts of oxygen
loss were equal to those of fluorine. Oxygen could be
degraded by the breaking of only one bond, the oxygen
then forming a free radical. The free radicals produced
by scission of carbon-carbon bonds participated in
reactions leading to degradation and crosslinking. 9 refs.
CANADA
Accession no.700200
Item 280
47, No.1, Sept.1998, p.72-5
TEMPERATURE-MODULATED DIFFERENTIAL
SCANNING CALORIMETRY. II.
DETERMINATION OF ACTIVATION ENERGIES
Zhong Jiang; Hutchinson J M; Imrie C T
Aberdeen,University
Alternating differential scanning calorimetry (ADSC), a
commercial development of temperature-modulated
differential scanning calorimetry, was used to determine the
activation energy associated with the relaxation processes
in polycarbonate in the region of the glass transition. In this
procedure the frequency of the temperature modulation is
varied over a range of approximately one decade, and the
mid-point of the step change in the complex heat capacity is
evaluated. In these experiments, two different amplitudes
of temperature modulation were employed. The results were
in agreement with each other, and in good agreement with
published values. Ripples seen on the Fourier-transformed
signals are attributed to the mode of the data analysis, and
not to noise on the data. 7 refs.
WESTERN EUROPE
Accession no.700165
Item 281
Materials World
6, No.10, Oct.1998, p.617-9
THROWING LIGHT ON FIBRES AND
COMPOSITES
Young B
Manchester,University
The use is discussed of Raman spectroscopy to monitor
the stresses and strains on individual fibres in composite
materials. New instrumentation has caused rapid growth
in the use of Raman spectroscopy for materials
characterisation, including the introduction of charged-
coupled device cameras which offer significant
improvements in sensitivity and very low noise, and also
holographic notch filters which are used to remove the laser
line and allow single monochromators to be used. Both
these developments are incorporated in the Raman imaging
microscope developed by Renishaw in collaboration with
Leeds University Physics Department. Its use is described
with reference to aramid fibre reinforced PP. 5 refs.
RENISHAW PLC
WESTERN EUROPE
Accession no.699334
Item 282
Farbe und Lack
104, No.10, 1998, p.93/8
German
CALORIMETRY
Haessler R
Dresden,Institut fuer Polymerforschung
The use of modulated DSC for improved interpretation
of product characteristics under thermal effects was
investigated. Tgs, for example, which are masked by post-
curing or enthalpy relaxation, could be detected in a single
measurement and compared. The separation of complex
transitions in multicomponent systems into individual
parts such as melts, transition temps. and relaxations was
shown to be feasible. The potential for use of modulated
DSC in the field of epoxy resins was demonstrated using
examples of the determination of Tg near the regions of
enthalpy relaxation, melt and post-curing. 7 refs.
WESTERN EUROPE
Accession no.699054
Item 283
Structure and properties of Oriented Polymers. Second
Edition.
London, Chapman & Hall, 1997, p.234-68. 9
NUCLEAR MAGNETIC RESONANCE
Speiss H W
Max-Planck-Institut fuer Polymerforschung
Edited by: Ward I M
(Leeds,University)
The basics of solid state NMR are outlined and the site-
selective information available from multi-dimensional
NMR spectra about molecular order and dynamics in
oriented polymers is illustrated with specific experimental
examples. 55 refs.
WESTERN EUROPE
Accession no.697739
Item 284
Structure and properties of Oriented Polymers. Second
Edition.
London, Chapman & Hall, 1997, p.181-233. 9
INFRARED DICHROISM, POLARISED
FLUORESCENCE AND RAMAN
SPECTROSCOPY
Bower D I
Leeds,University
Edited by: Ward I M
(Leeds,University)
The three spectroscopic techniques for studying
molecular orientation in polymers described in detail
use polarised electromagnetic radiation. The principles
of the techniques are outlined, relevant theory and
experimental details described, and a selection of results
presented. 79 refs.
WESTERN EUROPE
Accession no.697738
Item 285
Polymer
39, No.20, 1998, p.4973-6
EFFECTS OF SUBSTRATE INTERACTIONS IN
THE LIQUID CHROMATOGRAPHY OF
POLYMERS
Kosmas M K; Bokaris E P; Georgaka E G
Ioannina,University
The elution behaviour of PMMA samples was studied
through two liquid chromatographic columns, one
containing a substrate of silica covered with trimethylsilyl
groups and the other a substrate of pure silica. Both
substrates had the same pore size and the solvent was the
same for both columns. The results were discussed and
they showed that the polymer-surface interactions
changed when the nature of the substrate was changed.
14 refs.
WESTERN EUROPE
Accession no.696588
Item 286
15, No.1, 1st Jan.1998, p.93-9
SYSTEMATIC STUDY ON THE STABILITY OF
SELECTED POLYMER ANTIOXIDANTS IN EU
OFFICIAL AQUEOUS AND ALTERNATIVE
FOOD SIMULANTS USING HPLC
Demertzis P G; Franz R
Fraunhofer Institute for Food Technol. & Packag.
Details are given of the stability of five commercial
antioxidants in food simulants and in an alternative fat
simulant. Analysis was performed using a rapid HPLC
method with UV detection. 23 refs.
WESTERN EUROPE
Accession no.695963
Item 287
Colloid & Polymer Science
276, No.7, July 1998, p.565-9
DESCRIPTION OF THE GLASS TRANSITION
MEASURED BY TEMPERATURE MODULATED
Schawe J E K
Ulm,University
The temp. modulated DSC (TMDSC) technique could be
used for heat capacity spectroscopy in the low frequency
range. The measured property was the complex heat
capacity. The frequency-dependent relaxation transition
measured by TMDSC occurred in the temp. range of the
thermal Tg. The non-equilibrium of the glassy state thus
influenced the TMDSC curves. Experimental evidence
was the dependence of the shape of the heat capacity curve
on the thermal history. A theoretical description of the
influence of the non-equilibrium state on the spectroscopic
curves, based on the Tool-Narayanaswamy-Moynihan
model, is presented. 23 refs.
WESTERN EUROPE
Accession no.695591
Item 288
Composites Plastiques Renforces Fibres de Verre
Textile
No.21, May/June 1997, p.48-54
French
DURABILITY OF COMPOSITES: HOW TO
ACHIEVE RELIABLE ACCELERATED AGEING
Siampiringue N; Gaumet S; Lemaire J
Centre National dEvaluation de Photoprotection
The use of accelerated ageing tests and
spectrophotometric techniques in studying the
photooxidative degradation of unsaturated polyester resins
and glass fibre-reinforced composites is examined.
Results of accelerated and natural ageing tests are
compared, and criteria to be taken into account in
achieving accelerated test results representative of reality
are discussed. 5 refs.
WESTERN EUROPE
Accession no.695308
Item 289
7, No.3, July/Sept.1997, p.19-23
Portuguese
FAILURE ANALYSIS OF MATERIALS BY
ADVANCED MICROSCOPIC TECHNIQUES
Chinaglia C R; Correa C A
Sao Carlos,Universidade Federal
Failure analysis techniques allowing the determination
of the chemical composition of a sample and its correlation
with the observed fracture mode are examined. Topics
discussed include the use of SEM in studying fracture in
mineral filled thermoplastics, secondary electron imaging
in obtaining information on sample topography,
backscattered electron imaging in studying filler
dispersion in polymer matrices, and energy dispersive X-
ray spectroscopy in determining the chemical composition
of the fillers or contaminants responsible for fracture
initiation. 5 refs.
BRAZIL
Accession no.695299
Item 290
Journal of Polymer Science : Polymer Physics Edition
36, No.12, 15th Sept.1998, p.2165-75
DESCRIPTION OF THERMAL RELAXATION OF
POLYSTYRENE CLOSE TO THE THERMAL
GLASS TRANSITION
Schawe J E K
Ulm,University
Using spectroscopic methods at relatively high frequency,
the alpha-relaxation was measured in the thermodynamic
equilibrium. In the caloric case this phenomenon is called
thermal relaxation transition. Using a conventional
differential scanning calorimeter, the transition of the
equilibrium (the melt) into a nonequilibrium (the glassy
state) was measured. This effect is called thermal glass
transition. Temperature-modulated DSC curves in the
glass transition region were described using the Tool-
Narayanaswamy-Moynihan model. 54 refs.
WESTERN EUROPE
Accession no.694872
Item 291
36, No.12, 15th Sept.1998, p.2103-9
RAPID DETERMINATION OF COMONOMER
CONTENT, CRYSTALLINITY, AND LONG
SPACING BY MULTIPLE-PULSE PROTON NMR
IN ETHYLENE-VINYL ALCOHOL
COPOLYMERS
Perez E; Cerrada M L; Vanderhart D L
Instituto de Ciencia y Tecnologia de Polimeros;
US,National Institute of Standards & Technology
Capitalising on the superior sensitivity of proton NMR,
relatively rapid estimates of three parameters, namely,
comonomer content, crystallinity, and long spacing, were
determined for three ethylene-vinyl alcohol copolymers
using solid state proton NMR measurements. Multiple-pulse
techniques were utilised (a) in conjunction with magic angle
spinning for measuring comonomer content, (b) in
conjunction with a relaxation time measurement for
determining crystallinity, and (c) in conjunction with a
relaxation time-based spin diffusion measurement for
determining the long spacing. These three parameters,
extracted from data collected in a total spectrometer time of
about 20 min., and were compared with similar parameters
obtained using more conventional DSC, small angle X-ray
scattering (including synchrotron), and solution-state NMR
measurements, with good agreement. 23 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; USA;
WESTERN EUROPE
Accession no.694867
Item 292
Smart Materials & Structures
7, No.4, Aug. 1998, p.557-68
IN SITU CURE MONITORING USING OPTICAL
FIBRE SENSORS. A COMPARATIVE STUDY
Powell G R; Crosby P A; Waters D N; France C M;
Spooncer R C; Fernando G F
Brunel University; Cranfield,University
A comparative study is presented for different types of
optical fibre sensor developed to monitor the cure of an
epoxy resin system. The sensors were based on
transmission spectroscopy, evanescent wave spectroscopy
and refractive index monitoring. 19 refs.
WESTERN EUROPE
Accession no.694840
Item 293
Polymer Testing 97. Day 3: Chemical Analysis.
Conference proceedings.
Shawbury, 7th-11th April 1997, Paper 4. 9T
RAMAN SPECTROSCOPY OF POLYMERS
Williams K P J; Wilcock I C
Renishaw plc
(Rapra Technology Ltd.; Plastics & Rubber Weekly;
European Plastics News)
Raman spectroscopy is now coming of age as a routine
analytical method. Advances in Raman technology have
meant that robust, user-friendly equipment can be
manufactured at a reasonable cost. These advances are
described, together with applications of Raman imaging
microscope systems to polymer analysis. 11 refs.
WESTERN EUROPE
Accession no.694712
Item 294
International Polymer Processing
13, No.2, July 1998, p.142-8
PEROXIDE INDUCED CROSSLINKING AND
DEGRADATION OF POLYAMIDE
Yu Q; Zhu S
McMaster University
Peroxide-induced crosslinking and degradation of nylon
12 were investigated using ESR. Various reaction
mechanisms are proposed. 20 refs.
CANADA
Accession no.694268
Item 295
199, No.8, 1998, p.1623-9
THERMAL STABILITY AND
CRYSTALLISATION KINETICS OF PEEK
Chen J-Y; Chen M; Chao S-C
Taiwan,National Sun Yat-Sen University
TGA, dynamic rheological analysis and polarised light
microscopy were used to assess thermal stability of PEEK.
Emphasis is given to the effect of melting temperature on
thermal stability. 23 refs.
CHINA
Accession no.694246
Item 296
Injection Molding
6, No.8, Aug. 1998, p.56/9
MATERIALS ANALYST: PART 13.
PERFORMANCE PROBLEMS: WHEN THE
PELLETS DONT MATCH THE PARTS
Sepe M
The use of differential scanning calorimetry and
thermogravimetric analysis as analytical tools in part
failure determination is applied. Problems are examined
in part performance of moulded 30% glass-reinforced,
low-viscosity PEI and a second part moulded from PPS
with proprietary additives to improve wear resistance. The
importance of checking the composition of the basic
material is stressed.
USA
Accession no.693205
Item 297
69, No.11, 12th Sept.1998, p.2175-85
IR SPECTROSCOPY AS A QUANTITATIVE AND
PREDICTIVE ANALYSIS METHOD OF
PHENOL-FORMALDEHYDE RESOL RESINS
Holopainen T; Alvila L; Rainio J; Pakkanen T T
Joensuu,University; Dynoresin Oy
A set of resin samples was characterised by IR and carbon-
13 NMR spectroscopy. The suitability of IR spectroscopy
for the quantitative analysis of resins was evaluated by
statistical methods using the NMR reference data as
calibration. The values of interesting properties, e.g. the
amount of free phenol and the formaldehyde-to-phenol
molar ratio, of the resins being similar to the calibration
resins were predicted from the IR spectra. The predicted
results were compared with those observed by carbon-13
NMR spectroscopy. 15 refs.
FINLAND; SCANDINAVIA; WESTERN EUROPE
Accession no.692990
Item 298
33, No.13, 1st July 1998, p.3245-9
XPS MONITORING OF THE REMOVAL OF AN
AGED POLYMER COATING FROM A METAL
SUBSTRATE BY TEA-CARBON DIOXIDE
LASER ABLATION
Cottam C A; Emmony D C; Cuesta A; Bradley R H
Loughborough,University; Aberdeen,Robert Gordon
University
X-ray photoelectron spectrometry was used to observe
the changes in surface chemistry during the removal of
paint from a zinc coated steel substrate using TEA-carbon
dioxide laser ablation. Laser ablation at both plasma and
sub-plasma fluences were investigated and their relative
merits discussed. The laser was shown to be effective in
paint removal and was not impaired by ageing in the paint.
32 refs.
WESTERN EUROPE
Accession no.692055
Item 299
70, No.15, 1st Aug.1998, p.3298-303
IMPROVEMENTS IN POLYMER
CHARACTERIZATION BY SIZE-EXCLUSION
CHROMATOGRAPHY AND LIQUID
CHROMATOGRAPHY AT THE CRITICAL
CONDITION BY USING ENHANCED-FLUIDITY
LIQUID MOBILE PHASES WITH PACKED
CAPILLARY COLUMNS
Hao Yun; Olesik S V; Marti E H
Ohio,State University; Ashland Chemical Co.
The use of the above combination of techniques is
described and results obtained for samples of PS, PMMA,
styrene-methyl acrylate copolymers and functionalised
PS are presented and discussed. 32 refs.
USA
Accession no.691471
Item 300
Polymer
39, No.22, 1998, p.5293-300
QUANTITATIVE CARBON-13 SOLID-STATE
NMR AND FT-RAMAN SPECTROSCOPY IN
NOVOLAC RESINS
Ottenbourgs B; Adriaensens P; Carleer R; Vanderzande
D; Gelan J
Limburg,University
A qualitative and quantitative study of the curing behaviour
of a high-ortho novolac resin with paraformaldehyde under
different conditions was conducted. The degree of cure as
a function of the formaldehyde/phenol ratio, the degree of
conversion and the final structure after curing were
determined on the basis of a quantitative carbon-13 solid
state NMR with cross-polarisation and magic angle
spinning. The spin-lattice relaxation time was measured
as a probe to follow the evolution of cure. Fourier
transform-Raman spectroscopy was proposed as a
qualitative tool to follow the degree of crosslinking in this
high-ortho novolac. 54 refs.
WESTERN EUROPE
Accession no.689414
Item 301
Antec 98. Volume II. Conference proceedings.
Atlanta, Ga., 26th-30th April 1998, p.1415-7. 012
IN SITU SPECTROSCOPY OF CO2-INDUCED
PLASTICISATION OF GLASSY POLYMERS
Kazarian S G; Brantley N H; Eckert C A
Georgia,Institute of Technology
(SPE)
In situ spectroscopy is used to study the plasticisation of
glassy polymers by high-pressure and supercritical CO2.
The methodology for in situ spectroscopic analysis of the
interactions between CO2 and polymers is described. The
changes in IR spectra of CO2 incorporated into various
polymers indicate a specific interaction between CO2 and
polymer functional groups. Increased polymer segmental
mobility is also observed, indicative of the plasticisation
phenomenon. Implications of these discovered molecular
interactions are discussed. 25 refs.
USA
Accession no.687565
Item 302
QUANTITATIVE ANALYSIS OF CHEMICAL
BLOWING AGENTS BY DSC
Prasad A; Shanker M
Millennium Petrochemicals Inc.
(SPE)
It is shown that differential scanning calorimetery (DSC)
can be used to determine quantitatively the level and
composition of chemical blowing agents such as
azodicarbonamide (azo) in commercial formulations.
DSC can also be used to obtain the onset of decomposition
temperature and the rate of decomposition of azo in the
presence of group II and group IV metal salt activators.
DSC has the potential to detect the level of undecomposed
blowing agents present in processed foam products and
to qualitatively determine the degree of dispersion of the
blowing agent and the activators in commercial
formulations. Advantages of DSC over the currently used
EGA technique are ease of operation, shorter analysis time
and detection of azo concentrations as low as 1%. 12 refs.
USA
Accession no.687551
Item 303
APPLICATION OF GC/MS IN
THERMOPLASTICS PROBLEM SOLVING
Shaker D C; Kim H C
LNP Engineering Plastics
(SPE)
The use of GC/MS (gas chromatography/mass spectrometry)
in the thermoplastics problem solving area is outlined. GC/
MS is a hyphenated technique; i.e. it combines the two
techniques, chromatography and spectroscopy. In this
procedure, a material is introduced into the GC, components
are separated and sent to the MS where they are ionised, and
the resulting particles are separated by mass. The applications
of GC/MS to solving complex problems are discussed
through positive identification of base resins, contamination,
odours and solvents.
USA
Accession no.687499
Item 304
TEMPERATURE GRADIENT INTERACTION
CHROMATOGRAPHY OF POLYMERS
Chang T; Lee W; Lee H C; Mays J W; Harville S;
Frater D J
Pohang,University of Science & Technology;
Alabama,University at Birmingham
(SPE)
Temperature gradient interaction chromatography (TGIC)
is a conventional reversed phase BPLC technique, but the
column temperature is varied during elution. A very fine
and reproducible control of interaction between polymer
chains and the stationary phase can be achieved by changing
the column temperature. Under a suitable temperature
programming, this method provides a far superior resolution
to conventional size exclusion chromatography. In addition,
elution in TGIC is more sensitive to molecular weight alone.
Thus it provides an excellent route to separating branched
polymer molecules of similar hydrodynamic volume but
differing molecular weight. 8 refs.
KOREA; USA
Accession no.687496
Item 305
CALORIMETRY TO STUDY REACTING
POLYMER SYSTEMS
Van Mele B; Van Assche G; Van Hemelrijck A
Brussels,Free University
(SPE)
Modulated (temperature) differential scanning calorimetry
(MTDSC or MDSC) is used to simultaneously study the
evolution of heat flow and heat capacity for the isothermal
and non-isothermal reactions of polymer systems. An
epoxy-anhydride thermosetting system is used as an
example. Vitrification and devitrification steps are
observed. The heat flow phase during isothermal and
nonisothermal cure is always small, but its evolution
contains information on relaxation phenomena, vitrification
and devitrification, in the course of the chemical reaction.
Modelling of the (heat flow related) chemical kinetics and
the (heat capacity related) mobility restrictions contributes
to a better understanding of the reaction mechanism and
reaction kinetics up to a high degree of chemical
conversion. The use of MTDSC as a tool for a quantitative
construction of the vitrification curve in Temperature-Time-
Transformation and Continuous-Heating-Transformation
diagrams is illustrated. 20 refs.
WESTERN EUROPE
Accession no.687483
Item 306
PRACTICAL ANALYSIS TECHNIQUES OF
POLYMER FILLERS BY FOURIER
(FTIR)
Coles B J; Hall C J
Hauser Inc.
(SPE)
The identification of polymers by FTIR is often
complicated by the presence of fillers. However for kaolin
clay, an FTIR analysis should be able to identify the filler
and predict its concentration using a standard curve. The
resulting percentage is more reliable than a simple ash,
which may change the chemical composition of the filler.
2 refs.
USA
Accession no.687418
Item 307
38, No.6, June 1998, p.922-5
IDENTIFICATION OF OFF-FLAVOUR
COMPOUNDS IN HDPE WITH DIFFERENT
AMOUNTS OF ABSCENTS
Villberg K; Veijanen A; Gustafsson I
Jyvaskyla,University; Borealis AB
Details are given of the addition of zeolite to HDPE
drinking water pipes in an attempt to eliminate odours
and to remove odour-causing compounds. The system
used for analysis of volatile organic compounds was a
gas chromatographic/mass spectrometric sniffing system.
Purge and trap techniques were used to introduce the
volatile, off-flavour components into the gas
chromatograph. 16 refs.
FINLAND; SCANDINAVIA; SWEDEN; WESTERN EUROPE
Accession no.686400
Item 308
Polymer
39, No.19, 1998, p.4665-73
SURFACE GLASS TRANSITION BEHAVIOUR
OF AMORPHOUS POLYMER FILM BY
SCANNING FORCE MICROSCOPY AND
SURFACE SPECTROSCOPY
Kakiyama T; Tanaka K; Takahara A
Kyushu,University
The surface molecular motion of amorphous polymeric
solids was measured by lateral force microscopy, scanning
viscoelasticity microscopy, and differential X-ray
photoelectron spectroscopy. Data are given for PS and
styrene-methyl methacrylate copolymers. 35 refs.
JAPAN
Accession no.686392
Item 309
73, No.487, Jan.1997, p.26-31
Spanish
TEMPERATURE MODULATED DIFFERENTIAL
SCANNING CALORIMETRY: A STEP FORWARD
IN STUDYING THE THERMAL PROPERTIES
OF POLYMERS
Perena J M
Instituto de Ciencia y Tecnologia de Polimeros
The principles of temperature modulated DSC are
described, and a number of examples are presented of its
application to studies of the thermal properties of plastics.
Some limitations of the technique are also examined. 6
refs.
WESTERN EUROPE
Accession no.686251
Item 310
70, No.13, 1st July 1998, p.456A-61A
CHARACTERISING SYNTHETIC POLYMERS
BY MALDI MS
Kuang Jen Wu; Odom R W
Evans C.,& Associates
An review is given of the use of matrix-assisted laser
desorption/ionisation time-of flight (MALDI TOF) mass
spectroscopy to determine MWDs and structures of
synthetic organic polymers, including the ion desorption
mechanism, synthetic polymer analysis, molecular weight
analysis, and its use in calibration of GPC profiles. 30
refs.
USA
Accession no.686157
Item 311
15, No.2, 1998, p.217-28
EFFECTS OF PACKAGING AND STORAGE
CONDITIONS ON VOLATILE COMPOUNDS IN
GAS-PACKED POULTRY MEAT
Eilamo M; Kinnunen A; Latva-Kala K; Ahvenainen R
VTT Biotechnology & Food Research;
Finland,Technical Research Centre
Volatile compounds released by raw chicken legs packed
in modified atmosphere packages were determined to
develop a spoilage indicator for monitoring the shelf life
of raw chicken. The effects of four packaging factors
(headspace volume, oxygen transmission rate of the
package, residual oxygen and carbon dioxide
concentration) and three storage factors (temperature,
illumination and storage time) on the amounts of volatile
compounds in the headspace of gas packages containing
two chicken legs were studied. Statistical experimental
design was applied and a linear screening design
comprising 18 experiments (fractional factorial) was
utilised. Volatile compounds in package headspace were
determined by gas chromatography/mass spectrometry.
The results were compared with the results of sensory
evaluation and microbial determinations. 8 refs.
FINLAND; SCANDINAVIA; WESTERN EUROPE
Accession no.686119
Item 312
International Journal of Adhesion & Adhesives
18, No.3, 1998, p.193-8
USE OF XPS AND TOF-SIMS TO INVESTIGATE
ADHESION FAILURE OF A CATIONIC
RADIATION CURED COATING ON
GALVANISED STEEL
Leadley S R; Watts J F; Rodriguez A; Lowe C
Surrey,University; Becker Industrial Coatings
Details are given of coating delamination in a hot, humid
environment for a cationic radiation cured coating of
cycloaliphatic epoxy resin. X-ray photoelectron
spectroscopy and time-of-flight mass spectroscopy of the
delaminated surface showed that the phosphorus
hexafluoride anion of the photoinitiator segregates to the
interface. The durability of the coating was improved by
reformulation with a reduced concentration of
photoinitiator. 7 refs.
WESTERN EUROPE
Accession no.684932
Item 313
Antec 98. Volume I. Conference proceedings.
METHODS FOR THE MEASUREMENT OF
CRYSTALLINITY OF PREFORMS AND
BOTTLES MADE FROM PETP
Bashir Z; Al-Alouish I; Al-Raqibah I; Ibrahim M
SABIC Corp.
(SPE)
PETP has established itself as a material for making
lightweight, clear and tough bottles. Ideally, a preform
with zero or very low crystallinity (for purposes of clarity)
is sought, while the final bottle should have high
crystallinity (for enhancing gas barrier and mechanical
properties). Monitoring crystallinity is thus important. An
attempt is made to evaluate methods of crystallinity
measurement using density, differential scanning
calorimetry and modulated differential scanning
calorimetry to study the crystallinity of preforms and
bottles. The applicability and appropriateness of each
technique for different PETP sample types, and
interpretation problems are also discussed. 20 refs.
SAUDI ARABIA
Accession no.684627
Item 314
30, No.5, 1998, p.439-43
DIRECT DETERMINATION OF MOLECULAR
WEIGHT DISTRIBUTION BY SIZE EXCLUSION
CHROMATOGRAPHY(SEC) WITH 750 MHZ
PROTON NMR DETECTION (ON-LINE SEC-
NMR)
Ute K; Niimi R; Hongo S; Hatada K
Osaka,University
The above on-line SEC-NMR technique was used to
analyse MWDs of isotactic PMMAs with Mn ranging
from 3270 to 22,200. The molec.wt. of the polymer in
flowing eluate was determined directly (without a
conventional calibration procedure) from he relative
intensity of NMR signals due to the end group and
repeating units. The MWD determined in this manner was
proved to be accurate by SEC-NMR experiments on
uniform isotactic PMMAs consisting of exactly 23, 40
and 80 repeating units. Investigation was also undertaken
to optimise flow rate and NMR parameters for quantitative
SEC-NMR measurements. The signal-to-noise ratio of
750 MHz SEC-NMR spectra was 9.2 times that obtained
previously with 500 MHz SEC-NMR operated under
similar conditions. 17 refs.
JAPAN
Accession no.684613
Item 315
Shawbury, Rapra Technology Ltd., 1996, pp.150.
95.00. 30cms. 9511
ENVIRONMENTAL STRESS CRACKING OF
PLASTICS
Wright D C
This book reviews the factors which influence
environmental stress cracking, and examines the current
state of knowledge regarding specific categories of
plastics. The book is divided into three main sections
focusing on the prediction of ESC and assessment by
testing, factors that influence ESC and data on specific
plastics. Methods for the experimental evaluation of
environmental stress are described. This book is
available for purchase from Publication Sales, Rapra
Technology Ltd.
Accession no.683806
Item 316
12, No.5, 1998, p.507-21
EFFECT OF CURING TEMPERATURE ON THE
ADHESION STRENGTH OF POLYAMIDEIMIDE/
COPPER JOINTS
Cho J H; Kong D I; Park C E; Jin M Y
Pohang,University of Science & Technology;
Korea,Research Institute of Chemical Technology
The adhesion strength of polyamideimide/copper joints
was investigated as a function of the curing temperature
and time. The effects of copper oxide formed by thermal
treatment and alkaline treatment on the adhesive strength
of the joints were examined. The locus of failure of the
joints was also studied by SEM and X-ray photoelectron
spectroscopy. 21 refs.
KOREA
Accession no.682955
Item 317
38, No.4, April 1998, p.566-72
DYNAMIC AND ISOTHERMAL
THERMOGRAVIMETRIC ANALYSIS OF A
POLYCYANURATE THERMOSETTING SYSTEM
Zacharia R E; Simon S L
Pittsburgh,University
Isothermal and dynamic thermogravimetric analysis
(TGA) were performed on a polycyanurate thermosetting
material. The effects on thermal stability of the copper
naphthenate catalyst were studied by comparing two
systems with different amounts of catalyst. Tests were
performed isothermally at temperatures ranging from 200-
240C for times up to one week. Dynamic tests were also
performed at rates of 0.1 C/min to 40 C/min at
temperatures ranging from 180 to 600C. Results
demonstrate the difficulties of extrapolating dynamic TGA
data to use conditions to predict long-term thermal
stability. 14 refs.
USA
Accession no.681689
Item 318
34, No.2, Feb.1998, p.163-70
STUDY OF TALC-ADDITIVE INTERACTIONS
BY COMBINED TGA-FTIR SYSTEM
Bertin D; Boutevin B; Rigal G; Fourty G
Montpellier,Ecole Nationale Superieure de Chimie;
Talcs de Luzenac SA
By using combined TGA/FTIR thermogravimetric
analysis, accurate real time qualitative and quantitative
data can be obtained for thermal decomposition of
polymers. It was used to study interactions between an
additive and a filler (talc), highlighting a degradation
phenomenon of additive by talc, and this phenomenon
depended on the structure and chemical composition of
talc. This procedure also applied to analysis of degradation
of other additives by talc. Thus, polymer formulations
will rapidly be optimised in various areas of filled
polymers. 12 refs.
WESTERN EUROPE
Accession no.681630
Item 319
Journal of Polymer Science : Polymer Chemistry
Edition
36, No.9, 15th July 1998, p.1363-71
MACROMOLECULES AT THE CRITICAL
ADSORPTION POINT. II. ROLE OF COLUMN
PACKING: BARE SILICA GEL
Berek D; Janco M; Meira G R
Slovak,Academy of Sciences; INTEC CONICET
Data are presented manifesting the role of column
packings from the point of view of both their pore size
and surface chemistry. Bare silica gels that are the most
commonly used LC CAP column packings and model
macromolecules, viz. narrow PMMA, were investigated.
20 refs.
ARGENTINA; SLOVAK REPUBLIC; SLOVAKIA
Accession no.681599
Item 320
20th Annual Anniversary Meeting of the Adhesion
Society. Conference proceedings.
Hilton Head Island, S.C., 23rd-26th Feb.1997, p.519-
21. 8(10)
USING XPS TO INVESTIGATE FIBRE/MATRIX
CHEMICAL INTERACTIONS AT THE
INTERFACE IN CARBON FIBRE REINFORCED
COMPOSITES
Weitzsacker C L; Xie M; Drzal L T
Michigan,State University
Edited by: Drzal L T; Schreiber H P
(US,Adhesion Society)
With composites expanding into areas from aerospace to
recreation, different matrices are being investigated to
tailor composites to specific uses. The degree of adhesion
between the fibre and matrix, influenced by chemical
reactions, mechanical interactions and topography at the
fibre/matrix interface, has been recognised as a critical
factor in determining the performance of fibre-reinforced
composites. The interaction and chemical reaction of
functional groups in the matrix with functional groups at
the fibrer surface contribute to the adhesion. Direct
analysis of the fibre/matrix interface by surface analytical
methods such as X-ray photoelectron spectroscopy is not
trivial due to the thickness of a matrix layer over fibres
and the complexity of the matrix system. Indirect analysis
of the matrix/fibre interface is possible using model
compounds which represent functional groups where
differences in results are indicative of reaction between
fibre and matrix. The matrix functional groups that may
chemically react with the fibre surface can be separated
and investigated individually. Mixtures of model
compounds can be used to investigate functional groups
reactions between the components, and with the fibre
surface. Model compounds based on epoxy, polyimide,
polyphenylene sulphide and vinyl ester matrices are
investigated to characterise the chemical reactions at the
fibre/matrix interface. XPS is used to characterise both
the carbon fibre surfaces and the reacted carbon fibre
surfaces. The model compounds representative of each
of these matrices demonstrate the range of possible
reactions and interactions possible between the fibre and
matrix, ranging from no reaction to distinct chemical
reactions. 4 refs.
USA
Accession no.681439
Item 321
Cleanrooms
12, No.5, Suppl. May 1998, p.S13/20
APPLICATION OF FTIR FOR MONITORING
CLEANROOM AIR AND PROCESS EMISSIONS
Zazzera L; Reagen W
3M Co.
The use of FTIR monitoring methods for HAP, VOC, PFC
and HFC emissions for identification and quantification
in process exhaust and in clean room air, is discussed. A
summary is included of the various protocols, test methods
and references for the use of FTIR spectroscopy to
generate verifiable data. Results of field trials and
laboratory study trials are presented, which demonstrate
its value as a monitoring method in the semiconductor
industry
USA
Accession no.679498
Item 322
70, No.8, 15th April 1998, p.1563-8
POLYMER ANALYSIS BY MICRO-SCALE SIZE-
EXCLUSION CHROMATOGRAPHY(SEC)/
MALDI TIME-OF-FLIGHT MASS
SPECTROMETRY WITH A ROBOTIC
INTERFACE
Nielen M W F
Akzo Nobel Central Research
A report is presented on the development of a micro-scale
SEC system in which the MALDI matrix solution is
coaxially added to the column effluent and directly spotted
onto the MALDI targets in a robotic interface. Each spot
corresponds to the 10-s elution window from the micro-
SEC column, thus yielding a narrow polymer distribution
which is amenable to characterisation by MALDI mass
spectroscopy. The performance of the system is
demonstrated by the characterisation of a polybisphenol
A carbonate and a complex dipropoxylated bisphenol A/
adipic acid/isophthalic acid copolyester resin. 29 refs.
Accession no.679150
Item 323
38, No.2, Feb.1998, p.265-73
DSC STUDIES ON THE CRYSTALLISATION
CHARACTERISTICS OF POLY(ETHYLENE
TEREPHTHALATE) FOR BLOW MOULDING
APPLICATIONS
Daw-Ming Fann; Huang S K; Jiunn-Yih Lee
Taiwan,National University of Science & Technology
The crystallisation behaviour of blow moulded PETP
bottles, which helps determine the products transparency,
was investigated by DSC dynamic cooling experiments
that simulated the cooling that occurs in the injection blow
moulding manufacturing process. DSC measurements
were used to obtain information on related aspects, such
as the ease of crystallisation from glassy and molten states
and crystallinity in the products. An Avrami equation was
used for calculation of the crystallisation kinetic
parameters. 40 refs.
TAIWAN
Accession no.678858
Item 324
TAPPI 1997 Polymers, Laminations and Coatings
Conference. Conference Proceedings. Book 1.
Toronto, Ontario, 24th-28th Aug.1997, p.173-82. 012
INFLUENCE OF MINERAL FILLERS ON THE
PROCESSING OF LLDPE FILMS
Ansari D M; Higgs R P
ECC International Ltd.
(TAPPI)
A study was made of the thermal properties and melt
rheology of linear LDPE masterbatches filled with
calcium carbonate, talc and calcined clay. Films were
prepared by extrusion blowing and temperature changes
were monitored along the bubble. Filler distribution within
the films was assessed by optical and electron microscopy.
Rheological properties of the diluted masterbatches were
evaluated over four decades of shear rate. The mineral
fillers increased cooling rates and improved bubble
stability. Coarser calcium carbonate grades gave the
greatest improvement, while fine grades and talc had little
effect. Micrographs revealed the level of interparticle
contact and alignment of anisotropic particles which gave
rise to the observed differences. Filler type and content
did not significantly influence shear rheology at the shear
rates associated with film extrusion. 17 refs.
CANADA; EUROPEAN COMMUNITY; EUROPEAN UNION;
UK; USA; WESTERN EUROPE
Accession no.677503
Item 325
TAPPI 1997 Polymers, Laminations and Coatings
Conference. Conference Proceedings. Book 1.
Toronto, Ontario, 24th-28th Aug.1997, p.35-44. 012
EFFECT OF TITANIUM DIOXIDE ON
EXTRUSION STABILITY
Merkley J H
Eastman Chemical Co.
(TAPPI)
Rheological techniques for following the degradation and
changes in molecular weight and MWD of titanium
dioxide-filled polyolefins during extrusion coating are
examined. These include measurements of the crossover
point between loss modulus and storage modulus and the
variation in complex viscosity versus frequency curves
seen in the rotational mechanical spectrometer curves,
variations in viscosity versus shear rate seen in the
capillary extrusion rheometer curves, and shifts in the
DMTA curves.
CANADA; USA
Accession no.677489
Item 326
Edition
36, No.5, 15th April 1998, p.851-60
PEROXIDE INDUCED CROSSLINKING AND
DEGRADATION OF PVC
Yu Q; Zhu S; Zhou W
McMaster University
Peroxide induced crosslinking and degradation of PVC
were investigated using an on-line ESR technique. The
reaction variables included temperature, peroxide type and
concentration. The mechanism involved in the reaction
was determined base on the radical information. The gel
content and swelling ratio were also measured. 38 refs.
CANADA
Accession no.674965
Item 327
Journal of Materials Science Letters
17, No.6, 15th March 1998, p.511-3
EVIDENCE OF MOLECULAR ORIENTATION IN
POLY(3-BUTYLTHIOPHENE) FILMS BY
ELECTRON SPIN RESONANCE
MEASUREMENTS
Pawlicka A; Walmsley L; Faria R M; Nascimento O R
Sao Paulo,University; Paulista,Universidade Estadual
It was demonstrated that ESR could show evidence of
molecular orientation in films of poly(3-butyl thiophene),
making ESR useful to study orientation in conjugated
polymers when it is wished to avoid radiation damage or
for a non-destructive investigation before X-ray
measurements. 11 refs.
BRAZIL
Accession no.674766
Item 328
Macromolecules
30, No.25, 15th Dec.1997, p.7970-6
DSC, FT-IR, AND ENERGY DISPERSIVE X-RAY
DIFFRACTION APPLIED TO THE STUDY OF
THE GLASS TRANSITION OF POLY(P-
PHENYLENE SULPHIDE)
Caminiti R; DIlario L; Martinelli A; Piozzi A; Sadun C
Roma,Universita La Sapienza; Roma,Istituto Nazionale
per la Fisica della Materia
The glass transition of PPS was studied by means of DSC,
FTIR spectroscopy and energy dispersive X-ray diffraction.
All of the techniques showed the alpha-transition of the
polymer. The results of the different techniques were
consistent if the onset temperature for the DSC experiments
was taken as representative of the glass transition. The glass
transition temperature was found to vary as a function of
the heating rate. The activation energy of the glass transition
process was calculated by means of a theoretical model.
The results were discussed. 47 refs.
WESTERN EUROPE
Accession no.672088
Item 329
Kunststoffe Plast Europe
88, No.2, Feb.1998, p.34-5
WHAT HAS GONE WRONG?
Sass A
NRW GmbH
Practical case studies are used to demonstrate how useful
differential scanning microscopy analysis can be for
material testing and damage analysis on plastics and plastic
parts. It measures the physical and chemical properties of
the plastic as a function of temperature. Information gained
by use of the analytical tool is examined, and case studies
relating to fluctuating material quality through the use of
recyclate, and the oxidation of PP water pipes are discussed.
WESTERN EUROPE
Accession no.671875
Item 330
Industrial & Engineering Chemistry Research
37, No.3, March 1998, p.1140-53
SHEATH-CORE DIFFERENCES CAUSED BY
RAPID THERMOOXIDATION DURING MELT
BLOWING OF FIBRES
Kelley S L; Shambaugh R L
Oklahoma,University
A technique based on intrinsic viscosity measurements
was developed for measuring sheath and core molecular
weights during melt blowing of fibres. A mathematical
model is described which accounts for rapid diffusion and
thermooxidation. Experimental molecular weight
measurements for PP fibres were compared with
theoretical predictions. 29 refs.
USA
Accession no.670584
Item 331
Polymer Bulletin
40, No.2-3, Feb./March 1998, p.227-34
COMPATIBILISATION OF POLYSULPHONE/
POLYAMIDE BLENDS BY REACTIVE
POLYSULPHONES. EVIDENCE FOR
COPOLYMER FORMATION
Weber M; Heckmann W
BASF AG
Melt blending studies using polysulphone with different
functional groups and polyamide were performed in a batch
type mixer. Blends were investigated by solvent extraction
and TEM. Model experiments revealed the possibility to
compatibilise these blends by reactive blending techniques
using functionalised polysulphones. 14 refs.
WESTERN EUROPE
Accession no.670478
Item 332
36, No.1, 15th Jan.1998, p.133-41
NEW APPROACH FOR ESTIMATING THE
RECRYSTALLISATION RATE AND
EQUILIBRIUM MELTING TEMPERATURE
Hong Gyun Kim; Robertson R E
Michigan,University
A method was described for measuring the heat and rate
of crystallisation following partial melting. The method
uses a specific sequence of temperatures with a differential
scanning calorimeter, and the melting and recrystallisation
processes were confirmed by optical observations. The
method was applied to poly(butylene terephthalate). The
melting temperatures obtained from recrystallisation were
used in the Hoffman-Weeks equation to deduce 236 C as
the equilibrium melting temperature for PBTP. 22 refs.
USA
Accession no.669994
Item 333
Composites Science & Technology
57, No.8, Aug.1997, p.975-83
EFFECTS OF SILANE COUPLING AGENTS ON
THE INTERPHASE AND PERFORMANCE OF
GLASS-FIBRE REINFORCED POLYMER
COMPOSITES
Wu H F; Dwight D W; Huff N T
A single filament model of a commercial glass fibre-
reinforcement manufacturing process was used to apply
methacryloxy and amino silanes with one, two and three
silanols to two different glass fibres in a molecular model.
Surface analyses by angular-dependent X-ray
photoelectron spectroscopy, electric-kinetic analysis, and
contact-angle measurements were used to characterise the
surface coatings. The micro-indentation technique was
used to evaluate fibre-matrix interfacial adhesion.
Changes observed in surface chemistry, micromechanics,
and composite properties as functions of silanol type are
correlated. Data includes molecular models of coupling
agent on E-glass surface, chemisorption of coupling agent
into glass surface, isoelectric point values for each
treatment, composite flexural strength, composite TS, and
composite interfacial shear strength before and after 3-
days in boiling water. Matrix was polyester resin (E-701
from Owens Corning). 22 refs. (Presented at 6th Int. Conf.
on Composite Interfaces, Microphenomena in Advanced
Interfaces, Zichron Yaacov, Israel, 5th-8th May 1996).
USA
Accession no.669950
Item 334
Polymer Bulletin
39, No.6, Dec.1997, p.721-7
COMPARISON OF CALIBRATION WITH PPG
AND PS STANDARDS IN SIZE EXCLUSION
CHROMATOGRAPHY MEASUREMENTS FOR
CHARACTERISATION OF OLIGOLACTONE
MACROMONOMERS
Schoch M; Gopp U; Steurich S; Sandner B
Halle,Martin-Luther-Universitat
The calibration of size exclusion chromatography
measurements for the determination of the molecular
weights of oligolactone macromonomers was carried out
using PPG and PS as standards. Results are compared
with those obtained by end-group analysis with proton
NMR14 refs.
WESTERN EUROPE
Accession no.669429
Item 335
70, No.1, 1st Jan.1998, p.131-5
USE OF MALDI-TOF TO MEASURE
MOLECULAR WEIGHT DISTRIBUTIONS OF
POLYDISPERSE POLYMETHYL
METHACRYLATE
Rashidzadeh H; Baochuan Guo
Cleveland,State University
Using PMMA samples, some of the causes of mass
discrimination encountered in the MALDI-TOF analysis
of polydisperse polymers were investigated. It was found
that detector saturation could be a major instrumental
factor causing mass discrimination. This was due to the
strong signals of matrix-related ions and low-mass
oligomer ions. The matrix effect as another source of mass
discrimination was analysed quantitatively. 34 refs.
USA
Accession no.666829
Item 336
Polymer
39, Nos.6-7, 1998, p.1439-43
TEMPERATURE MODULATED DSC STUDY OF
POLYETHYLENE TEREPHTHALATE
CRYSTALLIZATION. II. APPLICABILITY TO
NON-ISOTHERMAL PROCESS
Toda A; Tomita C; Hikosaka M; Saruyama Y
Hiroshima,University; Kyoto,Institute of Technology
The non-isothermal crystallisation of PETP was examined
by temp. modulated DSC(TMDSC). A new analytical
model of TMDSC was applied to the process, taking
account of the response of exothermic heat flow to temp.
modulation in an apparent heat capacity of complex
quantity. By examining the frequency dependence of the
apparent heat capacity, the applicability was successfully
examined for the non-isothermal process. The method was
capable of determining the temp. dependence of crystal
growth rate from TMDSC data analysis. The results were
in good agreement with the dependence determined from
literature values of spherulite growth rate measured by
optical microscopy. 12 refs.
JAPAN
Accession no.666765
Item 337
29, No.11, 1997, p.910-3
FRACTIONATION OF PEO STAR SAMPLES BY
SUPERCRITICAL FLUIDS
Cansell F; Botella P; Six J-L; Garrabos Y; Tufeu R;
Gnanou Y
CNRS
Details are given of the use of supercritical fluids for the
fractionation of PEO. The fractionation of a binary mixture
of star and linear chains of PEO was studied. 25 refs.
WESTERN EUROPE
Accession no.666545
Item 338
Polymer
39, No.2, 1998, p.255-66
INVESTIGATION OF PHYSICAL AGEING IN
POLYMETHYLMETHACRYLATE USING
POSITRON ANNIHILATION, DIELECTRIC
RELAXATION AND DYNAMIC MECHANICAL
THERMAL ANALYSIS
Davis W J; Pethrick R A
Strathclyde,University
Physical ageing of PMMA was studied using positron
annihilation lifetime spectroscopy (PALS), dielectric
relaxation spectroscopy (DRS) and dynamic mechanical
thermal analysis (DMTA) and the results obtained from
these techniques were compared. A correlation existed
between the free volume as measured by PALS and the
changes which occurred in the DRS and DMTA data. It
was concluded that thermorheologically simplicity was
probably an oversimplification for this system and that
physical ageing was associated with a redistribution, not
just a shift, of molecular relaxation processes. The
relaxation distribution changed as the glass transition
temperature was approached. The free volume distribution
probably changed during ageing, but it was not possible
to quantify these changes from the PALS study. 43 refs.
WESTERN EUROPE
Accession no.665913
Item 339
67, No.3, 18th Jan.1998, p.487-500
SURFACE ENERGY MAPPING OF KEVLAR
FIBRES BY INVERSE GAS
CHROMATOGRAPHY
Rebouillat S; Donnet J B; Guo H; Wang T K
Du Pont (UK) Ltd.; Ecole Nationale Superieure de
Chimie de Mulhouse
The surface energy characteristics of three Kevlar fibres
were systematically studied using two inverse gas
chromatography (IGC) techniques, i.e. at an infinite probe
dilution and at a finite probe concentration, with the latter
allowing a unique mapping of the surface energy levels,
which complements greatly the more traditional
characterisation of the highest energy sites. The standard
thermodynamic parameters, such as the free energy and
the adsorption enthalpy and entropy, as well as the
dispersive and the specific component of the fibre surface
energy, were determined from the retention behaviour at
zero coverage of selected molecules of various polarity.
Using the second IGC approach, i.e. at finite
concentration, the isotherms for the adsorption of n-octane
and n-hexylamine on the three selected Kevlar fibres were
constructed by the one peak method. 29 refs.
WESTERN EUROPE
Accession no.665736
Item 340
67, No.3, 18th Jan.1998, p.449-53
COMPATIBILITY STUDY OF
POLYCARBONATE-POLYVINYL
PYRROLIDONE BLEND USING HIGH
RESOLUTION SOLID STATE NUCLEAR
MAGNETIC RESONANCE
da Silva E P; Tavares M I B
Rio de Janeiro,Universidade Estadual do Norte
Fluminense; Rio de Janeiro,Universidade Federal
The combining NMR techniques in the solid state permit
the evaluation of the polymeric systems homogeneity. In
polycarbonate-polyvinyl pyrrolidone blends, the response
of proton spin-lattice relaxation time in the rotating frame
was the determinant to obtain information on the transition
when the quantity of polyvinyl pyrrolidone is close to 40
wt% and a better organisation of amorphous phase was
detected. 13 refs.
BRAZIL
Accession no.665732
Item 341
51, No.12, Dec.1997, p.1823-5
INVESTIGATION OF CHEMICAL
INTERACTIONS AT THE STEEL/POLYMER
INTERFACE BY FT-IR DIFFUSE
REFLECTANCE SPECTROSCOPY
Bistac S; Vallat M F; Schultz J
Institut de Chimie des Surfaces et Interfaces
Interactions between a steel surface and an ethylene-vinyl
acetate copolymer grafted with maleic anhydride were
investigated by FTIR diffuse reflectance spectroscopy.
The failed surfaces obtained after a mechanical separation
of the polymer/steel assemblies were analysed. A two-
step mechanism was proposed: the opening of the
anhydride cycle by a hydrolysis reaction, leading to the
formation of a carboxylic diacid, followed by the reaction
of the acid with some oxidised metallic elements present
at the metal surface. This study underlines the contribution
of FTIR reflectance techniques to the understanding of
adhesion mechanisms. 7 refs.
WESTERN EUROPE
Accession no.665698
Item 342
51, No.12, Dec.1997, p.1784-90
DEPTH PROFILING STUDY OF EFFECT OF
ANNEALING TEMPERATURE ON POLYMER/
POLYMER INTERFACES IN LAMINATES
USING CONFOCAL RAMAN
MICROSPECTROSCOPY
Hajatdoost S; Olsthoorn M; Yarwood J
Sheffield,Hallam University; Utrecht,University
The effect of annealing temperature on molecular
interactions at the interface of polymer laminates was
reported. Depth profiling was carried out using confocal
Raman microspectroscopy to study polyacrylonitrile/
polyvinyl alcohol and polyacrylonitrile/polyacrylic acid
laminates. The laminates were annealed at 65, 75 and 90C.
It was demonstrated that the degree of hydrogen bonding
interaction between the nitrile and alcohol groups near
the interfacial region changes between laminates annealed
at different temperatures. For comparison, Raman
mapping of a polyacrylonitrile-polyvinyl alcohol blend
was used to study the interactions between the polymers
in this (disordered) system. 29 refs.
NETHERLANDS; UK; WESTERN EUROPE
Accession no.665697
Item 343
51, No.11, Nov.1997, p.1741-4
CHARACTERISATION OF DENTURE ACRYLIC
RESIN SURFACES MODIFIED BY GLOW
DISCHARGES
Suzer S; Ozden N; Akaltan F; Akovali G
Bilkent,University; Ankara,University; Middle
East,Technical University
Resin samples prepared by compression moulding using
a PMMA denture base material were exposed to radio
frequency glow discharges to improve the wettability of
the material. FTIR reflectance, X-ray photoelectron
spectroscopy and contact angle measurements were used
to characterise the changes introduced by the glow
discharge plasma. 18 refs.
TURKEY
Accession no.665695
Item 344
51, No.11, Nov.1997, p.1736-40
GENERALISED TWO-DIMENSIONAL FOURIER
TRANSFORM INFRARED PHOTOACOUSTIC
SPECTRAL DEPTH-PROFILING ANALYSIS
Jiang E Y; McCarthy W J; Drapcho D L; Crocombe R
A
Bio-Rad Laboratories Inc.
A new application of generalised two-dimensional
correlation spectroscopy in photoacoustic depth-profiling
analysis. Both rapid-scan and step-scan photoacoustic
spectroscopy (obtained by using the software-based
digital signal processing technique) of multilayer samples
were used to calculate generalised two-dimensional
correlation maps. Advantages of this unambiguous
analysis method in enhancing spectral as well as depth
resolutions, over conventional two-dimensional
correlation and other spectral depth-profiling methods,
were discussed. 31 refs.
USA
Accession no.665694
Item 345
51, No.11, Nov.1997, p.1668-77
RAPID-SCAN TWO-DIMENSIONAL FT-IR: AN
EFFICIENT APPROACH TO DYNAMIC
INFRARED SPECTROSCOPY
Steeman P A M
DSM Research
A new and efficient mode of operation is presented that
involves a continuous rapid-scan FTIR spectrometer, the
measurement technique relying completely on the
utilisation of the digital signal processor for data
acquisition and manipulation. Experimental and
mathematical details were discussed. Application of the
rapid-scan technique was illustrated with some results for
a styrene-acrylonitrile/butadiene copolymer. 17 refs.
Accession no.665692
Item 346
51, No.11, Nov.1997, p.1593-6
RAMAN IMAGING OF DENTAL ADHESIVE
DIFFUSION
Wieliczka D M; Kruger M B; Spencer P
Missouri,University
Using micro-Raman spectroscopy, chemical and
morphological information on the dentin/adhesive
interface was collected with minimal sample preparation.
Results provided direct evidence of an adhesive
preparation and demineralisation depth for two adhesive
systems. 17 refs.
USA
Accession no.665691
Item 347
Injection Molding
5, No.12, Dec. 1997, p.44-5
MATERIALS ANALYST: PART 3. LOT-TO-LOT
VARIATION
Sepe M
Dickten & Masch Mfg.Co.
The use is examined of thermogravimetric analysis as an
analytical tool for the diagnosis of part failure in injection
moulding. The consistent performance of an ethylene
vinyl acetate copolymer was evaluated and the need to
separate the component parts of the material to test for
the amount of vinyl acetate in the compound is discussed
in order to develop a thermal history. Once this history is
established, a customer can institute an incoming QC test
on the materials composition rather than by adjusting
the process for each new lot and performing product
testing after the parts have been produced.
USA
Accession no.664180
Item 348
57, No.3, 1997, p.313-24
THERMOANALYTICAL STUDY OF THE
EFFECT OF EAA AND STARCH ON THE
THERMOOXIDATIVE DEGRADATION OF
LDPE
Bikiaris D; Prinos J; Perrier C; Panayiotou C
Thessaloniki,University
The effect of ethylene-acrylic acid copolymer (EAA) and
plasticised starch (PLST) on the thermooxidative
degradation of LDPE was examined. The course of
oxidation was followed using TGA to monitor the weight
changes during heating and DSC to study the heat changes
taking place during oxidation. Three types of blend were
examined: LDPE-plasticised starch, LDPE-EAA and
LDPE-starch-EAA blends. All blends contained cobalt
stearate as prooxidant. 36 refs.
WESTERN EUROPE
Accession no.664073
Item 349
Pitture e Vernici
73, No.17, 1997, p.38-43
English; Italian
RELEASE OF VOLATILE DERIVATIVES FROM
INITIATORS IN RADIATION CURING
Visconti M; Cattaneo M; Li Bassi G
Lamberti SpA
Details are given of the development of a technique for
the direct evaluation of volatile organic compounds during
the radiation curing process. This method was used to
evaluate the release of benzaldehyde from commercially
available alpha-hydroxyketones during curing. 8 refs.
WESTERN EUROPE
Accession no.663242
Item 350
Iranian Journal of Polymer Science & Technology
10, No.2, Summer 1997, p.35-46
Persian
APPLICATIONS OF HIGH-RESOLUTION
SOLID-STATE CARBON 13 NMR
SPECTROSCOPY TO POLYMERS
Farahmand F G; Morshedian J
Iran,Polymer Research Centre
A brief review is given of the theory and applications of
carbon 13 NMR to polymer analysis. Mention is made of
conformational analysis, polymer reactions in solid state,
analysis of crosslinked systems, homogeneity of polymeric
blends, analysis of surface species, and variable temperature
carbon 13 NMR solid state spectroscopy. 37 refs.
IRAN
Accession no.663219
Item 351
69, No.23, 1st Dec.1997. p.4872-7
SAMPLE PRECONCENTRATION USING ION-
EXCHANGE POLYMER FILM FOR LASER
ABLATION SAMPLING INDUCTIVELY
COUPLED PLASMA ATOMIC EMISSION
SPECTROMETRY
Wing Tat Chan; Yip H H G
Hong Kong,University
An efficient sample pretreatment/introduction technique
for the inductively coupled plasma atomic emission
spectrometry (ICP-AES) using ion exchange for analyte
preconcentration and matrix separation and laser ablation
sampling for sample introduction was developed.
Ammonium pyrrolidone dithiocarbamate-PS films were
coated on glass plates for analyte preconcentration. 32 refs.
HONG KONG
Accession no.662915
Item 352
Pigment & Resin Technology
26, No.6, 1997, p.370-7
FTIR SPECTROSCOPY OF LAC RESIN AND ITS
DERIVATIVES
Sarkar P C; Shrivastava A K
Indian Council of Agricultural Research; Ranchi
College
Fourier transform infrared spectroscopy was applied to
the study of lac resin, a complex natural resin of insect
origin, and some of its derivatives. The results obtained
by this method are compared with those from earlier
studies that used classical methods of chemical analysis.
Experiments include the preparation of hard and soft
resins, dewaxed lac, ammoniated lac, lac acetal,
halogenated lac, hydrolysed lac, rebuilt lac (rebulac), and
the preparation of lac metal salts. It is found that FTIR
has several advantages over classical methods, but that
FTIR data requires supplementing by other instrumental
techniques such as FT-Raman spectroscopy and solid state
nuclear magnetic resonance. 21 refs.
INDIA
Accession no.662758
Item 353
Journal of Vinyl and Additive Technology
3, No.3, Sept.1997, p.249-55
PRACTICAL GUIDE TO THE IDENTIFICATION
OF MONOMERIC PLASTICIZERS IN
FLEXIBLE PVC COMPOUNDS
Kozlowski R R; Gallagher T K
Aristech Chemical
The performance of a flexible PVC compound is often
defined by its plasticiser content and composition and a
simple, accurate and fast method of plasticiser
identification could, therefore, be an effective quality
control and benchmark performance test in new product
development studies. Gas chromatography was shown to
provide the most effective identification method and it
was demonstrated that it could be complemented by IR
spectroscopy, liquid chromatography and physical
observations to confirm identity. 4 refs.
USA
Accession no.661993
Item 354
Macromolecules
30, No.21, 20th Oct.1997, p.6674-6
HIGH-RESOLUTION CALORIMETRY STUDY
OF THE ORDER-DISORDER TRANSITION IN A
DIBLOCK COPOLYMER MELT
Voronov V P; Buleiko V M; Podneks V E; Hamley I W;
Fairclough J P A; Ryan A J; Mai S M; Liao B X; Booth C
Russian Academy of Sciences; Leeds,University;
UMIST; Manchester,University
A new method is reported for locating the order-disorder
transition in a diblock copolymer, namely high-resolution
calorimetry, and the result compared with determinations
by small-angle X-ray spectroscopy and rheology. 13 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; RUSSIA; UK;
WESTERN EUROPE
Accession no.658801
Item 355
Polymer Science Series A
39, No.8, Aug.1997, p.953-7
STUDY OF SOLUBLE POLYAMIC ACIDS AND
POLYESTER IMIDES BY METHODS OF
EXCLUSION LIQUID CHROMATOGRAPHY
Nesterov V V; Kudrysvtsev V V; Svetlichnyi V M;
Gazdina N V; Belnikevich N G; Kurenbin O I;
Zhukova T I
St.Petersburg,Institute of Macromol.Compounds
The molecular and conformation characteristics of a series
of polyamic acids and polyester imides, obtained by high-
temp. imidisation of polyamic acids in N-
methylpyrrolidinone or m-cresol, were studied by
viscometry and exclusion liquid chromatography. The
differences in the molec.wts. of the products of polyamic
acid imidisation in N-methylpyrrolidinone and m-cresol
were explained by the different characters of inactivation
of the anhydride groups. 20 refs. (Full translation of
Vys.Soed.A, 39, No.8, 1997, p.1387-91)
RUSSIA
Accession no.658622
Item 356
Macromolecules
30, No.18, 8th Sept.1997, p.5285-9
FURTHER APPLICATION OF A PROCEDURE
FOR MOLECULAR WEIGHT AND
MOLECULAR WEIGHT DISTRIBUTION
MEASUREMENT OF POLYDISPERSE
POLYMERS FROM THEIR MATRIX-ASSISTED
LASER DESORPTION/IONISATION TIME-OF-
FLIGHT MASS SPECTRA
Vitalini D; Mineo P; Scamporrino E
Istituto per la Chimica e la Tecnol.dei Mat.Pol.;
Catania,Universita
A recently reported off-line procedure to estimate
molecular weight averages and MWD index, also for
polydisperse polymers, directly from their matrix-assisted
laser desorption/ionisation time-of-flight mass spectra
(MALDI-TOF) was applied to poly(bisphenol A-
carbonate), a poly(ether-sulphone resin) and
poly(dimethylphenylene oxide), all having a wide
polydispersity index. The molecular weight and MWD
obtained values were compared with those determined
by GPC or supplied by makers. A structural
characterisation of these polymers was also performed
by examining their MALDI-TOF mass spectra. 29 refs.
WESTERN EUROPE
Accession no.657168
Item 357
Injection Molding
5, No.10, Oct. 1997, p.60/2
MATERIALS ANALYST: PART 2. BRITTLE PPO
Sepe M
The use is described of differential scanning spectroscopy
(DSC) as an analytical tool in the diagnosis of part failure.
Degradation of the polymer during processing is
examined, and the example is investigated of a 30% glass
reinforced PPO which showed brittleness and for which
the causes of failure were revealed by means of DSC
analysis.
USA
Accession no.655661
Item 358
Vol.119, July 1997, p.317-24
CHEMICAL ANALYSIS OF POLYMERS USING
TRANSMISSION ELECTRON MICROSCOPY/
ELECTRON ENERGY-LOSS SPECTROSCOPY:
THE EXAMPLE OF POLY(ETHYLENE
TEREPHTHALATE)
Varlot K; Martin J M; Quet C; Kihn Y
Lyon,Ecole Centrale; CEMES-LOE
Electron energy-loss spectroscopy analysis of PETP was
performed in the analytical TEM to evaluate the
possibility of chemical analysis of the polymer at sub-
micrometre scale. Due to irradiation damage, it was
necessary to work at the lowest possible electron dose,
and with the specimen cooled to liquid nitrogen
temperature. In the acquired spectra, an identification of
the different chemical bondings in agreement with X-ray
absorption near-edge spectroscopy experiments is
proposed. 14 refs.
WESTERN EUROPE
Accession no.653745
Item 359
Vol.119, July 1997, p.309-15
CARBON-13, MAGNESIUM-25 AND BORON-11
SOLID STATE NMR STUDY OF A FIRE
RETARDED ETHYLENE-VINYL ACETATE
COPOLYMER
Pecoul N; Bourbigot S; Revel B
Ecole Nationale Superieure de Chimie de Lille; Centre
Commun de Mesures RMN
Flame retardance of ethylene-vinyl acetate copolymer can
be achieved using magnesium hydroxide incorporated in
the polymeric matrix. The adduct of a small amount of
zinc borate as synergistic agent in the formulation
increases the fire-proofing properties. Multinuclei solid-
state NMR appears as a means to characterise materials
before and after combustion. It was shown that
endothermic dehydration, water vapour evolved and
formation of a glassy coating provided the flame
retardancy of interest to the polymer matrix. 12 refs.
WESTERN EUROPE
Accession no.653744
Item 360
Vol.119, July 1997, p.269-76
QUANTITATIVE ATR-FTIR SPECTROSCOPY AT
POLYMER SURFACES: SORPTION AND
MOLECULAR CONFORMATION
Mueller M; Schmitt F J
Dresden,Institute of Polymer Research
Adsorption and diffusion phenomena at or within polymer
systems were investigated by surface sensitive ATR-FTIR
spectroscopy. For a systematic description, a study was
made of (1) the competitive adsorption and desorption
behaviour of proteins on polymer surfaces, (2) swelling
of hydrophilic polymers by water molecules, which can
be accompanied by conformational changes, and (3)
induced orientational changes of hydrophobically
modified polypeptides by apolar solvents. 10 refs.
WESTERN EUROPE
Accession no.653740
Item 361
Vol.119, July 1997, p.227-34
INELASTIC NEUTRON SCATTERING STUDIES
OF POLYETHYLENE AND N-ALKANES
Parker S F
Rutherford Appleton Laboratory
High quality inelastic neutron scattering (INS) spectra of
randomly oriented polycrystalline PE, polydeutero-
polyethylene and highly oriented polyethylene are
presented and a number of new features described. 9 refs.
WESTERN EUROPE
Accession no.653736
Item 362
Vol.119, July 1997, p.157-64
INFRARED ABSORPTION SPECTRA OF
POLYMERS FROM CLASSICAL MOLECULAR
SIMULATION
Soldera A; Dognon J P
CEA/Le Ripault
A method is proposed to predict the IR spectra of
amorphous polymers. Based on classical molecular
simulation and Kramers-Kronig relations, it allows the
computations of absorption and transmittance spectra of
polymer films in near and middle infra-red domains with
good agreement with experimental data. 22 refs.
WESTERN EUROPE
Accession no.653730
Item 363
Vol.119, July 1997, p.79-87
CREEP RATE SPECTROSCOPY USING A LASER
INTERFEROMETER AS ULTRA-HIGH
RESOLUTION TECHNIQUE FOR STUDY OF
RELAXATIONS
Peschanskaya N N; Yakushev P N; Sinani A B;
Bershtein V A
Russian Academy of Sciences
An original laser interferometry creep rate spectroscopy
(CRS) method was developed and used as the low-
frequency and high-resolution technique for studying
microplasticity and relaxations in different materials
including brittle ones. New possibilities for CRS for
polymers are demonstrated. 13 refs.
RUSSIA
Accession no.653722
Item 364
Vol.119, July 1997, p.49-63
POTENTIAL OF TWO-DIMENSIONAL NEAR-
INFRARED CORRELATION SPECTROSCOPY
IN STUDIES OF PRE-MELTING BEHAVIOUR OF
NYLON 12
Ozaki Y; Yongliang Liu; Noda I
Kwansei-Gakuin,University; Procter & Gamble Co.
This review paper discusses the potential of generalised
two-dimensional near-infrared correlation spectroscopy
in studies of pre-melting behaviour and hydrogen bonds
of nylon 12. A study on dissociation and hydrogen bonds
of N-methylacetamide is also reviewed as a model
compound study of nylon 12. FTIR spectra were measured
over a temperature range of 30-150C where gradual
weakening of inter- or intramolecular associative
interactions and decrease of local order leading to the
eventual fusion of nylon 12 crystals are observed. 24 refs.
JAPAN; USA
Accession no.653720
Item 365
Vol.119, July 1997, p.25-48
UNDERSTANDING POLYMERS BY
VIBRATIONAL SPECTROSCOPY: SOME
RECENT ADVANCES IN THEORY AND
EXPERIMENT
Meier R J
DSM Research
A rapid scan version of two-dimensional spectroscopy is
introduced and applied to study the phases of an
acrylonitrile-butadiene-styrene polymer system. Some
recent advances in the application of computational
chemistry to the evaluation of vibrational spectra are
presented. Some specific applications are discussed. 31 refs.
Accession no.653719
Item 366
International Journal of Polymer Analysis and
Characterization
3, No.4, 1997, p.369-79
HPLC QUANTIFICATION OF THIOETHER
ANTIOXIDANTS IN POLYETHYLENE AFTER
DISSOLUTION OF POLYMER UNDER
PRESSURE IN ALIPHATIC SOLVENT
Macko T; Furtner B; Lederer K
Leoben,Montan-Universitat
A new method is described for the quantitative
determination of some sulphur-containing antioxidants in
PE. The polymer matrix is dissolved in hot n-heptane/
isopropyl alcohol, 97/3 v/v at 160 deg.C under elevated
pressure (0.33 MPa) and precipitated by cooling. The
solution is injected directly into a normal-phase silica gel
column flushed with the same solvent as used for the
dissolution of the polymer. This method gives high recovery
of the antioxidants, good repeatability of the analysis and
a low detection limit of 0.011 mg 4,4'-thiobis(3-methyl-6-
tert-butylphenol) (Santonox R) /1 g PE; 0.074 mg
ditetradecyl-beta,beta-thiodipropionate (Chimox 14) / 1
g PE; and 0.125 mg dioctadecyl-beta,beta-thiodipropionate
(Irganox PS 802) /1 g PE. 23 refs.
Accession no.653220
Item 367
Vol.118, June 1997, p.383-8
FREE VOLUME STUDIES IN MISCIBLE
POLYMER BLEND SYSTEMS
Campbell J A; Goodwin A A; Ardi M S; Simon G P;
Landry-Coltrain C J T
Monash,University; Eastman Kodak Co.
A brief review is presented of the published literature
relating to the use of positron annihilation lifetime
spectroscopy in studying the effects of miscibility on the
free volume of miscible, amorphous polymer blends.
Studies of a fully miscible polyvinyl phenol/PVAC blend,
a partially miscible polyphenyl methacrylate/
polycarbonate blend and a largely immiscible PS/PVAC
blend are reported. The results indicate that miscible
blends tend to show a negative deviation of free volume
size, and to a lesser degree free volume fraction, on mixing
due to the intimacy of packing of the blend component
macromolecules. The largely immiscible blend shows
positive deviation of free volume size which is ascribed
to additional free volume at the interface. 13 refs.
AUSTRALIA; USA
Accession no.652994
Item 368
Edition
35, No.12, 15th Sept.1997, p.2431-9
ESR STUDY ON CHEMICAL CROSSLINKING
REACTION MECHANISMS OF PE USING A
CHEMICAL AGENT. II. EFFECT OF PHENOLIC
ANTIOXIDANTS
Yamazaki T; Seguchi T
Hitachi Cable Ltd.; Japan,Atomic Energy Research
Institute
The effect of antioxidant on the reaction mechanism of
chemical crosslinking of PE with dicumyl peroxide at high
temperatures was investigated by ESR. The antioxidant
reacted with the alkyl radicals in PE formed by the thermal
decomposition of dicumyl peroxide above 120C and
disturbed the crosslinking. 10 refs.
JAPAN
Accession no.652659
Item 369
51, No.8, Aug.1997, p.1176-8
QUANTITATION OF POLYETHYLENE GLYCOL
CONCENTRATION USING RAMAN
SPECTROSCOPY
Melendez Y; Schrum K F; Ben-Amotz D
Purdue,University; Maryville College
Raman spectroscopy is used to quantitate the amount of
polymer in solution, in particular polyethylene glycol
dissolved in chloroform. For various chain lengths and
polymer weight fraction ranges, it is shown that the ratios
of peak intensifies in the C-H stretching region may be
used to quantitate polymer weight fraction with about 1%
uncertainty. For low polymer weight fraction ranges (0-
10%), the relationship between Raman intensity and
polymer weight fraction is essentially linear, while at
higher ranges (0-50%) the intensity follows a nonlinear
function derived from basic concentration relationships
and indicates a universal scaling with polymer chain
length. 10 refs.
USA
Accession no.652414
Item 370
Polymer
38, No.17, 1997, p.4381-5
SEPARATION AND IDENTIFICATION OF
ETHYLENE-PROPYLENE BLOCK
COPOLYMER
Junting Xu; Linxian Feng; Shilin Yang; Yinan Wu;
Yiqing Yang; Xiangming Kong
Zhejiang,University; Shanghai,Research Institute of
Petrochemical Technology
A commercial impact resistant PP alloy was fractionated
using the temperature rising elution fractionation
technique and several ethylene-propylene block
copolymers with different ethylene contents were
obtained. The block structure of the fractions was
identified by combining the fractionation results with
carbon-13 NMR spectroscopy and DSC results. Some
transition segments were found between PE and PP
segments in the block copolymers. With increasing elution
temperature, the number and kind of transition segments
decreased, together with the length and melting
temperature of the PE segment in the block copolymer
fractions. 18 refs.
CHINA
Accession no.651909
Item 371
Analyst
122, No.8, Aug.1997, p.777-81
DETERMINATION OF FINISHING OILS IN
ACRYLIC FIBRES BY NEAR-INFRARED
REFLECTANCE SPECTROMETRY
Blanco M; Coello J; Fraga J M G; Iturriaga H;
Maspoch S; Pages J
Barcelona,Universidad Autonoma
The potential of near-infrared diffuse reflectance
spectrometry for quality control analyses in the textile
industry is explored with a view to the quantification of
finishing oils in acrylic fibres by partial least-squares
regression, using a rotary cuvette system for recording
spectra. Calibration is performed with a set of samples
that encompasses every source of variability, and the
wavelength region where absorption is mostly due to the
oil is used to construct several models from which that
leading to the minimum relative standard error for a
sample test set is selected. The results provided by various
mathematical treatments used to minimise scattering
resulting from the differential linear density of the samples
reveal no significant differences between prediction
errors. The model is used to quantify levels of finishing
oil in routinely manufactured samples for a period of six
months, during which time two batches show poor
predictions due to a new component appearing in the
product. Modification of the calibration model to account
for this component substantially increases robustness and
allows the accurate quantification of all batches
manufactured after the model is developed. 28 refs.
WESTERN EUROPE
Accession no.651451
Item 372
Analyst
122, No.9, Sept.1997, p.101R-15R
ANALYTICAL EXTRACTION OF ADDITIVES
FROM POLYMERS
Vandenberg H J; Clifford A A; Bartle K D; Carroll J;
Newton I; Garden L M; Dean J R; Costley C T
Leeds,University; ICI; Newcastle,University of
Northumbria
Plastics contain many other small molecules as well as
the polymer itself. These include additives to alter the
polymer properties or prolong the life of the polymer,
such as plasticisers, antioxidants and UV light absorbers.
There may also be processing aids, residual monomers,
low molecular weight oligomers and inadvertent
contaminants present. It is important for the manufacturer
and regulators to know the level of these materials in the
polymer to ensure the product is fit for its intended
purpose. Food contact plastics are regulated by maximum
concentrations allowable in the plastic, which applies to
residual monomers and processing aids as well as
additives. There are some methods for determining
concentrations of additives without extraction from the
polymer, such as nuclear magnetic resonance
spectrometry, UV spectrometry and UV desorption-mass
spectrometry. However, in order to determine the levels
in the polymer, it is usually necessary to extract the
compounds quantitatively from the plastic before analysis.
A review is presented of the available extraction
WESTERN EUROPE
Accession no.651430
Item 373
69, No.16, 15th Aug.1997, p.3304-13
QUANTITATIVE ANALYSIS OF PESTICIDES IN
POST-CONSUMER RECYCLED PLASTICS
USING OFF-LINE SUPERCRITICAL FLUID
EXTRACTION(SFE)/GAS
CHROMATOGRAPHY-ECD
Nerin C; Batlle R; Cacho J
Zaragoza,University
The SFE of several organochlorine and organophosphorus
pesticides and two metabolites from recycled plastics was
studied. The recycled plastics, used as agricultural soil covers,
were a mixture of LDPE and EVA. The SFE was optimised
and compared with the classical sonication and total
dissolution extraction methods. The plastic was extracted
with supercritical carbon dioxide under different extraction
conditions, depending on the physical matrix characteristics.
Average recoveries of the eleven chemicals studied ranged
from values greater than 90% with an overall relative
standard deviation of 4.3% for plastics films to values lower
than 40% with an overall standard deviation of 7.2% for
plastics pellets. The variables affecting the whole extraction
process and the results obtained in the comparison between
the three extraction methods are discussed. 45 refs.
WESTERN EUROPE
Accession no.650545
Item 374
33, No.7, July 1997, p.1135-42
FOURIER TRANSFORM INFRARED
SPECTROSCOPY APPLIED TO THE STUDY OF
PVC DECOMPOSITION
Beltran M; Marcilla A
Alicante,Universidad
The process of PVC decomposition was studied by FTIR
under dynamic conditions. The IR spectra were directly
obtained from PVC films pyrolysed in-situ in a specially
designed infra red cell. A qualitative description of the
changes observed in the spectra was presented. 35 refs.
WESTERN EUROPE
Accession no.650382
Item 375
Vol.118, June 1997, p.261-5
HIGH PERFORMANCE LIQUID
CHROMATOGRAPHY CHARACTERIZATION
OF MACROMOLECULES
Chang T; Lee H C; Lee W
Pohang,University of Science & Technology
A new chromatographic method for polymer molecular
weight characterisation, temperature gradient interaction
chromatography, is described. Fine and reproducible
control of interaction between polymer chains and the
alkyl chain bonded silica packing material can be achieved
by varying the column temperature. The method can be
used to characterise binary polymer mixtures, where one
component is separated by the size exclusion mechanism
and the other is simultaneously separated by the
interaction mechanism in a single isocratic elution. The
application of this technique to the characterisation of PS
and PS/PMMA mixtures is examined. 12 refs.
KOREA
Accession no.649987
Item 376
Macromolecules
30, No.13, 30th June 1997, p.3781-7
CHARACTERISATION OF POLYESTERS BY
MATRIX-ASSISTED LASER DESORPTION
IONISATION MASS SPECTROMETRY
Williams J B; Gusev A I; Hercules D M
Pittsburgh,University
A series of aliphatic polyesters, characterised by
asymmetric oligomer distributions, heteroterminated linear
chains, and cyclic oligomers, were studied using MALDI.
Structural characterisation results were compared with
those from fast atom bombardment mass spectrometry,
electrospray ionisation mass spectrometry, NMR and end-
group titration. MALDI molecular weight determination
was contrasted with those from GPC and NMR. 23 refs.
USA
Accession no.649761
Item 377
Shawbury, Rapra Technology Ltd., 1997, pp.120. 12
ins. 15/4/97. Rapra Review Rept. No.95, vol.8, No. 11
1997,
THERMAL ANALYSIS OF POLYMERS
Sepe M P
Dickten & Masch Mfg.Co.
Edited by: Dolbey R
Rapra Review Report No.95
A review is presented of the techniques involved in the
thermal analysis of polymers. Techniques discussed
include differential scanning calorimetry, differential
photocalorimetry, thermogravimetric analysis,
thermomechanical analysis, dynamic mechanical analysis,
dielectric, thermally stimulated current/relaxation map
analysis analysis, and thermal conductivity analysis. 381
refs.
WESTERN EUROPE
Accession no.647258
Item 378
65, No.3, 18th July 1997, p.595-600
MOLECULAR WEIGHT OF POLYETHYLENE
GLYCOLS BY VAPOR PRESSURE
OSMOMETRY: AN ALTERNATIVE DATA
TREATMENT
Sabadini E; Assano E M; Atvars T D Z
Campinas,Universidade Estadual
The number-average molec.wt. of some polyethylene
glycols was analysed using vapour pressure osmometry.
This technique generally worked with a plot of the
difference in electrical resistance/concentration versus
concentration and the molec.wt. was determined by the
calibration constant obtained from the curve intercept. It
was demonstrated that this method induced a high
dispersion of the data, which could be minimised using a
plot of difference in electrical resistance versus
concentration.. More precise values of molec.wt. could
thus be obtained and the number-average molec.wt. of
several polyethylene glycols could be directly obtained
from the ratio between the curve slopes obtained for a
standard and the polymer sample. 10 refs.
BRAZIL
Accession no.645677
Item 379
Speciality Chemicals
17, No.5, June/July 1997, p.165/70
MAKING LIQUID CHROMATOGRAPHY MORE
ACCESSIBLE
Kuehler T C; Sellen M; Lavold T; Batt J; Langridge J;
Raso R; Rontree J A
Astra Hassle AB; Micromass AB; Micromass UK Ltd.
Until recently, mass spectrometry was regarded as a highly
sophisticated technique requiring careful use of the
instrument by a sole operator, and demanding meticulous
sample preparation by the chemist. However, moves
towards open-access, chemist-operated systems have been
reported on mass spectrometers equipped with a variety
of ionisation modes. The reliability and robustness of
atmospheric pressure ionisation, the ease and speed of
source tuning, the fact that it is unnecessary to optimise
the source conditions for each sample individually and
the reproducibility of results have made API techniques
the ionisation methods of choice. Details are given. 5 refs.
SCANDINAVIA; SWEDEN; UK; WESTERN EUROPE
Accession no.645281
Item 380
57, No.2, 1997, p.135-49
THERMAL DEGRADATION KINETICS OF
POLYPROPYLENE. III.
THERMOGRAVIMETRIC ANALYSIS
Chan J H; Balke S T
Toronto,University
Thermogravimetric data were obtained for the pyrolysis
of polypropylene, and several previously published
interpretation methods were applied to the data. The wide
temperature range used in this work (45-580C)
encompassed a change in the decomposition mechanism
and this greatly limited the utility of the methods. To
accommodate this mechanism change, the data were
treated as a pseudo-first order reaction. The lower
activation energy occurring at lower degradation
temperatures was attributed to scission of the weak links
in the polymer. The higher activation energy was similar
to the carbon-carbon dissociation energy and was
associated with random scission throughout the polymer.
47 refs.
CANADA
Accession no.645116
Item 381
57, No.2, 1997, p.113-25
THERMAL DEGRADATION KINETICS OF
POLYPROPYLENE. I. MOLECULAR WEIGHT
DISTRIBUTION
Chan J H; Balke S T
Toronto,University
A kinetic model for the thermal degradation of PP was
developed and fitted to MWD data obtained by high
temperature size exclusion chromatography. In a series
of ampoule experiments, reaction temperatures of 275-
315C were examined with reaction times of up to 48 h. A
single-parameter version of the model, containing an
apparent rate constant, was found to provide excellent
fits of all MWDs. Values of the parameter varied with
both temperature and reaction time. 35 refs.
CANADA
Accession no.645114
Item 382
69, No.13, 1st July 1997, p.2485-95
MASS SPECTROMETRIC INVERSE GAS
CHROMATOGRAPHY: INVESTIGATION OF
POLYMERIC PHASE TRANSITIONS
Panda S; Bu Q; Huang B; Edwards R R; Liao Q; Yun K
S; Parcher J F
Mississippi,University
An improved inverse gas chromatographic method
involving the use of a mass-specific detector for
determination of the Tg of polymeric materials is
described. This new method allows the use of several
probe solutes simultaneously with an automated, closed-
loop injector and stepped temperature programming. The
result is a single continuous chromatogram for each probe
solute over a range of temperatures encompassing the Tg.
Several different methods for the exact determination of
Tg from the chromatogram were investigated. Two new
methods were also proposed for the evaluation of Tg from
either the temperature dependence of the second moments
of the elution peaks for probe solutes or simple inspection
of the variation of elution peak height (width) with
temperature. 51 refs.
USA
Accession no.645093
Item 383
69, No.12, 15th June 1997, p.15R-28R
COATINGS
Anderson D G
Witco Corp.
A review is presented of analytical techniques applicable
to the examination of coatings, raw materials and
substrates since 1995. The most highly referenced areas
were found to be IR spectroscopy, NMR, HPLC, thermal
analysis and gas chromatography. 704 refs.
USA
Accession no.640310
Item 384
Polymer Bulletin
38, No.6, June 1997, p.681-8
SEPARATION OF BLOCK COPOLYMERS FROM
PARENT HOMOPOLYMERS BY MEANS OF
CRITICAL ADSORPTION POINT
Janco M; Berek D; Onen A; Fischer C H; Yagci Y;
Schnabel W
Slovak Academy of Sciences; Istanbul,Technical
University; Hahn-Meitner-Institut Berlin GmbH
The principle underlying the above method is described
and results of its application to block copolymers
consisting of methyl methacrylate and tetrahydrofuran
blocks are presented and discussed. The technique is
shown to be suitable for characterisation of block
copolymers with regard to the presence of homopolymer
and multiblock (triblock) fractions. 5 refs.
SLOVAK REPUBLIC; SLOVAKIA; TURKEY; WESTERN
EUROPE
Accession no.640169
Item 385
Antec 97. Volume III. Conference proceedings.
Toronto,27th April-2nd May 1997,p.3588-92. 012
FOURIER TRANSFORM INFRARED MICRO
SPECTROSCOPY MAPPING. APPLICATIONS
TO VINYL SIDING INDUSTRY
Garcia D; Black J
Elf Atochem North America Inc.
(SPE)
Fourier transform IR (FTIR) spectroscopy is a powerful
analytical technique capable of yielding high quality
information with a spacial resolution as low as 10 microns.
When coupled with an automated mapping stage, it can
offer unique evaluation capabilities. A number of
applications of FTIR spectroscopy mapping to the vinyl
siding industry are described. Examples focus on
determining, in single sample mapping experiments, the
compositional changes associated with capstock to
substrate transition and evaluating the degradation species
and level observed during weathering exposure
throughout the thickness of the siding panel. 4 refs.
USA
Accession no.639927
Item 386
Toronto, 27th April-2nd May 1997, p.2310-4. 012
QUANTITATIVE ANALYSIS OF LDPE/LLDPE
BLEND USING DSC AND FTIR METHODS
Prasad A; Mowery D
Quantum Chemical Co.
(SPE)
A blend of LDPE and LLDPE is widely used for blown
film applications. For quality control an accurate and rapid
method is required to identify the type and composition
of alpha-olefin in an LDPE/LLDPE blend. A rapid,
accurate and new test method is developed which utilises
DSC and FTIR techniques. The melting point of LDPE
varies with density and usually is in the range of 106 deg.C
to 112 deg.C for film grade resins. The DSC thermogram
of LLDPE is characterised by a broad range of melting
with a lower melting peak around 106 deg.C to 110 deg.C
and a higher one in the range of 120 deg.C to 124 deg.C.
In the blend with LDPE, the ratio of the two endothermic
peak heights changes. At a given weight percent of LDPE,
this ratio depends on the type of LLDPE. The separate
calibrations for butene-1, hexene-1, and octene-1 LLDPEs
are developed to quantify the blend composition from
DSC thermograms provided the alpha-olefin type is
identified by a rapid method such as FTIR. 17 refs.
USA
Accession no.638387
Item 387
Shawbury, Rapra Technology Ltd., 1992, pp.112. 12ins.
30/6/97. Rapra Review Rept. No.61, Vol.6, No.1, 1992.
FOOD CONTACT POLYMERIC MATERIALS
Sidwell J
Edited by: Dolbey R
Rapra Review Report No.61
A review is presented of the current and proposed
European legislation on materials in contact with food,
as well as the latest technological advances. With
reference to legislation, details are given of EC directives
issued, their implementation, FDA regulations, recycling
and waste management legislation. Technical
developments in food contact materials cover barrier
polymers in multilayer packaging films, migration of
species from food contact materials, and methods of
analysis of multilayer food contact materials. 485 refs.
WESTERN EUROPE
Accession no.637749
Item 388
Polymer
38, No.12, 1997, p.3035-43
CHARACTERIZATION OF POLYETHYLENE
TEREPHTHALATE AND POLYETHYLENE
TEREPHTHALATE BLENDS
Fox B; Moad G; van Diepen G; Willing I; Cook W D
CSIRO,Div.of Chemicals & Polymers;
Monash,University
A method was developed for direct determination of the
molec.wt. of the PETP component in PETP/ABS blends
by GPC. The technique was used to demonstrate that an
observed deterioration in the mechanical properties, e.g.
Izod impact strength, of PETP/ABS blends on processing
could be correlated with a decrease in the molec.wt. of
the PETP component. Various methods for evaluating the
molec.wt. and the chemical microstructure of PETP were
examined. The use of NMR spectroscopy as a means of
quantitatively identifying end groups and comonomers
that were present at the 1-4% level in commercial PETP
was critically evaluated with reference to the stability of
PETP and PETP end groups in various NMR solvents.
New proton NMR chemical shift assignments for
cyclohexanedimethanol units are presented and the
reactivity of hydroxy end groups in trifluoroacetic acid
mixtures is examined. 34 refs.
AUSTRALIA
Accession no.636573
Item 389
Polymer Testing
16, No.2, 1997, p.193-8
NMR CARBON-13 HIGH RESOLUTION STUDY
OF POLY(ETHYLENE-CO-VINYL ACETATE)
Stael G C; Tavares M I B
CCT/UENF
EVA was analysed by carbon-13 high-resolution using
NMR employing solution and solid state techniques. The
analyses of this copolymer by solution NMR permitted
the copolymer composition to be obtained, and using
solid-state NMR, a study of molecular mobility was
carried out. Both studies were made to correlate the
structure and properties. 9 refs.
BRAZIL
Accession no.634101
Item 390
Trends in Polymer Science
5, No.3, March 1997, p.97-102
CHARACTERISATION OF POLYMER BLENDS
BY INVERSE GAS CHROMATOGRAPHY
Al-Saigh Z Y
Ohio,State University
A brief review is presented of the use of inverse gas
chromatography to characterise polymer blends.
Comparisons between data from inverse gas
chromatography and DSC are discussed. 23 refs.
USA
Accession no.632110
Item 391
Polymer News
22, No.1, Jan.1997, p.15
POLYMER ANALYSIS AND
CHARACTERISATION. SOLID STATE NMR: IS
IT BECOME TRULY POPULAR?
Garbassi F
EniChem SpA
A very brief review is presented of specific areas where
solid state NMR can contribute to polymer analysis.
Mention is made of polymer morphology, interactions,
dynamics and polymer reactions. 10 refs.
WESTERN EUROPE
Accession no.632071
Item 392
69, No.4, 15th Feb.1997, p.618-22
COMPOSITION AND MICROSTRUCTURE
ANALYSIS OF CHLORINATED
POLYETHYLENE BY PYROLYSIS GAS
CHROMATOGRAPHY AND PYROLYSIS GAS
CHROMATOGRAPHY/MASS SPECTROMETRY
Cheng-Yu Wang F; Smith P B
Dow Chemical Co.
A pyrolysis gas chromatography method was developed
to determine the composition and microstructure of
chlorinated PE (CPE). The method used specific aromatic
compounds which were formed through
dehydrochlorination of trimers after pyrolysis of CPE
polymers at elevated temperatures. The composition and
microstructure calculation was based on the difference
between the levels of ethylene and vinyl chloride trimers
formed. The composition of CPE polymers used in this
study was corroborated with carbon-13 NMR results and
the manufacturers product specification. 23 refs.
USA
Accession no.629089
Item 393
Biomaterials
18, No.5, March 1997, p.415-9
DETECTION OF PEROXY SPECIES IN ULTRA-
HIGH MOLECULAR WEIGHT
POLYETHYLENE BY RAMAN SPECTROSCOPY
Chenery D H
Smith & Nephew Group Research Centre
Samples of gamma-sterilised UHMWPE were examined
using infra-red and Raman spectroscopies. The purpose
of this study was to detect the peroxy intermediates by
the novel use of Raman spectroscopy to confirm that
oxidation proceeded by this mechanism. 16 refs.
WESTERN EUROPE
Accession no.625483
Item 394
Polymer
38, No.1, 1997, p.1-7
CALORIMETRY: 6. THERMAL
CHARACTERISATION OF MULTICOMPONENT
POLYMERS AND INTERFACES
Hourston D J; Song M; Hammiche A; Pollock H M;
Reading M
Loughborough,University of Technology;
Lancaster,University; ICI Paints
A quantitative thermal method, based on the differential
of heat capacity signal from modulated temperature
differential scanning calorimetry, was described for
determining the weight fraction of interface and the extent
of phase separation in polymer materials. The interface
was modelled as discrete fractions, each with its own
characteristic increment of heat capacity. The materials
used to demonstrate the range of the method were PS
blended with poly(phenylene oxide) (PPO), pure PS, pure
PPO, a styrene-isoprene-styrene triblock copolymer (SIS),
SIS blended with PPO, PMMA/poly(vinyl acetate) blends
and PVC sandwiched with poly(n-butyl acrylate). Two-
phase and four-phase systems were used. The calculated
results agreed well with experimental results for two- and
four-phase systems. 20 refs.
WESTERN EUROPE
Accession no.621625
Item 395
69, No.1, 1st Jan.1997, p.66-71
CRITICAL CONDITION USING ENHANCED-
FLUIDITY LIQUID MOBILE PHASES
Souvignet I; Olesik S V
Ohio,State University
The use of enhanced-fluidity liquid mixtures of THF and
carbon dioxide for liquid chromatography at the critical
condition was examined. For PS polymers, the molec.wt.
range that could be analysed at the critical condition was
compared for THF/carbon dioxide and other common liquid
mixtures. As enhanced-fluid liquids were highly
compressible, it was possible to reach the critical condition
by changing the pressure of the THF/carbon dioxide
mixture. Approaching the critical condition by pressure
variation was compared with that possible with temp.
changes. Pressure variation was a more accurate and
reproducible means of reaching the critical condition than
temp. variation. Finally, THF/carbon dioxide mixtures were
used as mobile phases at the critical condition for PS to
characterise styrene-methyl acrylate copolymers. 25 refs.
USA
Accession no.620015
Item 396
Shawbury, Rapra Technology Ltd., 1995, pp.108. 12ins.
18/7/95. Rapra Review Rept. Vol.7, No.11, 1995,
MOLECULAR WEIGHT CHARACTERISATION
OF SYNTHETIC POLYMERS
Holding S R; Meeham E
Rapra Technology Ltd.; Polymer Laboratories Ltd.
Edited by: Dolbey R
Rapra Review Report No. 83
Techniques are examined for the determination of the
molecular weight distribution and molecular weight averages
of synthetic polymers. The use is discussed of gel permeation
chromatography in combination with other techniques such
as light scattering and viscometry to provide information
about the molec.wt. of a polymer and potentially significant
information on the composition of copolymers and blends.
The use of solution viscosity is also examined as a valuable
quality control technique. 411 refs.
WESTERN EUROPE
Accession no.556661
Item 397
60,No.9,1st May 1988,p.932-7
IDENTIFICATION OF DYES IN SOLID
POLYMETHYL METHACRYLATE BY MEANS
OF LASER DESORPTION FOURIER
TRANSFORM ION CYCLOTRON RESONANCE
MASS SPECTROMETRY
Hsu A T;Marshall A G
OHIO STATE,UNIVERSITY
It is demonstrated that the above technique can detect and
identify (by chemical formulae) dyes in solid PMMA
commercial plastics at concentrations at least on order of
magnitude lower (0.1% vs 1-2wt%) than those obtained
by the best currently-available alternative method (ATR
Fourier transform IR spectrometry). Both untreated and
redissolved PMMA can be characterised, in the presence
and absence of up to three dyes in a single sample. 44 refs.
USA
Accession no.357996
Item 398
Oxford, Pergamon Press Ltd., 1984, pp.ix,445.
LS.24.50. 9ins. 2copies. 12/7/85. Analytical Chemistry
Vol.8. 91T
ANALYSIS OF PLASTICS
Crompton T R
This book covers all aspects of the analysis of plastics by
chemical and physical methods. It is divided into eight
chapters which each deal with a particular polymer or
group of polymers:- polyolefins, polypropylene, higher
alkene polymers, styrene polymers, chlorine-containing
polymers, methacrylates, polybutadienes, polyesters and
polyethers. The techniques discussed include
spectroscopy, chromatography, fractionation,, X-ray
diffraction, autoradiography, DTA, TGA and DSC.
UK
Accession no.280400
Item 399
Weinheim, Verlag Chemie GmbH, 1981, pp.XV,687.
12ins. 22/3/82. R.ROOM. 91T
ATLAS OF POLYMER AND PLASTICS
ANALYSIS. VOL.3....ADDITIVES AND
PROCESSING AIDS: SPECTRA AND METHODS
OF IDENTIFICATION. 2ND REV.EDN.
Scholl F
The spectroscopic and chromatographic data that are
required for the identification of plastics additives and
processing aids are presented. Over 1300 IR spectra and
60 UV spectra are included. The functions and
compositions as well as the physical and chemical
methods of identification of the following materials are
discussed: plasticisers, fillers, pigments, antioxidants, UV
stabilisers, optical brighteners, antistatic agents,
biostabilisers, flame retardants, lubricants, accelerators,
hardeners and blowing agents. 608 refs.
Accession no.211056
Item 400
Members Rept.49 Shawbury, 1980, pp.12. 12ins.
2copies. 26/6/80. 91T
CHROMATOGRAPHY - ANALYTICAL
APPLICATIONS IN THE RUBBER AND
PLASTICS INDUSTRIES
Sidwell J A
Rubber & Plastics Research Assn.of Gt.Britain
RUBBER & PLASTICS RA.MEMBERS REPT.049
This report details some of the high-performance liquid
chromatography work carried out at RAPRA and reviews
reported in the literature. 11 refs.
RUBBER & PLASTICS RESEARCH ASSN.OF
GT.BRITAIN
Accession no.154074
Subject Index
Subject Index
A
ABS, 160 164 207 225 345 365 388
398
ABSORPTION, 56 226 297 306 374
382
ABSORPTION SPECTRA, 274
ABSORPTION SPECTROSCOPY,
358 362
ACCELERATOR, 399
ACCURACY, 131
ACETIC ACID, 76 266
ACETONE, 185 224 266 311
ACETONITRILE, 21 266
ACID, 277 288
ACOUSTIC MICROSCOPY, 126
ACRYLATE, 269
ACRYLIC, 199
ACRYLIC ACID COPOLYMER,
172 217 348
ACRYLIC POLYMER, 33 172 255
299 314 335 371 384 397
ACRYLIC-MELAMINE RESIN, 44
175
ACRYLONITRILE, 119
ACRYLONITRILE COPOLYMER,
57
ACRYLONITRILE-STYRENE
COPOLYMER, 72 110 220 345
ACTIVATION ENERGIES, 49 75
146 169 280 288 317 328 380
381
ADDITIVE, 29 36 71 89 99 107 108
112 124 128 132 151 161 171
178 181 199 201 206 225 226
250 272 288 289 302 306 318
324 325 353 366 372 377 387
391 397 399
ADHESION, 32 61 62 145 157 167
176 202 223 231 236 237 247
249 312 316 341 346
ADHESIVE, 9 20 62 167 168 179
272 346
ADSORPTION, 46 56 65 93 103
178 203 210 221 241 285 319
339 360 384
ADSORPTION
CHROMATOGRAPHY, 105 210
AEROPLANE, 36 62 121
AFFINITY CHROMATOGRAPHY,
50 97
AGEING, 66 80 86 88 112 148 152
274 288 298 309 338 377
ALCOHOL, 56 235 288
ALCOHOLYSIS, 39
ALKYD RESIN, 237
ALPHA TRANSITION, 245 290
328
ALUMINIUM, 126 168 179 223 266
ALUMINIUM HYDROXIDE, 211
ALUMINIUM OXIDE, 6
AMINE, 36 48 130 151 161 178 272
AMMONIUM PYRROLIDONE
DITHIOCARBAMATE, 351
AMMONIUM SALT, 258
AMORPHOUS, 14 54 74 78 99 117
141 170 207 213 274 283 340
362 367
ANISOTROPY, 13 256 324
ANNEALING, 24 54 74 101 135
136 277 308 338 342
ANTI-STICK AGENT, 6
ANTIMONY, 95
ANTIOXIDANT, 65 86 93 107 132
171 183 195 286 288 366 368
372 387 399
ANTISTATIC AGENT, 399
AQUEOUS, 46 198 223 232
ARAMID FIBRE, 281
AROMA, 56 57
AROMATIC, 48 125 192 278 288
299 392
ATMOSPHERIC PRESSURE, 50
206 222
ATOMIC ABSORPTION
SPECTROSCOPY, 177
ATOMIC EMISSION
SPECTROSCOPY, 95 177 218
273 351
ATOMIC FORCE MICROSCOPY,
30 38 44 58 59 62 108 115 118
142 145 154 167 179 191 219
277
ATTENUATED TOTAL
REFLECTANCE
SPECTROSCOPY, 43 61 69 126
257 262 301 360
AUGER ELECTRON
SPECTROSCOPY, 13
AUTOMATION, 46 50 212 278 382
AUTOMOTIVE APPLICATION, 44
56 62 67 175 202 212 236 329
AUTOOXIDATION, 169
B
BACKSCATTERED ELECTRON
IMAGING, 289
BAG, 266
BAGASSE, 100
BAND STRUCTURE, 262
BARIUM SULPHATE, 40
BARRIER PROPERTIES, 56 57 86
94 168 387
BENZENE, 382
BETA RELAXATION, 325
BIAXIALLY ORIENTED, 104
BIOCOMPATIBLE, 42
BIODEGRADABLE, 37 112 267
387
BIODETERIORATION, 5 37 112
246 267 387
BIOMATERIAL, 42 46 246 262
BIOMEDICAL APPLICATION,
262
BIREFRINGENCE, 257 284
BISPENTAMETHYLPIPERIDYL
SEBACATE, 66
BISPHENOL A, 200 222 272 356
BISPHENOL A COPOLYMER,
189
BISPHENOL A DIGLYCIDYL
ETHER, 178
BISPHENOL A EPOXY RESIN,
11
BISPHENOL A
POLYCARBONATE, 4 29 78
135 159 322 367
BISPHENOL DIGLYCIDYL
ETHER, 178
BLEND, 11 12 15 25 47 58 60 63
64 69 72 77 91 98 107 110 112
125 137 139 146 147 151 156
186 188 193 209 213 220 228
234 246 309 331 340 347 348
363 367 375 377 386 388 390
391 394
BLOCK COPOLYMER, 127 193
274 354 370 384 394
BLOW MOULDING, 313 323
BLOWING AGENT, 302 399
BLOWN FILM, 324 386
BODY ARMOUR, 281
BOILING POINT, 120 185 266
BONDING, 32 168 202
BONDING AGENT, 168 179
BONNET, 329
BOTTLE, 57 131 212 266 313 323
BOUND WATER, 51
BOUNDARY LAYER, 81
BRANCHING, 18 35 60 102 200
216
BRITTLE, 41 62 271 289 357 363
BROMINE CONTAINING
COPOLYMER, 273
Subject Index
BUCKET, 67
BUILDING APPLICATION, 7 385
BULK MOULDING
COMPOUND, 202
BUMPER, 67
BUTYL ACRYLATE
COPOLYMER, 28 198
BUTYL METHACRYLATE
COPOLYMER, 166 190
BUTYLENE COPOLYMER, 102
113
C
CALCINED CLAY, 324
CALCIUM CARBONATE, 65 211
289 324
CALCULATION, 8 14 77 98 114
149 162 172 190 227 276 277
285 290 310 323 328 330 337
344 362 382 390 392 394
CALIBRATION, 6 47 173 190 208
216 229 238 270 297 309 310
319 334 378 392
CALORIMETRY, 9 61 64 65 74 88
133 150 154 186 290 302 305
313 354 359
CAPILLARY
ELECTROPHORESIS, 46 50
97
CAPILLARY GAS
CHROMATOGRAPHY, 76
CAPILLARY RHEOMETRY, 324
325
CAR, 56 67
CARBON 13, 130 193 209 265
268 297 359 370 389 392
CARBON BLACK, 40 93
CARBON DIOXIDE, 57 298 301
311 373 395
CARBON DISULPHIDE, 311
CARBON FIBRE-REINFORCED
PLASTIC, 36 178 182 196 231
320
CARBONYL GROUP, 274 288
CARBOXYLIC ACID, 288 341
CASTING, 94 262 367
CELLULAR MATERIAL, 80 84
85 97 302
CELLULOSE, 43 82 263
CELLULOSE ACETATE, 79
CELLULOSE NITRATE, 46 79
185
CEMENT, 276
CHAIN LENGTH, 272 274
CHAIN SCISSION, 274 380
CHAR, 194
CHEMICAL BONDING, 358
CHEMICAL COMPOSITION, 25
72 80 89 103 107 146 159 172
197 198 211 213 229 232 289
318
CHEMICAL FORCE
MICROSCOPY, 58
CHEMICAL IONISATION MASS
SPECTROSCOPY, 222
CHEMICAL REAGENT, 53 334
CHEMICAL RECYCLING, 39
CHEMICAL RESISTANCE, 57
175
CHEMICAL STRUCTURE, 1 8 12
16 25 31 47 49 51 53 56 66 68
73 77 83 89 93 98 102 103 114
130 133 140 152 158 159 164
166 168 180 200 222 228 229
243 264 268 269 274 275 277
283 284 286 291 300 301 308
310 317 318 328 331 334 337
355 356 364 365 368 370 376
382 391
CHEMILUMINESCENCE, 88
CHEMOMETRIC ANALYSIS, 140
216
CHINA CLAY, 226 306
CHITIN, 246
CHLORINATED
POLYETHYLENE, 146 392
CHLORINE, 17 194 373
CHLORODIFLUOROETHANE,
337
CHLOROFORM, 3 208 369 382
CHROMATOGRAPHIC
ANALYSIS, 66 81 86 89 96 97
105 112 119 137 141 152 171
191 194 229 235 303 304 366
375 382 384
CHROMATOGRAPHY, 3 21 25 28
29 30 34 35 39 40 46 50 52 53
55 56 60 66 71 72 75 80 81 84
86 87 89 96 97 102 103 105
107 108 112 113 114 116 119
120 124 128 137 141 152 158
159 160 166 169 171 172 174
183 185 186 190 191 194 195
200 203 204 206 208 210 218
222 229 233 235 239 240 241
242 243 259 264 273 278 285
295 299 303 304 307 310 311
314 319 322 325 334 349 353
355 356 366 372 373 375 376
379 381 382 383 384 388 395
398 399
CHROMIC ACID, 61
CHROMOGEN, 16 288
CLAY, 324
CLEARCOAT, 27 44 175
CLOUD POINT, 12 98 125
COATED FIBRE, 179
COATED METAL, 157 227
COATING, 19 27 44 62 66 121 126
138 163 168 174 175 185 217
222 223 227 236 237 239 255
259 266 298 312 325 359 383
COBALT STEARATE, 348
COHESION, 94 145 167
COLOUR, 274 288
COLOURANT, 181
COLUMN CHROMATOGRAPHY,
233 375
COLUMN PACKING, 50 203 235
241 319 375
COMBUSTION, 359
COMPATIBILITY, 63 90 209 331
340
COMPLEX VISCOSITY, 325
COMPOSITE, 10 13 17 36 62 79
81 82 90 100 134 141 176 178
179 182 196 197 199 202 211
231 234 258 265 271 281 288
289 296 318 320 333 339 357
377
COMPOSITION, 72 73 100 122
123 130 220 241 243 389 392
394
COMPUTER AIDED ANALYSIS,
46 67 108 173 174 214 309
COMPUTER MODEL, 144 152
174 338
COMPUTER SIMULATION, 248
367
CONCENTRATION, 55 102 105
129 130 183 197 215 224 250
262 283 300 311 317 339 353
378
CONE CALORIMETER, 150 359
CONFOCAL RAMAN
MICROSPECTROSCOPY, 168
342
CONFORMATIONAL
ANALYSIS, 360
CONTACT ANGLE, 37 61 202
217 277 333 343
CONTACT LENS, 265
CONTAINER, 57 266 278
CONTAMINATION, 17 128 160
181 289 357
COOLING, 57 67 139 309 323 324
358
COOLING RATE, 57 126 207 309
323 324
COPOLYESTER, 204 322
COPOLYETHERSULPHONE, 47
COPOLYMER COMPOSITION,
28 57 70 94 198 210 220 370
Subject Index
COPPER, 61 316 317
CORONA TREATMENT, 205
CORRELATION
SPECTROSCOPY, 344 364
CORROSION, 255 271
CREEP RATE SPECTROSCOPY,
363
CRESOL, 355
CRITICAL CONCENTRATION,
241
CRITICAL POINT, 103 395
CRITICAL SOLUTION
TEMPERATURE, 125
CROSS-POLARISATION, 193 209
268 300
CROSSLINK, 83 279
CROSSLINK DENSITY, 179 269
CROSSLINKED, 110 179 221 250
CROSSLINKING, 9 10 20 24 27
36 46 48 49 73 85 115 134 161
180 187 265 272 279 288 294
300 309 326 368 377
CROSSLINKING AGENT, 222
288
CRYSTALLINE, 2 59 143 147 283
313
CRYSTALLINITY, 2 13 24 42 54
57 62 63 64 69 94 102 113 114
117 122 126 131 139 143 147
168 257 260 274 277 281 291
309 313 323 357 364 367 377
391
CRYSTALLISATION, 2 9 12 13
22 24 26 52 54 57 59 74 78 107
117 122 131 136 139 147 148
155 170 246 261 295 309 323
329 332 336 386
CRYSTALLISATION
TEMPERATURE, 136 309
CRYSTALLITE, 57 139 260
CURE TEMPERATURE, 2 48 161
CURE TIME, 36 265 309
CUREMETER, 134
CURING, 8 20 27 36 68 73 83 89
138 144 149 161 163 178 182
187 247 248 265 269 272 300
305 309 312 316 349 377
CURING AGENT, 36 151 161 178
182 222 250 272 288 317
CYCLOHEXANE, 21 263 285
D
DATA ANALYSIS, 13 216 237 267
291 319
DATA COLLECTION, 291 345
DEBONDING, 236
DECANE, 382
DEFECT, 67 88 126 289 329
DEFORMATION, 41 59 67 249
277 283
DEGRADABLE, 37 112 267 387
DEGRADATION, 4 16 39 44 58
65 66 80 85 86 87 88 92 94 101
112 119 135 148 152 164 175
183 189 194 195 213 228 244
258 266 267 274 279 288 294
298 302 309 311 318 325 326
330 338 347 357 374 377 380
385
DEGRADATION PRODUCT, 4 17
34 75 87 112 128 152 175 183
194 274 279 288
DEGRADATION
TEMPERATURE, 194 269 380
DEGREE OF BRANCHING, 18 35
DEGREE OF CROSSLINKING, 9
27 300 377
DEGREE OF CRYSTALLINITY,
143 313
DEGREE OF CURE, 10 36 269
DEHYDROCHLORINATION, 146
392
DELAMINATION, 255 312
DENSITY, 18 52 56 106 131 168
179 216 231 261 289 313 367
DENTAL APPLICATION, 172 247
276 343 346
DEPOLYMERISATION, 39 165
266
DEPTH PROFILING, 205 333 342
344
DERIVATIVE
THERMOGRAVIMETRY, 380
DESORPTION, 71 93 104 210 310
360
DETECTION LIMIT, 56 174 289
DIACID, 288 341
DIBUTYL PHTHALATE, 76
DIBUTYL SEBACATE, 277
DICHLOROXYLENE, 48
DICHROISM, 284
DICUMYL PEROXIDE, 368
DICYANATE POLYMER, 11
DIELECTRIC ANALYSIS, 9 377
DIELECTRIC CONSTANT, 46
237 338
DIELECTRIC PROPERTIES, 46
245 338
DIELECTRIC RELAXATION
338
DIELECTROMETRY, 9
DIETHYLENE GLYCOL, 26 121
266
DIFFERENTIAL
INTERFERENCE
MICROSCOPY, 324
DIFFERENTIAL
PHOTOCALORIMETRY, 377
CALORIMETRY, 2 6 7 8 10 11
12 15 17 18 20 22 24 29 36 41
51 54 56 63 64 65 74 77 78 83
85 88 94 95 98 101 110 113 114
122 125 126 131 133 134 135
136 139 144 146 147 149 154
155 161 163 164 170 186 187
207 211 213 220 245 246 252
253 254 258 261 267 269 276
277 280 282 287 290 291 296
302 305 309 313 323 324 328
329 332 336 348 357 367 370
377 382 386 387 390 394 398
DIFFERENTIAL THERMAL
ANALYSIS, 2 6 7 8 10 12 15
17 18 20 22 24 29 36 41 54 56
63 64 65 74 77 78 83 88 94 95
98 101 110 113 114 122 125
126 131 133 134 136 139 144
146 147 149 154 155 161 163
164 170 186 187 207 211 213
231 245 246 252 253 254 258
267 269 276 277 280 287 290
291 296 302 309 313 323 324
328 329 332 336 348 357 367
370 377 382 386 387 390 398
DIFFUSE REFLECTANCE
SPECTROSCOPY, 341
DIFFUSION, 9 56 80 99 124 125
264 274 346 351 360 372 387
394
DIFFUSION COEFFICIENT, 56
99 111 224
DIGITAL ANALYSIS, 10
DIGLYCIDYL ETHER
BISPHENOL A, 200
DIMETHYL FORMAMIDE, 21 77
DIMETHYL ISOPHTHALATE,
208
DIMETHYL SULPHOXIDE, 342
DIMETHYL TEREPHTHALATE,
39 208
DIPHENYLMETHANE
DIISOCYANATE, 9
DISCOLOURATION, 288
DISPERSION, 181 217 289 361
DISTILLED WATER, 56
DISTORTION, 20 260
DISTRIBUTION, 60 102 338
DOMESTIC APPLIANCE, 80
DOUGH MOULDING
COMPOUND, 211
DRAW RATIO, 117 257 283 284
Subject Index
DRINKING WATER, 183 307
DUCTILE FAILURE, 289
DYE, 16 397
DYNAMIC, 71 144 317 323 374
DYNAMIC DIFFERENTIAL
SCANNING CALORIMETRY,
11
DYNAMIC INFRARED
SPECTROSCOPY, 345
DYNAMIC LIGHT
SCATTERING, 111
DYNAMIC MECHANICAL
ANALYSIS, 36 56 73 83 92
114 134 161 196 245 269 309
377
DYNAMIC MECHANICAL
THERMAL ANALYSIS, 325
338 367
DYNAMIC PROPERTIES, 179
317 325
DYNAMIC SPECTROSCOPY,
345
DYNAMIC VISCOELASTIC
PROPERTIES, 101
E
ELECTRICAL CONDUCTIVITY,
38
ELECTRICAL INSULATOR, 271
ELECTRICAL PROPERTIES, 38
46 338 378
ELECTROCHEMICAL
IMPEDANCE
237 255
ELECTRODIALYSIS, 97
ELECTROKINETIC
CHROMATOGRAPHY, 46
ELECTROKINETIC
POTENTIAL, 333
ELECTRON DISPERSIVE X-RAY
ANALYSIS, 6
ELECTRON ENERGY LOSS
ELECTRON IONISATION MASS
SPECTROMETRY, 206
ELECTRON MICROSCOPY, 2 5
13 63 82 108 129 181 289 324
ELECTRON SCANNING
MICROSCOPY, 2 5 13 63 82
108 129 181
ELECTRON SPECTROSCOPY
FOR CHEMICAL ANALYSIS,
61
ELECTRON SPIN RESONANCE
326 327 368
ELECTRONIC APPLICATION, 5
ELECTROPHORESIS, 46 50 97
ELECTROSPRAY IONISATION,
190 222 229 376
ELEMENTAL ANALYSIS, 15 115
160 194 351
ELUENT, 203 235 375
ELUTION, 35 46 203 210 266 285
370 375 382
ELUTION CHROMATOGRAPHY,
50
ELUTION FRACTIONATION, 52
ELUTION VOLUME, 35 285 310
356
EMISSION, 56 87 174 321
END GROUP, 36 102 130 151 229
274 314
END-GROUP ANALYSIS, 190
200 334 376 388
ENDOTHERM, 54 56 74 78 94
125 136 139
ENDOTHERMIC, 235 245 276
309 329 359
ENERGY ABSORPTION, 207
ENERGY CONTENT, 357
ENERGY DISPERSIVE X-RAY
ANALYSIS, 108 129 289 328
ENGINEERING APPLICATION,
309 367
ENTHALPY, 36 64 74 125 179 187
276 282 309 339 354 375
ENTROPY, 339 375
ENVIRONMENTAL SCANNING
ELECTRON MICROSCOPY,
324
ENVIRONMENTAL STRESS
CRACKING, 315
EPICHLOROHYDRIN, 272
EPOXY NOVOLAC RESIN, 11
EPOXY RESIN, 10 11 20 32 36 47
62 68 144 145 149 151 157 161
178 179 182 199 200 222 249
255 269 272 282 292 305 309
312 320
EQUIPMENT, 6 46 138 194 197
218 309 335 379
ERROR ANALYSIS, 13
ETHANOL, 56 311
ETHERSULPHONE
COPOLYMER, 47
ETHYLENE ACRYLIC ACID
COPOLYMER, 51 348
ETHYLENE-BUTYLENE
COPOLYMER, 52
ETHYLENE CONTENT, 370 392
ETHYLENE COPOLYMER, 22 60
63 102 113 154 209 259 348
359 389
ETHYLENE GLYCOL, 39 266
ETHYLENE-HEXENE
COPOLYMER, 52
ETHYLENE-PROPYLENE
COPOLYMER, 69 274 370
ETHYLENE TEREPHTHALATE
COPOLYMER, 131
ETHYLENE-VINYL ACETATE
COPOLYMER, 57 70 100 209
226 251 270 306 341 347 359
373 389
ETHYLENE-VINYL ALCOHOL
COPOLYMER, 56 57 94 291
387
ETHYLIDENE VINYL
PYRROLIDONE, 250
EVANESCENT WAVE
EXCLUSION
34 35 40 41 50 52 55 60 97 102
103 108 112 114 116 158 166
204 210 229 239 240 243 299
314 322 334 355 375 381
EXOTHERM, 85 323
EXOTHERMIC, 54 276 309 329
336
EXTENDER, 121
EXTRACTION, 71 97 128 171 185
195 266 331 372 373
EXTRACTION
CHROMATOGRAPHY, 97
EXTRUSION, 6 7 40 70 72 183
188 195 225 254 266 324 325
F
FADING, 288
FAILURE, 17 30 36 167 178 182
254 271 289 296 341 347 357
FAILURE ANALYSIS, 36 108 145
167 254 289 329
FAST ATOM BOMBARDMENT
MASS SPECTROSCOPY, 376
FATTY ACID, 232
FIBRE, 31 33 43 82 100 178 179
182 231 256 260 330 339 371
FIBRE GLASS, 76 176 197
FIBRE OPTIC, 36
FIBRE-REINFORCED PLASTIC,
36 100 141 178 231 258 281
320
FIELD EMISSION SCANNING
TRANSMISSION ELECTRON
MICROSCOPY, 289
FIELD-FLOW
FRACTIONATION, 35 97
FILLED, 179 318 325
Subject Index
FILLER, 17 43 45 65 81 90 93 184
207 211 226 289 306 307 318
324 325 399
FILLER CONTENT, 81 90 324
FILLER DISTRIBUTION, 289 324
FILM, 1 3 16 27 37 38 40 41 49 56
57 61 62 65 86 92 102 104 106
115 117 118 135 142 148 156
167 168 186 205 246 257 262
266 269 288 289 308 324 327
349 351 362 373 374 386 387
FINITE ELEMENT ANALYSIS,
108
FIRE RETARDANT, 359
FLAME IONISATION, 185
FLAME RETARDANT, 95 152
211 218 273
FLAMMABILITY, 150 173 273
359
FLASH CHROMATOGRAPHY,
97
FLASH PYROLYSIS, 4
FLAVOUR, 183
FLEXIBLE, 84 277 283 353
FLOATATION, 97
FLOW INJECTION ANALYSIS,
50
FLOW MICROCALORIMETRY,
93
FLOW RATE, 50 143 233 324 372
FLUORESCENCE, 17 293
FLUORESCENCE
FLUOROPOLYMER, 279 387
FOAM, 80 84 97 302
FOOD-CONTACT
APPLICATION, 124 177 195
208 264 286 387
FOOD PACKAGING, 57 124 168
195 266 278 311
FORMULATION, 30 108 164 174
217 312
FOURIER TRANSFORM
INFRARED SPECTROSCOPY,
1 3 6 8 11 24 25 26 29 30 34 36
40 41 60 63 64 72 77 83 88 92
93 94 98 102 107 108 113 117
126 135 136 150 153 156 160
161 163 165 169 170 173 181
189 190 213 215 216 226 228
246 249 250 252 259 262 264
271 274 275 277 288 300 306
309 316 318 321 328 341 343
344 345 352 360 364 374 381
385 386 397
FRACTION, 35 170 204 394
FRACTIONATION, 28 52 97 107
113 337 370 398
FRACTURE, 67 82 98 178 236
271 289
FRACTURE MORPHOLOGY, 2
13 54 61 98 115 191 319 346
391 394
FREE ENERGY, 339
FREE RADICAL, 45 266
FREE VOLUME, 18 56 99 338
367 382
FREEZING POINT, 324
FREQUENCY, 78 118 179 255 256
287 309 325 336
FUEL TANK, 56
FUNCTIONAL GROUP, 36 83 274
331
FUNGUS, 5
FURAN RESIN, 199
FURNITURE, 274
G
GAMMA-IRRADIATION, 4 99
133 393
GAS, 67 80 277 311
GAS BARRIER, 56 57 168
GAS CHROMATOGRAPHY, 3 4
30 34 39 53 56 66 71 72 75 76
80 81 84 87 90 96 107 112 119
120 124 128 132 141 143 160
174 183 185 186 191 194 195
198 208 217 218 221 232 235
250 270 273 278 303 307 311
339 349 353 373 382 383 390
392 398
GAS DIFFUSION, 274
GAS LIQUID
CHROMATOGRAPHY, 97
GAS-PHASE, 67 80 277 311
GAS PIPE, 277
GAS TRANSMISSION, 311
GEL, 46 319 326
GEL ELECTROPHORESIS, 97
GEL PERMEATION
113 137 152 169 172 190 200
233 259 264 295 310 325 334
356 376 383 388 396 399
GELATION, 7 73 134 161 294
GLASS, 145 167 276 351
GLASS CONTENT, 296
GLASS FIBRE, 76 176 197
GLASS FIBRE-REINFORCED
PLASTIC, 17 179 202 211 231
271 288 296 333
GLASS TRANSITION
TEMPERATURE, 12 15 18 20
29 36 49 51 56 74 77 81 85 94
101 106 110 114 117 122 135
149 155 161 163 164 170 179
207 213 220 249 261 269 280
282 287 290 305 308 309 323
328 338 357 367 377 382 390
394
GLOW DISCHARGE, 343
GLOW DISCHARGE
SPECTROSCOPY, 202
GRAVIMETRIC ANALYSIS, 23
82 85 93 94 152 189 196 211
244 258 296 317 347 377 380
H
HEADSPACE ANALYSIS, 311
HEADSPACE
CHROMATOGRAPHY, 185
HEAT CAPACITY, 20 74 78 125
161 179 220 253 261 276 280
287 290 309 324 336 394
HEAT DEGRADATION, 23 26 29
75 76 83 152 160 163 189 192
194 196 244 266 273 318 325
380 381
HEAT FLOW, 36 155 245 252 261
276 309 324
HEAT INSULATION, 80 276
HEAT RESISTANCE, 11 24 26 57
85 126 163 196 228 266 267
269 295 317 377
HEAT STABILITY, 146 196
HEAT TREATMENT, 57 119
HEATING, 36 179 187 244 266
309 323 348 354
HEATING RATE, 36 54 144 179
309 328 332 348 380
HELIUM, 57
HETEROGENEITY, 25 217 268
HETEROGENEOUS, 129 146 170
HEXANE, 240 319
HIGH DENSITY
POLYETHYLENE, 52 56 57 63
87 91 102 109 112 128 132 143
164 195 212 214 307 357 372
392
HIGH IMPACT PS, 48
39 46 76 97 165 171 183 195
200 222 233 238 239 242 247
264 266 286 304 337 366 375
383 399 400
HIGH TEMPERATURE, 62 107
277 381
HIGH RESOLUTION, 179 209
289 340 354 363 389
HINDERED AMINE, 3 31 66 123
225
Subject Index
HINDERED PHENOL, 41
HIP JOINT, 42
HOMOGENEITY, 100 289 340
HOT STAGE MICROSCOPY, 2
181
HUMIDITY, 44 56 57 309
HYDROFLUOROCARBON, 321
HYDROGEN BONDING, 77 94
99 114 342 364
HYDROGEN CHLORIDE, 34 48
194 228
HYDROLYSIS, 34 58 59 165 319
341 352
HYDROPHILICITY, 46 51 360
HYDROPHOBICITY, 37 46 360
375
HYDROXYBENZENE, 75 297
300
HYDROXYETHYL
METHACRYLATE
COPOLYMER, 46
HYDROXYL GROUP, 36 69
I
IDENTIFICATION, 30 79 121 128
132 212 214 353 370 397
ILLUMINATION, 311
IMAGING, 13 67 88 168 179 275
289 346
IMIDAZOLE, 262
IMIDISATION, 8 355
IMMERSION, 178 223 237
IMMISCIBLE, 188 367 394
IMMUNOELECTROPHORESIS,
97
IMPACT PROPERTIES, 56 63 231
370 388
IMPLANT, 219 262 393
IMPURITY, 221
INDUCTION PERIOD, 41 88
INDUCTIVELY COUPLED
PLASMA SPECTROMETRY,
351
INELASTIC NEUTRON
SCATTERING, 361
INFRARED ABSORPTION, 36
274 362
INFRARED CAMERA, 67
INFRARED DICHROISM, 284
INFRARED SPECTROSCOPY, 1 3
8 11 14 17 24 26 29 33 34 36 39
41 43 51 60 63 66 69 72 77 79
85 88 92 93 94 98 108 113 126
135 142 150 153 156 160 161
163 164 165 169 172 173 181
184 186 188 189 207 215 216
225 226 228 230 244 246 249
250 256 257 259 262 264 269
271 274 275 277 284 294 297
301 306 316 318 321 328 341
343 344 345 353 360 362 364
365 371 374 381 383 385 386
387 393 399
INFRARED THERMOGRAPHY,
67
INJECTION MOULDING, 67 160
231 296 357
INK, 239
INSULATION, 80 276
INTERACTION, 90 167 178 235
249 285 311 318 341 342 364
INTERACTION PARAMETER,
220 235 285
INTERCHAIN PACKING, 135
INTERFACE, 178 179 182 206 229
236 322 341 342 346 367 394
INTERFACIAL ADHESION, 333
INTERFACIAL DEBONDING, 167
INTERFACIAL INTERACTION,
90 167 178
INTERFACIAL PROPERTIES, 81
90 111 141 167 178 249 320 342
INTERFEROMETRY, 13 275 363
INTERNAL MOULD RELEASE,
202
INTRINSIC VISCOSITY, 29 172
266 330
INVERSE GAS
141 143 191 217 235 339 382
390
ION CHROMATOGRAPHY, 97
218
ION CYCLOTRON RESONANCE,
397
ION EXCHANGE, 50 97 351
IONISATION, 46 50 206 222 379
IRON OXIDE, 112
IRRADIATION, 4 40 92 153 358
IRRADIATION DEGRADATION,
133
ISOELECTRIC POINT, 46 333
ISOMERISATION, 11 288
ISOPHORONE DIISOCYANATE,
121
ISOTACHOPHORESIS, 46
ISOTACTIC, 129 133 274 314
ISOTHERM, 67 178 309 339
ISOTHERMAL, 36 78 117 125 276
317 338 348 375
ISOTROPY, 117
K
KAOLIN, 226 306
KEVLAR, 191
KINETIC, 8 10 45 73 83 125 377
KINETICS, 3 23 52 73 75 94 144
149 302 317 323 332 363 380
381
L
LAC RESIN, 352
LACQUER, 185
LAMELLAE, 78 139
LAMINATE, 56 57 168 182 266
342
LAMINATED FILM, 57 168 266
293
LANGIVIN EQUATION, 3 46 50
60 75
LASER, 62 212 236 298 351 397
LASER INDUCED
DECOHESION
SPECTROSCOPY, 236
LASER INTERFEROMETRY, 363
LASER IONISATION MASS
SPECTROMETRY, 6
LASER LIGHT SCATTERING, 35
200
LASER RAMAN
SPECTROSCOPY, 168
LATERAL FORCE
MICROSCOPY, 308
LATEX, 46 156 174 193 198
LEACHING, 183
LEAD, 201
LEAST-SQUARES ANALYSIS,
70 214 345
LENS, 219 265
LIFETIME PREDICTION, 108
255 377
LIGHT ABSORPTION, 229 274
LIGHT DEGRADATION, 3 40 129
153 196 274 288
LIGHT MICROSCOPY, 181 295
LIGHT SCATTERING, 111 116
117 172 203 238 260 310 396
LIGHT STABILISER, 3 31 123
132 288
LIGHT STABILITY, 3 288
LIGNOCELLULOSE, 82
LINEAR LOW DENSITY
POLYETHYLENE, 57 92 107
139 186 216 225 324 386
LINEAR REGRESSION
ANALYSIS, 144
LIQUID CHROMATOGRAPHY,
21 25 35 39 46 50 55 76 97 103
105 108 124 159 165 171 183
195 200 203 206 210 222 229
233 238 239 240 241 242 243
Subject Index
247 264 266 285 286 299 304
319 337 353 355 366 375 379
383 384 395
LIQUID CRYSTAL POLYMER,
309 367 387
LIQUID NITROGEN, 358
LOW DENSITY
POLYETHYLENE, 3 57 86 87
139 143 164 168 186 207 214
266 324 325 348 372 373 386
LOW FREQUENCY, 126 363
LOW MOLECULAR WEIGHT,
128 375
M
MAGIC ANGLE, 209 268 283 291
300 340
MAGNESIUM-25, 359
MALDI-TOF SPECTROSCOPY,
28 103 127 137 158 159 166 204
310 322 335 356 376
MALEIC ANHYDRIDE, 82
MALEIC ANHYDRIDE
COPOLYMER, 28 341
MAPPING, 69 275 289 339 342
344
MASS SELECTIVE DETECTOR,
76 218
MASS SPECTROMETRY, 4 6 13
28 30 50 75 103 107 112 127
132 178 186 192 194 204 222
229 266 278 307 311 376 379
382 392 396 397 398
MASS SPECTROSCOPY, 28 66 72
84 86 103 121 124 127 128 137
153 158 159 166 177 185 190
195 202 204 206 244 250 270
273 303 310 312 322 335 356
376 399
MATRIX, 36 82 141 178 182 351
359
MATRIX-ASSISTED LASER
DESORPTION, 28 103 127 137
158 159 166 204 310 322 335
356 376
MDI, 9
MECHANICAL DEGRADATION,
266
MECHANICAL PROPERTIES, 9
40 41 56 61 62 63 65 67 82 84
86 91 114 115 126 151 163 168
178 179 182 207 231 249 256
269 271 277 281 288 289 296
309 315 316 324 325 333 353
365 370 388
MECHANICAL RECYCLING, 195
MECHANICAL SPECTROSCOPY,
325
MEDICAL APPLICATION, 42 262
MELAMINE-FORMALDEHYDE
RESIN, 159 365
MELT, 54 170 254 282 290 354
MELT TRANSITION, 267
MELTING, 2 24 54 78 79 136 155
179 209 252 309 332
MELTING POINT, 12 52 56 63 94
114 164 266 295 324
MELTING TEMPERATURE, 20 57
179 207 309 323 332 370
MEMBRANE OSMOMETRY, 396
METAL, 177 179 298 341
METAL ADHESION, 62 223 341
METAL COATING, 62 255
METAL SALT, 352
METALLISED FILM, 168 266 387
METHACRYLATE COPOLYMER,
190
METHACRYLIC ACID
METHACRYLIC ESTER
COPOLYMER, 190
METHACRYLIC ESTER
POLYMER, 45 245
METHANOL, 39 56 76 171 266
METHANOLYSIS, 39
METHYL ACETATE, 185
METHYL ACRYLATE
COPOLYMER, 33 172 299 395
METHYL ETHYL KETONE, 285
METHYL METHACRYLATE, 288
METHYL METHACRYLATE
COPOLYMER, 28 33 166 198
308 384
METHYLBENZENE, 56 185 241
261
METHYLENE CHLORIDE, 266
MICROANALYSIS, 179 231 289
MICROBIAL DEGRADATION, 5
MICROCALORIMETRY, 154
MICRODIELECTROMETRY, 9
MICROEXTRACTION, 71 185
MICRORAMAN
MICROSCOPY, 2 13 16 27 38 41
58 59 61 98 111 125 126 142
145 168 179 181 213 231 256
257 277 289 295 308 324 387
MICROSTRUCTURE, 13 58 60
168 170 198 274 370 388 392
MICROTOMY, 168
MICROWAVE, 112 128 262
MICROWAVEABLE, 266 387
MID-INFRARED
SPECTROSCOPY, 362
MIGRATION, 46 65 183 264 266
288 387
MINERAL FILLER, 45 288 289
324
MISCIBILITY, 12 64 77 98 125 146
209 213 220 309 367 390 391
394
MOBILE PHASE, 50 375 395
MODEL, 28 105 149 152 172 216
290 311 319 336 341 360 381
382 394
MODULATED DIFFERENTIAL
10 36 74 125 131 135 161 220
261 282 309 377 394
MODULATED TEMPERATURE
THERMOMECHANICAL
ANALYSIS, 20
MOISTURE CONTENT, 6 51 148
266 309
MOLAR MASS, 25 35 102 103 107
140 159
MOLECULAR
CONFIGURATION, 117 130
135 168 328 338 355 367
MOLECULAR INTERACTION,
178 220 342 375
MOLECULAR MOBILITY, 26 268
301 389
MOLECULAR ORIENTATION,
257 281 284 327 360
MOLECULAR STRUCTURE, 1 8
12 16 25 31 47 49 51 53 56 66
68 72 73 77 80 83 89 93 98 101
102 103 107 114 130 133 140
146 152 158 159 164 166 168
172 180 197 198 200 211 213
222 228 229 232 243 264 268
269 274 275 277 283 284 286
289 291 300 301 308 310 317
318 328 331 334 337 355 356
364 365 368 370 376 382 391
MOLECULAR WEIGHT, 1 28 29
42 46 50 52 54 55 62 73 89 102
112 113 114 116 120 127 128
130 158 164 166 172 185 190
200 204 210 222 224 235 239
243 285 310 314 319 322 323
325 330 332 334 337 355 356
375 376 378 381 382 388 395
396
MOLECULAR WEIGHT
DISTRIBUTION, 102 116 190
200 204 224 310 314 319 322
325 356 375 381 396
MONITORING, 5 70 149 174 188
223 261 272 298 311 321 348
MONOETHYLENE GLYCOL, 39
266
Subject Index
MONOMER, 124 229 269 270 387
MORPHOLOGY, 2 13 54 61 63 98
115 118 136 191 213 256 309
319 346 367 391 394
MOULDING, 134 225 343
MULTI-ANGLE LASER LIGHT
SCATTERING, 35 200
MULTILAYER, 168 266 344 387
MULTILAYER FILM, 57 168
MULTIPLE PULSE NMR, 291
MULTIVARIATE ANALYSIS, 216
MUNICIPAL WASTE, 128
N
N-METHYL-2-PYRROLIDONE,
355
NANOCOMPOSITE, 62
NAPHTHA, 215
NATURAL FIBRE, 82
NATURAL FIBRE-REINFORCED
PLASTIC, 141
NATURAL POLYMER, 232 352
NEAR-INFRARED
CORRELATION
SPECTROSCOPY, 364
NEAR-INFRARED
225 362 371
NITROCELLULOSE, 46 79 185
NITROGEN, 57 76 95
NITROGEN-CONTAINING
POLYMER, 250
NON-DESTRUCTIVE TEST, 19
32 67 106 126 157 327
NOVOLAC RESIN, 73 300
NUCLEAR MAGNETIC
RESONANCE, 1 22 28 30 31
32 34 57 60 68 73 77 100 108
113 114 123 130 138 148 162
169 172 180 189 193 201 209
212 246 248 251 265 268 272
283 291 297 300 314 331 334
340 350 359 370 372 376 383
388 389 391 392
NUMBER-AVERAGE
MOLECULAR WEIGHT, 130
375 378
NYLON, 33 56 57 79 125 164 168
192 199 207 225 231 309 331
NYLON 1010, 24
NYLON-12, 294 364
NYLON-6, 33 56 57 132 207 387
NYLON-6,6, 17 33 57 130 231 329
O
ODOUR, 57 183 307
OIL, 194 277
OLIGOMER, 26 46 103 124 172
190 192 238 242 264 266 335
ON-LINE MEASUREMENT, 314
OPTICAL FIBRE, 36 188 292
OPTICAL MICROSCOPY, 2 13 41
98 125 142 181 213 289 324
387
OPTICAL PROPERTIES, 1 3 47
57 162 181 199 200 206 263
274 288 292 293 323 332 350
362 375
OPTIMISATION, 50 102 105 171
233 318 373
ORGANOLEPTIC PROPERTIES,
57 183
ORIENTED, 104 117 283 284 361
387
ORTHOPAEDIC APPLICATION,
393
OSCILLATING DIFFERENTIAL
7
OSMOMETRY, 29 46 200 378
OVEN STABILITY, 266
OXIDATION, 40 41 61 66 88 94
104 129 152 153 205 266 269
274 288 325 329 348 381 393
OXYGEN, 57 104 153 262 274
311
OXYGEN ABSORPTION, 104
387
OXYGEN BARRIER, 56 57 168
P
PACKAGING, 5 57 128 131 168
212 264 266 278 323 387
PACKAGING FILM, 57 168 266
387
PAINT, 62 174 185 217 255 298
PAPER, 266 387
PAPER CHROMATOGRAPHY, 97
PARACRYSTALLINE, 102 207
213 315
PARTIAL LEAST SQUARES, 215
216
PARTICLE BEAM ANALYSIS,
206
PARTICLE PACKING, 324
PARTICLE SIZE, 13 45 50 81 225
233 319 324 372 375
PARTICLE SIZE
DISTRIBUTION, 62 324
PEAK INTENSITY, 168 178 260
289 392
PELLET, 216 266 296 373
PERMEABILITY, 56 57 168 237
PERMITTIVITY, 338
PEROXIDE, 294 326
PEROXY COMPOUND, 393
PESTICIDE, 373
PH, 46 50 130 183
PHARMACEUTICAL
APPLICATION, 46 221
PHASE BEHAVIOUR, 267 340
365
PHASE SEPARATION, 110 125
156 391 394
PHENOL, 75 297 300
PHENOL-FORMALDEHYDE
RESIN, 73 297 300
PHENOLIC ANTIOXIDANT, 183
PHENOLIC RESIN, 83 199 300
PHOSPHORUS, 95 312 373
PHOTOACOUSTIC
PHOTOCALORIMETRY, 377
PHOTOCHEMICAL
DEGRADATION, 288
PHOTOCROSSLINKING, 45 187
PHOTODEGRADATION, 16 19
65 66 274 279
PHOTOELECTRON
100 104 121 167 175 176 196
197 202 205 277 279 298 308
312 316 320 333 343
PHOTOINITIATOR, 27 312
PHOTOISOMERISATION, 288
PHOTOLYSIS, 153
PHOTON CORRELATION
SPECTROSCOPY, 224
PHOTOOXIDATION, 40 129 153
274 288
PHOTOVOLTAIC PROPERTIES,
38
PHTHALATE, 288
PHTHALOCYANINE GREEN, 65
PHYSICAL AGEING, 101 135 213
309 338
PHYSICAL PROPERTIES, 12 42
52 56 63 94 114 164 188 215
216 236 259 266 295 324 353
382
PIGMENT, 65 121 181 217 225
236 237 325 399
PIPE, 52 183 277 307 329
PLANT FIBRE, 82
PLASMA TREATMENT, 61 69
106 230 262 298 343
PLASTICISATION, 36 56 301 348
PLASTICISER, 33 34 120 184 258
277 353 387 399
PLASTICS WASTE, 87 211 212
PLATE-OUT, 6
Subject Index
POLARISATION, 256 257 284
POLARISED CONFOCAL
RAMAN MICROSCOPY, 257
POLARISED FLUORESCENCE,
284
POLARISED LIGHT
MICROSCOPY, 181
POLARISED OPTICAL
MICROSCOPY, 13
POLARISING MICROSCOPY,
168
POLARITY, 50 203 339
POLYACETAL, 164
POLYACRYLAMIDE, 46 240
POLYACRYLATE, 245 269
POLYACRYLIC, 249 343
POLYACRYLIC ACID, 46 172 342
POLYACRYLIC IMIDE, 387
POLYACRYLONITRILE, 33 79
119 342
POLYALPHA-
METHYLSTYRENE, 153
POLYAMIC ACID, 355
POLYAMIDE, 33 56 57 79 125
164 168 192 199 207 225 231
309 331
POLYAMIDE-1010, 24
POLYAMIDE-12, 159
POLYAMIDE-6, 33 56 57 132 165
207 387
POLYAMIDE-6,6, 17 130
POLYAMIDE-IMIDE, 316
POLYAMINE, 46 272
POLYANILINE, 46 115
POLYARAMIDE, 191 339
POLYARYL ETHER KETONE,
213
POLYARYLATE, 367
POLYBENZIMIDAZOLE, 79
POLYBENZYL
METHACRYLATE, 35
POLYBIBENZOATE, 309
POLYBISGLYCIDYL
METHACRYLATE, 247
POLYBUTYL ACRYLATE, 156
394
POLYBUTYL METHACRYLATE,
21 376
POLYBUTYL THIOPHENE, 327
POLYBUTYLENE
NAPHTHALATE, 98
POLYBUTYLENE
TEREPHTHALATE, 164 273
POLYCAPROLACTONE, 147 267
390
POLYCARBONATE, 14 57 62 72
79 99 101 199 207 245 273 280
309 340 356 363 367 382 398
POLYCYANATE, 11
POLYCYANURATE, 317
POLYDEUTEROPOLYETHYLENE,
361
POLYDICYANATE, 11
POLYDIMETHYLPHENYLENE
OXIDE, 356
POLYDIMETHYLSILOXANE,
140
POLYDISPERSITY, 29 35 127 137
204 224 325 335 356
POLYEPICHLOROHYDRIN, 390
POLYEPOXIDE, 10 20 32 36 47
62 68 144 145 149 151 157 161
178 179 182 199 200 222 249
255 269 272 282 292 305 309
312 320
POLYESTER RESIN, 199 204 288
POLYESTER-URETHANE, 114
POLYESTERIMIDE, 355
POLYETHER, 54 66 158 235 238
242 384 398
POLYETHER SULPHONE, 75
125 151 356
POLYETHER-ETHERKETONE,
54 79 126 213 295 315
POLYETHER-URETHANE, 90
POLYETHERETHERKETONE, 79
126
POLYETHERIMIDE, 64 79 98 192
296 367 387
POLYETHERSULPHONE, 75 125
151 356
POLYETHYL ACRYLATE, 58
POLYETHYL METHACRYLATE,
390
POLYETHYLENE, 42 52 56 57 60
61 63 65 79 87 91 92 99 102
107 109 112 128 132 139 143
146 148 154 157 164 168 181
186 188 195 199 207 212 214
216 225 249 256 260 263 266
267 283 293 307 315 324 325
344 348 357 361 365 366 368
370 372 373 386 392 393 398
400
POLYETHYLENE GLYCOL, 46
233 310 369 378
POLYETHYLENE GLYCOL
TEREPHTHALATE, 26
POLYETHYLENE
NAPHTHALATE, 387
POLYETHYLENE OXIDE, 125
154 235 337
POLYETHYLENE
TEREPHTHALATE, 2 12 26
39 40 57 63 64 74 76 79 106
117 118 131 136 157 164 168
207 212 214 257 261 263 266
269 283 293 309 323 336 357
358 382 388 398
POLYFLUOROETHYLENE, 79
164 180 279 296
POLYHYDROXYBUTYRATE, 59
POLYHYDROXYBUTYRIC
ACID, 246
POLYHYDROXYETHYL
METHACRYLATE, 172 248
POLYHYDROXYKETONE, 349
POLYHYDROXYSTYRENE, 77
367
POLYIMIDE, 5 23 79 196 199 320
355
POLYIONENE, 57 276
POLYISOCYANATE, 9
POLYKETONE, 54
POLYLACTIC ACID, 267
POLYMERIC FLAME
RETARDANT, 218 273
POLYMERIC MOULD RELEASE
AGENT, 202
POLYMETHACRYLATE, 45 245
398
POLYMETHACRYLIC ACID, 15
141
POLYMETHACRYLONITRILE,
141
POLYMETHYL
METHACRYLATE, 14 21 116
132 137 141 159 166 178 204
219 220 221 224 229 240 241
284 285 289 299 301 304 314
319 335 338 343 363 375 382
384 394 397 398
POLYMETHYLENE OXIDE, 79
POLYOL, 84 110
POLYOXYETHYLENE, 154
POLYOXYMETHYLENE, 79
POLYPHENYLENE, 398
POLYPHENYLENE ETHER, 79
152 220 367
POLYPHENYLENE OXIDE, 79
152 220 357 367 394
POLYPHENYLENE SULPHIDE,
79 170 296 320 328
POLYPHENYLENE
TEREPHTHALAMIDE, 339
POLYPHENYLMETHACRYLATE,
367
POLYPHENYLSULPHONE, 79
POLYPROPYLENE, 31 41 57 59
79 87 88 91 102 104 109 112
118 123 128 129 132 133 168
171 183 188 205 206 207 212
214 249 264 281 284 289 293
329 330 370 380 381 398
Subject Index
POLYPROPYLENE GLYCOL,
334
POLYPROPYLENE GLYCOL
MALEATE, 288
POLYPROPYLENE OXIDE, 103
POLYPYRROLE, 46
POLYSTYRENE, 14 21 35 46 48
57 58 79 82 85 87 118 141 153
156 159 160 164 166 203 207
212 214 220 230 245 278 290
299 304 308 315 334 351 363
367 375 382 394 395 398
POLYSULPHONE, 75 79 99 125
331
POLYTETRAFLUOROETHYLENE,
79 164 180 279 296 363
POLYTETRAMETHYLENE
OXIDE, 384
POLYTHIOPHENE, 38
POLYURETHANE, 19 66 79 80 84
89 110 157 158 163 169 187
199 207 255
POLYVINYL ACETATE, 79 199
209 220 268 270 367 394
POLYVINYL ALCOHOL, 1 46 51
57 284 342
POLYVINYL CARBAZOLE, 162
POLYVINYL CHLORIDE, 6 7 17
57 79 87 108 141 145 146 167
184 194 201 207 212 214 227
228 254 262 315 326 353 374
385 392 394
POLYVINYL ESTER, 320
POLYVINYL METHYL ETHER,
363
POLYVINYL PHENOL, 77 367
POLYVINYL PYRROLIDONE, 46
77 248 250 340
POLYVINYLBENZENE, 79 85 87
118 153 212 290 315
POLYVINYLCARBAZOLE, 162
POLYVINYLIDENE CHLORIDE,
57 168 387
POLYVINYLIDENE FLUORIDE,
12 79 277 390
POLYVINYLPYRROLIDONE, 46
77 248 250 340
PORE SIZE, 50 241 285 319 375
POROSITY, 50 126 142 203 241
285 319 367 375
POSITRON ANNIHILATION
LIFETIME SPECTROSCOPY,
19 99 338 367
POST-CONSUMER, 195 214 266
373
POTABLE WATER, 183 307
POTASSIUM BROMIDE, 262 271
POWDER, 126 175 194
POWDER COATING, 222
PRE-TREATMENT, 176 197 215
223 351
PRECIPITATION, 35 266
PRESSURE, 50 56 171 194 206
222 236 395
PRINCIPAL COMPONENTS
ANALYSIS, 216
PROBE, 179 339 382
PROBLEM PREVENTION, 30
181 296 303
PROCESSING, 115 168 199 207
209 231 254 261 323 325 329
373 388
PROPYLENE, 264
PROPYLENE COPOLYMER, 18
22 69 102
PROPYLENE-ETHYLENE
PROTECTIVE COATING, 217
255
PROTON MAGNETIC
RESONANCE, 265 291 314
388
PROTON SPIN RELAXATION,
209 268
PULSED NMR, 272
PURITY, 120 192
PYROLYSIS, 4 75 83 87 119 192
194 212 234 270 273 296 303
374 380 392
PYROLYSIS GAS
107 132 198 218 221 232 250
270 392
PYROLYSIS-IR
SPECTROPHOTOMETRY, 4
PYROLYSIS MASS
SPECTROMETRY, 4 192
Q
QUALITATIVE ANALYSIS, 195
QUALITY, 183 311 361
QUALITY CONTROL, 67 131 329
347 353 357 386
QUANTITATIVE ANALYSIS, 102
171 179 184 195 221 278 373
QUENCHING, 101 117 135 261
363
R
RADIATION CURING, 269
RADIO FREQUENCY
DISCHARGE, 343
RADIOLYSIS, 4
RAMAN SPECTROSCOPY, 16 27
30 33 42 47 69 70 108 109 129
140 151 168 182 212 214 215
216 256 257 263 281 284 288
293 300 342 346 365 369 393
RAPID SCAN, 344 345
REACTIVITY, 151 274 388 392
REARVIEW MIRROR, 67
RECLAIM, 289
RECOVERY, 319
RECRYSTALLISATION, 54 136
309 332
RECYCLABILITY, 57 88 266 387
RECYCLATE, 64 91 122 195 329
373
RECYCLING, 39 57 64 88 91 122
128 165 195 211 212 231 266
373 387
REFLECTANCE
REFRACTIVE INDEX, 1 106 190
200 229 292 375
REFRIGERATOR, 80
REGRESSION ANALYSIS, 144
214 215 216 224 345
REINFORCED PLASTIC, 13 17
36 79 81 90 100 134 141 176
178 179 182 196 197 199 202
211 231 234 271 281 288 296
318 320 333 339 357 377
RELATIVE HUMIDITY, 44 56 57
309
RELAXATION, 74 282 287 290
309 363
RELAXATION MAP ANALYSIS
SPECTROSCOPY, 377
RELAXATION SPECTRA, 325
RELAXATION TIME, 209 291
340
RELAXATION TRANSITION,
290
RELEASE AGENT, 202
REPEATABILITY, 347
REPRODUCIBILITY, 6 46 347
375
RESIDENCE TIME, 266 325 357
RESIDUAL ADDITIVE, 221
RESIDUAL CATALYST, 129
RESIDUAL STRESS, 67 316
RESOLUTION, 50 118 229
RETENTION TIME, 119 222
RETENTION VOLUME, 143 375
REVERSE OSMOSIS, 97
REVERSE-PHASE
233
REVIEW, 13 55 59 71 79 107 199
205 212 283 284 310 350 363
364 365 367 372 377 383 387
Subject Index
390 391 396
RHEOLOGICAL PROPERTIES,
10 20 29 41 46 73 149 161 163
217 266 295 324 325 338 354
RHEOMETRY, 10 324 325
RHEOPHOTOACOUSTIC
SPECTROSCOPY, 249
ROPE, 281
ROTATING FRAME, 209 268 340
ROUND ROBIN TEST, 173
S
SAMPLE PREPARATION, 13 72
123 124 207
SAMPLE SIZE, 72 124 143
SAMPLING, 13 71 72 123 124 207
233 351
SAN, 110 147 207 220 284 315
345
SATURATED POLYESTER, 26 49
106 114 204 229 267 322 336
367 376 388 398
SCANNING ELECTRON
MICROSCOPY, 2 5 6 13 59 61
62 63 82 98 108 129 181 202
231 289 316 324 358
SCANNING PROBE
MICROSCOPY, 59 179
SCISSION, 4 152 274 380
SCRAP POLYMER, 122 128 214
231
SEALANT, 247
SEALING, 387
SEAT, 274
SECONDARY AMINE, 36 151
SECONDARY ANTIOXIDANT,
93
SECONDARY ION MASS
202 312
SECONDARY STABILISER, 228
SEMICONDUCTOR, 321
SEMICRYSTALLINE, 102 106
122 207 213 235 315
SENSITIVITY, 118 291
SENSOR, 20 292
SEPARATION, 35 55 97 105 128
243 341 351 370 375 384
SEQUENCE ANALYSIS, 50
SHEAR, 9 178 182 324 325 333
SHEET, 186
SHEET MOULDING
COMPOUND, 202 211
SHELF LIFE, 57 311 387
SHELLAC, 232 352
SHIFT FACTOR, 209
SIDING, 385
SILICA, 6 21 40 45 46 90 203 289
319 375
SILICA GEL, 241 319
SILICATE, 65 81
SILICONE POLYMER, 204 284
SIMULATED BODY FLUID, 34
SIMULATION, 34 134 149 323
362 367
SIZE EXCLUSION
34 35 40 50 52 55 60 97 102
103 108 112 114 116 158 166
204 229 239 240 243 299 314
322 334 375 381
SIZING, 176
SMALL-ANGLE, 117 291 354
SMOKE EMISSION, 76 150 173
SOFTENING TEMPERATURE,
179
SOFTWARE, 67 195 344
SOL-GEL, 53
SOLAR ENERGY
APPLICATION, 38
SOLID STATE, 193 209 268 283
291 300 340 359 389
SOLUBILITY, 56 79 90 97 114
115 160 372 375
SOLUTE, 50 235 382
SOLUTION, 21 46 55 77 115 116
130 178 224 268 291 351 367
389
SOLUTION CASTING, 94 262
367
SOLUTION VISCOSITY, 396
SOLVENT, 21 29 35 56 113 124
130 185 203 210 235 259 261
266 285 349 360 366 369 375
388
SOLVENT EXTRACTION, 266
331
SOLVENT PERMEABILITY, 56
SOXHLET EXTRACTION, 112
SPECIFIC HEAT, 20 122 207 309
324 354
SPECIFIC VOLUME, 18
SPIN-PROBE ANALYSIS, 45
SPIN RELAXATION, 209 268 300
SPOILAGE INDICATOR, 311
STABILISER, 3 40 41 66 86 183
184 201 225 228 288 372
STABILITY, 24 26 57 85 126 163
196 228 266 267 269 295 317
324 377
STANDARD, 120 183 184 392
STAR-BRANCHED, 35
STARCH, 112 267 348
STARCH POLYMER,
STATIC HEAD SPACE GAS
CHROMATOGRAPHY, 71
STATIONARY PHASE, 50 203
235 375
STEEL, 223 341
STEP-SCAN PHOTOACOUSTIC
SPECTROSCOPY, 344
STEREOREGULARITY, 168
STERIC EXCLUSION
CHROMATOGRAPHY, 41
STERILISATION, 42 393
STORAGE, 309 311
STORAGE TIME, 311
STRAIN, 315 325 365
STRENGTH, 9 167 269 315
STRESS, 67 168 182 281 289 315
316 325
STRESS CRACKING, 271
STRESS-STRAIN PROPERTIES,
61 231 281 325
STRUCTURAL ADHESIVE, 62
STRUCTURAL ANALYSIS, 168
STRUCTURE-PROPERTY
RELATIONSHIP, 209 269 389
STYRENE, 199 278 288
STYRENE-ACRYLONITRILE
COPOLYMER, 72 110 147 207
220 284 315 345
STYRENE COPOLYMER, 28 69
127 198 299 308 363 395
STYRENE-ISOPRENE-
STYRENE BLOCK
COPOLYMER, 394
STYRENE-METHACRYLIC
ACID COPOLYMER, 81
SUB-GLASS TRANSITION, 170
SUBSTRATE, 126 223 236 262
285 298
SULPHUR DIOXIDE, 75
SUPERCRITICAL, 39
SUPERCRITICAL FLUID
SUPERCRITICAL FLUID
EXTRACTION, 97 171 372
373
SUPERCRITICAL GAS, 301
SURFACE ANALYSIS, 19 30 37
38 44 58 59 62 67 69 118 175
178 179 202 219 289 324 333
SURFACE AREA, 197 324
SURFACE CHEMISTRY, 93 298
319
SURFACE ENERGY, 52 141 217
235 277 339
SURFACE PROPERTIES, 42 44
106 118 179 191 196 217 219
277 308 312 360 383
SURFACE TREATMENT, 61 62
81 168 176 178 182 197 205
Subject Index
223 230 262 277 298 343 371
SURFACTANT, 46 65 233
SURGICAL APPLICATION, 219
393
SWELLING, 15 237 250 326 360
SYNCHROTRON RADIATION,
291
SYNTHETIC FIBRE-
REINFORCED PLASTIC, 281
T
TALC, 65 318 324
TAPE, 284
TAPPING MODE ATOMIC
FORCE MICROSCOPY, 58
TASTE, 57
TEMPERATURE DEPENDENCE,
49 99 135 146 147 170 196 259
269 308 336 354 364 382
TEMPERATURE GRADIENT
INTERACTION
CHROMATOGRAPHY, 304
375
TEMPERATURE MODULATED
CALORIMETRY, 54 78 136
252 253 280 287 290 309 336
TEMPERATURE PROFILE, 67
324
TEMPERATURE
PROGRAMMED
ANALYTICAL PYROLYSIS,
273
TEMPERATURE RANGE, 207
317 364 380 382
TEMPERATURE RISING
ELUTION FRACTIONATION,
370 396
TENSILE PROPERTIES, 40 41 61
63 65 86 114 115 231 277 315
333
TEREPHTHALIC ACID, 76
TERTIARY AMINE, 36 151
TEST SPECIMEN, 236 346 351
358
TESTING, 19 43 58 59 62 71 79
96 108 112 120 123 124 134
145 174 182 183 184 185 195
206 208 254 255 270 288 293
304 315 321 329 332 345 347
357 363 365 379 382 398
TETRAHYDROFURAN, 29 35
240 241 319 395
TEXTILE APPLICATION, 371
THERMAL AGEING, 88 152
THERMAL ANALYSIS, 7 20 26
36 54 56 67 78 83 92 95 110
133 134 144 147 149 154 155
170 179 186 187 189 207 245
252 258 267 269 270 305 309
313 324 325 367 377 383 386
394
THERMAL CONDUCTIVITY, 80
179 309 324 377
THERMAL DEGRADATION, 23
26 29 75 76 83 85 152 160 163
189 192 194 196 244 258 266
273 318 325 380 381
THERMAL DIFFUSIVITY, 179
324 394
THERMAL FIELD-FLOW
FRACTIONATION, 35
THERMAL HISTORY, 57 135 136
207 245 254 262 287 309
THERMAL IMAGING, 67
THERMAL INSULATION, 80 276
THERMAL MECHANICAL
ANALYSIS, 196 377
THERMAL RELAXATION, 282
290
THERMAL RESISTANCE, 196
THERMAL STABILITY, 11 24 26
57 85 126 163 196 228 266 267
269 295 317 377
THERMAL TRANSITION, 56 78
220 282 290 309
THERMAL VOLATILISATION
ANALYSIS, 189
THERMALLY STIMULATED
CURRENT, 323 377
THERMOANALYTICAL, 348
THERMODYNAMIC
PROPERTIES, 21 90 122 155
169 172 220 235 290 339
THERMOGRAM, 36 67 323 348
370
THERMOGRAVIMETRIC
ANALYSIS, 2 8 12 15 17 23 24
26 29 48 82 83 85 93 94 98 146
152 163 164 189 192 194 196
211 228 231 244 258 267 269
295 296 316 317 318 326 330
347 348 377 380 381 398
THERMOLYSIS, 189
THERMOMECHANICAL
DEGRADATION, 266
THERMOMECHANICAL
PROPERTIES, 179 269
THERMOOXIDATIVE
DEGRADATION, 41 94 152
269 348
THERMORHEOLOGICAL
PROPERTIES, 338
THICKNESS, 27 56 62 67 168 179
236 255 257 263
THIN LAYER
TIE LAYER, 168
TIME, 54 61 94 135 209 223 253
261 268 277 289 317 338 354
394
TIME DEPENDENCE, 125 196
360
TIME OF FLIGHT, 103 127 137
158 159 166 178 202 204 229
310 312 322 335 356 376
TIME RESOLVED
SPECTROSCOPY, 170
TITANIUM DIOXIDE, 40 65 217
237 325
TOLUENE, 56 185 241 261 319
TOTAL ORGANIC CARBON, 183
TOXICITY, 173 195
TRACE ELEMENT, 177
TRANSITION PHENOMENA,
254
TRANSITION PROPERTIES, 203
269 340 354
TRANSITION TEMPERATURE,
179
TRANSMISSION ELECTRON
MICROSCOPY, 2 5 13 59 63
82 108 129 181 213 289 331
358
TRANSMISSION
TRANSPARENCY, 57 236 323
TRANSPORT PROPERTIES, 56
115
TRIAZINE, 40
TRICHLOROBENZENE, 29
TRICHLOROMETHANE, 29
TRIETHYLAMINE, 298
TRIFLUOROACETIC ACID, 388
TROUBLESHOOTING, 30 181
296 303
TWO-DIMENSIONAL, 55 58 209
233 242 275 283 344 345 364
365
U
UHMWPE, 260 393
ULTRA-HIGH RESOLUTION
SPECTROSCOPY, 363
ULTRASONIC, 112 126 272
ULTRAVIOLET ABSORPTION,
229 274
ULTRAVIOLET CURING, 27 269
349
ULTRAVIOLET DEGRADATION,
16 19 196
ULTRAVIOLET IRRADIATION,
Subject Index
19 40 44 196
ULTRAVIOLET RESISTANCE,
57 196
ULTRAVIOLET SPECTRA, 3 41
65 86 157 264 372 383 399
ULTRAVIOLET
SPECTROSCOPY, 1 3 41 46 65
86 115 157 288 372
ULTRAVIOLET STABILISER,
225 288 399
UNIT CELL, 13 168
UNPLASTICISED POLYVINYL
CHLORIDE, 254
UNSATURATED POLYESTER,
82 199 204 288 333
UV VIS SPECTROSCOPY, 1 46
115 288
V
VACUUM DISTILLATION, 97
185
VACUUM PYROLYSIS, 87 194
VAPOUR PERMEABILITY, 56
168
VAPOUR PHASE OSMOMETRY,
396
VAPOUR PRESSURE
OSMOMETRY, 29 200 378
VARNISH, 174
VEHICLE BONNET, 329
VEHICLE MIRROR, 67
VIBRATIONAL
SPECTROSCOPY, 14 16 17 26
27 30 33 36 39 42 43 47 51 69
70 85 108 109 129 140 142 150
151 156 164 168 172 173 182
184 186 188 207 212 214 215
216 225 226 230 244 256 257
263 269 274 281 284 288 293
297 300 318 342 345 346 353
365 369 393
VINYL ACETATE, 251 270
VINYL ACETATE COPOLYMER,
209 359 389
VINYL ACETATE-ETHYLENE
359
VINYL CHLORIDE, 199 392
VINYL CYANIDE, 119
VINYL CYANIDE COPOLYMER,
57
VINYL ESTER RESIN, 320
VINYL GROUP, 274
VINYL PYRROLIDONE
COPOLYMER, 46
VISCOELASTICITY, 20 219 308
VISCOMETRY, 29 200 203 355
VISCOSITY, 10 29 46 149 172 266
324 325 330
VISIBLE SPECTROSCOPY, 1 46
115 288
VITRIFICATION, 78 161 290
VOLATILE CONTENT, 72 185
VOLATILE ORGANIC
COMPOUND, 84 174 185 255
278 321
VOLATILISATION, 72 97
VOLUME FRACTION, 13 227
231 324 332 367
W
WASTE, 87 122 128 211 212 266
387
WATER, 39 56 61 266 360
WATER ABSORPTION, 51 56 237
309
WATER CONTENT, 6 51 148
WATER PERMEABILITY, 56 237
WATER PIPE, 307 329
WATER TREE GROWTH RATE,
148
WATER VAPOUR
PERMEABILITY, 56 168
WAVE NUMBER, 168
WAVELENGTH, 44 207 288
WAX, 232
WEATHERING, 44 62 86 92 222
385
WEIGHT AVERAGE
MOLECULAR WEIGHT, 375
WEIGHT CHANGE, 348
WEIGHT FRACTION, 176 394
WEIGHT GAIN, 56
WEIGHT LOSS, 56 94 164 267
296 347 380
WETTABILITY, 37 343
WIDE ANGLE, 117 213 260
WIDE ANGLE X-RAY
SCATTERING, 24
WINDOW, 7
WOOD FIBRE-REINFORCED
PLASTIC, 9 82 141 258
X
X-RAY ANALYSIS, 6 108 129 212
231 289 328 383
X-RAY DIFFRACTION, 13 41 57
83 92 95 117 213 260 277 291
327 328 398 399
X-RAY FLUORESCENCE, 17 399
X-RAY FLUORESCENCE
SPECTROSCOPY, 108
X-RAY NEAR EDGE
ABSORPTION
SPECTROSCOPY, 358
X-RAY PHOTOELECTRON
100 121 145 167 175 176 196
197 202 277 279 298 308 312
316 320 333 343
X-RAY RESISTANCE, 104 279
X-RAY SCATTERING, 13 24 41
57 83 92 95 117 213 260 277
291 327 328
X-RAY SPECTROSCOPY, 13 37
48 63 100 108 121 167 175 176
196 197 202 277 279 298 308
312 316 320 328 333 343 354
358
XENON LIGHT, 274
Y
YELLOWING, 288
YOGHURT POT, 278
YOUNGS MODULUS, 40 114
168 231 256 269 309 365
Z
ZEOLITE, 307
ZIEGLER CATALYST, 102 129
ZINC, 298
ZINC BORATE, 359
ZIRCONOCENE, 365
Subject Index
DOCUMENTS DIRECT
(Document Delivery Service)
The Polymer Library (www.polymerlibrary.com) is the worlds most comprehensive collection of information on
the rubber, plastics, composites and adhesives industries. The fully searchable database covers approximately 500
regular journals as well as conference proceedings, reports, books, company brochures and data sheets.
Almost all the articles selected for the database can be ordered in full text through our document delivery department.
Non-patent requests are usually despatched within 24 hours of receipt (Monday to Friday).
We have a large collection of literature directly related to the industries we serve and can offer a personal
service with minimal bureaucracy, based on detailed knowledge of our stock.
Many of the documents held at Rapra are not available via other services. This is particularly the case for our
extensive and unique collection of company literature and data sheets.
We offer a fast turnaround service (within one working day) combined with a range of delivery options. Some
full text documents are available as PDF files which can be downloaded immediately
SPEED OF DELIVERY
Non-patent documents are despatched from Rapra within 24 hours of receipt (Monday - Friday) of request using
first class mail within the UK, and airmail for the rest of the world. If you request e-mail or fax service, delivery will
be within hours anywhere in the world.
HOW TO ORDER
Orders can be made by post, fax, telephone, e-mail, on-line via the website database (http://www.polymerlibrary.com),
or through an online host.
When ordering please include your full company details and which documents you require, quoting one of the following:
1. Accession Number or Copyquest number or,
2. Full Bibliographic Details
Please include which payment method you wish to use and how you wish to receive the article (i.e. e-mail,
post, fax, etc.)
Documents can be ordered from Rapra online using the appropriate command of your online host. In this case we
will issue you with an invoice and statement every three months.
For further information, please see www.rapra.net/absdocs/copyquest.htm or contact Sheila Cheese or Jackie
McCarthy on +44 (0)1939 250383 or e-mail documents@rapra.net.
PLEASE TURN OVER FOR PAYMENT METHOD OPTIONS AND ORDER FORM
CREDIT CARD PAYMENTS
This is preferable for people who only intend to use our service occasionally. The prices are per copy inclusive of
postage and packaging if appropriate. Pre-payment is required by Credit Card payment.
Delivery Method Price
E-mail, Ariel, Fax, First Class / Airmail Post 10 / Approx. US$15 or 17 (UK & Overseas) + VAT
PDF files Prices Please refer to online order form for details
(these may vary each publisher sets price)
ANNUAL DEPOSIT ACCOUNTS
A more cost effective way to use our service is to open an annual deposit account. (Web subscribers can use their
web subscription for both web access and document delivery)
The minimum amount required to open an account is 200 / Approx. US$290 or 330 (UK & Overseas)
Delivery Method Price
E-mail, Ariel, Fax, First Class / Airmail Post Documents are only priced at 7 / Approx. US$10 or 12 per item
PDF files Prices Please refer to online order form for details
(these may vary each publisher sets price)
Please Note: Any money remaining in an annual deposit account after 12 months is void.
Patents are charged at a standard price of 10 / Approx. US$15 or 17.
ORDER FORM
I would like to open/renew a deposit account for the following amount ___________________________________
I would like to order the following documents _______________________________________________________

_____________________________________________________________________________________________
PAYMENT
Name: ____________________________________________________
Company: _________________________________________________
Address: __________________________________________________
_________________________________________________________
_________________________________________________________
Telephone: _____________________ Fax: ______________________
Rapra Technology Limited
Shawbury, Shrewsbury, Shropshire SY4 4NR, United Kingdom
Tel. +44 (0)1939 250383 Fax: +44 (0)1939 251118
E-mail: documents@rapra.net
Remittance enclosed
(use only for opening or renewing annual deposit accounts)
(If paying by cheque, please make payable to Rapra Technology Ltd. in
Sterling/US$/Euros via UK banks only or make payment direct to
Account No: 05625025, Sortcode: 55-50-05, National Westminster Bank Plc,
8 Mardol Head, Shrewsbury, Shropshire, SY1 1HE, UK)
Please invoice my company (use only for opening or renewing

annual deposit accounts)
Please deduct from my annual deposit account (use this option

when ordering documents if you already have a deposit account)
Account Number _______________________________________
Please charge my credit card

American Express / Visa / Mastercard (delete as appropriate)
Card Number:
Signature: ______________________ Exp. date: ______________
IMPORTANT - Value Added Tax (VAT)
The above prices do not include VAT. Customers in EU member countries may be
liable to pay VAT if their Registration Number is not supplied. Please enter your EU
Registration Number (VAT - BTW - IVA - TVA - MWST - MOMS - FPA) below:
VAT Number:

Analysis of Plastics

Enviado por

Dados do documento

Direitos autorais

Formatos disponíveis

Compartilhar este documento

Compartilhar ou incorporar documento

Opções de compartilhamento

Você considera este documento útil?

Este conteúdo é inapropriado?

Direitos autorais:

Formatos disponíveis

Analysis of Plastics

Enviado por

Direitos autorais:

Formatos disponíveis

Rapra Review Reports

Expert overviews covering the science and

Please invoice my company

Please charge my credit card

I would like to order the following documents _______________________________________________________

Please invoice my company (use only for opening or renewing

Please deduct from my annual deposit account (use this option

Please charge my credit card

Você também pode gostar