CHAPTER 3 METHODOLOGY and EXPERIMENTAL DESIGN

3.1

INTRODUCTION

The previous chapter summarised the literature review on aggregate for concrete
manufacturing, concrete in general, and the use of concrete in acoustic barriers. The
specific focus of the literature review was an evaluation of:

recycling of concrete waste

usage and properties of RC Aggregate

concrete technology issues resulting from the use of RC Aggregate in new concrete

testing and research techniques used in concrete technology and material science to
examine the basic physical and mechanical properties, especially those related to
porosity of aggregate and concrete

use of non-destructive techniques including neutron scattering in the examination of

microstructure of cementitious materials

use of concrete in acoustic products specifically in acoustic barriers for urban

freeways; and

acoustic properties and acoustic testing of concrete barriers

The review of literature has been authenticated through ongoing personal contact with
professionals representing the concrete industry. They include concrete recyclers,
concrete product manufacturers as well as researchers in the relevant research fields that
include technical staff operating scientific instruments.

Consulted professionals

included members of the following organisations:

Division of Building, Construction and Engineering, Commonwealth Scientific
Industrial and Research Organisation (CSIRO), Melbourne
Physics Department and Waste Management Group, Australian Nuclear Science
Technical Organisation (ANSTO), Lucas Heights, Sydney
Acoustic Laboratories, RMIT University, Melbourne
Concrete Institute of Australia (CIA), Victorian Branch, Melbourne
Cement and Concrete Association of Australia, Melbourne
Recycling Industries Pty. Ltd., Alex Fraser Group, Laverton North, Melbourne
Westkon Precast Concrete Pty. Ltd, Sunshine, Melbourne
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Hollow Core Concrete Pty. Ltd., Laverton North, Melbourne

Unicrete Industries Pty. Ltd., Braybrook, Melbourne
Boral Testing Services (Concrete Laboratories), Boral Resources Pty Ltd, Thornbury,
Melbourne
Vicroads, Environmental Services, Kew, Melbourne
Geoscience Australia, Symonston, Canberra
University of Melbourne
Monash University, Melbourne
New York City Transit Authority, New York
The following chapter outlines the experimental and developmental program that was
devised for this research project. The experimental program was aimed at examining
and gaining an understanding of the engineering properties of RC Aggregate and RA
Concrete and differentiating these alternative materials from commonly used natural
aggregate and standard concrete.

The experimental program also included an

examination of physical properties of fine aggregate, and the effect on durability of

concrete. The developmental program aimed at utilizing inherent properties of RC
Aggregate in the development of less-fines RA Concrete and the use of such concrete
in acoustic barriers. The research gained from the experimental and developmental
programs that have been devised, was the result of literature surveys, guidance from
standard test procedures and consultations with professionals in related fields.
The experimental and developmental components of this research project were divided
into four distinctive stages:
EXPERIMENTAL
An examination of physical properties and the effect of fine aggregate grading on
durability of concrete
An examination of RC Aggregate physical and mechanical properties

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DEVELOPMENTAL
The development of RA Concrete and examination of its physical, mechanical and
acoustic properties
The development of a pre-cast RA Concrete acoustic barrier and examination of its
acoustic properties

3.2

EXPERIMENTAL and DEVELOPMENTAL PROGRAM - OVERVIEW

The experimental design and developmental program was divided into four stages. The
first two stages were associated with an assessment of existing materials and
differentiating between commonly used natural aggregate for concrete and alternative
recycled concrete aggregate, whereas the final two stages were associated with the
development of new products made from selected RC Aggregate. Table 3.2.1 presents
definitions of the four major stages of the experimental and developmental programs
whereas Figure 3.2.1 further outlines the project stages by introducing major phases of
the project.

Table 3.2.1 Experimental design program - major stages

Stages
Stage definition
EXPERIMENTAL
Stage 1
Investigation of impact of fine aggregate grading on durability of concrete
Stage 2
Examination of RC Aggregate and limited investigation of quarry sourced local
basalt (Natural Aggregate)
DEVELOPMENTAL
Stage 3
Development and examination of RA Concrete and limited examination of NA
Concrete (control concrete)
Stage 4
Development and examination of RA Concrete acoustic barrier

The initial stages of the experimental program of this research project aimed at
examining RC Aggregate properties in order to obtain necessary data, enabling the
design of RA Concrete mixes, and allowing a thorough characterisation of the concrete.
Furthermore, it also included testing of an acoustic barrier that was developed to utilise
some inherent or purposely modified properties of RC Aggregate and RA Concrete.

3-3

Normal density
NA Concrete
(+)

Natural (N)
Aggregate

No-fines
NA Concrete

Fine
Aggregate

(+)

RC
Aggregate

Normal density
RA Concrete
No-fines
RA Concrete

Less-fines
RA Concrete
Stage 1

Stage 2

Stage 3

Acoustic
Barrier
Stage 4

Figure 3.2.1 Outline of the experimental and developmental program

The four main stages of the experimental and developmental programs were further
divided into a number of phases where each phase dealt with a specific property of
either; the aggregate, concrete, or acoustic barrier. In some instances, control samples
of natural aggregate (local basalt) and concrete made from such aggregate were deemed
as necessary for comparison purposes.

Table 3.2.2 outlines all stages of the

experimental program; properties examined at each stage; and testing methods or

procedures used.

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Table 3.2.2 Project stages and properties tested

Stages
Stage 1
Stage 2

Stage 3

Stage 4

Stage
definition
Fine Aggregate
RC Aggregate
and/or
N Aggregate

RA Concrete
and/or
NA Concrete

Acoustic
Barrier

Properties & research techniques

EXPERIMENTAL
Particle size distribution - PSD
Composition (cpr content)
Elemental composition SEM
Cement content in aggregate fines
Impurities and foreign material
Particle size distribution PSD
Particle density
Bulk density
Water absorption
Porosity SANS
Porosity BET
Consistency and workability slump test
Microstructure development SEM
Mass per Volume
Compressive strength
Durability VPV
Porosity / micro-cracks SEM
Porosity SANS
Porosity BET
DEVELOPMENTAL
Interconnected air voids content
Sound absorption impedance tube
Design and manufacture
Sound absorption reverberation room

Test
procedures
AS1141.11
Procedure #1
SEM
AS1141.72
Procedure #2
AS1141.11
AS1141.6.1
AS1141.4
AS1114.6.1
SANS
BET
AS1012.3.1
SEM
AS1012.12.1
AS1012.9
AS1012.21
SEM
SANS
BET
Procedure #3
AS1935
AS3600
AS1045

In the first two stages, the fine and coarse aggregates were examined from a strength,
durability, and acoustics requirements perspective to provide data for further use in the
development of an optimum concrete mix design.

The decision to use the 14/10mm

RC Aggregate as a coarse fraction necessitated the use of a well graded fine aggregate.
As a consequence, it was necessary to examine locally available fine aggregate from
major suppliers of concrete sand in the Melbourne metropolitan area. The particle size
distribution of concrete sands from six different sources were examined in order to
derive the fineness modulus (FM), often used as a supplementary parameter
characterising fine aggregate.
Furthermore, RC Aggregate was examined to quantify foreign materials such as bricks,
wood, plastic, metal, etc in the aggregate. An excessive amount of contaminants was
3-5

perceived to have a potentially deleterious effect on the strength and durability of

concrete made from RC Aggregate.
Basic engineering properties of RC Aggregate such as particle size distribution, water
absorption and particle density were investigated in order to assist in the concrete mix
design, as well as to expand the existing body of knowledge on this material. This was
followed by a more detailed examination of porosity of the aggregate which was
deemed to influence physical and mechanical properties of RC Aggregate.
The 14/10mm RC Aggregate was tested for its paste/aggregate composition i.e. the
relative amounts of cement paste residue (cpr) and natural rock in the aggregate. The
relative amount and quality of cpr was perceived to influence particle density,
aggregates overall porosity and water absorption. The paste/aggregate composition of
the aggregate was examined in accordance with an in-house method developed by the
author (see Appendix 1), that included a combination of mechanical separation, visual
inspection and subsequent mass measurements of each constituent. Relative amounts of
cement paste residue and natural aggregate were also examined by mapping images
obtained from a Scanning Electron Microscopy (SEM) examination. Within SEM and
micro-cracks examinations, backscatter images were taken at very low magnifications
(15 to 30 times). Photographs of concrete specimens that were cut and used for other
tests were also examined.
Apart from the investigation of paste/aggregate composition of RC Aggregate, an
elemental and compound composition examination of cement paste residue of the
aggregate was also carried out. Although the area examined by the SEM is relatively
small and could perceived to be less representative, it was recognised that this test could
give a valid indication of elemental and compound composition along with evidence of
any chemical contaminants present in cement paste residue of RC Aggregate.
Crushed cement paste residue and fines of RC Aggregate were also examined for
elemental composition using the Scanning Electron Microscopy examination. The fines
were also examined to investigate re-cementing properties of the aggregate.
Following basic characterisation, more detailed tests were then employed to examine
the porosity of cement paste residue of RC Aggregate. A non-destructive neutron
3-6

scattering method, the Small Angle Neutron Scattering (SANS) was used to examine
total porosity and fractal dimensions of pore structure. This was followed by BrenauerEmmett-Tellers (BET) nitrogen adsorption method to determine the volume, size and
surface area of pores. Table 3.2.3 summarises the properties that were tested, along
with the number and size of test samples of natural and RC Aggregate.

Table 3.2.3 RC Aggregate and Natural Aggregate examination summary

Aggregate type
and property
examined
Fine aggregate
PSD
Coarse aggregate
Aggregate
composition
Elemental
composition

Test
procedures

Number of
samples per
test

Frequency of tests
/ total number of
tests

Sample size

AS1141.11

500g

Procedure #1
(Appendix 1)
SEM

1 in 4 months, 12
lots, 35
1 in 6 months
18

1.5kg

Cement content
Foreign materials
and impurities
PSD

AS1141.72
Procedure #2
(Appendix 1)
AS1141.11

1
1
2

Particle density
Bulk density
Water absorption
Porosity
Porosity

AS1141.6.1
AS1141.4
AS1141.6
BET
SANS

2
2
2
5 10
7

2-3

4
Every month
32
Every month
(64+6)70
24
24
24
21
7

Slabs
2 x 20 x 20mm
Powder ~2g
Powder ~ 80g
5kg
2kg
2kg
~ 15kg
2kg
~ 5mm
6 x 6 x 6mm

The third stage of the project dealt with the development and characterisation of RA
Concrete, with a specific focus on the investigation into an optimum relationship
between porosity of RC Aggregate and physical and mechanical properties of RA
Concrete. Initially the development of RA Concrete included devising concrete mix
designs of normal density concrete of various compressive strengths ranging from
15MPa to 40MPa, which later was limited to a compressive strength of RA Concrete of
25MPa. In addition, mix designs of no-fines RA Concrete were devised, and properties
investigated. Control samples of concrete made from natural aggregate (local basalt)
for both normal density and no-fines concrete were also prepared and examined. A
concept of less-fines concrete emerged, resulting in the development of a two-layered
concrete viz. solid and porous.

Methods of mix proportioning of less-fines RA

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Concrete were devised, and samples with various relative thickness of solid and porous
layers were investigated.
The scope of the RA Concrete examination and adopted procedures related to a type of
concrete classified as; normal density, no-fines or less-fines. Plastic properties of
less-fines and no-fines RA Concrete were assessed by a visual inspection, whereas in
the case of normal density concrete, consistency and workability of fresh concrete were
tested by a standard slump test. Properties of hardened concrete, such as mass per
volume, compressive strengths and apparent volume of permeable voids (VPV) were
tested in the Concrete and Fluid Mechanics laboratories at Swinburne University of
Technology (SUT) using standard equipment.
Samples used for examining the microstructure development in RA Concrete using
SEM were cut from test specimens using a concrete saw. Samples were examined for
the presence of micro-cracks and microstructure development with a specific focus on
the boundary zone between new cement paste and cement paste residue of the
aggregate. Some of the slab-like specimens used in SANS experiments were also
examined by SEM to determine elemental composition.
Porosity characteristics of RA Concrete including total volume of pores in concrete
matrix, volume of micropores, pore size distribution and specific surface area were
determined using the BET nitrogen adsorption method.

A supplementary non-

destructive SANS method was also used to examine pore structure and to determine the
fractal mass, a parameter describing roughness of pores in RA Concrete.

The

Australian Nuclear Science and Technology Ogranisation (ANSTO) facilities at Lucas

Heights were used to prepare and test concrete specimens over the period of 1999 to
2002.
A less-fines RA Concrete of various relative thicknesses of solid and porous layers
was then examined to gauge concrete durability using the VPV method. The amount of
partly interconnected air voids in porous layers was measured using the water
displacement method.

Sound absorption of less-fines RA Concrete was then

determined through the impedance tube method.

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Although a 28-day continuous moist curing regime was adopted in the case of all test
specimens of NA and RA Concrete, an allowance for alternative curing by PE sheet
wrapping was made. A limited number of the slab-like specimens prepared with D2O
were cured for 56 days in deuterium oxide. Table 3.2.4 presents an outline of the
testing program for the concrete examination, the frequency of tests, and number and
size of test specimens.
Table 3.2.4 RA and NA Concrete development and examination summary
Concrete type &
property
examined
Normal density
Consistency
Microstructure
development
Mass per volume

Testing
procedures

Number of
samples per
test

AS1012.3
SEM

1
2-3

Compressive
strength (fc)
Durability - VPV

AS1012.9

Porosity /
microcracks
Porosity

SEM

AS1012.12.1

AS1012.21

SANS

Frequency of tests
/ total number of
tests

Every batch
1 in 4 months
11
3
Every batch / mix
design 40
3
Every batch / mix
design 40
2 or 3
Selected mixes
(sliced into 4) 12
2-3
1 in 4 months
11
10
1 per year
20

Porosity
No-fines
Consistency
Microstructure
Mass per Volume

BET

5-10 particles

1 in 4 months 34

Visual
SEM
AS1012.12.1

2-3
3

Compressive
strength
Durability - VPV
Less-fines
Consistency
Mass per volume
Interconnected air
voids
Sound absorption

AS1012.9

AS1012.21

2 (sliced in 4)

Every batch
1 in 4 months
Every batch / mix
design
Every batch / mix
design
Selected mixes 10

Visual
AS1012.12.1
Procedure #3
(Appendix 1)
AS1935

1
3
1

Every batch
12
34

Sample size

~ 0.025m3
3 x 20 x 20mm
150 x 300mm
150 x 300mm
100 x 200mm
3 x 20 x 20mm
Powder ~2g
5 x 5 x 5mm
2 x 20 x 20mm
~ 5mm
~ 0.025m3
2 x 20 x 20mm
150 x 300mm
150 x 300mm
100 x 200mm
~ 0.025m3
83 x 150mm
83 x 150mm
100 x 200mm
83 x 150mm

The final stage of the project consisted of the design, development and testing of a
prototype and commercially manufactured acoustic barrier made from the 14/10mm RC
Aggregate. The requirements set for acoustic barrier design were to best utilize the
3-9

physical and mechanical characteristics of the less-fines RA Concrete and its ability to
absorb and reflect sound energy. A total of approximately 11m2 of the barrier prototype
was manufactured in pre-cast panels, in the Concrete and Heavy Structures laboratories
at Swinburne University of Technology. Panels were air cured for 28 days, before
being transported and tested at the Acoustic Laboratory at RMIT University in
Melbourne.

The same design and similar production procedures were applied to

commercially manufactured barriers at Westkon Precast Concrete Pty Ltd. Panels sized
1 x 4 metres were manufactured, air cured, and cut into three parts to enable their
placement in the reverberation chamber. The reverberation room method was used to
measure the sound absorption coefficient of the prototype, and of commercially
manufactured barriers (SAA, 1988). Table 3.2.5 summarises the final stage of the
project experimental and developmental program.

Table 3.2.5

Prototype and commercially manufactured acoustic barrier

examination summary

Property

Testing
procedure

Sound absorption
Sound absorption

AS1045
AS1045

Number of
samples
per test
12
9

Frequency of
tests / total
number of tests
1
1

Sample size
150 x 850 x 1250mm
150 x 1000 x 1300mm

The experimental program of the project also included the use of the Australian Small
Angle Neutron Scattering (AUSANS) facilities at ANSTO, Lucas Heights. The SANS
technique was used to determine the pore structure of the RC Aggregates cement paste
residue, and microstructure of RA Concrete in a range of pore sizes ranging between
10 and 100. The SANS experimental program was employed to supplement the
BET nitrogen adsorption examination of microstructure of the aggregate and concrete
which can measure porosity in the range of pore sizes between 17 and 3m. Apart
from the standard specimen preparation for SANS testing, some specimens were
prepared and cured with deuterium oxide (D2O).

The curing regime for samples

prepared with H2O was a 28-day continuous curing in light water, whereas specimens
prepared with D2O were continuously cured for 56 days in deuterium oxide.
The SANS experimentation was carried out in four rounds: September 1999, March
2000, May 2001, and January 2002.

Initially, irregularly shaped samples of RC

Aggregate particles were investigated, then cubic samples 6 x 6 x 6mm were cut from
3-10

the aggregate, and finally two lots of the slab-like 2 x 25 x 25mm samples of RA
Concrete were prepared and examined.

Table 3.2.6 shows the AUSANS testing

program.

Table 3.2.6
Round
1999
2000
May 2001
May 2001
January 2002
January 2002

AUSANS sample suite

Shape and size of

samples
Irregular aggregate
Cubic 6 x 6 x 6mm
Slabs 2 x 25 x 25mm
<150m powder
Slabs 2 x 25 x 25mm
(H2O made)
Slabs 2 x 25 x 25mm
(D2O made)

No. of
samples
4
7
10
6
4
6

Moisture conditions
Oven dry
Oven dry, H2O, D2O
Oven dry, H2O, D2O
Oven dry
Oven dry, H2O, D2O,
50% H2O + 50% D2O
D2O, oven dry, H2O,
50% H2O + 50% D2O

Concurrently with the AUSANS experimentation, the pore structure of RC Aggregate

and RA Concrete was examined using the Brunauer-Emmett-Teller (BET) nitrogen
adsorption technique, which was chosen to measure pore size distribution in a range
partially overlapping with SANS.

Controlled standards were created for natural

aggregate (local basalt), and of the cement pastes of water/cement ratios of 0.2, 0.4, and
0.8.

These standards were used as the benchmark porosity for subsequent

characterization of the aggregate and concrete. The pore structure of the cement paste
residue of RC Aggregate, and those of RA Concrete were then compared with control
standards. Six lots of test specimens were prepared and examined at the Micromeretics
Laboratory at Swinburne University of Technology.

Some tested specimens were

previously examined by the non-destructive SANS technique. Table 3.2.7 shows an

experimental design program of the BET nitrogen adsorption experiments.

Table 3.2.7

BET nitrogen adsorption test program

Samples
Natural aggregate (na), 0.2 cp
0.8 w/c new cement paste (0.8 cp)
0.4 w/c new cement paste (0.4 cp)
RC Aggregate cement paste residue
(rca-cpr), old cp +na, na + old cp
0.8 cp + rca-cpr
0.4 cp + rca-cpr

Examination date & number of samples

May Oct April May June Dec
2
1
2
10
6
1
3
3

Jan
2

3-11

The following sections present details of research methods and test procedures adopted
in the experimental and developmental programs of the project. Account or reference is
given to experimental setup, laboratory equipment, detailed procedures, and laboratory
reports requirements.

3.3

FINE AGGREGATE

The quality and properties of fine aggregate including aggregate grading amongst other
factors have an influence on the durability of concrete. In Victoria, it is preferred to
express the durability of hardened concrete as the apparent volume of permeable voids.
To formulate durable concrete made from alternative coarse aggregate, the cement paste
surrounding RC Aggregate has to be of the highest possible quality. The purpose of
examining the grading of fine aggregate was to select an aggregate that would yield the
highest quality of cement paste in new concrete. Subsequently, properties of the six
different concrete sands used in the Melbourne metropolitan area were investigated.
The particle size distribution (PSD) was examined and one single parameter known as
the fineness modulus (FM) was derived for each of the fine aggregate. Table 3.3.1
presents the sources of fine aggregate.

Table 3.3.1
Source 1
Pronto
Langwarrin

Source 2
Pioneer
Heatherton

Fine aggregate sources

Source 3
CSR
Lyndhurst

Source 4
Pronto
Yea

Source 5
Boral
Langwarrin

Source 6
Boral
Bacchus Marsh

Representative samples were obtained directly from a stopped conveyor belt at various
concrete production plants. A sampling frame was used and procedures described in the
Australian Standard AS1141.3.1-1996 Methods for sampling and testing aggregate,
Method 3.1: Sampling aggregates were followed. Three samples of 5kg each, per
every supplier, were obtained in five equal increments. Samples were bagged and
labeled. In addition, an adequate amount of fine aggregate to produce nine (9) concrete
test specimens was obtained.

3-12

3.3.1 Particle Size Distribution

The Australian Standard AS 1141.11 1996 Methods for sampling and testing
aggregates, Method 11: Particle size distribution by sieving procedures was followed
to determine the grading of fine aggregate. A standard sieve set ranging between the
4.75mm sieve to 0.075mm was used. Test portions of 500g were used and the sieve set
was hand agitated. Tests were performed at the Geotechnical Laboratory at SUT.
A parameter known as fineness modulus (FM) of sand was then estimated using the
particle size distribution data. The FM is a sum of cumulative percentages retained on
the standard sieves (0.150, 0.300, 0.600, 1.18, 2.36 and 4.75mm) divided by 100
(Nawy, 1997).

3.4

NATURAL (N) COARSE AGGREGATE

Any natural aggregate chosen for this research project had to bear a resemblance to
grading characteristics of the 14/10mm RC Aggregate, of which the examination was
the main purpose of this research. Ideally, shape and surface texture of N Aggregate
should also be similar to those of RC Aggregate, although differences in raw materials
used for the production of the aggregates made it difficult to match those characteristics.
Local basalt supplied by the Boral Quarry Pty Ltd was deemed suitable on the basis of
similar particle size distribution.
Sampling of N Aggregate was in accordance with the Australian Standard AS1141.3.11996 Methods for sampling and testing aggregate, Method 3.1: Sampling aggregates.
Representative samples were obtained directly from a stopped conveyor belt at concrete
production plants.

A sampling frame was used to obtain the 15kg representative

samples in five equal increments. To obtain the required grading, some single sized
aggregate had to be added to the aggregate supplied by Boral Quarry Pty Ltd. Test
portions for specific tests were derived using a sampler divider.

3-13

3.4.1 Particle Size Distribution

The Australian Standard procedures described in AS1141.11-1996 Methods for
sampling and testing aggregates, Method 11: Particle size distribution by sieving was
followed to determine the grading of N Aggregate. Test portions of 2kg were used. A
standard sieve set, and hand agitation was used. Particle size distribution tests were
performed when comparison data to those of RC Aggregate had to be generated. In
total, six samples were tested over a period of three (3) years. Tests were conducted at
the Geotechnical Laboratory at SUT.

3.4.2

Elemental Composition

A semi-quantitative analysis of the natural aggregate in slab-like samples prepared for

SANS or other SEM samples where micro-cracks were examined was performed. The
data was used to establish standards for an elemental and compound composition of
natural aggregate.
The SEM examination was performed using a JEOL JSM840 Scanning Electron
Microscope equipped with EDS (Energy Dispersive X-ray Analysis), under the
guidance and assistance of Mr. Hans Brinkies at the Electron Microscopy Laboratory at
Swinburne University of Technology, (SEM, 1999). The same equipment and technical
support was used in other experiments involving SEM. Section 3.5.4 outlines the
testing procedures and sample preparation regime.

3.5

RECYCLED CONCRETE (RC) AGGREGATE

The coarse aggregate used in this research project is a commercially available product
known as 14/10mm RCA. The aggregate is manufactured by Recycling Industries Pty
Ltd at the Alex Fraser Group of Companies. At present, the 14/10mm RC Aggregate is
being used as a partial substitute for coarse aggregate in various types of concrete,
including low strength concrete for footpaths or construction of residential slabs
manufactured by Hi-tech Concrete Pty Ltd in Melbourne. The choice of this aggregate
3-14

was based on results of previous investigations into concrete recycling by the author,
and also instigated by the request of the industrial partner of the project. It has been
decided that this aggregate would be the most suitable for the production of concrete
acoustic barriers.
Representative samples of RC Aggregate were obtained by the author or supplied by the
company from its stockpiles at the concrete recycling plant at Laverton North, Victoria.
Sampling from the side of the stockpile was carried out with the use of a board and
shovel, and samples were placed in sealed plastic bags. Procedures described in the
Australian Standard AS1141.3.1-1996 Methods for sampling and testing aggregate,
Method 3.1: Sampling aggregates were followed. The 20kg samples were obtained in
five equal increments. Sample portions for specific tests were reduced using a sample
divider.

The frequency of specific tests was accordingly adjusted to the relative

importance of examined property to the overall objectives of the project.

3.5.1

Cement Paste Residue (cpr) Content

Determination of the content of cement paste residue in RC Aggregate was carried out
in accordance with procedures devised by the author (see Appendix 1).

Initially,

particles of clean natural aggregate, aggregate coated with cement paste, and fragments
of cement paste residue were segregated. Particles of aggregate coated with more than
approximately 10% of cement paste residue were then broken to smaller pieces until
natural aggregate and cpr were separated. Test portions of 1.5kg were used. Test
portions were reduced from combined samples collected over a three month period
between January 1999 and October 2001. A total of thirty two (32) representative
samples of RC Aggregate were reduced to twelve (12) test portions. The tests were
carried out at the Concrete Laboratory at Swinburne University of Technology.
RC Aggregate composition was also determined from area mapping of RA Concrete
samples, which were cut for some other tests, mainly in the VPV and SANS
examinations.

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3.5.2

Impurities and Foreign Materials Content

Occurrence of any other materials other than natural aggregate and cement paste residue
in RC Aggregate may adversely affect compressive and tensile strength, abrasion
resistance, surface finish, and durability of new concrete.

The content of foreign

materials in RC Aggregate was assessed by a method devised by the author (see

Appendix 1). The classification of foreign materials in RC Aggregate is listed as
follows:
A. Brick particles
B. Plasterboard pieces (gypsum)
C. Mortar (cement-lime)
D. Wood pieces
E. Other organic matter such as grass, paper, etc
F. Clay particles
G. Bitumen
H. Plastic
I. Steel fibre-reinforcement
J. Glass
K. Pebbles or other aggregate coated with paint or other protective coating
L. Miscellaneous (paint, foam, etc)
Foreign materials were then further classified as lighter or as heavier than 1,000kg/m3.
Light impurities such as wood, other organic matter and plastic, tend to adversely affect
the durability and surface finish of concrete. A simple test was devised to determine the
weight of particles and isolate particles lighter than 1,000kg/m3. All foreign material
was submerged in water, separated, oven dried and weighed.
The frequency of occurrence of each class of foreign material in 14/10mm RC
Aggregate was recorded and, along with other information on the quality of the
aggregate, shared with the industry partner.
A total of thirty two (32) samples of the 14/10mm RC Aggregate were examined
between January 1999 and August 2001. The visual assessment of RC Aggregate,
3-16

classification of foreign materials, and determination of their content by weight was

carried out at the Geotechnical Laboratory at SUT.

3.5.3

Cement Content in RC Aggregate Fines

One of the assumptions developed during the early stages of the project was that
particles smaller than 75m might contain traces of unhydrated cement, as some of the
RC Aggregate is produced from relatively fresh concrete waste. A modified method
was adopted to determine any content of cement in aggregate fines. The method
described in the Australian Standard AS1141.72-1996 Methods for sampling and
testing aggregate, Method 72: Cement content of cement stabilised materials was
modified by the author. The modification included removal of the fines, and subsequent
substitution of the stabilised cement with RC Aggregates fines.
Fine particles smaller than 75m were removed from the RC Aggregate through
sieving. A total of eight (8) samples were prepared where three (3) samples were used to
derive a calibration curve, and five (5) to determine the amount of unhydrated cement in
the aggregate.

The calibration curve was derived using 14/10mm RC Aggregate

without particles smaller than 75m and GB cement. A portion of 20g of cement was
used, which is equivalent to 0.5% of cement content. The GB cement was chosen as it
has a relatively high content of pozzolanas and exhibits a mineral composition that is
closer to the elemental and compound distinctiveness of RC Aggregates fines, as the
SEM examination had indicated.
The test portions consisted of 4kg of 14/10mm RC Aggregate, plus 80g of particles of
75m or below. The 80g portion size was derived from an average content of 2% in all
of the RC Aggregate samples. There were no other deviations from the standard
procedures. Tests were conducted at the Chemistry Laboratory at SUT.

3-17

3.5.4

Microstructure and Elemental Composition

The Scanning Electron Microscopy was used to examine elemental (based on assumed
compound) composition of cement paste residue of RC Aggregate, and to examine the
aggregates microstructure (SEM, 1999). The SEM was predominantly used to identify
micro-cracks in the aggregate itself, and in the transition zone between new paste and
RC Aggregate.
Solid slab-like samples and powder samples were examined. The solid samples, 3mm
thick, 20 x 20mm, were cut from larger RC Aggregate particles, collected at the
Laverton North concrete recycling plant during the crushing process of concrete waste,
or alternatively, cut from the concrete made from 14/10mm RC Aggregate. Powder
samples were grinded to particles below 150m with the use of a laboratory grinder.
The instrument used was the JEOL JSM840, which is a conventional type of Scanning
Electron Microscope, equipped with EDS (Energy Dispersive X-ray Analysis). This
conventional type of SEM requires nonconductive samples to be made conductive. A
carbon coater was used to coat solid samples of RC Aggregate with evaporated high
purity carbon. Carbon coated solid samples were mounted on aluminum disks. Some of
the aggregate were immersed in resin. Powder samples were attached to a double-sided
carbon tape, and mounted on aluminum pin type SEM mounts.
A total of 24 solid and 6 powder samples were examined.

To assure the best

representation of the population of RC Aggregate cement paste residue in these

samples, a number of specific areas of up to 50mm2 were selected. A total of forty (40)
areas of different sizes were examined. The SEM examination of each sample started
with an analysis of Back-scatter Electron (BSE) images of RC Aggregate cement paste
residue surface at low magnifications (15 times), which followed by an EDS of the
selected areas.
The Backscatter Electron images were obtained with an atomic number contrast. At
low magnifications (e.g. 15 times), areas of approximately 48mm2 (8mm x 6mm) were
analysed, whereas at higher magnifications (e.g. 500 times), areas of approximately
3-18

0.0005mm2 (25m x 20m) were assessed.

Dark areas on the BSE images are

representative of elements with a low mean atomic number, such as calcium, whereas
lighter areas are representative of elements with a high mean atomic number, such as
iron.

Elemental spectra were produced, which quantified elements present in the

analyzed areas. Subsequently, a semi-quantitative analysis of elements in their assumed

compound composition was performed, and results obtained. Although the analysis was
semi-quantitative, as the examined samples were not compared against known
standards, the method was assumed as adequate for comparative purposes. To ensure a
high standard and validity of data, the operational conditions of the instrument were
kept constant.
Observations on micro-cracks using BSE images at low magnifications were recorded.
Chosen areas were further analyzed, and some of the BSE images stored as TIFF files.
Elemental spectra and qualitative analysis results were copied as pictures on Microsoft
Word documents.

3.5.5

Particle Density

Standard procedures in accordance with the Australian Standard AS 1141.6.1 2000

Methods for sampling and testing aggregates, Method 6.1: Particle density and water
absorption weighing-in-water method were followed in order to determine the
particle density of RC Aggregate.

This method also allows the determination of

apparent particle density (A), particle density on a dry basis (D), and on a saturatedsurface-dry basis (S). 2kg test portions were examined.
Each test portion was reduced from the combined samples of the three monthly
sampling periods. A total of twelve (12) samples were examined at the Geotechnical
Laboratory at SUT.

3.5.6

Bulk Density

The compacted bulk density of oven dried RC Aggregate was examined.

The

procedures of the Australian Standard AS1141.4-2000 Methods for sampling and

testing aggregates, Method 4: Bulk density of aggregate was followed.

A ten (10)
3-19

litre cylindrical watertight measure was used to determine the compacted bulk density.
A total of fifteen (15) samples were examined between January 1999 and August 2003
at the Geotechnical Laboratory at SUT.

3.5.7 Particle Size Distribution

Determination of RC Aggregate grading followed procedures of the Australian Standard
AS1141.11-1996 Methods for sampling and testing aggregates, Method 11: Particle
size distribution by sieving. The standard sieve set was hand agitated. Two test
portions of approximately 2kg were obtained from monthly samples over a period from
January 1999 to August 2001, and in late 2003. A total of sixty four (64) tests were
examined at the Geotechnical Laboratory at SUT.

3.5.8

Water Absorption

Water absorption of RC Aggregate was determined in accordance with the Australian

Standard AS 1141.6.1 2000 Methods for sampling and testing aggregates, Method
6.1: Particle density and water absorption weighing-in-water method. The 2kg test
portions, obtained from combined three monthly samples over a three (3) year period
were tested. A total of twelve (12) samples were examined. Water absorption was
examined at the Geotechnical Laboratory at SUT.
Water absorption of the aggregate was also determined during the SANS experimental
program. RC Aggregate absorption of light water (H2O) and heavy water (D2O) was
investigated. Although the size of the SANS specimens (6 x 6 x 6mm) was relatively
small and could be less representative, the results that were obtained as a by-product in
the SANS examination were used for comparative purposes. A total of seven (7)
samples were examined at ANSTO laboratories at Lucas Heights.
3.5.9 BET Porosity
Porosity of RC Aggregate in terms of specific surface area, pore size distribution, and
pore volume, was examined using the Brenauer-Emmett-Teller BET nitrogen adsorption

3-20

method (SUT, 1999).

Porosity in pore size, ranging between 17 and 3m, was

examined.
The ASAP 2000 instrument was used with two independent vacuum pump systems; one
for degassing; and one for analysis. The range of pressure measurements varied from 0
up to 950mmHg. Powder and solid samples were placed in sample tubes and examined.
Each solid sample consisted of approximately ten (10) pieces of aggregate and powder
sample weight was approximately four (4) grams. Control standards were established
for cement pastes of 0.2, 0.4, and 0.8 water/cement ratios, either from purposely
prepared pastes or by using the known standards. Samples of RC Aggregate for the
porosity examination using the BET nitrogen adsorption method were selected on a
visual basis.

The cement paste residue samples were classified as either; highly,

moderately, or slightly weathered.

The BET nitrogen adsorption examination of RC Aggregate and then of RA Concrete
was performed under the guidance and assistance of Mr. David Lewis, at the
Micromeretics Laboratory at SUT.

3.5.10 SANS Porosity

The Small Angle Neutron Scattering technique was used to examine the porosity in pore
sizes ranging between 10 and 100. The Australian Small Angle Neutron Scattering
(AUSANS) facilities at the Australian Nuclear Science Technical Organisation
(ANSTO) at Lucas Heights were used to prepare and test RA Concrete samples
(ANSTO, 1999). The SANS results were also used to determine the fractal mass of
pore structure of RC Aggregates cement paste residue. The SANS experimental
program was chosen to complement the BET nitrogen adsorption method, in order to
obtain corresponding data on microstructure of the aggregate.
Examination of RC Aggregate porosity using the SANS technique was carried out in
September 1999 and March 2000.

Initially, irregularly shaped samples of RC

Aggregate particles were investigated, followed by cubic 6 x 6 x 6mm samples. RC

Aggregate cubes were cut out of cement paste residue. All samples were tested in oven
3-21

dried conditions. Table 3.5.1 presents the SANS testing program of RC Aggregate,
cement paste residue.
Table 3.5.1 SANS experiments (1999 and 2000 - sample suite
Month & year
Sep 1999
March 2000

Shape and size of samples

Irregular aggregate
Cubic 6 x 6 x 6mm

No. of samples
4
7

Moisture conditions
Oven dry
Oven dry, H2O, D2O

The SANS investigation was carried out in accordance with ANSTO procedures under
the guidance and assistance of Dr Robert Knot, from the Australian Nuclear Science
Technical Organisation. The same procedures and facilities were also used in the
examination of concrete as outlined in Section 3.6.7 and Section 3.7.7 of this document.

3.6

NATURAL AGGREGATE (NA) CONCRETE

Two types of NA Concrete; normal density, and no-fines concrete were investigated. In
the investigation of compressive strength and volume of permeable voids, concrete
samples were prepared in accordance with the Australian Standard AS1012.8.1-2000
Methods of testing concrete, Method 8.1: Method for making and curing concrete
Compression and indirect tensile test specimens.
All of the NA Concrete samples were prepared at the Concrete Laboratory at Swinburne
University of Technology. Concrete was placed in layers in cylindrical moulds, which
were clamped securely to a vibrating table. Concrete was compacted through the use of
a laboratory vibrating table at a frequency of 50Hz. After initial storage and subsequent
demoulding, specimens were continuously cured in lime-saturated water at a
temperature of 232C for a period of 28 days. Representative concrete specimens for
BET and SANS porosity examinations were cut out of the compressive strength
samples, or cast in specially prepared moulds.
The frequency of preparing and testing of NA Concrete samples was dependent on the
projects overall objectives and availability of the BET and AUSANS facilities. Plastic
and hardened properties of NA Concrete were investigated.

3-22

3.6.1

Workability and Consistency

Workability and consistency of fresh concrete was examined using a slump test in
accordance with the Australian Standard AS1012.3.1-1998 Methods of testing concrete,
Method 3.1: Determination of properties related to the consistency of concrete
Slump test. In the case of normal density NA Concrete, the slump test was performed
on every batch of concrete made using standard procedures and equipment. With
reference to the no-fines NA Concrete, a slump test by observation was deemed to be
valid.

3.6.2

Compressive Strength

The compressive strength of normal density and no-fines NA Concrete was determined
following procedures of the Australian Standard AS1012.9-1999 Methods of testing
concrete, Method 9: Determination of the compressive strength of concrete
specimens. Portland cement mortar capping was adopted for normal density concrete,
and restrained natural rubber capping for no-fines concrete was used to ensure a high
standard of test specimens, and integrity of compression strength test results. Three
specimens per concrete batch were cast, cured and crushed. Cylinders of 150mm in
diameter and 300mm in height were used. All specimens were tested after the 28 day
period of continuous moist curing in the lime-saturated water.

3.6.3

Mass per Volume

All of the NA Concrete specimens prepared for compression strength (three per test)
test, and the VPV (two per test) investigation, were measured and weighed in
accordance with the Australian Standard AS1012.12.1 1998 Methods of testing
concrete, Method 12.1: Determination of mass per unit volume of hardened concrete
rapid measuring method to determine the mass per volume. A total of twelve (12)
samples (representing 36 specimens) of N40, and eight (8) samples (representing 24
specimens) of N25 were examined at the Concrete Laboratory at SUT.

3-23

3.6.4

Apparent Volume of Permeable Voids

The Australian Standard AS1012.21 1999 Methods of testing concrete, Method 21:
Determination of water absorption and apparent volume of permeable voids in
hardened concrete procedures were followed to determine the volume of
interconnected void space in hardened NA Concrete. Specimens of 100mm in diameter
were cut into four equal slices, oven dried to a constant mass, immersed, and boiled in
water. The VPV of 40MPa natural aggregate concrete was examined when the fine
aggregate for this research project was investigated. Six (6) samples; two specimens
each, were examined at that stage.

In addition, the VPV of N25 Concrete was

investigated, to derive a control set of data on volume of interconnected void space in

concrete of a comparable mix design to those of RA25 Concrete. A total of twelve (12)
samples were examined.
The VPV examination of NA Concrete was performed at the Concrete and Fluid
Mechanics laboratories at SUT.

3.6.5

Water Absorption

Water absorption of NA Concrete was determined to create a standard set of data for
comparison purposes. Water absorption was examined in accordance with Australian
Standard AS1012.21 1999 Methods of testing concrete, Method 21: Determination
of water absorption and apparent volume of permeable voids in hardened concrete.
Water absorption of NA Concrete was examined using the same samples as in the
apparent VPV examination.

3.6.6 BET Porosity

Specific surface area, pore size distribution and pore volume of NA Concrete was
examined using the Brenauer-Emmett-Teller BET nitrogen adsorption method (SUT,
1999). Porosity ranging between 17 and 3m was examined in order to establish a
control standard for concrete porosity to be compared with porosity of recycled concrete
3-24

aggregate, and recycled aggregate concrete. The BET measurements were also used to
supplement and compare SANS results of porosity on the same specimens. Samples of
cement pastes of water/cement ratios of 0.4 and 0.8 were prepared, and BET porosity
determined to establish control samples of porosity for comparison purposes.
Instrumentation, sample preparation and test parameters as described in section 3.5.9 of
this document, also apply to the NA examination using BET nitrogen adsorption.

3.6.7

SANS Porosity

The AUSANS instrument at Lucas Heights was used to examine porosity of NA

Concrete.

Sample preparation and testing procedure outlined in the AUSANS

procedures were followed (ANSTO, 1999).

Samples of new cement paste were

prepared. A number of pastes of w/c ratios of 0.2, 0.4, and 0.8 were investigated. Two
cement paste samples per every water cement ratio were prepared. The 0.2 w/c ratio
samples were prepared using a superplasticiser (Type HWR). The data obtained from
the SANS investigation of cement paste formed a benchmark for future porosity
comparison purposes, between SANS porosity data obtained from RA Concrete and RC
Aggregate examinations.

3.6.8

Interconnected Air Void Content in No-Fines NA Concrete

Interconnected air void ratios in no-fines NA Concrete were examined using a water
displacement method developed by the author (see Appendix 1). A glass dish with
marked increments of volume was used. Samples of no-fines concrete were slowly
submerged into a known volume of water to a specified porous layer thickness. The
volume of displaced water due to the presence of concrete was recorded. Ratio of voids
and aggregate for a specific thickness of the no-fines concrete was calculated. The
Fluid Mechanics Laboratory at SUT was used.

3-25

3.7

RECYCLED AGGREGATE (RA) CONCRETE

Batches of RA Concrete were prepared either at the Concrete Laboratory at Swinburne

University of Technology, or at the Boral Concrete Laboratory at Thornbury. Methods
described in the Australian Standard AS1012.8.1-2000 Methods of testing concrete,
Method 8.1: Method for making and curing concrete Compression and indirect
tensile test specimens were followed in preparing, sampling, and curing of concrete
specimens. Standard cylinder moulds; 100mm and/or 150mm in diameter were used.
Concrete was placed in layers in the moulds, which were attached to a vibrating table,
and compacted at a frequency of 50Hz. After the initial 24 hour period of storage and
demoulding, RA Concrete samples for compressive and VPV testing were cured under
standard moist curing conditions (100% RH and 232C) in lime-saturated water.
Laboratory curing tanks were used, and all specimens were cured for 28 days with the
exception of specimens used for acoustic tests. Samples for the impedance tube test,
and the SANS test were wrapped in two polyethylene plastic bags, and stored in the
laboratory at a controlled temperature of 232C. Table 3.7.1 summarises the curing
regimes employed in the RA Concrete experimental program (also applicable to any
other concrete made from natural aggregate in this research project).

Table 3.7.1 Curing regime of concrete test specimens

Tests / Curing
Compressive strength
Volume of permeable voids
Impedance tube
Reverberation chamber

3.7.1

Bath-cured
Yes
Yes
-

Sealed-cured
Yes
-

Air-cured
Yes

Workability and Consistency

Workability and consistency of fresh RA Concrete was examined by the means of a

slump test in accordance with the Australian Standard AS1012.3.1-1998 Methods of
testing concrete, Method 3.1: Determination of properties related to the consistency of
concrete Slump test. In the case of normal density RA Concrete, the slump test was
performed on every batch of concrete made using standard procedures and equipment.

3-26

However, due to the workability and consistency of the less-fines and no-fines RA
Concrete, the slump test was conducted by visual observation.

3.7.2

Microstructure Development

Examination of the microstructure of RA Concrete was conducted with the use of a

Scanning Electron Microscopy complying with standard SEM procedures (SUT, 1999).
There was a specific focus on the detection of micro-cracks in the transition zone
between new cement paste and RC Aggregate. Solid slab-like 20mm x 20mm samples
3mm thick were examined. The samples were cut from larger RA Concrete specimens
made from 14/10mm RC Aggregate. Solid samples were coated with purified carbon
and mounted on sample holders.
A total of six (6) solid samples were examined. In these samples, specific areas of
approximately 1mm2 were selected, which were assumed to best represent the interface
zone in RA Concrete. A total of twenty five (25) areas were examined. Visual
assessments and observations of micro-cracks on studied images at low magnifications
were recorded.

3.7.3

Mass per Volume

Mass per volume of RA Concrete was determined using procedures in accordance with
the Australian Standard AS1012.12.1 1998 Methods of testing concrete, Method
12.1: Determination of mass per unit volume of hardened concrete rapid measuring
method. All of the concrete specimens that were used for testing compressive strength
and VPV were used to record and calculate mass per volume of hardened concrete. The
measurements were taken on saturated surface-dry specimens. Three (3) specimens per
concrete batch, a total of forty two (42) were examined.

3-27

3.7.4

Compressive Strength

To determine the compressive strength of RA Concrete, The test specimens were

prepared and cured in accordance with the Australian Standard AS1012.8 2000
Methods of testing concrete, Method 8: Method for making and curing concrete
compression, indirect tensile and flexure test specimens, in the laboratory or in the
field.
Three (3) specimens for every batch or for every concrete mix design were prepared.
Two sizes of standard cylinder specimens were used, depending on availability of
moulds. When compressive strength tests were performed at the commercial laboratory,
cylinders of 100mm in diameter and 200mm in height were used. Cylinders of 300mm
in diameter and 300mm in height were used for tests conducted at Swinburne University
of Technology.
Compressive strength of RA25 concrete was determined in accordance with a testing
method described in Australian Standard AS1012.9 1999 Methods of testing concrete,
Method 9: Determination of the compressive strength of concrete specimens.

3.7.5

Apparent Volume of Permeable Voids

The apparent volume of permeable voids in RA Concrete was determined using a

testing method set out in the Australian Standard AS1012.21 1999 Methods of testing
concrete, Method 21: Determination of water absorption and apparent volume of
permeable voids in hardened concrete. This method allows determining the volume of
interconnected void space of concrete which is emptied during oven drying and filled
with water during subsequent immersion and boiling.
For selected batches of concrete, two test cylinders 100mm in diameter were prepared.
After a required curing period, each 200mm high sample was cut into four equal slices
(approximately 50 mm thick) with a concrete saw.

A laboratory water bath with a

heater was used to boil portions of concrete specimens.

3-28

The VPV examination was performed at the Concrete and Fluid Mechanics laboratories
at Swinburne University of Technology and at the Boral Concrete Laboratory at
Thombury.

3.7.6 BET Porosity

Specific surface area, pore size distribution, and pore volume of RA Concrete was
examined using the Brenauer-Emmett-Teller nitrogen adsorption method in accordance
with standard BET Procedures (SUT, 1999).

Porosity in the pore diameter range

between 17 and 3m was examined. In some cases, the BET measurements were
intended to supplement and compare the SANS results of porosity of the same
specimens. Selected SANS specimens which underwent a non-distractive examination
using neutron scattering were then used to examine the porosity in an extended range
using BET nitrogen adsorption.
Samples were sourced from broken pieces of RC25 Concrete used in compressive
strength tests. They were further crushed in a laboratory crusher to obtain particles of
approximately 4 to 5mm in diameter. The RA Concrete samples were then segregated
and classified as either containing more than 50% of cement paste residue and new
cement paste (samples designation; old cpr + na), or samples containing less than 50%
of cement paste residue with visible traces of concrete sand or pieces of fresh cement
paste, or traces of natural coarse aggregate (samples designation; na + old cpr). Solid
samples consisting of small aggregate pieces were placed in testing tubes, degassed, and
tested using the ASAP 2000 instrument. Generated standards of RC Aggregate were
used for comparison and analysis.

3.7.7

SANS Porosity

Following an examination of irregularly shaped and cubed samples of RC Aggregate

porosity using the SANS technique, the third lot of samples were prepared and
examined in May 2001.

A total of ten (10) solid samples of RA Concrete were

prepared. The sample suite included: specimens of neat cement paste of different w/c

3-29

ratios and a mixture of cement paste residue of RC Aggregate and fresh cement pastes
of various w/c ratios (see Table 3.7.1).
Table 3.7.1 AUSANS - May 2001 experiments - sample suite
Samples group
RCA1 (6) samples
prepared using H2O and
cured in H2O

RCA2 (4) samples

prepared using H2O and
cured in H2O
RCA9

Sample
1
2
3
4
5
6
1
2
3
4
5

Sample designation and description

neat 0.2 cement paste (cp)
neat 0.4 cp
neat 0.8 cp
0.2 cp + 1g of recycled concrete aggregate (rca)
0.4 cp + 1g of rca
0.8 cp + 1g of rca
neat 0.4 cp
neat 0.8 cp
0.4 cp + 1g of rca
0.8 cp + 1g of rca
Powder cpr1-1&2, cpr2-1&2, cpr3-1&2

All samples were prepared and cured with H2O.

Samples were tested at various

moisture conditions, oven dried, saturated in H2O, saturated in D2O, and saturated in a
mixture of 50% of D2O and 50% of H2O. Samples of powdered RC Aggregate were
also tested. Table 3.7.3 demonstrates designations and the moisture conditions of the
samples of the May 2001 testing round.

Table 3.7.3 AUSANS - May 2001 experiments - sample moisture conditions

AUSANS Sample
designation
RCA1
RCA2
RCA3
RCA4
RCA5
RCA6
RCA7
RCA8
RCA9

Samples moisture conditions

oven dried samples (six samples)
oven dried samples (four samples + Al + background)
RCA1 saturated in H2O
RCA2 saturated in H2O
RCA1 saturated in D2O
RCA2 saturated in D2O
RCA1 saturated in 50%D2O & 50%H2O
RCA2 saturated in 50%D2O & 50%H2O
Powder

The first lot of samples designated as RCA1 were wrapped in aluminium foil and placed
in sample holders of the UASANS instrument. Initially, the neutron beam transmission
was measured for 300 seconds, then each sample was subjected to radiation of an
intensive beam of neutrons for two periods of 3,600 seconds each, and scattered neutron
were detected using the AUSANS detector. After the first lot of samples were scattered,
they were soaked in light water for 12 hours and scattered as RCA3, then dried and
3-30

subsequently soaked in heavy water, and scattered as RCA5, and then oven dried for 12
hours and soaked in a 50/50 mixture of light and heavy water before being subjected to
radiation of an intensive beam of neutrons for 2 hours per sample, as RCA7. A similar
sequence of radiation, soaking and drying was employed to examine the second lot of
the SANS samples RCA2, RCA4, RCA6 and RCA8 respectively. As part of the SANS
experimentation, the absorption of light and heavy water was investigated. The testing
schedule of the May 2001 SANS round of experiments is presented in Appendix 2.
The fourth round of the SANS experiment also included the preparation and curing of
some of the samples using D2O. All samples were solid slabs, which included neat
cement paste samples of w/c ratios of 0.4 and 0.8. Other samples consisted of known
amount of cement paste residue of RC Aggregate of previously determined elemental
composition embedded in fresh cement paste.

Table 3.7.4 presents RA Concrete

samples examined in January 2002.

Table 3.7.4 AUSANS - January 2002 experiments - sample suite
Samples group
RCA11 (6) samples
prepared using D2O and
cured in D2O

RCA12 (4) samples

prepared using H2O and
cured in H2O
RCA19 (2) samples

Sample
1
2
3
4
5
6
1
2
3
4
1
2

Sample description
neat 0.4 cement paste (cp)
0.4 cp+ 1g of natural aggregate (na)
0.4 cp + 1g of recycled concrete aggregate (rca)
0.4 cp + 0.5g of (rca)
0.8 cp
0.8 cp + 0.5g of (rca)
neat 0.4 cp
neat 0.8 cp
0.4 + 1g of (rca)
0.8 + 1g of (rca)
neat 0.8 cp
0.8 + natural aggregate (na)

The SANS samples were examined at various moisture conditions in order to

investigate the influence of light, heavy, and 50/50 mixture of light and heavy water on
the scattering profile of the same samples. Table 3.7.5 presents moisture conditions of
the SANS sample suite of the January 2002 testing round.

3-31

Table 3.7.5 AUSANS - January 2002 experiments - sample moisture conditions

Samples group
RCA11
RCA12
RCA13
RCA14
RCA15
RCA16
RCA17
RCA18

Samples moisture conditions

saturated D2O (five samples)
oven dried samples (four samples + Al foil)
RCA11 dry (after 11h)
RCA12 saturated in D2O (after 11h)
RCA11 saturated in H2O
RCA12 saturated in H2O
RCA11 saturated in 50%D2O & 50%H2O
RCA12 saturated in 50%D2O & 50%H2O

As in the third round of SANS experiments, a group of samples was subjected to

radiation of an intensive neutron beam under various moisture conditions such as; oven
dried, soaked in D2O, H2O or 50/50 solution of light and heavy water. The testing
schedule and sample preparation for the January 2002 SANS experiments is presented
in Appendix 2.
Neutron scattering experimentation using the SANS technique was performed in
accordance with the AUSANS procedures (ANSTO, 1999).

Total porosity was

estimated with the use of a program developed at Geoscience Australia in Canberra.

The program called PRINSAS allows estimating total porosity of examined concrete
specimens (Hinde and Radlinski, 1999 2003).
The SANS data was analyzed with the help of Dr Alan Hinde and Dr Andrzej Radlinski,
using computer facilities at GeoScience Australia in Canberra, and with the help of Dr
Laurie Aldridge of ANSTO at Lucas Heights.

3.7.8

Fractal Mass

Fractal mass, a measure of the roughness of pores in two-phase material, was estimated
from SANS data using Microsoft Excel and Origin software. The fractal mass was
calculated from a SANS scattering profile on a log-log scale. Fractal mass is a slope of
the line of best fit in a plot of scattering intensity log (I), versus scattering wave vector
log (I(Q)).

3-32

3.7.9

Interconnected Air Void Content in No-Fines RA Concrete

A water displacement method (see Appendix 1) was used to examine interconnected air
voids in all of the no-fines and less-fines RA Concrete samples. The procedures
described in section 3.6.8 apply.

3.8

LESS-FINES RECYCLED AGGREGATE CONCRETE

The experimental program described above, aimed at differentiating natural aggregate

and RC Aggregate and increasing the understanding of differences between NA
Concrete and RA Concrete of compressive strengths of 25MPa and 40MPa.
The next phase in this research project aimed at taking advantages of these differences
and developing a product that best utilizes the inherent properties of RC Aggregate.
The developmental program outlined below aimed at:
1. Material (less-fines RA Concrete) development using the impedance tube method,
2. Product (acoustic barrier) development which involved
a. Research testing of a prototype barrier developed at Swinburne University of
Technology, and
b. Commercial product manufactured at Westkon Precast Concrete Pty Ltd
3. Simulation of acoustic character of barrier installation (Harding, 2004)
The development of the less-fines RA Concrete followed an investigation of the
performance of 14/10mm RC Aggregate in normal density, and in no-fines concrete. A
good understanding of RA Concrete, especially of the potential of no-fines concrete to
entrap and dissipate energy of sound waves, led to an investigation of a two-layered
concrete. The no-fines layer would allow sound waves to enter into the concrete matrix,
whereas the solid layer would provide structural strength of the two-layer less-fines
RA Concrete, and also provide a reflective surface to allow sound waves to resonate.
This structure was further employed in acoustic barriers.
The normal density and no-fines RA Concrete was prepared and examined in
accordance with various Australian Standards as described in sections 3.6 and 3.7 of
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this document, with the only exception being the compaction of no-fines RA Concrete,
where special plates were used to compact each layer of concrete in a cylindrical mould.
Two methods of achieving two-layered less-fines concrete were investigated. In the
first method, the concrete mix design has a deficiency of fine aggregate and the two
layered structure is developed by over-vibration of such concrete.

In the second

method, the normal density concrete is placed first and compacted, followed by the
placement of no-fines concrete in the porous layer, concluding with screeding with a
plank of timber.
The mix designs of less-fine RA Concrete were based on the required relative
thickness of porous and solid layers. The amount of cement paste had to be sufficient to
coat coarse aggregate in the porous layer and to fill available space between coarse
aggregate in the solid layer.

3.8.1

Interconnected Air Void Content

The method introduced in Section 3.6.8, and described in Appendix 1 applies.

Interconnected air void content was examined on all impedance tube samples, with
porous layer thicknesses ranging between 40 and 90 millimeters.

3.8.2

Sound Absorption Impedance Tube Method

Sound absorption capacities of the less-fines RA Concrete were determined in

accordance with the Australian Standard AS1935-1999 Method for the measurement of
normal incidence sound absorption coefficient and specific normal acoustic
impedance of acoustic materials by the tube method.
The size of cylindrical test specimens was; 83mm in diameter, and 150mm in overall
height. The specimens were of varying relative thickness of porous and solid layers. A
total of 10 samples were tested at the Applied Physics Acoustic Laboratory at RMIT
University in Melbourne.

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3.9

PROTOTYPE and COMMERCIALLY PRODUCED BARRIER

The ultimate purpose of this research project, other than a thorough examination of
commercially manufactured 14/10mm RC Aggregate, was to develop and manufacture
a concrete acoustic barrier with the use of such aggregate. On the basis of preliminary
results, it was concluded that the less-fines RA Concrete with solid layer compressive
strength of 25MPa is adequate to manufacture an acoustic barrier. Based on sound
absorption characteristics of the less-fines concrete samples of different thicknesses of
porous layers obtained by the impedance tube method, it was decided that the prototype
barrier consists of a combination of panels of different porous layer thicknesses. The
prototype acoustic barrier (acoustic system) had been designed to have three sets of
panels of different porous layer thicknesses: 40mm, 60mm, and 80mm. The one-pour
method of the fines deficient concrete was used to manufacture twelve (12) panels.
Concrete used for the prototype was classified as less-fine and over-vibration was
required to allow the development of two distinctive layers viz. solid and porous.
Further to the development of the barrier prototype, a commercial acoustic barrier was
developed. The commercially manufactured barrier consisted of three (3) panels. The
size of each panel was 1 meter by 4 meters. The designed thickness of porous layer was
40 mm. The two-pour method was used to manufacture panels of the acoustic barrier.
The solid layer was produced from the normal density RA Concrete using reclaimed
aggregate supplied by Boral Resources Pty Ltd, and the porous layer was made from the
no-fines RA Concrete using the 14/10mm RC Aggregate.
In both the prototype and commercially manufactured barriers, the major objectives
were to test production methods and to investigate acoustic performance of the barrier
using the reverberation room method.

3.9.1

Sound Absorption Reverberation Room Method

Procedures, instrumentation, and requirements with reference to test specimens for the
measurement of sound absorption of the less-fines RA Concrete acoustic barrier in a

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reverberation room are described in the Australian Standard AS1045 1988 Acoustics
Measurement of sound absorption in a reverberation room.
According to the standard, the barrier had to have an area ranging between 10m2 and
12m2 if the barrier is tested in reverberation rooms with a volume less than 250m3. The
samples (panels) shall be of rectangular shape, with the ratio of width to length between
0.7 and 1. Table 3.9.1 presents the acoustic barrier panels used in the determination of
sound absorption coefficient using the reverberation room method.

Table 3.9.1 Sound absorption examination of less-fines RA Concrete acoustic

barrier using reverberation room method
Acoustic Barrier
Prototype
Commercially manufactured

Number
of panels
12
3 cut in
3 parts

Panel size

Date of test

150 x 850 x 1250mm

150 x 1000 x 1300mm

October 2002
November 2003

Panels of the barrier were placed directly on the floor of the reverberation room, and
care was taken to ensure a distance between the boundary of the panels and the room
did not exceed 1 meter, and that the edges of the panels adjacent to the room boundaries
were parallel.
The

instrumentation

including

signal

generator,

source

filter,

loudspeakers,

microphones, measuring filter, amplifiers, and recording equipment complied with

standard requirements. The test signal was generated in a bandwidth of one-third
octave, and the source and measuring filters were used to maintain the one-third octave
bandwidth in a desired range of frequencies between 63Hz and 2,000Hz.
The acoustic testing of barriers was performed at a constant temperature of 25C, and
relative humidity of 55%.
The measurements of reverberation times as a function of time in a reverberation
chamber with the barrier, and without the barrier, were recorded and followed by the
calculation of equivalent sound absorption area (As). Sound absorption coefficient is
obtained by dividing As by the surface area of the barrier. Two measurements of
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reverberation time were obtained; the first with the barrier and the second one of an
empty room.
Reverberation room tests were conducted by Mr. Peter Dale and Mr. John Watson at the
Acoustic Laboratories at RMIT University, which is the NATA Registered laboratory
No 1421.

3.10

CONCRETE MIX DESIGN

Special concrete mix design procedures were considered unnecessary and proportioning
of RA Concrete was based on similar principles as for ordinary Portland cement
concrete. The initial mix designs were based on a mixture of different approaches such
as gap grading (Stewart, 1951), so-called British method (DOE, 1988), the CONAD
method (Day, 1999), and trial mix method. The author sought advice on final concrete
mix designs from a local concrete manufacturer, (Boral, 1999). Some corrections to
concrete mix proportions were based on the differences in specific gravity (particle
densities) of the natural coarse aggregate and RC Aggregate 2.7 and 2.2 respectively.
To overcome a potential influence of variable water absorption of RC Aggregate on
plastic and hardened properties of RA Concrete, a pre-wetting of the aggregate was
employed.

3.11

PROTOTYPE BARRIER DESIGN

The prototype and commercially manufactured acoustic barriers made from selected RC
Aggregate were developed to provide an optimum balance between sound absorption
capabilities and structural integrity. The two layered barrier panels were design to
withstand design loading, in accordance with the Australian Standard AS 1170.1-2002
Structural design actions, Part 1: Permanent, impose and other actions and AS
1170.2-2002 Structural design actions, Part 2: Wind actions.
The formwork for the manufacturing of precast panels was designed in accordance with
the Australian Standard AS3610-1995 Formwork for concrete.

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The design of reinforcement, cover to reinforcement, and concrete strength followed

procedures of the Australian Standard AS3600-2001Concrete Structures. Concrete was
specified and delivered in accordance with the Australian Standard AS1379-1997
Specification and supply of concrete.
In the production of concrete panels, two methods were employed. The prototype
barrier (12 panels of approximately 1m2) was manufactured in laboratories at
Swinburne University of Technology. A small laboratory drum mixer was used to
produce concrete for the prototype barrier. The formwork and steel reinforcement were
prepared at the Heavy Structure Laboratory. The less-fines RA25 Concrete mix was
used, and the one-pour method was employed to place concrete. Over-vibration was
employed to allow control segregation of concrete and development of two distinctive
layers. Air curing of concrete panels was employed.
The commercially manufactured acoustic barrier consisted of three precast panels, each
4m2 in area. A standard steel formwork used in the precast concrete industry was used.
Standard procedures were used to fix steel reinforcements and place lifting points. The
two-pour technique was employed to place RA40 Concrete in the formwork. Firstly, a
layer of the normal density concrete was placed and compacted, which followed
placement of a layer of the no-fines RA Concrete made from 14/10mm RC Aggregate.
The normal density concrete made from reclaimed 20mm graded aggregate, and nofines concrete used in the production of commercially manufactured barriers was
delivered by Boral Resources (Concrete) Pty Ltd.

3.12

LIMITATIONS and OMISSIONS

The experimental and developmental program presented in this chapter reflects the core
experimental work of the project. The author is aware that the program could include
other tests to characterise RC Aggregate such as:

alkali reactivity of the material to assess the potential of a silica-alkali reaction in

RA Concrete

permeability tests to complement porosity assessment of the aggregate, and to better

estimate the durability of RA Concrete
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weak particles content including clay lumps, soft and friable particles in RC
Aggregate

aggregate soundness and evaluation by exposure to a sodium sulfate solution

a complete knowledge of the original concrete used to make the RC Aggregate

including its strength, cement content, water/cement ratio, air content, density, type
of aggregate, etc,.

However, laboratory space availability along with time, precluded the inclusion of such
tests in this projects experimental program.
The experimental program of RA Concrete would ideally include tests to examine
properties of concrete such as: indirect tensile strength (Brazil or splitting test),
flexural strength, shrinkage to complete mechanical properties characterisation of RA
Concrete and permeability to further contribute to durability characteristics.
There are also properties of the acoustic barrier that the author would like to examine in
more detail; such as impact resistance of the porous layer, compressive strength of core
concrete specimens obtained from the barrier and volume of permeable voids of core
concrete specimens obtained from acoustic barrier panels. The author would also like to
manufacture another set of barriers, test it in the reverberation room, install a
demonstration barrier, and perform field durability and acoustic effectiveness tests.

3.13

SUMMARY

This chapter presented the research methodology and the experimental design program
adopted in order to fulfill the main objectives of the project. The chapter outlined the
four major stages and the main phases of the experimental program, which was devised
with the help of professionals in related engineering disciplines from various
commercial, educational and scientific organizations.
The brief overview of the project methodology followed a more detailed description of
rationale of each of the research techniques employed, methods used at each phase,
sampling procedures, sample sizes and locations of where the tests were performed.
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The methodology described investigations into fine aggregate, natural and recycled
concrete coarse aggregates, concrete made from these aggregate, and an investigation of
the final product, the less-fines RA Concrete acoustic barrier.
The following chapter presents a summary of results along with a data analysis based on
the methodology and experimental design program described in this chapter.

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CHAPTER 3 METHODOLOGY and EXPERIMENTAL DESIGN ............................1

3.1
INTRODUCTION ............................................................................................1
3.2
EXPERIMENTAL and DEVELOPMENTAL PROGRAM - OVERVIEW ....3
3.3
FINE AGGREGATE ......................................................................................12
3.3.1
Particle Size Distribution ........................................................................13
3.4
NATURAL (N) COARSE AGGREGATE.....................................................13
3.4.1
Particle Size Distribution ........................................................................14
3.4.2
Elemental Composition...........................................................................14
3.5
RECYCLED CONCRETE (RC) AGGREGATE ...........................................14
3.5.1
Cement Paste Residue (cpr) Content.......................................................15
3.5.2
Impurities and Foreign Materials Content ..............................................16
3.5.3
Cement Content in RC Aggregate Fines.................................................17
3.5.4
Microstructure and Elemental Composition ...........................................18
3.5.5
Particle Density .......................................................................................19
3.5.6
Bulk Density ...........................................................................................19
3.5.7
Particle Size Distribution ........................................................................20
3.5.8
Water Absorption....................................................................................20
3.5.9
BET Porosity...........................................................................................20
3.5.10
SANS Porosity ........................................................................................21
3.6
NATURAL AGGREGATE (NA) CONCRETE.............................................22
3.6.1
Workability and Consistency ..................................................................23
3.6.2
Compressive Strength .............................................................................23
3.6.3
Mass per Volume ....................................................................................23
3.6.4
Apparent Volume of Permeable Voids ...................................................24
3.6.5
Water Absorption....................................................................................24
3.6.6
BET Porosity...........................................................................................24
3.6.7
SANS Porosity ........................................................................................25
3.6.8
Interconnected Air Void Content in No-Fines NA Concrete..................25
3.7
RECYCLED AGGREGATE (RA) CONCRETE...........................................26
3.7.1
Workability and Consistency ..................................................................26
3.7.2
Microstructure Development ..................................................................27
3.7.3
Mass per Volume ....................................................................................27
3.7.4
Compressive Strength .............................................................................28
3.7.5
Apparent Volume of Permeable Voids ...................................................28
3.7.6
BET Porosity...........................................................................................29
3.7.7
SANS Porosity ........................................................................................29
3.7.8
Fractal Mass ............................................................................................32
3.7.9
Interconnected Air Void Content in No-Fines RA Concrete ..................33
3.8
LESS-FINES RECYCLED AGGREGATE CONCRETE...........................33
3.8.1
Interconnected Air Void Content ............................................................34
3.8.2
Sound Absorption Impedance Tube Method .......................................34
3.9
PROTOTYPE and COMMERCIALLY PRODUCED BARRIER ................35
3.9.1
Sound Absorption Reverberation Room Method.................................35
3.10 CONCRETE MIX DESIGN ...........................................................................37
3.11 PROTOTYPE BARRIER DESIGN................................................................37
3.12 LIMITATIONS and OMISSIONS..................................................................38
3.13 SUMMARY ....................................................................................................39

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Figure 3.2.1 Outline of the experimental and developmental program ............................4

Table 3.2.1 Experimental design program - major stages.................................................3
Table 3.2.2 Project stages and properties tested ...............................................................5
Table 3.2.3 RC Aggregate and Natural Aggregate examination summary....................7
Table 3.2.4 RA and NA Concrete development and examination summary .................9
Table 3.2.5 Prototype and commercially manufactured acoustic barrier examination
summary...............................................................................................................10
Table 3.2.6 AUSANS sample suite............................................................................11
Table 3.2.7 BET nitrogen adsorption test program....................................................11
Table 3.3.1 Fine aggregate sources ............................................................................12
Table 3.5.1 SANS experiments (1999 and 2000 - sample suite......................................22
Table 3.7.1 Curing regime of concrete test specimens ...................................................26
Table 3.7.1 AUSANS - May 2001 experiments - sample suite ......................................30
Table 3.7.3 AUSANS - May 2001 experiments - sample moisture conditions ..............30
Table 3.7.4 AUSANS - January 2002 experiments - sample suite .................................31
Table 3.7.5 AUSANS - January 2002 experiments - sample moisture conditions .........32
Table 3.9.1 Sound absorption examination of less-fines RA Concrete acoustic barrier
using reverberation room method ...........................................................................36

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