CHAPTER 1

1.0 Introduction
1.1 Background
The

industrial training provides

the

place for the student to gain

lots of knowledge and experience in the actual industry situations. I, Nur Amna
binti Johari, identity

card

no.

920826-06-5524,

matrix

no.

112958,

undergraduate student at Universiti Sains Malaysia, Engineering Campus Nibong

Tebal. I am studying Polymer Engineering at School of Materials and Mineral
Resources Engineering. Industrial Training (EBP350) is the compulsory subject
the

third

year

student to

complete

the degree

in

bachelor

of

polymer

engineering. I am doing the industrial training under Physical Lab Department at

Rubberflex Sdn. Bhd., a latex thread manufacturer. I have been supervised by Mr.
Abul Kasim, an Executive.
1.2 Aims and Objectives
The following objectives constitute the framework of our training subject:

Linking academic training at universities with practical training during

graduate started working. To provide exposure to students to adjust to the
working world.

The close relationship between employment and university sector

Increasing confidence about the role of a professional engineer in the

actual situation. Opportunity to practice the theories that students learn in
real work situations.

Enhance skills and increase the efficiency of communication with employers

and
colleagues.

1 |I N DUS TR I A L TRA I N I N G R

EPORT

CHAPTER 2
2.0 Training Schedule
Week
Week 1

Schedule
- Introduction to types and colour of product.
- Standard Operation Procedure (SOP) and hands-on training;
i.

T50

ii.

Talcum

iii.

Water extract

iv.

Single test

v.

Colour

shade vi.
Week 2

pH

- Testing;
i.

Break test multiple loop, single

loop. ii.

VRS multiple and single

loop.
iii.
Week 3

Single thread test using Wilson Method.

- Determination
of defects on threads.
Bio-lab
i.

Determination of acetic and formic acid content in

thread. ii.
Week 4

Machine maintenance

- Natural Ageing
i.

2013 sample analysis

ii.
Week 5

- Ozone
Analysis
i.
ii.

Week 6

Test using Break Test, VRS and Newton Test

Static
Dynamic

- Accelerated Ageing
- Competitor
i.

NRT

ii.

HVFILA

iii.

Longtex

iv.

Swasthy

v.
Worldflex vi.
Week 7

- Roundex
Filing
i.
ii.

Week 8

Defect samples.
Product sample; count-based

- Chemical laboratory
i.

Alkalinity

ii.

Potassium Hydroxide (KOH)

Number iii.

pH value

iv.

Viscosity

v.

Mechanical Stability Test (MST)

3|INDUSTRIAL TRAINING REPORT

vi.

Dry Rubber Content (DRC)

vii.

Total Solid Content (TSC)

viii.

Volatile Fatty Acid (VFA)

Number ix.

Swelling set

- Raw materials
i.

ii.

Preparation of
emulsion

Preparation od

dispersion iii.
Week 9

Preparation

- Report Compilation
of solution

4|INDUSTRIAL TRAINING REPORT

CHAPTER 3
3.0 Company Background
3.1 Rubberflex
Bhd.
Rubberflex

Sdn.

produces

quality

rubber

threads

for

various

applications

in

various industries. Rubberflex strive for consistency in quality and to meet

customers stringent quality

and

delivery requirements.

With their worldwide

distribution network and established manufacturing facility, they deliver products

in a myriad of specifications according to each clients requirement.

5 |I N DUS TR I A L

EPORT

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3.1.1 Product Application

Rubberflex products are used in a wide range of application in various
industries. These include :
i. Sport wear: Shorts and tracksuits
ii. Undergarments: Men and Women briefs, brassieres, hosieries, socks
and garters
iii. Packing Materials: Meat and other food stuff, luggage straps,
books, stationaries
iv. Industrial Webbing: Furniture, trampoline, bungee
cords v. Medical Products: Bandages
vi. Sports and healthcare accessories: Ankle/knee/elbow guard, hip/waist
braces vii. Diapers products: Baby diapers and adult diapers
viii. Fashion: Hair bands, wrist bands, costume jewellery

3.2 Contact Address

RUBBERFLEX SDN.BHD.
Lot 2, Kawasan Perindustrian Bentong,
28700 Bentong,
Pahang Darul Makmur
Malaysia
Phone No: +609 222 4611
Fax No: +609 222 5300

HEAD OFFICE
RUBBERFLEX SDN. BHD.
21st Floor UBN Tower, Box No 48
No 10 Jalan P.Ramlee
50250 Kuala Lumpur
Tel: +603 2072 0011
Fax: +603 2078 5103
Website: www.rubberfle x.co m. my
E-mail: info@rubberf le x.co m. my

CHAPTER 4
4.0 Organization Structure

QUALITY CONTROL DEPARTMENT ORGANISATION

CHART 2014
LEELA SAMUEL
QA/QC
MANAGER
ABUL KASIM
SMJ QA/QC
EXECUTIVE

QUALITY CONTROL
12 SUPERVISORS
2 SR.LAB
ASSITANT
28 LAB ASSITANT

QUALITY ASSURANCE
1 EXECUTIVE PRE
SHIPMENT
3 QA-PRE ISO
1 EXECUTIVE

QUALITY
ENGINEERING
1
SUPERVISO
R

PHYSICAL LABORATORY FACTORY 2

ABUL KASIM
SMJ
Head of Physical
Laboratory

QUALITY CONTROL
QUALITY ASSURANCE
RESEARCH & DEVELOPMENT
3 SUPERVISORS
1 BLOCK LEADER
11 LAB ASSISTANT
2 GRAPH TESTER

1
EXECUTIV
E

1
SUPERVISO
R

CS
R
1 PRACTICAL
TRAINEE

CHAPTER 5
5.0 Project Overview
1. Standard Operation Procedure (SOP) and hands-on training on physical testing;
i.

T50

ii.

Talcum

iii.

Water extract

iv.

Single test

v.

pH

vi.

Colour shade

2. Conduct testing on thread;

i.

Break test multiple loop, single

loop. ii.

VRS multiple and single

loop.
iii.

Single thread test using Wilson Method.

3. Determination of defects on threads.

CHAPTER 6
6.0 Raw Materials
Latex on its own is not strong enough to make products. Crosslink can be
introduced either using chemical method or by radiation. The chemical method;
involves introducing chemicals (or ingredients) that could react with rubber main chain
and tie rubber molecules together. The reaction takes place at unsaturated sites (double
bond) in rubber main-chain.
Process of addition of chemicals to the latex is called compounding. Latex
containing these chemicals is called compounded latex. Most chemicals added to the
latex are in solid form therefore these chemical have to be dispersed in water first
before added to the latex. The dispersion for dispersed chemicals is prepared by
grinding them together with the dispersing agent in water. The chemicals used in latex
compounding can be divided into three general classifications:
1. Surface active agents
2. Liquid phase modifier
3. Elastomer or rubber phase modifier

Table 1: The chemical ingredients used in latex compounding.

Exclus ive to latex

Common with dry rubber

Stabilizers

Sulphur

Dispersing agents

Accelerator

Wetting agents

Activator

Emulsifie
r
Thickener

Antioxidants
Filler/P
igments

Coagulant/Gelling agent

6.1 Surface active agents (surfactants)

These surfactants are used

to convert water insoluble solid and water

immiscible compounding ingredients to water compatible systems that can be mixed

with the latex without upsetting the colloidal stability of the latex system.
Surface active agents normally used in latex compound either anionic (produce
negative ions) or non-ionic (does not ionise and active over wide pH range). pH
of latex compound is normally maintained around 9-10.5.
These surface active agents can be further classified as:
1. Emulsifying agents used to disperse immiscible liquids in water
2. Dispersing agents used to disperse insoluble solids usually in powder
form in water by placing an electrical charge on the individual particles
3. Wetting agents lower the interfacial tension to permit wetting out of dry
powders
The surfactants added to latex compound as aqueous solutions in order to
ensure fast and even dispersion. Surfactants should be used as carefully as
possible because their

retention

in

the

finished

products

increase

the

hydrophilic properties of the products thus giving it tendency to swell in water.

All surfactants act as release agents, impairing the adhesion of the rubber to treated
substrate.
6.1.1 Emulsifying agents
This class of surfactants is used to emulsify oily additives. These
oily additives include paraffinic and
waxes, solid tackifiers

and

naphthenic oils,

antioxidants.

The

most

liquid

tackifiers,

commonly

used

emulsifier is anionic carboxylate soaps such as lauric acid, oleic acid and
caprylic acid. Other fatty acid such as rosin acid, tall oil, stearic acid and
castor oil may also be used. Non- ionic emulsifier is not often used because
of low solubility and cloud point (solubility

decrease

with

increasing

temperature). Emulsion stabilising agents must be used when emulsion is

prepared to prevent the destabilization of the emulsion. These emulsion

stabilizing agents are usually latex protective colloids or thickener.

Example:

Caseinates,

cellulose

derivatives,

sodium

polyacrylates,

polyvinyl pyrollidone, sodium alginates

Some fine-particle solids such as bentonite clay, zinc oxide and

hydrated aluminium silicate.

6.1.2 Dispersing agents

These are surface active agents used to disperse substance in
powder form, the dispersing agent that most widely used
salt

of

the condensation product of naphthalene--sulphonic acid and

formaldehyde (such as sodium

dispersing

is sodium

agents

are

methylene-bis-naphthalenesulphonate).

The

added to the mixture of water and the solid to be

dispersed before grinding.

6.1.3 Wetting agents
The wetting agents is used for impregnation and coating processes.
Some wetting agent used with the dispersing agents to better disperse the
solids

in water. Some popular wetting agents are alkyl and alkyl aryl

sulphonates and sulphonated polyglycol ethers.

6.2 Liquid phase modifiers
The liquid modifiers are used to:
1. Protect the latex particles; classified as stabilisers

Maintaining the colloidal properties

Prevent

premature

coagulation

and

pre-floc

formation

during

latex compounding and processing

2. Modify certain liquid latex properties; classed as thickeners and wetting agents

The thickener impart desired flow characteristics to latex compounds

The wetting agents facilitate wetting ability and reduce interfacial tension

3. Converting liquid latex to solid; called coagulant or gelling agents

Chemicals that important to convert late into products

The heat sensitised gelling agents are included into this group of chemical

6.2.1 Stabilizers
This group of chemicals is used to ensure adequate processing stability
by maintaining the colloidal properties.

The chemicals classified under

this group are:

a) pH mdifiers (such as ammonia, caustic potash
(KOH), b) caustic soda (NaOH) and amines,
c) protective colloids (such as HMW materials casein, glue and
gelatin), d) surface active agents (such as carboxylates, sulphates etc)
6.2.2 Thickeners and wetting agents
Thickeners modify the viscosity of latex compound to achieve
desired flow properties. Often referred as the viscosity modifier that can be
divided into two groups:
a) Natural viscosity modifier from plants or
animal b) Synthetic viscosity modifiers
Most of these viscosity modifiers fall within the general class:
i. Water soluble hydrocolloids (hydrophilic, macromolecular and
water soluble)
Example: - Alginates algini acid obtained from various marine
algae a. Gum Arabic the sap from a certain varieties of acacia
tree
b. Casein obtained from raw protein of milk

c. Gelatin obtained from the connective tissues of animals

and fishes
ii.

Others

are

classed

as alkali-thickenable lattices (containing

particles that are capable of being swollen by the latex aqueous

phase when pH is raised to an appropriate value).
6.2.3 Gelling agents
Gelling agents is the chemicals that can promote destabilisation of
latex particles to form products. The classification of the gelling agents is
based on the rate of destabilisation of the latex particles.
Table 2: Various types of gelling agents.
Type
coagulants

Function
Destabilize rapidly

Examples
Acids, salts: Calcium nitrate,
calcium chloride

ge ling agents

Destabilize slowly

Sodium and/or potassium

silicofluoride

ge ling agents

Heat sensitizers

Agents partially destabilize

Cationic soap, diphenyl

prior to gelation

guanidine, quartenary amine

Destabilized at elevated

Ammonium nitrate,

temperature

ammonium
persulphate, ammonium
chloride

6.3 Elastomer phase modifiers

Elastomer phase modifier imparts finished latex products properties desired by
compounder. Most of the materials are in solid form and need to be dispersed in
water before added to latex. Materials are classified into several types according
to their function.

Table 3: Different types of elastomer phase modifiers

Type

Function

Vulcanising agents

Cross-link the rubber molecules in the latex

Accelerator

Speed up the cross-linking process

Activators

Activate the cross-linking process

Antioxidants

Provide protection to the products against degradation

Fillers

Modify physical properties and reduce costs

Pigments

Provide colour to the finished products

Softeners

Control modulus of the finished products

Re-odorants

Mask the rubber odour

6.3.1 Vulcanising agents

Chemical

added

to

the

latex

to

produce

cross-links.

Most

popular vulcanising agents is sulphur (added to the latex range of 0.5 2.0
pphr). The products made from sulphur containing latex compound will have
poorer thermal stability (the latex products dimensions change after heating).
Tetramethylthiuram
agents

disulphide

(TMTD)

is

another

vulcanising

(sulphurless or sulphur donor) used to produce thermally stable products.

6.3.2 Accelerators
Accelerators

control

the

rate

of

crosslinking

process.

Fast

accelerators used because the crosslinking process takes place at low

temperature. The amount of accelerator added to latex is in the range of
0.5-3.0 pphr. Examples of accelerators are dithiocarbamates and xanthates.

6.3.3 Activators
The most popular is zinc oxide which functions as an activator
to regenerate accelerator and to prevent retardation of vulcanisation because the
concentration of accelerator in the latex decrease as vulcanisation proceeds.
The addition of activator to latex compounds is to increase tensile strength
and modulus. Usually, the level of zinc oxide in latex compound is 0.5-2.5
pphr. The lowest level of ZnO will give transparency and highest level will
result

in

high modulus products.

ZnO

will also

produce zinc oxide

thickening effect because of its reaction with ammonia in the latex.

When preparing latex compound, it is not advisable to use too much
ZnO. Other activators are zinc stearate and zinc carbonate. They will
produce transparent products,

resulting latex compound

not prone to

thickening effects but they are more difficult to difficult to disperse in latex
compared with ZnO.
6.3.4 Antioxidants
Antioxidants

are

not

usually

necessary

in

latex

compounds.

Antioxidants added so that the rubber molecules in latex are not subjected to
any degradation step (chain scission as mastication in dry rubber) during
processing. In most lattices, natural or added antioxidants already present
that provide adequate protection against degradation. Accelerators (especially
ZDEC) have antioxidant activity. Good practice to add efficient antioxidant
range 0.5-2.0 pphr.
The antioxidants are added can be divided into two groups:
i. Amine compound - More effective antioxidants
- Good protection against oxygen, heat and light
- Tends to cause discolouration (staining effects)
ii. Phenolic compound - Less effective antioxidants
- Non-staining that suitable for all lattices

6.3.5 Fillers and Pigments

Fillers can be divided into two groups (see in Table 4):
a) Inorganic: no reinforcing add to reduce cost or to increase
weight, added to compound to colour it
b) Organic: reinforcing add to increase strength. Classified under
two groups:
i.

Those which are pre-formed as aqueous dispersion of

particles before addition to the latex compound.

ii.

Those which are formed by chemical reactions within the

latex aqueous phase following the addition of appropriate
reagents.

Table 4: Example of inorganic and organic fillers.

Inorganic

Organic

Kaolinite clays

High-styrene styrene-butadiene

Cheap and fine particle size, added

to the latex compound up to 400 pphr
Increasing

amount

will

increase the modulus

with

high

Widely

used

as

fillers

for latex formulations

These

lattices

are

anionic and alkaline in pH

amount

of

clay will be hard and have no rubbery

characteristics

reduce

the tensile strength of the product but

Products

copolymers lattices

and normally compatible

with most rubber lattices

White pigments

Graft copolymer lattices

Used to provide whiteness to the

latex products
Most
dioxide

effective

Sequences
rigid polymer

is titanium

have been
onto

the

of
segments
grafted

(usually 1-5 pphr)

Lithophone

latex
a

mixture

of

particles

rubbery polymer that is

zinc sulphide and barium sulphate

miscible

can also use to replace titanium

macromolecules

dioxide

Litophone is
cheaper.
Bentonite clays

latex compound
Silica
Hydrated

precipitated

silica

and

fume or pyrogenic silica

They are acidic, so care should
be taken to increase the pH by
addition of ammonia or KOH
Calcium carbonate
These

fillers

include

whitting,

ground chalks and ground limestones

Cheap

but

give

products

of

poor quality (tend to discolour)

It may reduce the colloidal stability
of the latex. Small amount of sodium
carbonate is usually added prior to the
addition to latex compound

18 | I N D U S T R I A L

with

TRAINING REPORT

the

Comprising the rubber

to be reinforced.

Not widely used as filler in

of

CHAPTER 7
7.0 Compounding
Preparation of solution
(water soluble
ingredient)

Latex compounding

Preparation of dispersions
(solid ingredients)
Emulsion preparation
(water insoluble
ingredients)
Figure 1: Schematic stages involves in latex
compounding.
7.1 Compounding Latex for Thread Production
Formulation

for

thread

production

is

usually

based

on

either

centrifuged or creamed latex. Creamed latex is preferred by some manufacturers

because of its better strainability and higher rubber content, but centrifuged lattices
are

used

successfully in many factories. Some manufacturers use a blend of

centrifuged and creamed lattices for thread production. Both HA and LA types of
latex are used for latex production. The major

requirements

for

thread

manufacturers are the mechanical stability, strainability, viscosity or a zinc oxide

viscosity value. The first two properties are relevant because the greater amount of
filtration which is required in the preparation of a thread mix. The other properties
affect extrusion of the mix.
A latex mix for use in the extrusion process should ideally possess the following
characteristics:
a)

A constant viscosity over several days storage

b)

The ability to gel rapidly at acid pH values and give a strong gel

c)

Freedom from air bubbles, coagulum and poorly dispersed materials

19 | I N D U S T R I A L

EPORT

TRAINING R

d)

The ability to dry and vulcanised rapidly to optimum physical properties

20 | I N D U S T R I A L

EPORT

TRAINING R

In addition to the above the mix should, again ideally, provide a

vulcanised thread having the following properties:
e)

High modulus and low tension set

f)

Minimal staining in contact with copper

g)

Good resistance to heating and laundering

In some cases the latex thread should also possess a good white colour and be

resistant to migratory staining and discolouration from antioxidants.

In practice, it is not possible to obtain all of the above characteristics to
equal extent from a single formulation. Some manufacturers produce a range of
latex threads e.g. standard and heat resistant type, from latex mixes of different
formulations.
The stabilizer system for the latex mix is usually based on fatty acid soap
and potassium hydroxide. Whilst this will not maintain the mix viscosity and
stability for a very long time, it is adequate for factory operation where the
storage time is usually between two and seven days. In addition, this system
provides a mix with fast gelation characteristics and gives thread high wet gel
strength.
The

majority of latex thread

dithiocarbamate and

benthiazole

compounds

system,

although

are

accelerated

in

respect

by the
of

copper

staining a compromise is normally necessary. Dithiocarbamate accelerators are the

main cause of copper staining but it is not possible to omit altogether without
scarifying

rate

of cure

and

therefore production

speed.

Consequently,

formulations for thread are usually designed to contain a minimum quantity of

dithiocarbamate with a thiozole as a major accelerator.
Also, it is usual to use zinc dibutyl dithiocarbamate rather than zinc
diethyldithiocarbamate. Since the former is believed to be less prone to staining.
For really effective protection against copper staining, however, formulations
which do not contain dithiocarbamate or thiurams must be used. With increasing
use of hot air dryers in home laundering the resistance of rubber threads to high
temperatures has become more important, vulcanising systems of the sulphurless or
less-sulphur types with better

heat resistance are necessary. A suphurless system containing a sulphur donor

such as dipentamethylenethiuram tetrasulphide (DPTT) may be employed.

Table 5: Latex thread formulation.

Ingredients

Normal

Heat resistant

Parts by weight
Natural rubber latex (60%)

166.7

166.7

Potassium laurate (20%)

2.5

2.5

Potassium hydroxide (10%)

4.0

4.0

Sulphur (50%)

3.5

4.0

ZMBT (50%)

3.0

3.0

ZBDC (50%)

0.5

1.0

Antioxidant 425 (40%)

5.0

5.0

Titanium dioxide (50%)

10-20

10-20

Zinc oxide (50%)

5.0

4.0

Drying and cure:

10-15 min, 130C

10-15 min, 35C

Dipentamethylenethiuram tetrasulphide
(50%)

The choice of antioxidant for latex thread is important, since thread has a
large ratio of surface area to bulk and is therefore relatively prone to oxidation. It is
normal to use highly substituted phenolic antioxidant such as Antioxidant 2246
or Antioxidant
425 or Wingstay L. Some of these antioxidants also improve protection against
ageing after detergent treatment. It is usual to add titanium dioxide to the
standard thread formulation for whiteness.

7.2 Preparation
Mix

of a Latex Thread

The preparation of a thread mix is similar to the preparation of other

latex mixes, but with the addition of three important operations: homogenisation,
deareation and filtration.
After mixing the solutions and dispersions with the latex, the mix is
matured by stirring it gently in a closed tank at a slightly elevated temperature.
The time will vary between four or five days at 5C and six to

hours at 40C.

Correct maturation is important since, in addition to the usually effect on cure

times, it also influences the gelling and extrusion behaviour of the thread. Under
matured latex mix tends to give gel in the form of an outer skin with a soft core
which will distort on passing over the rollers, while over-maturation results in too
low elongation of the freshly gelled thread to allow for the stretching which
occurs during subsequent processing, this leads to frequent breaking of the
thread, especially in the oven. After maturation, the mix is cooled to below
0C to stop further crosslinking. The mix is filtered through a 100 mesh nylon or
stainless steel filter before homogenisation.
Homogenisation of the mix is normally carried out through a pressure-jet
type homogeniser such as one of the APV-Gaulin machines. The effect of
greater mix homogeneity is believed to be two folds. Firstly, defects such as
rapidly varying thread diameter or blobbing which can be due to localised areas
of different viscosity, are likely

to

be

reduced.

Secondly,

it may give

reduced incidence of necking or

pearling. Once cause of this behaviour is thought to be an uneven state of cure
along the length of the thread. Such unevenness should be reduced by good
homogenisation and

correct

maturation.

Homogenisation

has

also

been

found, under optimum conditions, to reduce the viscosity of the mix by 20-50 %.
The de-areation and final filtration stages are necessary because the latex
mix has to flow through capillary tubes having a diameter of 1.0 mm or less. Pieces
of skin, floc, aggregates of compounding ingredients and air bubbles will produce
faults in the finished thread or cause breaks during the process.
It is necessary to carry out tests such as total solid content, viscosity and
degree of maturation on the prepared mix to ensure that it will perform consistently
fro m batch

to batch when processed on the extrusion plant. A mechanical stability test may also
be
performed to check that the compounding stage has had no adverse on mix stability.

Dispersions
Solutions

Latex

Mixin
g

Maturatio
n

Cool to below
20C

Filte
r
Homogeni
se

De-merate (75
mmHg)

Filte
r

Header
tank

Figure 2: Flow diagram for the reparation of a latex thread compound.

General principle concerning solutions, dispersion & emulsio ns :
1. The particle size of dispersion and droplet size of emulsions should
be comparable with latex particle size where they are to be added
2. The colloidal stability or dispersion and emulsions should comparable to
latex which they are to be added

3. The pH of solution, dispersions, and emulsions should be similar with

latex to which they are to be added

*if these three principles are not followed, the latex compound will not be
stable or resulting finished products will have poor properties
7.2.1 Preparation
Solutions

of

Aqueous

Aqueous solutions are prepared for compounding ingredients that water

soluble: those water soluble hydrocolloids (stabilizers or viscosity modifiers)
and some water

soluble

accelerators.

The

preparations

required

all

compounding ingredients to be dissolved in water. Method of achieving this

depends on type of compounding ingredients:a. Water soluble hydrocolloids
allowed to swell in the water first then the conditions changed to
make the hydrocolloids soluble.
b. Casein
solubility achieved by addition alkali to casein and water mixtur
7.2.2
Preparation
Emulsions
Emulsion is

of

a two-phase system consisting of fine droplets of one

liquid suspended in another liquid that incompletely miscible. For latex

compounds, emulsion usually oil in water emulsion.
Preparation
involves:

of oil in water

emulsion

making coarse suspension of oil droplets in water in the presence

of suitable emulsifying agent made by adding oil to water under
agitation

then subjected the coarse suspension to a refining process using

either colloid mills or emulsifiers or homogenisers

Two types of technique

emulsion:

to prepare oil in water

1. Direct method - Dissolve the emulsifying agent, colloid stabilise

thickener etc. in water) and then add oil under high speed stirring.

2. In-situ method - Carboxylate soap used as the emulsifying agent

and prepare two portions: a) fatty acid component of the soap,
dissolved in the oil to be emulsified, b) alkali component, dissolved in
water together with stabilizer and thickener. The oil phase then poured
into the aqueous phase with rapid stirring,

emulsification

occurs

spontaneously
Quality tests of emuls io ns - procedure
1. Fill 50 cm3 beaker with water and adjust pH to 9.5 with a 10% KOH
solution.
2. Place 1 drop of emulsion on the surface.
3. Observe the speed of spreading and if any oil film develops
4. A good emulsion will spread rapidly and no oil droplet/film on the
water surface.
Example
Table 6.1: Formulation for an oil-in-water emulsion (direct method).
Ingredients

Parts by weight
Dry

Wet

Oil

80

80

Sodium oleyl sulphate (10% m/m aqueous solution)

10

Sodium oleyl-anisiadine sulphate (10% m/m aqueous

20

20

70

solution)
Sodium carboxymethylcellulose (5% m/m aqueous
solution)
Water
Content active ingredients (% m/m)

40

Table 6.2: Formulation for an oil-in-water emulsion (in-situ method).

Ingredients

Part A

Part B

Parts by weight
Dry

Wet

Oil

80

80

Oleic acid

10

Morphine

20

Sodium carboxymethylcellulose (5%

20

70

m/m aqueous solution)

Water
Content active ingredients (% m/m)

40

7.2.3 Preparation of Dispersions

General principle of making aqueous dispersions
1. Proportion by mass of active ingredient in dispersion to simplify
the conversion

of

mass

of

active

ingredients

to

the

required

mass of dispersion.
2.

Preparation

of

initial

coarse

slurry

is

done

by

mixing

the

aqueous solutions of dispersing agents and colloid stabilizers with

water followed by addition of dry powder under high speed stirring.
Quality test of dispersion
1. Place one drop of dispersion on the top of a column of water contained
in a vessel such as measuring cylinder.
2. A good dispersion will form an opaque region at the top of vessel
3. A bad dispersion will sediment rapidly at the bottom of vessel.

Table 7: Example of 50% sulphur dispersion

Ingredients

Parts by weight

Sulphur

50

Anchoid

10% ammonium caseinate

30

Bentonite clay

Water

18

Total

100

7.2.4 Methods of Assessing the Degree of Vulcanisation

Swelling Set
1. Spread a thin film 0.003 and 0.01 in (dry) on a glass plate
2. Dry film with a fan for 1 hour
3. Dust film surface with talcum
4. Remove film from glass plate
5. Allow film to air dry (1 h) 23 + 2 C
6. Die out 1.5 inch diameter disc from film
7. Place the disc in petri dish with cyclohexane
8. Measure the diameter of disc in petri dish after 25 minutes by placing
dish
over graph paper with 0.00
division
9. Measure the diameter in two direction

7.3 Control of thread diameter

Control of the thread diameter or count

of the thread is essential in

production. The following parameters control the diameter of the thread:

a) The hydrostatic pressure on the latex thread compound in the
capillaries b) The internal diameter of the capillaries
c) The rubber content and viscosity of the latex compound
d) The rate at which the transfer rollers remove the thread from the acid bath
The first two factors are the main controls, whilst the third applies if
different compounds are run. The fourth factor provides a fine control of the thread
diameter.
The larger the diameter of the capillary, the large the thread obtained from
it. At a higher the hydrostatic pressure, a large thread diameter is obtained. As
the rubber content and viscosity are reduced, the thread diameter increases.
Table below summarise the effect of stretching on the wet gelled thread.
It is found that stretching the wet gel by 10-20 per cent decrease the thread
diameter by 5-9 per cent, and so affected a small degree of control over the final
count.
Table 8: Effect of stretching on thread diameter.
Degree of stretch (%)

Reduction of thread diameter (%)

10

20

30

12

40

15

50

18

100

29

CHAPTER 8
8.0 Manufacturing of latex thread
There are two routes to rubber thread manufacture. One of the established
methods involves the calendaring of a compounded rubber sheet and subsequently
cutting it into individual threads, norma ly referred as cut thread. The other method
is by extrusion and coagulation of appropriately compounded latex mix.
The term latex thread is normally applied to elastic thread produced by the
extrusion of

properly

matured

and

strained

natural

rubber

latex

compound.

Extrusion is the key operation in the manufacture of the latex thread and it is
the most sensitive in the manufacturing process. In the extrusion operation, a latex mix
is fed under pressure through a spinneret i.e. a glass capillary tube, which is immersed in
acid a round thread is formed with rapid gelling of the latex mix.
The latex filament is drawn through the bath by rollers. More rollers pull the
filament through washing baths into a curing and drying oven. On emergence from
the oven, the treads may be individually wound into bobbins, or more commonly,
formed into a ribbon. This process lends itself very readily to the continuous
production of endless length of threads.
Latex thread can be produced in diameters ranging from 1.3 mm (1/20 in) to 0.2 mm
(1/125 in) (known as

0 count and

5 count respectively), but the most common

range is from 0.85 mm (1/30 in) to 0.28 (1/90 in) (30-90 count). World demand for
latex thread is estimated at between 65000 to 70000 tonnes. It is widely used in
applications

such as clothing,

applications of latex thread

hosiery,

elastic

strapping and

include the production of shock

drive

belts.

Other

cords for parachutes

harness and elastic-cord for luggage strapping. The covered thread is also made into
open nets which are being increasingly used to replace string for holding joints of meat
together.
Latex thread is commonly used in the manufacture of latex catheters. A
length of suitable diameter is used as the former for the narrow inflation channel.
The thread can extracted easily when the catheter is complete because the vulcanised
thread does not adhere strongly to the deposit and when it is pulled longitudinally, its
diameter tends to decrease.

The present-day commercial process involves the simultaneous extrusion of 200400 threads

each from its

own nozzle,

closely spaced

and

in parallel.

Each

nozzle is dimensionally the same and each is connected to a common source of latex
mix to ensure uniformity of feed pressure. The spinnerets are made of precision-bore
glass tubing, and they must be kept clean. The spinnerets may be attached directly to
the manifold or connected in the acid bath, approximately 2 cm below the surface, so
that they are horizontal or slightly pointing upwards.

All the

capillary spinnerets

attached to the manifold should be matched both for length and bore otherwise
unequal flow rates will occur. The pressure is kept constant by maintaining the latex
source at a constant height above the orifices of the nozzles and a common roller
withdraws the threads are met. The coagulant most commonly used is a solution of acetic
acid at a concentration of 15-55 %. In general, weaker solutions are used for larger
diameter threads which are processed more slowly. One disadvantage of using a high
concentration of acid is that very efficient fume extraction facilities are required over the
coagulating bath. The acid is slowly circulated through the bath in the same d irection
as the threads by means of a pump, via a header tank and filter.
Ribbons are formed, usually from 40 filaments, by bringing the threads
into longitudinal contact and applying a small compressive force by means of a
roller. When properly prepared the individual threads in a ribbon adhere sufficiently
well to withstand normal handling but also may be easily separated, without damage,
before covering. Fully vulcanised threads have insufficient residual tack to prepare a
good ribbon and completely unvulcanised thread has too much, preventing the thread
being easily separated. For this reason, ribboning is normally carried out part way
through the oven. The latex threads can be readily separated from one another again to
recover their original individual nature. This is a particularly convenient form of supply
to feed a covering machine, that is, the machine which wraps covers of textile thread
around the rubber thread. Latex threads are used in garments in the covered

state

wrapped with one or two layers of textile (usually the latter). This winding is carried out
on special machines designed for the purpose.
The residual tack on latex thread means that the vulcanised threads may
cohere strongly, making handling difficult. It is therefore necessary to detackify the
thread through talc.

The curing oven is usually a multipass machine with three or sometimes five or
more fabric conveyer belts. Since the threads are not completely dry when they enter the
oven temperature of the initial zone is usually between 95- 00 C to avoid blistering of
the threads caused by rapidly expanding water vapour. The temperature is increased in
stages to values as high as 135- 40 C. The oven is heated by hot air from a heat
exchanger and the air flows in the opposite direction to that of the thread. The air
velocity should be kept low to avoid disturbance of the threads on the conveyer belts.
Batch Number
42842002;
4 year (2014)
28 week (week in the year)
4 day (Monday-1, Tuesday-2, Wednesday-3, Thursday-4, Friday-5, Saturday-6, Sunday-7)
20 machine
02 talcum (01-Silicone, 07-Meat Packaging)

CHAPTER 9
9.0 Chemical Laboratory
9.1 Chemical Laboratory
The properties of the latex are of interest because:
1. To gain better understanding of the physical and chemical nature of the latex.
2. To determine the fitness of a latex for a particular application; thread.
3.

To ensure the general quality of the latex

9.1.1 Total Solid Content (TSC)
Introductio n
Total solid content (TSC) is one of the tests that related to the
chemical composition in latex. It is define as the percentage by mass of the
whole latex, which is non-volatile under specified condition of drying in
open atmosphere at elevated temperature. Theoretically, in NR latex, the TSC
value is more less 60%. In general, latex is a dispersion of polymeric solids
in water or aqueous medium. It has two phases which are dispersed phase
and continuous phase. Mostly, the raw latex consist varies of chemical such
as proteins, resins and about 37% m/m rubber particle content.
Experime nta l Procedure
1. Different glass dishes are weighed.
2. All different samples are poured in different dishes respectively.
3. Again, the latex-filled dishes are weighed.
4. The dishes are swirled gently so that the latex can cover the dish bottom.
5. The dishes are put in the oven at 70C for about hours until the
samples
lost their whiteness.
6. The samples are took out from oven and let to be cooled at room
temperature before weighing.
7. The dish is relocated in the oven for 15 minutes and step 6 is repeated.
8. Steps 6 and 7 are repeated until the difference of loss in mass is less than
1mg

Calculat io n
The total solid content (TSC) value, expressed as a percentage by mass
is
obtained by using the formula following:
m1
x100
mo

TSC
Where,
m0 = mass of the test portion (g)
m1 = mass of the dried material (g)
9.1.2 Dry Rubber Content (DRC)
Introductio n

Production of natural product begins at the plantation where a slit is

made into the bark of the rubber tree to allow the flow of a milky sap. This
latex consist of water, polyisoprene and small quantities of other ingredients
such as protiens and carbohydrates (Andrew Ciesielski, 1999).
Dry rubber content (DRC) is simply defined as the percentage by mass
of the

latex,

which

is

coagulated

under

specified

conditions

of

colloidal destabilization by acid such as hydrochloric acid or acetic acid. It is

essential to apply the DRC process because it is indicator of the rubber content
in the latex.
The

DRC

value is slightly greater than the real rubber content

because a proportion of non-rubber substances are consist precipitates with

the rubber during colloidal destabilization. Nevertheless, the dry rubber
content is approximate to the true rubber substances compare to the total
solid content. It because
substances

while

non-volatile

and

the

latter

the differences

includes

between

the

these

non-volatile
two

rubber

indication

of

non-rubber substances in latex expressed as a percentages

of the mass of the whole latex.

Acetic acid is one of the latex destabilization agents. It is inorganic

acid that gives sour taste and pungent smell. In addition, acetic acid is a
weak acid where is only a partially dissociated acid in aqueous solution.
Acetic acid also physically in colourless liquid which absorbs water from
o

the environment and freeze at 16.5 C to crystalline solid state.

While sulphuric acid is a highly corrosive strong mineral acid. It
is a pungent-ethereal, colourless to slightly yellow viscous liquid which
is soluble in water at all
acid and

concentrations.

Sulphuric

acid

is

a diprotic

shows different properties depending upon its concentration.

Safety precautions

should be

strictly

observed

when

handling

it.

Moreover, it is hygroscopic, readily absorbing water vapour from the air.

Experime nta l Procedure
1. 2 different sample of NR latex are poured into labelled dishes respectively.
2. Sufficient water is added into the dishes to reduce the TSC of the
latex concentration to 20

1 % (m/m).

3. The dishes are rotated on smooth surface to let them dilute homogeneously.
4. 75

5 cm of 20g/dm acetic acid solution is added after 5 minutes in

both dishes.
5. The coagulated latex samples are depressed below the acid surface.
6. After 5 minutes, the dishes are placed on the steam bath for 15 30 minutes.
7. The small particle of the coagulated latex samples are collected by
rubbing with the main bulk.
8. The coagulated latex samples are soaked into different water so that they
are
not acidic when tested by using litmus paper.
9. The samples are then pressed to expel water and to obtain uniform
thickness less than 2mm.
10.The samples are washed and allowed to rinse before transferred into
drying oven.
11.The samples are dried at 70 C until no white patches.
12.The samples are cooled at ambient temperature then weighed.

13.The drying process is repeated at interval 15 minutes until the loss in

mass is less than 1 mg.
14.Steps 1-13 are repeated by replacing acetic acid with sulphuric acid
Calculat io n
DRC can be calculated by using:
DRC

m1
x100
mo

Where,
m0 = mass of dry coagulum in
gram m1 = mass of latex in gram
9.1.3 Mechanical Stability Test (MST)
Introductio n
MST can be defined as the ability if the latex to withstand the
colloidal destabilisative effects of mechanical influences such as shearing and
agitation. In the process, the latex compound is subjected to mechanical
agitation such as stirring. MST is only applicable to NR latex without
any

compounding ingredients. MST measures time of elapses before the

appearance of floccs when the latex is stirred. According to Perez (1993)

mechanical stability is also defined as

the

resistance

of

the

latex

to

flocculation during stirring or agitation. It is measured by the mechanical

stability time (MST) test in which latex is stirred rapidly (14000 rpm)
under standardized conditions (a test portion of the latex concentrate is
diluted to 55% by mass total solids content) and the time required for visual
flocculation to occur is noted. Expressed in seconds, this test allows the
behaviour

of the

latex

to

be

evaluated

during the course of the

different operations it undergoes during its transformation into a finished

product. The mechanical stability of natural latex should be

650 s.

Meyer (1953) reported that, when flocculation is visible, the time

taken is recorded, this being regarded as a measure of the mechanical stability.
The arrival of the end-point is preceded by a marked decrease in the depth
of the vortex around the stirring shaft, accompanied by loss of turbulence
and a change in the

sound of stirring action. Two methods are permitted for the determination of
the end-point:
I. palm of hand and
II. water-dispersibility.
Experime nta l
Procedure
1. 100g of latex concentrate is diluted to 55% TSC with appropriate
ammonia solution.
2. The diluted latex is warmed and stirred gently up to 36-37
C.
3. The latex is filtered through wire cloth and 80 g 0.5 g of the latex is
weighed into a container.
4. Check the temperature of the latex to be 351
C.
5. The container is located in position and the latex is stirred at the
rotational frequency of 14000 rev/min 200 rev/min throughout the test
until the end- point is passed.
6. The end-point is confirmed by the presence of an increased amount
of
flocculum in a sample taken after stirring the latex for an additional 15s.
Dilut io n
latex

of NR

The volume of ammonia added to the NR latex to reduce the TSC

value from 60.0% to 55.0% is obtained by using the equation 1 below.
M 1 V1
Where
1

= M 2 V2

M 1 = Molarity of Solution

M 2 = Molarity of Solution
2
V1 = Volume of Solution
1
V2 = Volume of Solution
2

Substitute the M1 value as 60.0% and M2 value as 55.0% with NR latex

volume of 100ml and the volume of ammonia obtained is 9.09ml. Hence,
9.09ml of ammonia solution is required to reduce the TSC of NR latex
from 60.0% to
55.0%.

The concentration of NR latex also will affect the MST. When dilution
of NR latex percentage increases,

it means that the little amount of

ammonia solution is needed. It will increase the formation of coagulant. More

diluted latex will affect the movement of latex particle to form coagulant.
By mechanical, those circumstances too liquid will reduce collision of latex
particles to form floccs due to low energy absorption rate.
Woon (2011) stated that another factor that will affect the MST
beside temperature is exposure to air (old latex). Longer exposure will make
the latex becomes not good hence reducing its stability. The aldehyde groups of
the rubber molecule could be oxidised forming carboxylic groups and this
ionised groups could in turn migrate to the rubber particle surface thereby
increasing the negative charge at the particle water surface. This is effect of
the latex absorbing the air (oxygen). Hence, always advice that after opening
the sample bottle, latex sample must be tested as soon as possible (within 24
hours).
According to Perez (1993), mechanical stability tends to decrease
during long periods of transportation and storage owing to the slow
hydrolysis of the stabilizers by ammonia. It is therefore necessary to be very
prudent when natural latex is received and found to have low mechanical
stability, for example, 600 s. Such latex is susceptible to the formation of
grains and wi l be filterable with difficulty. Manufacturers generally avoid
this problem by adding stabilizers such as an anionic fatty acid alcohol, for
example, lauryl sulphate.
9.1.4 Viscosity
Introductio n
Viscosity is a measure of the resistance of a fluid, which is
being deformed by either shear stress or tensile stress. Viscosity of the
latex largely contributes to the product thickness and it is depends on shear
rate, total solid content (TSC) and temperature. In Rubberflex, the spindle
size (1/60) used is fixed.

Viscosity depends largely on shear stress. When shear stress increases, the
viscosity will decrease. Besides that, the total solid content (TSC) of latex
also influences the viscosity of latex where the higher TSC will result
in higher viscosity value. Therefore the shear stress and TSC is investigated
in this testing as a factor that influences the viscosity of NR latex. The
viscosity of a latex sample is determined by means of a viscometer which
measures the torque produced on a specified spindle rotating at constant
rotational frequency and at low rate of shear while immersed to a specific
depth in the latex.
Experime nta l Procedure
1. The procedure to use the viscometer is studied.
2. Spindle size 1/60 is used where it is standardized for all different dilution.
3. 250 ml of NR latex is poured into a beaker and diluted to 30% from 60%
TSC.
4. The latex with new TSC value is tested for its viscosity value.
9.1.5 Alkalinity
Introductio n
Alkalinity is the measure of a solutions capacity to react with a
strong acid to a predetermined pH. The alkalinity of a solution is usually
made up of carbonate,

bicarbonate, and hydroxides.

Similar to

acidity,

the higher the alkalinity is, the more neutralizing agent is needed to counteract
it. Alkalinity is determined by titration with sulphuric acid to a pH of 4.5.
While these pH end - points are common in wastewater situations, other
end-points are often used depending on certain test or sample conditions.
In latex processing, ISO 125: 1990 (E) is used to determine the alkalinity.
Alkalinity refers to the free alkali content of latex and used to indicate the
amount of preservatives added for adequate preservation. Standard procedures
apply only to natural rubber latex. The general procedure is to titrate a
known weight of the latex with standard acid under conditions such that
coagulation is unlikely to occur. Titrations of latex concentrate with acid
electrometrically to pH 6 in the

presence of a stabilizer, and calculation of its alkalinity from the quantity of

acid that is required.
For HA preservative NR latex, the alkalinity should have at least 0.6
% (m/m) in the

latex system.

In this

experiment, the pH meter is

preferably to be used in determining the pH of the system rather than methyl

red. There is difficult to observe the colour changes of methyl red indicator
due to the opacity of the diluted NR latex hence it is difficult to ascertain the
end-point (Blackley, 1966).
Experime nta l Procedure
1. The pH meter is calibrated using the method specified in ISO 976.
2. 200 cm of water is filled in a 400 cm beaker.
3. 10g latex concentrate is added and stirred continuously.
4. The electrode is inserted.
5. Sulphuric acid is added drop by drop from the burette until the pH is
reduced to a value of 6.0 0.05.
6. The amount of sulphuric acid added is tabulated.
7. The determination is carried out in duplicate and the average
value is calculated.
Calculat io n of alkalinit y (ammonia preserved NR latex)
Alkalinity (as NH3 ) =

F1 = factor: 3.4 for H2 SO4

c = actual concentration per cubic decimeter
3

(0.05mol/dm ) V = volume in cubic centimeters of acid

used
M = mass of test portion in grams

9.1.6 Potassium Hydroxide (KOH) Number

KOH number can be explained as the number of grams of
potassium hydroxide equivalent to the anions present as ammonium salts in
the quantity of latex, which contains 100 grams of total solids. KOH number
also can determine

the quality of the NR latex. Some anions corresponding to the ammonium

ions, which assigned to the activity of the microorganism in latex before
adequate preservative

added.

Some

of these

anions

that enhance

the

colloidal stability of the latex will not determine the latex quality.
The basic principle of determining KOH number for NR latex is
reducing ammonia content in the latex to specified level by reaction with
formaldehyde, diluting with distilled water with given total solid content
(TSC)

and

then, titrating with carbonate-free aqueous KOH solution of

specified concentration.
The general objective is to determine the concentration of ammonium
ions in latex aqueous phase by titrating with hydroxyl ions. Ammonium is
weakly acidic, thus high end point of the titration. There are no suitable
colour-change indicators by which the end

point can be satisfactorily

detected. The reaction of ammonium and hydroxyl ions is as equation below:

NH4 + + HO- = NH3 + H2 O
Experime
Procedure

nta

1. The pH meter is calibrated by the method recommended in ISO 976.

2. The total solid content (TSC) and alkalinity of the NR latex are obtained .
3. Then, NR latex is weighed to the nearest 0.1g into a 400cm3 beaker
containing approximately 50g of total solids.
4. Next, the latex is diluted with distilled water to about 30% total solids.
5. The electrode is then inserted into the latex and 5cm3 of KOH
solution is slowly added while stirring slowly with the magnetic stirrer.
6. The resultant equilibrium pH reading is recorded.
3

7. Then KOH solution is added with increments of 1cm with continuous

stirring.
8. The equilibrium pH is recorded after each addition until the end-point has
been passed.
9. The end point of the titration is the point of inflexion of the titration
curve of pH value against volume of KOH.
10.Then, the graph of dpH against dV is plotted.

Value for KOH number for NR latex could be calculated by using below
equation:

C = Concentration of Potassium Hydroxide, mol/dm3

Where

V = Volume of KOH solution to reach an endpoint WT S = TSC of latex in terms of percentage

by mass M = mass of latex, in grams, g
The KOH number reflects the quality of the NR latex. The ideal
KOH number falls in between 0.4 to 1.0. Lower KOH number of NR latex
will shows the better quality of the NR latex.
There are few problems in determining the KOH number of the
latex which

when

measuring

KOH

number,

the

utilizing

process

of

acid from microorganism will interrupt the value. Somehow, the presence of
acid carbonate in the water source will result in different value of KOH number.
To maintain the colloidal stability of the latex, the stirring process needs to be
controlled in order to avoid flocculation due to agitation.

9.1.7 Volatile fatty Acid (VFA) Number

Introductio n
Volatile fatty acid (VFA) number is defined as the number of grams
of potassium hydroxide equivalent to

the volatile fatty acid in latex

concentrate containing 100g of total solids. VFA quantifies the concentration

of a particle subgroup of anions, which is included in the potassium
hydroxide number. It is used as an index for the quality of natural rubber
latex but more precise then the potassium hydroxide number because of more
discriminating. Bacteria on the carbohydrates in the latex use this test to
quantify the concentration of formic, acetic and propanoic acids, which are
produced due the attack. Hence, VFA

number test provides an indication of the extent of bacterial activities in the

NR latex, thus VFA number measures the state of preservation of NR latex. The
poor preservation results in lower quality of NR latex which resulted in high
value of VFA no.
The

volatile

fatty acid

number is determined by separating the

constituent of the aqueous phase from a specified mass of latex. It is then

subjected to steam distillation with a strong acid. After separation, it is titrated
with standard aqueous alkali solution. The volatile fatty acid number is high
and does not represent the volatile fatty acid content without correction.

Experime
Procedure

nta

1. First, 50g of latex concentrate is weighed into a beaker. Accurately, add

3

50cm of the ammonia sulphate solution from a pipette while stirring

the latex concentrate.
2. Then, the beaker is placed on the steam bath maintained at 70 o C and
continues
stirring the latex concentrate until it coagulates. The beaker is covered
with watch-glass and it is left on the bath for total period of 15 min.
3

3. The serum is decanted which exudes through a dry filter paper. 25cm of
the
3

filtered serum is pipetted into a dry 50cm conical flask.

4. 5cm3 of sulphuric acid solution is added to acidify it. It is mixed
well by swirling the flask.
5. Steam was passed through the steam jacketed distillation (Markham still) for
3

at least 15 min. 10 cm

of the acidified serum was introduced into the

inner tube with steam passing through the outer jacket of the steam outlet
open.
3

6. A 100 cm of graduated cylinder was placed under the tip of the condenser
to
receive the distillate.
7. The steam outlet was partially closed to divert steam into the inner tube.
Steam was passed gently at first, then was fully closed the steam outlet
until 100 cm3 of distillate has been collected.
8. The distillate was transferred to a 250 cm3 conical flask.

9. Solution was titrated with the diluted barium hydroxide using one of
the indicators (phenolphthalein) specified. The amount of the indicator
used to change the colour is recorded.
For dilut io n of barium hydroxide : 0.05 to 0.005 - mol/ dm3
By assuming the volume of barium hydroxide that is needed to use for
titration is
100 ml,
M1 = 0.05 mol/ dm3 , M2 = 0.005 mol/ dm3 , V2 = 100 ml

The amount of distilled water need to be added is 90.0

ml. VFA number calculat io n (example)
Table 9: Volume of barium hydroxide added in titration
Color Changes

Volume of Barium Hydroxide (ml)

Light pink

7.0

Dark pink

7.8

No changes to dark pink

12.8

Average

9.2

VFA number can be calculated by using equation below:

Where:
is the actual concentration, expressed in moles per cubic decimeter of
the
Barium Hydroxide solution.

is the volume in milliliters of barium hydroxide solution required to

neutralize
the distillate.
is the total solids content of the latex, expressed as a percentage mass of
the
latex concentrate.
is the mass in grams of the test portion.
is the dry rubber content, expressed as a percentage mass of the
latex
concentrate.
is the density in mega grams per cubic meter of the serum
134.64

is

factor

derived

from

the

relative

molecular

mass

of

potassium hydroxide, its equivalence to barium hydroxide and

those parts of the serum acidified and distilled.
Assume

TSC

(m/m) DRC

61.00 %
=

60.00

% (m/m)
Given

Found

0.005 mol/dm

1.02 Mg/m3

9.2 cm

50.00 g

The VFA No. is normally used to quantify or determine the

concentrations of acids presents such as formic and acetic acids that are due
to bacterial attack. These
microorganism

reaction

fatty
on

acids

are

formed

through

the carbohydrates present in latex and the

concentration of these anions in the latex indicates

the

extent

of

microorganism attack on the latex concentrate and indirectly measures the

quality of latex. The salts of acids present will reduce the colloidal stability
of latex concentrate and hence maximizing the coalescing of

latex particles, which lower the quality of latex concentrate. The higher the
VFA
number, the higher the amount of acids presents.
Carbon dioxide will produce bicarbonate and carbonate ions in ammoniapreserved NR latex. These ions will decrease the VFA number of NR latex.
The anions in carbonic acid will be more dominant to reduce mechanical
stability latex. Numbers of ammonia will form from the reaction of anions
from carbon dioxide and ammonium ion. The ammonia will react with
volatile fatty in and reduce VFA no. As the VFA no. decreases, the
volume of Barium Hydroxide required to be added on the serum also
reduced. Sulphuric acid was used to acidify serum before carrying out the
distillation process with Markham still and the function of this acid as
formation impurity with ammonia when distillation carried out.
VFA number (max) is 0.20(ISO2004). When VFA number of NR latex
is low, it shows that the latex is in good quality.
9.1.8 pH value
Objective
Testing using dried petri dish containing dried extracted water from
water extraction testing to test their pH in order to check whether the
latex thread containing high acidity or not. Basicly, the acceptable result are
pH 7 and above. We do not want thread to have high acidity (pH 1-pH 6).
Materials and apparatus
Dried petri dish from water extraction testing, pH meter (Mettler
Toledo), electrolyte solution, technical buffer solution.
Procedure
1. Take out the technical buffer solution (pH 4 and pH 7) and
electrolyte solution.

2. Calibrate the pH meter by using both pH 4 and pH 7 technical

buffer solution
3. Pour 5 ml distilled water in the dried petri dish and shake to have
the solution.
4. Put the solution in a small container and test it using electrode at the
pH
meter to know its pH

9.1.9 Swelling Set

Procedure
1. Spread a thin film 0.003 and 0.01 in (dry) on a glass plate
2. Dry film with a fan for 1 hour
3. Dust film surface with talcum
4. Remove film from glass plate
*Immersion of plate in water facilitate stripping with minimum
tearing or distortion
5. Allow film to air dry (1 h) 23 + 2 C
6. Die out 1.5 inch diameter disc from film
7. Place the disc in petri dish with cyclohexane
8. Measure the diameter of disc in petri dish after 25 minutes by placing
dish
over graph paper with 0.00
division
9. Measure the diameter in two direction

110

Reading

Figure 3: Graph paper

reading.

CHAPTER 10
10.0 Biology Laboratory
10.1 Determination of formic and acetic acid content
Procedure
1. Pour some sample (extracted water taken from water extraction testing) into
small bottle to be sent to bio-lab.

2. Inject 20 microLiter standard solution into the machine (results are based
on standard solution).
3. Next, inject 20 microLiter sample until we get the reading.
How to use machine?
1. Refresh machine using washing solution for 30 minutes.
2. Change to mobile phase solution for 30 minutes.

3. Inject standard solution until the result come out and proceed with samples.

4. Use washing solution for 30 minutes.

5. Change to storing solution for 30 minutes.

10.2 Preparation of HPLC Solution (Maintenance)

1. Standard Solution
i.

Prepare master mix by add 1 ml of 100% formic acid and 1 ml 100%

acetic acid into 100 ml distilled water.

ii.

Standard solution is done in 3 different ppm (100, 300 and 900 ppm).
iii.

For 100 ppm, put 0.5 ml of master mix in 50 ml distilled

water. iv.

For 300 ppm, put 1.5 ml of master mix in 50 ml

distilled water. v. For 900 ppm, put 4.5 ml of master mix in 50 ml

distilled water.
2. Mobile phase solution
i.

Weigh 2.72g of Potassium Dihydrogen @ orthophosphate and put in 1 L

distilled water.

ii.

Take out 50 ml of the mix, then add 50 ml

methanol iii.

Adjust the mixing to pH 3 and do

double filtration.
3. Washing solution
i.
ii.

Prepare 1 L distilled water.

Take out 100 ml of distilled water and add in 100 ml

methanol iii.

Do double filtration.

4. Storing solution
i.

Add 800 ml methanol in 200 ml distilled

water. ii.

Do double filtration.

Figure: formic and acetic acid use to prepare all solution.

Pipette (size: 1000 ml)

How to do double filtra t io n?

1.

2.

3.

4.

5.

6.

7.

CHAPTER 11
11.0 Physical Laboratory
11.1 Physical Testing
Since

conventional dumb-bell test

pieces cannot be cut from thread

specimens, the procedure for tensile tests must be modified. Details of the tests
for threads are given in various standards such as ISO 2321, BS 5421 Part 1 and
ASTM D2433 . The properties of most important for thread are count or diameter,
the Schwartz value and the elongation under a fixed load.
The count (size number) of a round thread is the number of threads which,
when placed side by side, measure 25.4 mm. The count of rubber thread is
determined indirectly, by measuring the thread density and then weighing a
precise length, usually
1 meter of thread.
The count is usually expressed as the median of the values for five test
pieces. It is customary to quote the count of a round thread, followed by the whole
even number which is nearest to the actual count of a square thread of equivalent
cross-sectional area (count of round thread 1.3 = actual count of square thread);
for example a round thread of count 50 is indicated as 50/56.
The density of thread, which normally varies from 0.95-1.11 g/cm3,
is determined by immersing the thread in a series of liquids of varying density
until it neither sinks nor rises. Mixture of ethanol (0.79 g/cm3) and ethylene
glycol (91.11 g/cm3) are used in this purpose.
The tensile strength and elongation at break are determined on a tensile
machine using special pneumatic grips to hold the thread. The stress retension of
the thread may be determined by measurement of the stress after holding the
thread extended at say
100% elongation for a specified time. It is convenient to use a loop of thread for
this
test.
The test for elongation under load measures the elongation produced when a
predetermined stress, usually 158 g/mm2 or 280 g/mm2, is applied to the thread.
Other

tests for thread include tensile strength, elongation at break and stress retension.
The heat ageing test consists of determining the Schwartz value of a sample of
thread. The loop test pieces are then stretched on a non-metallic frame of such
a size that the circumference of the loop is extended by 100 per cent. Whilst in this
condition, they are heated for 6 hours at

5C in a standard ageing oven and then

a lowed to recovered, still extended, for at least 16 hours in a standard

laboratory atmosphere. After this period, the loops are removed from the frame
and the Schwartz value is immediately re - determined. The percentage re-tension of
Schwartz value is quoted as the result. This procedure is considered to
results

closer to

give

those observed in service than conventional ageing tests,

because in garments the thread is nearly always extended even when the garment
is relaxed.
11.1.1 T50
Objective
Objective of doing T50 test is to determine the state of cure of
latex thread. Negative (-ve) temperature value indicates that the latex thread
is cured while positive (+ve) value indicates that the latex thread is not
cured. . This specification is normally in the range of -1 to -2 C for fine
gauge and MP while -6
C for big/course count.
Material and apparatus
Latex thread, acetone, T50 machine, thermometer, container, rubber stamp.
Procedure
1. Fill up the container with -38C acetone.
2. Mark the thread (2.5 cm) using rubber stamp.
3. Put the thread at the apparatus as shown (7.5 cm).
4. Pull the centre rod of the apparatus to 12.5 cm position and put the
apparatus in the acetone for 30 s.
5. After 30 s, immediately push the centre rod back to normal (7.5 cm).

6. Wait until the thread back to its initial length and record the temperature.

55 | I N D U S T R I A L

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11.1.2 Talcum
Objective
Objective of doing talcum testing procedure is to determine the
talcum content

in thread

represented

in percentage. Lower percentage

indicates that the latex sent to customers is good because customers do not
want to buy talcum. This test only done for talcum coated thread.

Table 10: The specification for talcum.

Count

Talcum percentage (%)

20 - 31

2.0 - 2.4

34 - 44

2.4 - 2.8

46 - 55

3.0 - 3.2

60 - 110

3.0 - 3.5

Diapers

3.0 - 3.2

Material and apparatus

Oven, latex thread samples, weighing machine, propyl alcohol, filter paper
Procedure
1. Separate the sample into individual threads and weigh.
2. Wash the thread sample using propyl alcohol (olive solution).
3. Put the washed sample on the filter paper.
4.

ocate them in the oven at 00 C for 4 hours.

5. Take out the sample and cool them down at room temperature.
6. Weigh the dried thread and calculate the percentage.
56 | I N D U S T R I A L

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7. Formula:
(weight of thread with talcum - weight of thread after dried) (weight of
thread with talcum)
Eg; (15.6224 - 15.1259) (15.6224) = 3.17

11.1.3 Water Extract

Objective
Objective of doing water extraction testing is to determine the water
content in latex. Lower water content (represent in percentage) will give
latex thread good quality.

Table 11: The specification of water extraction is:

Type of thread

Percentage (%)

NW/BL

1.8 2.5

HW/HB

1.5 2.0

XW/XB

0.8 1.2

MP

< 0.99

Fine Gauge

< 1.00

Material and apparatus

Latex thread, oven, filter paper, conical flask, dropper, petri dish
Procedure
1. Weigh empty petri dish.
2. Weigh 20 g latex thread sample using weighing machine.
3. Separate the individual threads and cut them into 1 mm long.
4. Put them in a beaker filled up with 200 ml distilled water.
5. Put the beakers in 00 C water bath for 1 hour.
6. Cool the beaker until the beaker is no longer warm.
7. Extract the water as shown using the apparatus.
*Extracted water in the beaker must achieve 200 ml. If it is not enough,
add distilled water in the sample-filled beaker and extract again until you
get 200 ml.
8. Fill the extracted water into small conical flask until the mark line and
then fill the water in the petri dish.
9.

ocate the petri dish in the oven at 00 C and leave for 4 ho urs.

10.Take out the petri dish and let it cool to room temperature. After
cooling, weigh the petri dish.
Formula: (initial weight of petri dish weight of petri dish after drying) 10
Eg:

(101.6754 101.3165) 10 = 2.5

11.1.4 Colour Shade

Eg: sample 1 :

L*
84.98 a*
0.58 b*
-4.17

sample 2 :

L* 23.44
a* 0.33
b* -0.43

sample 3 :

L*
51.37 a*
-0.35
b* -1.56

L* indicates the total brightness of a sample. If the sample is

white in colour, the total brightness is more than black colour. Example:
sample 1 and 2. L* value for sample 1 is 84.98, the value are much more
compared to L* value for sample 2, 23.44. This shows that sample 1
is white in colour and sample 2 is black in colour. a* indicates the
red/green colour. The a* value is not really important in latex thread
industry compared to paint industry. Both sample 1 and 2 show very
low a* value, means that the samples do not give red/green colour.
b* indicates blue or yellow colour. Latex thread industry is focusing
on this b* value because almost latex thread product are white in
colour and they tend to be become a bit blue or yellowish. For sample 1,

its b* value is less than -4, the colour are more to blue. While sample
2 (black sample), the value are really low, showing that it does not give
blue or yellowish colour.

11.1.5 pH
Objective
Testing using dried petri dish containing dried extracted water
from water extraction testing to test their pH in order to check whether
the latex thread containing high acidity or not. Basicly, the acceptable
result are pH 7 and above. We do not want thread to have high acidity
(pH 1-pH 6).
Materials and apparatus
Dried petri dish from water extraction testing, pH meter (Mettler
Toledo), electrolyte solution, technical buffer solution.
Procedure
1. Take out the technical buffer solution (pH 4 and pH 7) and
electrolyte solution.
2. Calibrate the pH meter by using both pH 4 and pH 7 technical
buffer solution.
3. Pour 5 ml distilled water in the dried petri dish and shake to have
the solution.
4. Put the solution in a small container and test it using electrode at the
pH
meter to know its pH

11.1.6 Ozone; Static and dynamic

Ozone is a colourless unstable toxic gas with a pungent odour and
powerful oxidizing properties which allows it to be detected at very low
amount. Ozone is formed from oxygen by electrical charges / ultraviolet and
differs from normal oxygen in having three atoms in its molecule, also
having density value up to 2.14 kilogram per meter cubic. Ozone is soluble
in water, sulphuric acid, carbon
rapidly

were

many

tetrachloride.

Ozone

molecule

react

chemical compound and is explosive in concentrated

amounts. Ozone is less abundant with a typical range of 20 to 100 ozone

molecules for each billion air molecules. Highest surface values resulted
when ozone is formed in air polluted by human activities.
Objective
Ozone climatic test chamber. This chamber is use to evaluate
ozone ageing resisting performance of rubber and the protective efficacy of
anti-ozone so as to take effective ozone-ageing resisting measures to extend
lifespan of the rubber product. Whole ozone generating and capture process
is performed in airtight loop, which guarantees the safety of people.
Apparatus
Ozone chamber and thread sample
Procedure
Static
1. Cut sample into 14 cm long (2 cm at each end is for gripping purpose).
2. Put the sample at the static sample holder and cut the overleft sample.
3. Set the timer and the temperature control as required.
Eg,

Timer: 3 min
Temperature: 40C
Ozone concentration: fixed at 50 pphm.

4. On all switches; ozone, temperature, static motor, fan and lamp.

5. Close the chamber and on the machine.

6. Observe the changes occur on the sample and record.
7. Off the machine and let the machine for 30 minutes for the machine to
clean up the ozone in the chamber before taking out the sample.

Dynamic
1. Cut sample into 20 cm long (2 cm at each end is for gripping
purpose).
2. Put the sample at the dynamic sample holder and cut the remaining
sample.
3. Set the timer, dynamic control and the temperature control as
required.
Eg

Timer: 3 min
Temperature: 40C
Dynamic counter:
5000
Ozone concentration: fixed at 50
pphm.

4. On all switches; ozone, temperature, dynamic motor, fan and

lamp.
5.
Close the chamber and on the
machine.
6. Observe the changes occur on the sample and
record.
7. Off the machine and let the machine for 30 minutes for the machine to
clean up the ozone in the chamber before taking out the sample.
11.1.7 Break test
Break test is done to check the tensile strength, elongation at break and
300% modulus of the thread. Tensile strength is the stress at which the
thread breaks when it is stretched under specified conditions. The value
is expressed in Kgf/cm2 or gm/mm2 and is referred to as the initial
cross-sectional area. Elongation at break is the increase of length of the
thread

at

break

when it is stretched

under

the specified

conditions,

expressed as the percentage increase of the original length. While 300%

modulus is the stress, measured in Kgf/cm2, calculated on the original
cross-sectional area, at a specified elongation (here at
300%) on an unmassaged
thread. Procedure

1. Prepare the multiple loop sample (Number or loop is depending on

count) Eg: Based on references, for count 42;
i.

(1 8.0) = 8 2 = 16 round, for both break test and VRS

test. ii.
iii.

cut and weigh filament

filament weight 3.2

m

eg : 298 3.2 = 953.6 (value to be key-in as

area) Multiple loop sample.

2. Select Break test after opening Trapeziumx.

3. Select Quick setting panel and key-in the area calculated before.

4. Put sample at the loop holder and re-zero the force and stroke column
by right-click.
5. Start the test.
6. Save the data.

11.1.8 VRS test

The Schwartz value of a thread is the mean modulus, on extension and
retraction during the sixth cycle of a sample of thread which has been
extended to and retracted

from an elongation 100% greater than the

elongation at which the modulus is required. For example, if a Schwartz

value at 300% elongation is desired the thread sample is extended from 0%
to 400% and back six times, and on the sixth cycle the force at 300% is
noted both on extension and retraction. The average of these two modulus
measurements is the 300% Schwartz value. It is usual to use special pneumatic
grips or to use knotted loops of thread for tensile testing. Massaged thread is
the subjection of the sample, before any readings are taken, to a number of
cycles of elongation to, and retraction from, an elongation greater than that
at which the readings will be made, in order to eliminate the effects of
storage on the physical properties of the thread and to reproduce as far as
possible the conditions of use.
Procedure
1. Prepare the multiple loop sample (Number or loop is depending on
count) Eg: Based on references, for count 42;
iv.

(1 8.0) = 8 2 = 16 round, for both break test and VRS

test. v.
vi.

cut and weigh filament

filament weight 3.2 m

eg : 298 3.2 = 953.6 (value to be key-in as area)

Multiple loop sample.

2. Massage the loop using the massage machine.

3. Select VRS test after opening Trapeziumx.

4. Select Quick setting panel and key-in the area calculated before.

5. Put sample at the loop holder and re-zero the force and stroke column
by right-click.
6. Start the test.
7. Save the data.

11.1.9 Break Newton test

Procedure
1. Based on references, for count 42;
i.

1 round, for both break test and VRS

test. ii.
iii.

cut and weigh filament

filament weight 3.2 m

eg : 298 3.2 = 953.6 (value to be key-in as
area) Single loop sample.

2. Select BreakN test after opening Trapeziumx.

3. Select Quick setting panel and key-in the area calculated before.

4. Put sample at the loop holder and re-zero the force and stroke column
by right-click.
5. Start the test.
6. Save the data.

11.2 Defects
i.

colour problem

ii.

high/low

separability iii.
iv.

overlap

soft/stiff

rubber v.

stick

thread
vi.

dry/wet paste built up

Example:
Types of defects
Bent thread

Wavy thread

Dirty thread

Split ribbon in box

Thick thread

Dirty ribbon

70 | I N D U S T R I A L

TRAINING REPORT

Sampl
e

CHAPTER 12
12.0 Research and Development (R&D activity)
12.1 Ageing
12.1.1 Natural ageing
With wax, without wax, different passage, with Rilox, NW Trial, HW Trial,
without Rilox, different curing belt speed, trial low maturation, direct
compound, different loading, silicone with wax and clay mixed.
Procedure
1.
Many samples are prepared as break, VRS test and Newton test
sample.
2. 3 of the samples are taken to do test (Break test, VRS and Newton
test respectively).
3. For 6 months in a row, 3 samples are taken to do testing per
month.
4.
The results are tabulated
analysed.
12.1.2
ageing

and

Accelerated

Accelerated ageing tests on rubber thread in a relaxed state are made in order
to determine the change in physical properties of a rubber thread subjected to
hot-air treatment at atmospheric pressure at a controlled temperature and for
a specified time. These accelerated-ageing tests have only a comparative
value and may not be taken as an exact indication of the storage life of
rubber threads, as the test conditions cannot reproduce all the various aspects
of storage.
In

Rubberflex,

this

accelerated

ageing

testing

is

mostly

done

to

compare competitors aged product with Rubberflex product. Competitors

sample supplied are mostly 3 months to 1 year age. In order to compare
with
thread
from
S T the
RIA
L TR
A I Rubberflex,
NING R
71 | I N D U
EPORT

fresh samples are taken and accelerated

ageing is done. Some sample are prepared and tested for its properties and
the remaining samples are stored in

72 | I N D U S T R I A L

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TRAINING R

oven (55 C) for 4, 48, 7 , 96 hours and wi l be prepared for testing after
the
period.
Table 12: Representation of hot-air treatment.
Hours

Representation (Months)

24

48

72

96

12

The ageing properties of a rubber thread are normally evaluated by

measurements of tensile strength, elongation at break and Schwartz value.
12.2 Competitors
The list below is also the manufacturers of latex thread. They are manufacturers
from Indonesia and Thailand, producing small quantity of rubber thread. Some
of these companies only produce small count latex thread.
1. NRT
2. HVFILA
3. Longtex
4. Swasthy
5. Worldflex
6.

Roundex

CHAPTER 13
13.0 Appendix
Appendix 1
OZONE CHAMBER DO
1. Read the manual in detail and follow the instructions.
2. Clean the unit regularly.
3. Use only genuine spares.
4. Attend immediately to anything unusual.
5. Maintain logbook to monitor operation of the unit.
6. Attend to repairs/services with qualified technicians only.
7. Tighten all screws after every two test cycles.
8. Keep the gear box and moving part well oiled.
9. Provide proper Earthing to the instrument.
10. If you observe any abnormal noise during operation, please contact Prestos
Service
personnel.
OZONE CHAMBER DONT
1. Neglect regular and preventive attention
2. Keep any tools or loose items on or inside the unit
3. Meddle with any setting or carry out adjustments without technical information
4. Run the unit without its cover
5. Do not open the door when Ozone is ON.
6. Ozone is highly inflammable; do not bring naked light near equipment
7. Do not inhale ozone directly from chamber
8. Do not do any repair work while the unit is running
9. The unit for a very long periods.