38

CHAPTER 3

MATERIALS AND METHODS

3.1 MATERIALS

The materials such as fine aggregate, coarse aggregate, water, fly

ash and alkaline solution were used in the research work. The methodology
adopted for the manufacturing of geopolymer concrete is also presented in
this chapter.

3.1.1 Fine Aggregate

Locally available river sand with fraction passing through 4.74 mm

sieve and retained on 600 sieve was used as a fine aggregate and tested as per
IS:2386. The physical properties of locally procured fine aggregate are
presented in Table 3.1. River sand confirms to grading zone II of IS: 383-
1970.

Table 3.1 Properties of fine aggregate

S.No Properties Results obtained

1 Specific gravity 2.64
2 Bulk density (kg/m3) 1961.7
3 Fineness Modulus 2.6
 39

3.1.2 Coarse Aggregate

Coarse aggregates confirming to graded aggregate of size 20 mm as

per IS: 383-1970. The coarse aggregates were tested as per the procedure
given in IS: 2386-1963 and the physical properties are given in Table 3.2.

Table 3.2 Properties of coarse aggregate

S.No Properties Results obtained

1 Specific gravity 2.64
2 Bulk density (kg/m3) 1629.7
3 Fineness Modulus 3.1

3.1.3 Water

Water is an important component of concrete. Potable tap water

available in the laboratory with pH value of 7.0 ± 1 and confirming to the
requirements of IS: 456-2000 was used in all experiments.

3.1.4 Fly Ash

In the experimental work, high calcium (class C) fly ash obtained

from batch II of Neyveli Lignite Corporation (NLC), Neyveli was used. Fly
ash is primarily silicate glass containing silica, alumina, iron, and calcium.
Minor constituents are magnesium, sulfur, sodium, potassium, and carbon.
The XRD patterns of the raw fly ash are shown in Figure 3.1.The main
mineral Crystalline compounds present in small amounts and large part of the
structure consists of amorphous content. The X-ray Fluorescence (XRF)
analysis and Scanning Electron Microscopy (SEM) were done at Central
Electro Chemical Research Institute, Karaikudi. The chemical compositions
of the fly ash determined by XRF analysis are given in Table 3.3. The
 40

chemical composition of the fly ash used in the experimental work is as per
the specification of ASTM. The SEM image of fly ash is shown in Figure 3.2.
From the figure, the shape of the fly ash particle is noted as spherical. The
properties of class C fly ash are shown in Table 3.4.

cps/eV
1.2
1.0

0.8

Fe Na Al
0.6 S O Mg Si S Ca Fe
Ca

0.4

0.2

0.0
2 4 6 8 10 12 14 keV

Figure 3.1 XRD of fly ash

Table 3.3 Chemical composition of class C fly ash

Oxides Composition, %
Observed value Specified as per ASTM
SiO2 25.69 25– 42
Al2O3 17.10 15– 21
Fe2O3 9.43 5.0 – 10
CaO 24.54 17– 32
Na2O 1.62 0.8– 6.0
MgO 4.06 4.0 – 12.5
SO3 4.25 0.4– 5.0
LOI 0.5 0.1– 1.0
 41

Figure 3.2 SEM image of fly ash

Table 3.4 Properties of fly ash

S.No Properties Results Obtained

1 Specific gravity 2.2
2 Fineness Modulus 3.2%
3 Specific surface m2/kg 319

3.1.5 Alkaline Solution

Xu & van Deventer (2000) confirmed that the addition of sodium

silicate solution to the sodium hydroxide solution as the alkaline activator
enhanced the reaction between the source material and the solution. Therefore
in the present study, a combination of sodium silicate solution and sodium
hydroxide solution were chosen as the alkaline liquid. Sodium based solutions
were chosen because they are cheaper than Potassium based solutions. The
sodium hydroxide solids were of commercial grade in flakes form with 97%
purity.
 42

The sodium hydroxide solution (NaOH) was prepared by

dissolving the sodium hydroxide flakes in water. The mass of NaOH solids in
solution was varied depending on the concentration of the solution expressed
in terms of molar, (M). For instance, NaOH solution with a concentration of
12M consisted of 12x40 = 480 grams of NaOH solids (in flakes form) per
litre of the solution, where 40 is the molecular weight of NaOH. Note that the
mass of NaOH solids was only a fraction of the mass of the NaOH solution,
and water is the major component.

The chemical composition of the sodium silicate solution was

Na2O=14.7%, SiO2 =29.4%, and water 55.9% by mass.

The sodium silicate solution and the sodium hydroxide solution

were mixed together at least one day prior of manufacturing geopolymer
concrete, Mandal et al. (2011).

3.2 MIXTURE PROPORTION

Based on the limited past research on geopolymer pastes available

in the literature, the following ranges were selected for the constituents of the
mixtures.

High calcium (ASTM class C) fly ash.

Alkaline liquid

Ratio of sodium silicate solution to sodium hydroxide solution,

by mass, was fixed as 2.5, Hardjito (2004).

Molarity of sodium hydroxide (NaOH) solution (8M, 10M,

12M, 14M and 16M).
 43

Varying the grades of concrete (GC-20, GC-30, GC-40, GC-

60).

The mix proportions were arrived based on the variables given in

the section. The aim was to arrive the mix ratios of GC-20, GC-30, GC-40,
and GC-60as per the Indian standard. The mix design for geopolymer
concrete was carried out as per IS 10262 – 2009. The mix design calculation
is given in Appendix A. Mix proportions of geopolymer concrete is given in
Tables 3.5.

Table 3.5 Mix proportions

Materials kg/m
3
Alkaline
Grade Fly Fine Coarse solution NaOH Na2SiO3
ash aggregate aggregate to binder
ratio
GC-20 383 567 1379 0.5 54.51 137
GC-30 479 536 1145 0.45 54.81 136.29
GC-40 527 522 1159 0.4 53.33 133.33
GC-60 530 505 1070 0.31 51.59 128.59

3.3 METHODOLOGY

Figure 3.3 shows the methodology of the present research on

geopolymer concrete
 44

Figure 3.3 Methodology

3.3.1 Mixing and casting

The mixing of geopolymer ingredients involves two general steps:

preparation of the alkaline activator solution and final mixing of all
ingredients. The alkaline activator solution was prepared about 24 hours
before final mixing with the other ingredients. The sodium hydroxide solution
and sodium silicate solution of desired quantity were mixed together in the
laboratory and left in room temperature one day earlier. The exothermic
reaction caused by the mixture of solutions produces heat; hence it requires
 45

cooling before adding to other ingredients. Coarse aggregates, fine aggregates

and the binder (fly ash) were dry mixed thoroughly in the mixing pan before
adding the activator solution. Premixed alkaline activator solution was then
added gradually until a consistent mixture was obtained. Figure 3.4 shows the
mixing and casting of geopolymer concrete specimens. Fresh concrete is the
state immediately after its preparation and this state is transient. This
condition seriously affects the behaviour of the final product. The fresh class
C fly ash based geopolymer concrete was dark in colour and shiny in
appearance. The mixtures were usually cohesive.

Figure 3.4 Mixing and casting of geopolymer concrete specimens

 46

3.3.2 Curing

Geopolymer concrete specimens were removed from the mould

after 4 hours of casting and cured at the room temperature of 28º C to 31º C.
These specimens were wrapped by polythene sheets as shown in Figure 3.5
during curing to prevent excessive evaporation.

Figure 3.5 Geopolymer specimens under curing

3.3.3 Tests on Geopolymer Concrete

The high calcium fly ash based geopolymer concrete had been
tested to find out the mechanical properties such as compressive strength and
split tensile strength. The durability tests such as sorptivity, water absorption,
sulphate resistance and acid resistance had been done. The flexural test on
reinforced geopolymer concrete beam had been tested under two point
loading. The analytical study on geopolymer concrete beam had been done
using ANSYS 14.5 software.
 47

3.4 FRESH PROPERTIES TESTS ON GEOPOLYMER

CONCRETE

3.4.1 Setting Time

The setting time of geopolymer paste were measured as that of

conventional concrete as per ASTM C 403. Setting time is an indication that
cementitious properties is developing and achieving certain degree of resistance
against penetration. Setting times were measured using vicat’s apparatus, based
on the depth of penetration of needle in the geopolymer paste. Initial setting time
is regarded as the time elapsed between the moment that the water is added to
the cement, to the time that the paste starts losing its plasticity. Final setting time
is the time elapsed between the moment the water is added to the cement, to the
time that the paste completely lost its plasticity.

3.4.2 Workability

One of the important fresh concrete properties which would affect

the strength of the hardened concrete is workability. Workability is defined as
the ease of placement of concrete with resistance to segregation. Here the
slump value of high calcium geopolymer concrete with varying molarity were
measured similar to ordinary concrete. Workability was carried out by slump
cone test for measuring consistency of geopolymer concrete. The slump was
determined according to Indian standard specifications IS: 1199-1959.
Compaction of fresh concrete in the cylinder steel moulds was achieved by
applying manual strokes in three equal layers. Initially the geopolymer
concrete had a stiff consistency. But with the addition of water, workability
increases.
 48

3.5 HARDENED TESTS ON GEOPOLYMER CONCRETE

Completely solidified state of concrete is called as hardened

concrete. The test procedures specified by IS: 516 – 1959 were strictly
followed. The strength of hardened concrete is assessed from compression
strength test and split tensile strength.

3.5.1 Compressive Strength Test

Compressive strength tests of class C fly ash based geopolymer

concrete were done on 150 x 150 x 150 mm cube specimens. It was prepared
using high calcium class C fly ash, fine aggregate, coarse aggregate and
alkaline solution. Geopolymer concrete cubes were cast in three layers, in
accordance to IS 10080-1982. Each layer was well compacted by a tamping
rod. After compaction, the top surface was covered with polythene sheet to
prevent from evaporation. The concrete cubes were demoulded after 4 hours
of casting. It was then left at ambient room temperature for curing. Then the
geopolymer concrete cubes were tested in a hydraulic compression testing
machine, as per IS: 4031-1982 (Part 6). The testing of geopolymer concrete
cubes in the compression testing machine is shown in Figure 3.6. The
compressive strength at failure is calculated using the Equation (3.1).
,=

(3.1)
 49

Figure 3.6 Geopolymer concrete cubes under testing

3.5.2 Split Tensile Strength

Split tensile strength is the one of the indirect methods developed

to determine the tensile strength of the concrete. The split tensile strength test
was carried out in accordance with IS: 5816-1999. The cylindrical specimens
of 150mm × 300mm size were cast and cured at ambient temperature. Central
lines were drawn on the opposite faces of the cylinders to ensure that they
were in the same axial plane. Specimens were placed in the Compression
Testing Machine. In this test, a compressive force is applied to concrete
specimen in such a way that the specimen fails due to tensile stresses induced
in it. The load was applied smoothly and continuously at nominal rate until
failure. The diametrical compressive load along the height of the cylinder was
applied and the ultimate load at failure or rupture was noted for calculation.
The testing of geopolymer concrete cylinders in the compression testing
machine is shown in Figure 3.7. The split tensile strength was calculated by
using Equation (3.2).
=

(3.2)
 50

Where,

fst = Split tensile strength in N/mm2

P = Ultimate load at failure in N

D = Diameter of cylindrical specimen in mm.

L = Length of cylindrical specimen in mm

Figure 3.7 Geopolymer concrete cylinder under testing

3.6 DURABILITY TESTS ON GEOPOLYMER CONCRETE

Durability is the ability of concrete to resist weathering action,

chemical attack and abrasion while maintaining its desired engineering
properties. It is known that durability increases the service life of the
structure. The service life and durability of a concrete structure strongly
depend on its material transport properties, such as permeability, sorptivity,
and diffusivity. Permeability controls deteriorations of concrete in the
aggressive environment, because the process of such deteriorations as
carbonation, chloride and sulphate attack is governed by the fluid
transportation in concrete.
 51

Sulphate attack is known to produce significant degradation in

concrete structures. Therefore, much attention was drawn to provide an
adequate protection for concrete in contact with surroundings with high
content of sulphate ions. Acid resistance is one of the essential properties for
structural materials. Sulphuric acid is one type of acid solution that is
frequently used to simulate the acid attack in sewer pipe systems. In such
systems, sulphuric acid attack is a particular problem as it is generated
bacterially from hydrogen sulfide. Based on the past studies, to evaluate the
acid resistance and sulphate resistance of high calcium fly ash based
geopolymer concrete specimens were soaked in sulphuric acid solution and
magnesium sulphate solution with selected concentration up to 80 days of
exposure.

The geopolymer mixes with 12 M of sodium hydroxide have

yielded high strength which was selected and opted for durability studies. The
following tests are carried out for assessing the durability properties of high
calcium fly ash based geopolymer concrete.

Sorptivity

Water absorption

Sulphate attack

Acid attack

3.6.1 Sorptivity Test

Sorptivity is the measure of water absorption rate front through the

unsaturated concrete under capillary suction. The sorptivity tests were
undertaken for cylindrical specimens with a 100 mm diameter and 50 mm
height in accordance with ASTM C-642. The cylinders after casting were
immersed in water for 45 days curing. After curing, the samples were dried in
 52

oven for 24 hours at 110°C temperature as shown in Figure 3.8. The

specimens were drowned with water level not more than 5 mm above the base
of specimen and the flow from the peripheral surface is prevented by sealing
it properly with non absorbent coating to maintain the uniaxial water flow
during the test as shown in Figure 3.9. The quantity of water absorbed in a
time period of 30 minutes was measured. Finally the Sorptivity co-efficient
was calculated using the Equations 3.3 given below.
=
Where,
(3.3)
S is the sorptivity in mm, t is the elapsed time in min.
=
W = change in weight = W2-W1

(3.4)

W1 is the oven dry weight of cylinder in grams, W2 is the weight of

cylinder after 30 minutes capillary suction of water in grams, A is the surface
area of the specimen through which water penetrated, D is the density of
water.

Figure 3.8 Specimens in oven at 110ºC

 53

Figure 3.9 Specimens immersed in water

3.6.2 Water Absorption Test

For water absorption test, 100 x 50 mm cylinders after casting were

immersed in water for 45 days curing. These specimens were then oven dried
for 24 hours at the temperature110°C until the mass became constant and

again weighed. This weight was noted as the dry weight (W 1) of the cylinder.
After that the specimen was kept in hot water at 85°C for 3.5 hours as shown

in Figure 3.10. Then the weight was noted as the wet weight (W 2) of the
cylinder. The water absorption was calculated by using the Equation 3.5.
% 100
(3.5)

Where, W1 is the oven dry weight of cylinder in grams, W 2 is the

wet weight of cylinder in grams after 3.5 hours.
 54

Figure 3.10 Specimens under hot water curing

3.6.3 Sulphate Resistance Test

The test procedure for sulphate resistance test was developed in

accordance to the procedure given in ASTM C 642. The sulphate resistance of
geopolymer concrete was evaluated by measuring the residual compressive
strength and change in mass after sulphate exposure. Test specimens for
sulphate resistance test were 150x150 x150 mm cubes and 100 x 200 mm
cylinders.

Geopolymer concrete specimens of all grades were immersed in

magnesium sulphate solution of 5% concentration, Bhakarev (2005) as shown
in Figure 3.11. The geopolymer concrete specimens were immersed in
magnesium sulphate solution on the third day after casting. The specimens
were kept fully immersed in these solutions, having four times the volume of
specimens for duration of 14, 28, 45and 80 days. In order to maintain the
concentration, the solution was replaced every week. Also the solution was
stirred every week to avoid deposits on the base. The effects of this solution
 55

on specimen were regularly monitored through visual inspection,

measurement of weight change and strength test. The surface of the cubes
were cleaned, weighed and tested in the compression testing machine.

Figure 3.11 Specimens soaked in magnesium sulphate solution

3.6.4 Acid Resistance Test

The test procedure for acid resistance test was developed in

accordance to the procedure given in ASTM C 642. The acid resistance of
geopolymer concrete was evaluated by measuring the residual compressive
strength and change in mass after sulphate exposure. Test specimens for acid
resistance test were 150x150 x150 mm cubes and 100x200 mm cylinders.
Geopolymer concrete specimens of all grades were immersed in 2 %
sulphuric acid solution on the third day after casting, Ariffin et al. (2013). The
specimens were kept fully immersed in these solutions, having four times the
volume of specimens for duration of 14, 28, 45 and 80 days. In order to
maintain the concentration, the solution was replaced every week. Also the
solution was stirred every week to avoid deposits on the base. The effects of
this solution on specimen were regularly monitored through visual inspection,
measurement of weight change and
 56

strength test as shown in Figure 3.12. The surface of the cubes were cleaned,
weighed and tested in the compression testing machine.

Figure 3.12 Specimens soaked in sulphuric acid solution

3.7 FLEXURAL TESTS ON GEOPOLYMER CONCRETE

In order to design an RC structural element, it is important to know

behaviour of reinforced concrete structures and an understanding of the basic
material properties. It is also important to get acquainted with the basic
concepts related to performance criteria in reinforced concrete design. The
aim of structural design is to design a structure so that it fulfills safety;
adequate serviceability includes stiffness and durability. In the design of
structures, better cracking resistance, ductility and energy absorption capacity
are expected because the attainment of ultimate load and large deformations
are realities in these structures.

The reinforced geopolymer beams were designed as under

reinforced as per IS 456 – 2000. The high calcium fly ash based reinforced
geopolymer concrete were prepared with 12M of sodium hydroxide and
 57

sodium silicate to sodium hydroxide ratio of 2.5. All grades of geopolymer

concrete beams with 1.25 % and 1.80 % tensile reinforcement are
experimentally investigated and compared. The experimental investigations
include the structural behaviour of concrete such as load carrying capacity,
ductility factor and energy absorption capacity.

3.7.1 Geometry and Reinforcement Configuration

All beams had been designed as under reinforced concrete. The

design procedures are shown in Appendix B. All grades of geopolymer beams
were of the same size 150 mm x 150 mm x 700 mm of Fe 500, 3Nos-10 mm
diameter bars (GCB 20-10, GCB 30-10, GCB 40-10 and GCB 60-10) and
3Nos-12 mm diameter bars (GCB 20-12, GCB 30-12, GCB 40-12and GCB
60-12) were used for flexural reinforcement at the bottom of beam, 2Nos-8
mm at the top of each beam and 6 mm diameter stirrups spaced 200 mm c/c
for shear reinforcement. The reinforcement details for these beams are shown
in Table 3.8 and Figure 3.13. The reinforcement ratios of 1.25% and 1.80%
were used. The mix proportions are shown in Table 3.6.

Table 3.6 Reinforcement details

S.No Beam Reinforcement Tensile

reinforcement
Specification Compression Tension
ratio, %
1. GCB 20-10 2 No 8 ø 3 No10 ø 1.25
2. GCB 20-12 2 No 8 ø 3 No12 ø 1.80
3. GCB 30-10 2 No 8 ø 3 No10 ø 1.25
4. GCB 30-12 2 No 8 ø 3 No12 ø 1.80
5. GCB 40-10 2 No 8 ø 3 No10 ø 1.25
6. GCB 40-12 2 No 8 ø 3 No12 ø 1.80
7. GCB 60-10 2 No 8 ø 3 No10 ø 1.25
8. GCB 60-12 2 No 8 ø 3 No12 ø 1.80
 58

Figure 3.13 Beam geometry and reinforcement details

3.7.2 Beam Casting and Curing

The coarse aggregates, fine aggregates and the binder (fly ash)
were dry mixed thoroughly in the mixing pan before adding the activator
solution. Premixed alkaline activator solution was then added gradually and
mixing was continued until a consistent mixture was obtained. Figure
3.14shows the casting of reinforced geopolymer concrete beam. Fresh
concrete mixtures were cast into beam mould. The moulds were filled in three
layers and each layer was compacted with 25 blows of hand compaction by
using compacting rod. Geopolymer concrete specimens were removed from
the mould after 5 hours of casting and maintained at the room temperature for
28 days. These specimens were wrapped by polythene sheets during curing to
prevent excessive evaporation.
 59

Figure 3.14 Casting of reinforced geopolymer concrete beam

3.7.3 Experimental Setup

All beams were tested under two point static loading. The span of
the beam was 750 mm. The loads were applied through load cell using a
hydraulic jack. During loading, the mid span deflection was measured using
dial gauge having a least count of 0.01 mm. Prior to placing the specimens in
the machine, the beam surfaces at the location of supports and loads were
smoothly ground to eliminate unevenness. All the specimens were given a
white wash in order to facilitate the marking of cracks. Deflections and the
applied load were recorded at every load increment. Cracks formed on the
faces of the beams were marked and identified. The failure mode of the
beams was also recorded. The experimental set up is shown in Figure 3.15.
The load at first crack, the ultimate load and the maximum deflection at the
ultimate load were noted.
 60

Figure 3.15 Flexural test set up of geopolymer concrete beam

3.8 ANALYTICAL MODELING USING ANSYS

Different methods have been utilized to study the response of

structural components. Experimental based testing has been widely used as a
means to analyze individual elements and the effects of concrete strength
under loading. But this method is extremely time consuming, and quite costly.
The use of finite element analysis to model these elements is much faster, and
extremely cost-effective. By understanding the use of finite element
packages, more efficient and better analyses can be made to fully understand
the response of individual structural components and their contribution to a
structure as a whole.

3.8.1 Finite Element Analysis

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Finite Element Analysis is a numerical method widely used to

analyze the concrete structures based on the use of the non-linear behaviour
of materials. Finite Element Analysis (FEA) provides a tool that can simulate
and predict the response of reinforced concrete members. Finite element
model proves to be computationally simple and better representation of the
actual behaviour of the members under various parametric conditions.

ANSYS is a general purpose finite element modeling packages for

numerically solving mechanical problems, including static / dynamic
structural analysis (both linear and non-linear). The ANSYS modeling
methodology is shown in Figure 3.16.

Fig 3.16: ANSYS modeling methodology

3.8.2 Creation of Model

SOLID 65 is used for the 3-D modeling of concrete. The element is

defined by eight nodes having three degrees of freedom at each node i.e.
translations in the nodal x, y and z directions, Ali Abbas (2010). Solid 65
element was used to model the concrete material, since it has capability of
both cracking in tension and crushing in compression. The material property
has to be defined before the creation of model. In this step of the
 62

preprocessor, the material model and the material property like linear, elastic
and isotropic were selected and the Young’s modulus and Poisson’s ratio
values were given. The model created by using ANSYS 14.5 is shown in
Figure 3.17.

Figure 3.17 Modeling in ANSYS

LINK8 is defined by two nodes which have been used for the
modeling of steel reinforcing bar. The 3-D spar element is a uniaxial tension-
compression element with three degrees of freedom at each node: translations
in the nodal x, y and z directions. The steel for the finite element model was
assumed to be an elastic-perfectly plastic material and identical in tension and
compression, Rohit Nair et al. (2015). The element is also capable of plastic
deformation.

Yield strength of longitudinal reinforcements and stirrups were 415

MPa. Poisson’s ratio of 0.3 was used.

The beam boundary conditions were needed to be applied at nodes

in the supports. The supports were modeled as rigid supports. Beam was
analysed as simply supported beam with two point loading. The load was
 63

applied at the point of application along the nodes by dividing the load with
the number of nodes appearing along the line of application.

In this research a convergence study was carried out to determine

an appropriate mesh density. Various mesh sizes were examined in ANSYS. It
was observed that the obtained ultimate load for mesh size 25 mm is nearest
to the ultimate load of experimental beam, Haider Alsaeq (2013).For this
reason, the mesh size equal to 25 mm was chosen for this study.