A

Seminar Report
on
“A CASE STUDY ON EVALUATION OF REACTIVITY OF CONCRETE
AGGREGATE”
Submitted in partial fulfilment for the degree of
MASTER OF TECHNOLOGY
(STRUCTURAL ENGINEERING)

Guided by: Submitted by:

Dr. TRILOK GUPTA DHEERAJ SHARMA
Department of Civil Engg. M.Tech II year
(Structural Engg.)

2018-2019
DEPARTMENT OF CIVIL ENGINEERING
COLLEGE OF TECHNOLOGY AND ENGINEERING
MAHARANA PRATAP UNIVERSITY OF AGRICULTURE AND TECHNOLOGY
UDAIPUR (RAJ.)
 CERTIFICATE

This is to certify that this seminar report entitled “A Case Study on Evaluation of Reactivity
of Concrete Aggregate” has been carried out under my guidance during the session 2018-2019
by “Mr. Dheeraj Sharma” student of final year M-tech (Structural Engg.), for the partial
fulfilment of the requirement for the award of degree of Master of Technology from the College
of Technology And Engineering, Maharana Pratap University of Agriculture and Technology,
Udaipur (Rajasthan) under my supervision.

Dr. Trilok Gupta

Department of Civil Engineering
College of Technology and Engineering
MPUAT, Udaipur (Raj.)

ii
 ABSTRACT

Alkali-aggregate reactions(AAR) occur between the alkali hydroxides in the pore solution of
concrete and certain minerals found in some aggregates. Two types of AAR reaction are
currently recognized depending on the nature of the reactivity minerals: alkali-silica reaction
(ASR) involves various types of reactive silica(SiO2) minerals and alkali-carbonate
reaction(ACR) involves certain types of dolomitic rocks(CaMg(CO3)2). Both types of reaction
can result in expansion and cracking of concrete elements, leading to a reduction in the service
life of concrete structures.
This report contain means to analyse the reactivity of concrete aggregates. For doing so
different methods are being studied, which include ultra-accelerated mortar bar tests (AAR-2),
Accelerated mortar bar tests (AMBT), Concrete prism test (CPT) and Nonlinear Impact
Acoustic Spectroscopy(NIRAS).
In a study, different types of granite aggregates were used for concrete and then tested to
evaluate the reactivity level of concrete by AAR-2 (the ultra-accelerated mortar bar test). The
result reviled that the granite rubble aggregates contained only few reactive rocks containing
amorphous silica.
On the other hand, another study carried out was to rapidly evaluate the alkali–silica reactivity
of aggregates using a Nonlinear Impact Resonance Acoustic Spectroscopy (NIRAS). In this
technique hysteretic and nonlinear elastic behaviour exhibited by concrete is associated with
the progress of damage such as that induced by the alkali–silica reaction (ASR). The results
showed that the NIRAS technique is capable of accurately characterizing the reactivity of the
aggregates and is more sensitive and faster than conventional methods.
The alkali-silica reactivity as well as alkali-carbonate reactivity of aggregate was evaluated
using the ASTM C 1260 and ASTM C 1105 respectively. The study revealed that the aggregates
susceptible to alkali-carbonate reactivity were also shown to be reactive due to the alkali-silica
reactivity.

iii
 TABLE OF CONTENTS

1 INTRODUCTION ....................................................................................................................................... 1

1.1 INTRODUCTION ....................................................................................................................................... 1

1.2 GENERAL APPROACH.............................................................................................................................. 1
1.3 TESTING TO DETERMINE AGGREGATE REACTIVITY ................................................................................ 2
1.3.1 Use of Field Performance History .............................................................................................. 2
1.3.2 Petrographic Assessment ............................................................................................................ 3
1.3.3 Accelerated Mortar Bar Test, ASTM C 1260 ............................................................................. 3
1.3.4 Concrete Prism Test .................................................................................................................... 4

2 LITERATURE REVIEW ............................................................................................................................ 5

3 CASE STUDYS .......................................................................................................................................... 7

3.1 CASE STUDY 1: DETERMINING REACTIVITY LEVEL OF GRANITE AGGREGATE FOR CONCRETE (AURIMAS,
ET AL., 2017) ..................................................................................................................................................... 7

3.1.1 Introduction................................................................................................................................. 7
3.1.2 Materials and Methods ................................................................................................................ 7
3.1.3 Test Methodology ....................................................................................................................... 8
3.1.4 Results and discussion ................................................................................................................ 9
3.1.5 Conclusions of Case Study 1 .................................................................................................... 12
3.2 CASE STUDY 2 RAPID EVALUATION OF ALKALI–SILICA REACTIVITY OF AGGREGATES USING A
NONLINEAR RESONANCE SPECTROSCOPY TECHNIQUE (CHEN, ET AL., 2010) .................................................... 13

3.2.1 Introduction............................................................................................................................... 13
3.2.2 Sample preparation ................................................................................................................... 13
3.2.3 NIRAS Experiment ................................................................................................................... 14
3.2.4 Results and discussions ............................................................................................................. 14
3.2.5 Conclusion of case study 2 ....................................................................................................... 18
3.3 CASE STUDY 3: EXPERIMENTAL INVESTIGATIONS TO EVALUATE THE ALKALI-CARBONATE REACTIVITY
AND ALKALI-SILICA REACTIVITY OF AGGREGATES (ISLAM, 2015) ................................................................... 19

3.3.1 Introduction............................................................................................................................... 19
3.3.2 Experimental procedure ............................................................................................................ 19
3.3.3 Results and discussion .............................................................................................................. 20
3.3.4 Conclusion of case study 3 ....................................................................................................... 23

4 SUMMERY ............................................................................................................................................... 25

5 REFERENCE ............................................................................................................................................ 26

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 LIST OF FIGURE

Figure 1 Summary of the Various Stages in the Process of Evaluation .................................................. 2

Figure 2. Digital dial indicator, Steel Container and Climatic Chamber respectively (Aurimas, et al.,
2017) ........................................................................................................................................ 9
Figure 3 Photo and Expansion of specimens with granite rubble fr.2/8 (Mix D) after 56 days in 1 M
NaOH solution (Aurimas, et al., 2017) .................................................................................. 11
Figure 4 Photo and Expansion of specimens with granite rubble fr.11/16 (Mix E) after 56 days in 1 M
NaOH solution (Aurimas, et al., 2017) .................................................................................. 11
Figure 5 Photo and Expansion of specimens with granite rubble fr.5/11 (Mix G) after 56 days in 1 M
NaOH solution (Aurimas, et al., 2017) .................................................................................. 12
Figure 6 Schematic plot of experiment setup........................................................................................ 14
Figure 7 Variation of normalized nonlinearity parameter with respect to exposure time (Chen, et al.,
2010) ...................................................................................................................................... 15
Figure 8 Variation of cumulative nonlinear parameter with increasing exposure period. (Chen, et al.,
2010) ...................................................................................................................................... 17
Figure 9 Correlation between cumulative nonlinearity parameters and AMBT expansion. (Chen, et al.,
2010) ...................................................................................................................................... 18
Figure 10 Expansion of mortar bars at 14, 28 and 56 days (Islam, 2015) ............................................ 21
Figure 11 Expansion of alkali-cured prisms at 80°C (Islam, 2015)` .................................................... 21
Figure 12 Expansion of water-cured prisms over test duration (Islam, 2015) ...................................................... 22

LIST OF TABLE

Table 1 Physical properties of granite rubble (Aurimas, et al., 2017) .................................................... 7

Table 2 Amount of materials per specimen ............................................................................................ 8
Table 3 Physical and mechanical characteristics of the specimens after 28 days (Aurimas, et al., 2017)
............................................................................................................................................... 10
Table 4 ASR classifications of the aggregates based on the failure criteria of ASTM 1293M1 (Islam,
2015) ...................................................................................................................................... 22
Table 5 ACR of the 14 investigated aggregates .................................................................................... 23

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 1 INTRODUCTION

1.1 Introduction

Alkali-aggregate reactions (AAR) occur between the alkali hydroxides in the pore solution of
concrete and certain minerals found in some aggregates. Two types of AAR reaction are
currently recognized depending on the nature of the reactive mineral; alkali-silica reaction
(ASR) involves various types of reactive silica (SiO) minerals and alkali-carbonate reaction
(ACR) involves certain types of dolomitic rocks (CaMg(CO3)2). Both types of reaction can
result in expansion and cracking of concrete elements, leading to a reduction in the service life
of concrete structures. (Michale, et al., 2008).

1.2 General Approach

The flow chart in Figure 1 shows the general sequence of testing and decisions that have to be
made when evaluating a source of aggregate for potential AAR. Prior satisfactory field
performance of the aggregate in concrete is considered in some cases to be sufficient for its
acceptance in new concrete. However, the use of field performance in the absence of testing
may not be sufficient to completely safeguard against damage due to AAR in new construction
because of the difficulties in assuring that the materials used in existing structures built ten to
twenty years ago are similar to those being proposed for use today. In most cases, it will be
necessary to conduct laboratory tests to determine whether or not the aggregate is deleteriously
reactive.
In the approach outlined by this report, the level of testing and the test limits vary depending
on the level of risk that is acceptable to the owner. However, in regions where AAR problems
are not infrequent and where the reactivity of aggregates are known to vary from source to
source, it may be necessary to implement a rigorous testing regime to establish aggregate
reactivity and evaluate preventive measures.
The proportion and the size of a particular type of reactive aggregate have also been found to
largely influence the expansive behaviour of ASR affected concrete, which are generally
observed as pessimism effects (Ichikawa 2009, Multon et al 2010, Multon et al 2008, Zhang
et al 1999, Gao et al 2013, Gracia-Diaz et al 2008)
 Select Aggregate
Source

Field Evidence Yes

Is it satisfactory?

No

Laboratory Tests No
Is the aggregate
deleteriously reactive?

Yes

ASR Type of Reaction

Is the expansion due to
ACR or ASR?

ACR

Alkali-Silica Reactivity Alkali Carbonate Reaction Non-Reactive

Take preventive measures or Avoid reactive components or Accept for use, no
do not use do not use precautionary measures
cessary

Figure 1 Summary of the Various Stages in the Process of Evaluation

1.3 Testing to Determine Aggregate Reactivity

1.3.1 Use of Field Performance History

Cores should be taken from a representative number of these structures and a petrographic
examination be conducted in accordance with ASTM C 856 to establish the following:
• The aggregate used in the structures surveyed is close in mineralogical composition to that
of the aggregate currently being produced.
• There is no evidence of damage due to AAR.
• The presence and quantity of fly ash or slag.
If the results of the field survey indicate that the aggregate is non-deleteriously reactive, the
aggregate may be used in new construction provided that the new concrete is not produced with
a higher cement alkali loading, lower amount of pozzolan or slag, or more aggressive exposure
condition than the structures included in the survey. (Michale, et al., 2008)

2
1.3.2 Petrographic Assessment

Petrographic examination of aggregates is conducted in accordance with ASTM C 295.

Petrography can reveal useful information about the composition of an aggregate, including
the identification and approximate quantification of reactive minerals. Petrography may be
used to classify an aggregate as potentially reactive, but expansion testing is required to
determine the extent of the reactivity and appropriate levels of prevention. Aggregates may be
accepted as non-reactive solely on the basis of petrography but there is certain level of risk
associated with such a decision as some reactive phases may not be detected by optical
microscopy. (Michale, et al., 2008)
Where a trained petrographer is examining aggregates from well-known and tested sources, it
is acceptable to use petrography to classify the aggregate reactivity on a routine basis. In
addition to looking for alkali-silica reactive minerals such as opal, chalcedony, cristobalite,
tridymite, strained and micro-crystalline quartz, and volcanic glass, petrographers should also
be vigilant as to the presence of mineralogical and textural features characteristic of alkali-
carbonate rocks. Deleterious alkali-carbonate reactive rocks are often characterized by a
microscopic texture consisting of dolomitic rhombs floating in a fine-grained matrix of calcite,
quartz and clay. However, there have been reports of deleterious ACR with rocks that do not
exhibit this “classic” texture (Ozol, 2006).

1.3.3 Accelerated Mortar Bar Test, ASTM C 1260

If the aggregate is not a quarried carbonate or it is a quarried carbonate with a composition that
falls outside of the region of “aggregates considered to be potentially reactive”.The next step
is to test the aggregate in accordance with ASTM C 1260. Coarse aggregates for this test have
to the crushed to sand size (< 5 mm) and then washed and graded to meet the grading
requirements of the test. Sands have to be washed and graded to meet the same grading
requirements. The test is intended to evaluate coarse and fine aggregates separately, and should
not be used to evaluate job combinations of coarse and fine aggregates. In this test, mortar bars
are produced with the aggregate being evaluated and at the age of two days the bars are
immersed into a solution of 1 M NaOH maintained at a temperature of 176oF (80oC) and the
length change of the bars is monitored. If the mortars do not expand by more than 0.10% after
14 days’ immersion in this solution, the aggregate is considered non-deleteriously reactive. If
the mortar bar expands by more than 0.10% at 14 days, the aggregate is considered to be
potentially reactivity and its reactive should be confirmed in ASTM C 1293 (CPT).
3
1.3.4 Concrete Prism Test

Concrete prism test (ASTM C 1293) is suitable for evaluating all aggregate types and is
considered to be the most reliable laboratory test for predicting field performance of
aggregates. If the aggregate being tested is a coarse aggregate it is blended with a non-reactive
fine aggregate and vice-versa, and the coarse-fine aggregate combination is used to produce
concrete prisms with a specified high alkali loading. The test is not intended for use with
specific job combinations of coarse and fine aggregate, however, it is generally considered
acceptable to do this, but the results are not applicable if either the coarse or fine aggregate is
changed during the job. (Michale, et al., 2008) The prisms are stored over water in sealed
containers at 100oF (38oC) and the length change is monitored periodically. If the prisms do
not expand by more than 0.04% after 1 year, the aggregate is considered non-deleteriously
reactive and may be used in concrete with no further testing (for AAR). If the prism expands
by more than 0.04% at 1 year, the aggregate is considered to be potentially reactive and
preventive measures are required if the aggregate is to be used in concrete construction.
If the aggregate tested was a quarried carbonate rock with a chemical composition that fell
within the region of “aggregates considered to be potentially reactive,” the concrete prisms
must be examined to determine whether alkali-carbonate reaction contributed to the expansion.
If damaging ACR is detected, either in isolation or in combination with ASR, the rock should
not be used in concrete without selective quarrying or aggregate beneficiation to remove the
reactive components. (Michale, et al., 2008)
There is generally a good agreement between the results of the accelerated mortar bar tests-
ASTM C 1260 and ASTM C 1567, and the concrete prism test (Thomas et al. 1999). In the
event of contrasting results between the AMBT and the concrete prism test (ASTM C 1293);
the results of the later are considered to be valid. However, the long duration of the test, 12
months for plain aggregate cement concrete and 2 years for concrete with pozzolans and slag,
to conclude an aggregate to be innocuous or reactive and for SCMs to be effective in containing
the deleterious expansions is a drawback.

4
 2 LITERATURE REVIEW

Concrete is made of coarse and fine aggregates, water and binding material. Over time,
investigations revealed that some aggregates used in concrete manufacturing cause reactions
that have an adverse effect on concrete structure (Esteves, et al., 2012). A lot of natural
aggregates are contaminated with amorphous silica and carbonates that both react with alkali
(Na and K). Alkali enter the cement mix from cementitious materials. This reaction is
commonly known as alkali induced corrosion reaction. (Ben, Nov 2013)

Alkali induced corrosion of concrete is the chemical reaction of alkali and aggregates. This
reaction occurs in concrete or mortar when reactive rocks from the aggregates combine with
sodium and potassium hydroxides emitted mainly from hardening cement binder. The reaction
product is hygroscopic gel, which through water absorption and expansion causes internal
stress that sometimes significantly exceeds the bearing capacity of concrete or mortar. Internal
stresses caused by reaction products result in micro cracking of concrete or mortar. (Michale,
et al., 2008)

Moreover, Researchers have found that the alkali-silica reaction occurs in the presence of
aggregates with reactive silica, high alkali pH and sufficient moisture (Opoka and Flint,1996),
Over a number of years, detailed investigations into alkali induced corrosion have led to the
conclusion that the process involves 3 components: amorphous hydrous and cryptocrystalline
SiO2 sodium and potassium, hydroxides and calcium hydroxide. (Kęstutis Barkauskas,1995).
Currently, the reactivity of aggregates is most commonly determined by expansion
measurement methods and petrographic analyses. Expansion measurement methods such as
accelerated mortar bar tests (AMBT) and concrete prism tests (CPT) are the most widely used
methods currently in practice. (Phair, et al., 1995)

However, AMBT has been criticized as an overly severe method, while the one-year test
duration of CPT reduces its usefulness for rapid identification of varying or marginal sources
Petrographic methods are usually used as supplementary, rather than independent, techniques
to assess the potential for reactivity (Chen, et al., 2010). For example, (Jacob,2008) used image
analysis techniques applied to scanning electron micrographs to characterize the “degree of
reaction”, correlating the changes in the microstructure with expansion measurements.

5
Lately, Study have been done to develop new test methods by trying to balance the trade-offs
between reliability and test duration. Nevertheless, nearly all of these new methods are still
based on the principle of length measurement, and the modifications are focused on the
experimental details, such as the size of the aggregates, size of the samples or the storage
temperature.

With compared to the ASR, a limited number of studies has been conducted on ACR of
aggregates. The past studies were lacked of whether the ACR of an aggregate is a variant of
ASR (Islam, 2015).

However, ASR damage in concrete not only leads to macroscopic changes such as the increased
length of unrestrained samples, but also alters the material properties at the microscopic scale.
For instance, experiments showed that the elastic modulus of alkali–silica gel is significantly
different from that of cement paste or aggregates, and that it varied under different internal
pressures (Chen, et al., 2010) .

The potentially reactive rocks shall be evaluated by means of petrographic analysis (Lindgard,
et al.,2012). The description of reactive rock from different countries is presented in RILEM
AAR-1 (Nixon, et al.,2015). According to RILEM AAR-1 rocks are classified into three
classes: Class I includes very unlikely to be alkali reactive aggregates, Class II includes alkali
reactivity uncertain aggregates, and Class III includes very likely to be alkali-reactive
aggregates.
The reactive silica content in rocks also varies. According to laboratory test results aggregates
can be classified by alkaline reactivity from fast to normal (5–20 years), slow (5–20 years) and
non-reactive (Lindgard, et al.,2010).

6
 3 CASE STUDYS

3.1 Case study 1: Determining Reactivity Level of Granite Aggregate for

Concrete (Aurimas, et al., 2017)
3.1.1 Introduction

The main aim of the research was to find the granite rubble reactivity level according to RILEM
AAR-2 test method. Granite rubble was considered to be a non-reactive aggregate, however,
depending on the quarry, granite may have various impurities including harmful minerals
containing active SiO2. The alkali – silica reaction is among the chemical reactions that have
a significant effect on the durability of concrete. During the alkali – silica reaction certain
forms of silica present in concrete aggregates react with high alkali content leading to formation
of hygroscopic gel that expands in humid environment and slowly, although strongly enough
degrades concrete structures. (Aurimas, et al., 2017)

3.1.2 Materials and Methods

Concrete mixes of 3 different fractions were used for the test presented in Table 1 Their
chemical and petrographic compositions of granite rubble have indicator value of 95% and 5%
for granite and diorite respectively.

Table 1 Physical properties of granite rubble (Aurimas, et al., 2017)

Granite rubble fraction Bulk density, kg/m3 Particle density, kg/m3

2/8 1480 2630
5/11 1530 2630
11/16 1450 2630

Physical properties of granite rubble are presented in Table 2. Portland cement CEM I 52.5 R
was used for the test. A very high quality superplasticizer MC-PowerFlow 3100 was added in
minute doses to produce the cement paste of the required plasticity. The superplasticizer is
based on polycarboxylate ether. The paste was mixed mechanically and compacted in forms by
a shaker. The specimens were kept in the moulds in humid conditions for 24 hours and
afterwards they were demoulded and hardened in water until the deformation testing. (Aurimas,
et al., 2017)
After 28 days of hardening in water mortar bars were bent and compressed by a press. The
flexural and compressive strength were determined according to LST EN 1015-11:2004.

7
 Table 2 Amount of materials per specimen

Flow diameter,
Mixture Cement (g) Aggregate (g) Water (ml) Plasticizer(g) W/C
mm
D 200 450 94 2.4 0.47 215
E 200 450 94 2.4 0.47 216
G 200 450 94 2.4 0.47 223

3.1.3 Test Methodology

In this research the reactivity of aggregates was tested according to RILEM RECOMMENDED
TEST METHOD: AAR-2 (the ultra-accelerated mortar-bar test). It was used to assess the level
of reactivity of the aggregates. According to AAR-2 method procedure mortar bars (40 mm ×
40 mm × 160 mm) hardened in water of 80 °C are kept in 1 M NaOH solution for 14 days at
80 °C and their expansion was measured. The ultra-accelerated AAR-2 can be used for testing
aggregate mixes, however, the aggregate particle size shall be from 125 mm to 4 mm. Coarse
aggregate was crushed by jaw crusher and washed. Washed samples are dried at 100–110 °C
for 16 hours. The mortar was made of 1-part cement and 2.25 parts aggregate. 600 g of cement
and 1350 g of dry aggregate was required for three prisms (40 mm × 40 mm × 160 mm). 6
prisms with each aggregate were molded (Aurimas, et al., 2017).
The water/cement ratio was 0.47. The mortar flow diameter must be from 205 to 220 mm.
Polycarboxylate-based superplasticizer was used to obtain the required mortar flow.
Superplasticizer was added at 0.2 % to the mortar containing granite rubble fraction 2/8 (Mix
D) and the flow diameter 215 mm was achieved. Superplasticizer was added at 0.2 % to the
mortar containing granite rubble fraction 11/16 (Mix E) and the flow diameter 216 mm was
achieved. Superplasticizer was added at 0.2 % to the mortar containing granite rubble fraction
5/11 (Mix G) and the flow diameter 223 mm was achieved. Mix compositions per one test
specimen are presented in Table 2. The mortar was made in accordance with cement class
requirements as per EN 196-1 (Aurimas, et al., 2017).
The elongation of specimens was measured by a digital dial indicator with the scale interval of
0.001 mm. The indicator was fixed in the frame where the prisms are placed. The frame and
indicator axles were inserted into the moulded holes at the ends of the specimen. Four prisms
with each aggregate were selected for the test. The length of the moulded prisms was measured
and the prisms were immersed into water at 80 °C. After 24 hours the prism lengths are
measured again (zero reading) and the specimens are placed into stainless steel containers with
1 M NaOH alkali solution at 80 °C. Containers with the specimens are placed into the climatic
chamber where (80 ± 2) °C temperature was maintained. The elongation of specimens was

8
measured regularly at the same hour of the day. When the specimens are removed after 24 ± 2
hardening in water at 80 °C temperature, the length, i.e. the zero reading (L0) was recorded;
this was a reference reading for further measuring of specimen expansion. After the specimens
are placed into 1 M NaOH alkaline solution at 80 °C, the specimen dimensions (Ln) are
recorded after 1, 3, 6, 9, 12, 14, 21, 28, 35, 42, 49, 56 days ± 2 hours (Aurimas, et al., 2017).

Figure 2. Digital dial indicator, Steel Container and Climatic Chamber respectively
(Aurimas, et al., 2017)

The linear expansion of each specimen was obtained by calculating the difference between the
length of the specimen at each period of measurement (Ln) and zero measurement (L0), to the
nearest 0.001 % of the effective length (Aurimas, et al., 2017), as follows:

Expansion = 100 ∙ (𝐿𝑛 – 𝐿0)

l
where:
L0 – measurement of the specimen just before immersion into sodium hydroxide solution;
Ln – a reading taken at each period of soaking in sodium hydroxide solution, n being the
number of days counted from the zero reading;
l – distance between the inner ends of the metal pins, measured to the nearest of 0.1 mm.

3.1.4 Results and discussion

The mortar density, compressive and flexural strength were measured in the tests. Portland
cement characteristics are presented.

9
Table 3 Physical and mechanical characteristics of the specimens after 28 days (Aurimas,
et al., 2017)

Specimen name Density, kg/m3 Flexural Strength, MPa Compressive Strength , MPa
D(fr. 2/8) 2324 10.8 64.7
E(fr. 11/16) 2314 11.6 65.2
G(fr. 5/11) 2321 10.1 62.6

The test of Specimen D mix with granite rubble fr. 2/8 after 56 testing days gave the results
presented in Figure 3. The average elongation after 14 testing days was 0.059 % and after 56
testing days the average elongation of the prisms was 0.111 %. The expansion of the prisms
occurs when the specimens are cured in 1 M NaOH alkaline solution at 80 °C. The expansion
was caused by the alkaline silica gel that develops in the specimen (Figure 3) .After 56 days of
testing gel deposits on the surface of the rods was the only evidence of alkali induced corrosion;
no surface cracking typical of alkaline induced corrosion was observed (Aurimas, et al., 2017).
The test revealed that granite rubble (fr. 2/8) was not heavily contaminated with reactive rock
and can be classified as Class I – very unlikely to be alkali reactive (expansion after 14 days
according to AAR-2 < 0.10 %) because no surface damage was observed in visual examination
of the specimens after the test (Aurimas, et al., 2017).
The results of tests of specimens with granite rubble fr. 11/16(Mix E) are presented in Figure
4. The average elongation after14 testing days was 0.066 % and after 56 testing days the
average elongation of the prisms was 0.110 %. The expansion of the prisms occurs when
specimens are immersed into 1 M NaOH solution at 80 °C. The expansion was caused by the
alkaline silica gel that develops in the specimen. Gel deposits on the surface were also observed
on the specimens of Mix E as on Mix D specimens; that was typical of alkali induced corrosion
(Figure 4). After56 days of testing gel deposits on the surface of the rods was the only evidence
of alkali induced corrosion; no surface cracking typical of alkaline induced corrosion was
observed (Aurimas, et al., 2017).
4Granite rubble (fr. 8/16) can be classified as Class I – very unlikely to be alkali-reactive
(expansion after 14 days according to AAR-2 < 0.10 %). Results of testing of the specimens
with granite rubble fr. 5/11 (Mix G) are presented in Figure 5. The average elongation after 14
testing days was 0.079 % and after 56 testing days the average elongation of the prisms was
0.112 %. The expansion of the specimens occurs when the prisms are immersed into 1M
NaOH solution at 80 °C. The expansion was caused by the alkaline silica gel that develops in
the specimen. Gel deposits on the surface were also observed on the specimens of Mix G; that
is typical of alkali induced corrosion (Figure 5). After 56 days of testing gel deposits on the

10
surface of the rods was the only evidence of alkali induced corrosion; no surface cracking
typical of alkaline induced corrosion was observed. Granite rubble (fr. 5/11) was not heavily
contaminated with reactive rock that causes alkali induced corrosion and concrete degradation;
therefore, it can be classified as Class I – very unlikely to be alkali-reactive (expansion after
14 days according to AAR-2 < 0.10 %) (Aurimas, et al., 2017).

Figure 3 Photo and Expansion of specimens with granite rubble fr.2/8 (Mix D) after 56 days
in 1 M NaOH solution (Aurimas, et al., 2017)

Figure 4 Photo and Expansion of specimens with granite rubble fr.11/16 (Mix E) after 56
days in 1 M NaOH solution (Aurimas, et al., 2017)

11
Figure 5 Photo and Expansion of specimens with granite rubble fr.5/11 (Mix G) after 56
days in 1 M NaOH solution (Aurimas, et al., 2017)

3.1.5 Conclusions of Case Study 1

The tests on granite rubble used for the tests revealed that:
 It contained few reactive rocks containing amorphous silica because after 14 days the
expansion did not exceed 0.1 % ((D Mix expanded by 0.059 %, E Mix expanded by
0.066 %, G Mix expanded by 0.079 %) according to RILEM AAR-2 test method.
 After 56 days of testing none of the test specimens demonstrated significant micro-
cracking and scaling specific to alkali corrosion.
 By visual examination we can say that granite rubble (fr. 5/11) was not heavily
contaminated with reactive rock that causes alkali induced corrosion and concrete
degradation; so it was very unlikely to be alkali-reactive (expansion after 14 days
according to AAR-2 < 0.10 %).
 Alkali induced corrosion tests with granite rubble did not show any signs of concrete
degradation evidenced by visually seen micro cracks, which spread in different
directions on the surface, and local scaling on the surface at reactive aggregate location.
Only surface gel deposits were observed. (Aurimas, et al., 2017)

12
3.2 CASE STUDY 2 Rapid evaluation of alkali–silica reactivity of aggregates
using a nonlinear resonance spectroscopy technique (Chen, et al., 2010)
3.2.1 Introduction

In this research a new nonlinear acoustic technique Nonlinear Impact Resonance Acoustic
Spectroscopy (NIRAS) was developed and used to characterize the alkali-reactivity of different
aggregates. Cementitious materials such as mortar and concrete exhibit a hysteretic and
nonlinear elastic behaviour in their constitutive relations. This hysteretic nonlinearity was
associated with interfacial deboning between the different constituents, and it changes with the
progress of damage such as that induced by the alkali–silica reaction (ASR) (Chen, et al., 2010).
One of the consequences of the hysteretic nonlinear property of these materials was the
decrease in resonance frequencies, with increased excitation amplitude. This shift in the
resonance frequency as a function of the material nonlinearity parameter can be used to directly
characterize the damage state of the material (Chen, et al., 2010). This research was focused
on the variation of the nonlinearity parameter during a standard accelerated mortar bar test
(AMBT) to assess the potential for alkali-reactivity of aggregates.

3.2.2 Sample preparation

Four fine aggregates, all from U.S. sources, were examined according to AASHTOT 303. The
difference between the accelerated mortar bar tests, AASHTO T 303 and the commonly used
ASTM C 1260, was only in the water-to-cement ratio, which were 0.50 and 0.47 respectively
(Chen, et al., 2010). The aggregates used for the tests were the following:
(1) A highly reactive aggregate from Texas with an expansion of 0.456% at 14 days
(2) A moderately reactive aggregate from Alabama with an expansion of 0.136% at 14 days,
(3) A marginally reactive aggregate from Georgia with an expansion of 0.098% at 14 days, and
(4) A non-reactive dolomitic aggregate from Georgia with an expansion of 0.069% at 14 days.

The mortar samples of dimensions 285×25×25 mm were cast according to standard procedures.
Three of which were used for expansion measurements, three for NIRAS tests, one for
compression testing to obtain elastic modulus values, and one for microscopy. A Type I cement
was used for preparing the samples and the mixing procedure was in compliance with
AASHTO T 303. The samples were cured at ∼100% relative humidity and 23 °C for 24 h. After
demoulding they were immersed in tap water and placed in an oven at 80 °C (176 °F) for

13
another 24 h. The first set of expansion measurements, compression tests and acoustic
experiments was then conducted to obtain the initial results at the end of the curing period.
(Chen, et al., 2010)
To induce ASR damage, mortar bars were then immersed in a 1 N NaOH solution at 80 °C
(176 °F), according to AASTHO T 303. Samples were then taken out of the solution at regular
intervals for expansion measurements, compression testing NIRAS testing, and microscopic
analysis.

3.2.3 NIRAS Experiment

In the NIRAS tests, mortar bar samples were cut to a length of 254 mm (10 in.). The samples
were then fixed at one end (embedded length was 25.4 mm (1 in.)) using a clamping device
and free at the other end (so that it was a beam with a fixed-free boundary condition). The
cantilever length of the beam was 228.6 mm (9 in.), and its thickness was 25.4 mm (1 in.). An
accelerometer was affixed to one surface near the free end, and the impact energy was applied
in the middle of the opposite surface with an instrumented hammer. (Chen, et al., 2010)The
impact signal and received vibration signal were captured and recorded by a digital
oscilloscope. A schematic diagram of the experimental setup was shown in Figure 6 Schematic
plot of experiment setup.

Figure 6 Schematic plot of experiment setup

3.2.4 Results and discussions

The linearity of the NIRAS experimental setup was first validated to quantify the instrument
nonlinearity for the system proposed to make these NIRAS measurements. The sensitivity of
the NIRAS technique for differentiating the ASR-damaged samples from the undamaged
14
control samples was then shown through a comparison with results from a conventional
resonance vibration (Chen, et al., 2010). Finally, the NIRAS technique was applied to
distinguish between four different aggregates of varying alkali–silica reactivity, and the results
are analysed and correlated to the accompanying expansion data and linear elastic modulus
measurements.
According to the (Chen, et al., 2010) the total nonlinearity from the mechanical fixture and
electronic devices was negligibly small, and thus the measured nonlinearity for mortar bars
presented later in the research was only due to the material, plus any damage to the material.

3.2.4.1 NIRAS measurements

The NIRAS measurements were used to determine if the NIRAS technique can be used to
distinguish aggregates with varying alkali-reactivity. Figure 7 shows the variation of
normalized nonlinearity parameters of four aggregates over the 14-day exposure period, where
the nonlinearity parameters were calculated by the slope of the linear relationship between the
shift of the resonance frequency and excitation magnitude. (Chen, et al., 2010) Similar to the
elastic modulus, the initial values of nonlinearity parameters for these four aggregates before
the exposure (day 0) were slightly different, and the normalization by the initial value on day
0 was enforced for the nonlinearity parameters at each exposure age to eliminate the effect of
different intrinsic material nonlinearity. The average of the three specimens were used in Figure
7 for all four aggregates and the standard deviation bar of aggregate #1 was also included.
(Chen, et al., 2010)

Figure 7 Variation of normalized nonlinearity parameter with respect to exposure time

(Chen, et al., 2010)

15
First, the nonlinearity parameter of the innocuous aggregate #4 remains below a small value of
2, indicating that the material nonlinearity due to ASR throughout the exposure period did not
significantly increase when compared to its initial value on day 0. The minor increase in
nonlinearity parameter of aggregate #4 could be due to the heating-and-cooling cycle during
tests or instrument nonlinearity. In contrast, the nonlinearity parameter of the highly reactive
aggregate #1 increases rapidly during the initial 4 days of exposure, reaching nearly 10 and
then decreases to a relatively stable value.
The large difference of nonlinearity parameters between aggregates #1 and #4 indicates that
the proposed NIRAS technique was sensitive to the ASR-induced damage of materials in these
experiments, and not the other potential nonlinearity sources. (Chen, et al., 2010)
In comparison, as shown in Figure 7, the nonlinearity parameters of aggregates #2, #3 and #4
increased steadily, and by day 6, the aggregates can be effectively distinguished from each
other. Particularly from day 2 to day 6, This relatively early differentiation of aggregate
reactivity was one potential advantage of the developed NIRAS method. Further research was
necessary to validate these results using aggregates with a wide range of reactivity. (Chen, et
al., 2010)
3.2.4.2 Physical interpretation of NIRAS results
The NIRAS technique has been shown to distinguish ASR-damaged samples from undamaged
samples and to distinguish among aggregates of varying alkali–silica reactivity. The measured
nonlinearity parameter was observed to increase with increasing damage due to ASR.
But, as seen in Figure 7, the nonlinearity parameters of aggregates #1 and #2 do not
monotonically increase with exposure, which was inconsistent with the increasing expansion
measured over time for these aggregates. Thus, it was imperative to inter-relate the variation
of the nonlinearity parameter with the changes occurring in the specimen during progressive
ASR. The nonlinearity parameter of aggregate #1 reaches its peak by 4 days of exposure and
decreases gradually afterwards, while the nonlinearity parameter of aggregate #2 has a slower
progression, reaching the maximum value by 6 days of exposure, and decreasing and
apparently stabilizing at low value by 10 days of exposure.
It was suggested that these ASR-induced changes in the microstructure may be responsible for
the initial increase and eventual decrease of the nonlinearity parameter. Again, the change of
material microstructure at different stages of ASR development may also contribute to the
increase-then-decrease of the hysteresis parameter observed by the NIRAS technique in Fig.
10. Recall that researchers have established that the ASR gel product has unique elastic

16
properties which differ from those of the aggregates and paste (Phair, et al., 1995).

Figure 8 Variation of cumulative nonlinear parameter with increasing exposure period.

(Chen, et al., 2010)

By examining the microstructure of concrete by (Chen, et al., 2010) a cumulative value (i.e.,
area under the nonlinearity parameter versus exposure time graph) would approximately
represent the total extent of gel and microcrack formation or a more generally-defined ASR
damage state. The variation of the cumulative nonlinearity parameter with increasing exposure
duration was plotted in Figure 8. The cumulative nonlinearity parameters show very good
correlations with measured AMBT expansions for all four aggregates, as shown in Figure 9
Also, it can be clearly seen from Figure 8 that the aggregates are distinguishable from each
other as early as day 6 which was not evident in the expansion measurements. Thus, such a
cumulative nonlinearity parameter can be used to differentiate aggregates of varying alkali
silica reactivity in a much shorter testing duration, compared to the expansion measurements.
Importantly, this cumulative nonlinearity parameter could be used to define prescriptive limits
on the value of nonlinearity parameter for classifying aggregates of varying reactivity.
However, further testing with a wide range of aggregates was required before these limits can
be defined.

17
 Figure 9 Correlation between cumulative nonlinearity parameters and AMBT expansion.
(Chen, et al., 2010)

3.2.5 Conclusion of case study 2

Based on the results of the study reported, the following conclusions can be made:
 We can conclude that the NIRAS technique was more Sensitive than conventional linear
acoustic methods and was capable of accurately characterizing the reactivity of The
aggregates examined.
 Furthermore, it was advantages over standard expansion measurements for
differentiating various aggregates having similar levels of reactivity, particularly at
early test ages.
 The observed downward shift of resonance frequency with an increased excitation level
was attributed to the nonlinearity in the mortar bar samples. The slope of the linear
relationship in the plot of resonance frequency shift versus excitation magnitude was
used to represent the state of ASR damage in mortar samples.
 It was shown that NIRAS was capable of distinguishing ASR damage in these samples
and was more sensitive to ASR damage compared to the conventional linear vibration
method.
 The proposed NIRAS technique was an effective on destructive testing tool to detect
and evaluate microstructural changes caused by ASR damage and could potentially be
used to assess damage states in concrete structures.

18
3.3 CASE STUDY 3: Experimental investigations to evaluate the alkali-
carbonate reactivity and alkali-silica reactivity of aggregates (Islam, 2015)
3.3.1 Introduction

In his experiment Islam evaluated the alkali-silica reactivity (ASR) and alkali-carbonate
reactivity (ACR) of the 14 aggregate groups quarried from different locations. In order to serve
the stated purpose, the investigated aggregate groups were tested in determining their alkali-
silica reactivity using the ASTM C 1260 at the ages of 2, 4, and 8 weeks, and the modified
ASTM C 1293 (prisms submerged in the 1N NaOH at 80°C) at the test durations of 4, 8 and
13 weeks. The aggregate prone to the alkali-carbonate reactivity was accessed using the ASTM
C 1105 at the ages of 3, 6 and 12 months. (Islam, 2015)

3.3.2 Experimental procedure

The aggregates utilized in this study were obtained from 14 different quarries. ASTM Type V
Portland cement with 21% SiO2, 3.6% Al2O3, 3.4% Fe2O, 63.1% CaO, 4.7% MgO, 0.84%
Na2Oeq, 2.6% SO, and 1.3% LOI was utilized as a sole cementitious material. (Islam, 2015)

3.3.2.1 Mortar bars for ASTM C 1260

The mortar bar specimens of dimensions 25.4 × 25.4 × 254 mm were prepared according to
ASTM C 1260 standard (2007) which consisted of 10% #8 sieve (2.3 mm), 25% #16 sieve
(1.18 mm), 25% #30 sieve (600 µm), 25% #50 sieve (300 µm), 15% #100 sieve (150 µm).
Water-to-cement ratio (by weight) of 0.47 and the aggregate-to-cement ratio of 2.15 were also
maintained. (Islam, 2015) The mortars were mixed in accordance with the requirements of
ASTM C 305 and moulded within a total elapsed time of not more than 2 minutes and 15
seconds. (Islam, 2015) The mortar bars were cured in a room maintaining 100% relative
humidity and a temperature of 38°C for a duration of 24 hours. The specimens were then
demoulded one at the time and their initial readings were taken before immersing in water at
80°C for 24 hours after which the zero readings were recorded.
Afterward, the mortar bars were submerged in a 1.0N NaOH soak solution in an air-tight plastic
container kept in an oven which maintained the temperature of 80 ± 1°C. Subsequent readings
were taken at the ages of 3, 6, 10 and 14 days, and after that one reading per week until the
immersion age was reached at 56 days. (Islam, 2015)

19
3.3.2.2 Concrete prisms for modified ASTM C 1293
Concrete prisms of dimensions 75 × 75 × 250 mm from each trial aggregate were also prepared
according to the requirements of ASTM C 1293 with an exception of Type V Portland cement,
as specified in Specification C 150, having a total alkali content of 1.25% Na2O. The absorption
and moisture content of the graded aggregates were included in the determination of the design
water-to-cement ratio. For each aggregate source, a constant volume of 0.0085 m3 concrete
was used to cast three prism specimens. After 24 hours of moist curing, the specimens were
placed in water at 80°C for 24 hours after which zero readings were taken. Three prisms were
then fully submerged in a 1.0N NaOH solution in an air-tight plastic containers held in an oven
maintaining the temperature of 80°C. The expansion readings of the specimens were taken
once a week until the immersion age was reached at 13 weeks.

3.3.2.3 Concrete prisms for ASTM C 1105

The mixture constituents of the prism specimens of ASTM C 1105 Concrete mixtures with a
volume of 0.3 ft3 were prepared for each of the aggregate quarries to cast three 3″ × 3″ × 11″
specimens. The prisms were stored at 100% relative humidity at room temperature. The change
in length was measured in one week intervals for the first three months, in two weeks’ intervals
for the next three months, and in 4 weeks’ intervals for the last six months. (Islam, 2015)

3.3.3 Results and discussion

3.3.3.1 Evaluation of ASR
The Samples were evaluated using ASTM C 1260 as the Figure 10 shows the mortar expansions
at the test durations of 14, 28 and 56 days. The mortar expansion increased with an increase in
test duration, and the increase in expansion varied widely depending on aggregate mineralogy.
The potential ASR reactivity of the aggregates was evaluated using the expansion limits of
mortar bars at the test durations of 14, 28 and 56 days.

The ASR classifications of the 14 trial aggregates were perfectly matched based on the 28-,
and 56-day expansion criteria of mortar bar, proposed by (Hooton and Rogers,1993) and
(Hooton,1995), and those proposed by (Islam,2010). The levels of ASR of the 11 of the 14
aggregate groups produced similar results at the three distinct test durations. (Islam, 2015) Of
the 14 aggregates, the four aggregates (A-A, D-D, E-E, and H-H) displayed innocuous
behaviour, and the seven aggregate groups (C-C, F-F, G-G, J-J, L-L, M-M, and N-N) were
found to be reactive based on the failure criteria of mortar bars at the test durations of 14, 28,

20
and 56 days. Overall, the ASR of the selected aggregates based on the extended immersion
ages provided more consistent results than that obtained at the early test duration. (Islam, 2015)

Figure 10 Expansion of mortar bars at 14, 28 and 56 days (Islam, 2015)

Figure 11 Expansion of alkali-cured prisms at 80°C (Islam, 2015)`

Now using Modified ASTM C 1293 Figure 9 shows the progression in prism expansion for the
1N NaOH at 80°C. As can be stated, the prism expansions increased with an increase in test
duration. However, expansion rate of prism specimens was lower than that of the mortar bars
due to the larger size of the specimens. (Islam, 2015) The levels of ASR of the trial aggregates
were determined based on the expansion limits of concrete prisms submerged in the1N NaOH
at 80 °C at the immersion ages of 4, 8, and 13 weeks.

21
Table 4 ASR classifications of the aggregates based on the failure criteria of ASTM 1293M1
(Islam, 2015)

Aggregate ID 4-week 8-week 13-week Potential ASR

(0.04%) (0.105%) (0.165%) reactivity
A-A I I I I
B-B R R R R
C-C R R R R
D-D R R R R
E-E I I I I
F-F R R R R
G-G R R R R
H-H I I I I
I-I R I I I
J-J R R R R
K-K R I I I
L-L R R R R
M-M R R R R
N-N R R R R
Notes: Prism submerged in the 1N NaOH at 80°C
I=Innocuous, R=Reactive

3.3.3.2 Evaluation of ACR

The standard test of ASTM C 1105 for the length change of concrete prisms due to alkali
carbonate reaction was conducted in a period of one year. Figure 12 Expansion of water-cured
prisms over test duration shows the 3-, 6- and 12-month prism expansions of the investigated
aggregate groups. As can be shown, the expansion of water-cured prisms due to ACR was very
low as compared to the alkali cured mortar bars and prisms due to the curing environment that
was less conducive for the AAR. The aggregates susceptible to ACR were determined using
the failure criteria of ASTM C 1105 of 0.015%, 0.025%, and 0.030% at the ages of 3, 6 and 12
months, respectively. (Islam, 2015)

Figure 12 Expansion of water-cured prisms over test duration (Islam, 2015)

22
The results are presented in Table 5. As can be shown, the four aggregate groups (F-F, K-K, L-
L and M-M) displayed the signs of ACR at the test durations of 3 months. Lengthening the test
duration to 6 months, the two aggregates (F-F and K-K) that were shown to be ACR reactive
at 3 months became innocuous at 6 months, and the behaviour of the L-L and M-M aggregate
groups was unaffected at the test duration of 6 months. When the prisms were cured in an
extended period of 12 months, the levels of ACR of all investigated aggregates produced
similar conclusions to those obtained at the 6-month testing period; the L-L and M-M
aggregates were reactive, whereas the remaining 12 aggregates were classified innocuous. It
was also observed that the late-age results were more consistent than those obtained at the early
stage.

Table 5 ACR of the 14 investigated aggregates (Islam, 2015)

Aggregate ID 4-month 6-month 13-week

(0.015%) (0.020%) (0.030%)
A-A I I I
B-B I I I
C-C I I I
D-D I I I
E-E R I I
F-F I I I
G-G I I I
H-H I I I
I-I I I I
J-J R I I
K-K R R R
L-L R R R
M-M I I I
N-N I I I
Notes: I=Innocuous, R=Reactive

3.3.4 Conclusion of case study 3

Based on the results of the study presented discussed, the following conclusions can be made:
 The study revealed that the aggregates susceptible to alkali-carbonate reactivity were
also shown to be reactive due to the alkali-silica reactivity. (Islam, 2015)
 Moreover, the high alkali soak solution (1N NaOH) elevated the alkali content of the
prisms which ultimately resulted in higher expansions for most aggregates during the
6-month testing period. (Islam, 2015) Utilizing the proposed expansion limits of ASTM
C 1293M1 of 0.105% at 8 weeks, and 0.165% at 13 weeks produced more reliable

23
 results than those generated at the early immersion age of 4 weeks.
 Of the 14 aggregate groups investigated, the four aggregate groups (F-F, K-K, L-L, and
M-M) displayed the signs of ACR at the immersion age of 3 months. Extending the test
duration to 6 and 12 months, the F-F and K-K aggregate groups were shown to be
innocuous, and the behavior of the remaining two aggregates (L-L and M-M) was still
reactive, and was unaffected by the test durations of 6 and 12 months.
 The two aggregates (L-L and M-M) having the 14-day mortar expansions of more than
0.80%, and 28-day prism expansions of 0.24% were classified as alkali carbonate
reactive based on the expansion limits of ASTM C 1105 at the test durations of 3, 6 and
12 months.
 It can be stated that the alkali-carbonate reactivity was an alternative of alkali-silica
reactivity. However, the ASR is not a variant of ACR (Islam, 2015).

24
 4 SUMMERY

Reactivity of aggregates is being a very sensitive issue when it comes to the damages it causes
to the structures, and it has high chances of coming into the action after many years of
construction.
The reactivity of aggregates is generally measured So, after analysing the case studies about
reactivity of aggregate, the following conclusions can be drawn:

 In case study 1, the results after the testing showed that the granite rubble aggregates
are not highly polluted with reactive particles containing amorphous silica that react
with sodium and potassium hydroxide causing alkali induced corrosion, furthermore
visual examination also did not show any surface damage.

 In case study 2, it was concluded that NIRAS technique is more Sensitive than
conventional linear acoustic methods and is capable of accurately characterizing the
reactivity of The aggregates examined. Furthermore, the results show advantages over
standard expansion measurements for differentiating various aggregates having similar
levels of reactivity, particularly at early test ages.

 In case study 3, it was pretty clear from the results that the 14 aggregate groups
investigated, the four aggregate groups displayed the signs of ACR at the immersion
age of 3 months. Extending the test duration to 6 and 12 months, so it can be stated that
the alkali-carbonate reactivity is an alternative of alkali-silica reactivity. However, the
ASR is not a variant of ACR.

25
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