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CHAPTER 3

EXPERIMENTAL PROGRAMME

3.1 General

This chapter presents the details of the developments in the process of


making fly ash based geopolymer concrete. The materials used for making
geopolymer concrete, mix proportions, manufacturing and curing of the test
specimens are explained. This is followed by a description of number and
types of specimens used, parameters tested and the various test procedures
adopted.

3.2 Materials

3.2.1 Fly ash

Fly ash is a fine powder recovered from the gases of burning coal
during the generation of electricity. These micron-sized earth elements consist
primarily of silica, alumina and iron. Fly ash particles are almost totally
spherical in shape, allowing them to flow and blend freely in mixtures. Fly ash
improves considerably the performance of binder paste and increases the
bonding action with aggregate and reinforcement. The properties of fly ash
may vary considerably according to several factors such as the geographical
origin of the source coal, conditions during combustion and sampling position
within the power plant. The major elemental constituents of fly ash are Si, Al,
Fe, Ca, C, Mg, K, Na, S, Ti, P and Mn. Nearly all naturally occurring elements
can be found in fly ash in trace quantities. Certain trace elements, including
As, Mo, Se, Cd and Zn, are primarily associated with particle surfaces. The
most abundant species in fly ash extracts are inorganic ions derived from Ca,
Na, Mg, K, Fe, S and C.
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Fly ash has been widely used as a partial replacement of cement in


concrete for over half a century. The benefits include saving of cement and
lowering of the heat of hydration in mass concrete (Baoju et al 2005). The use
of fly ash in concrete is economical and modifies the properties of concrete in
both the fresh and hardened states with improvements to workability, strength,
abrasion, heat evolution, shrinkage and reduces water reducing admixture
demands. In addition, the storage and disposal problem of fly ash, which is an
industrial waste or by-product is also solved by the use of fly ash in concrete;
otherwise, the fly ash has to be disposed of in landfills at a considerable cost.
It reduces cracking due to autogenous and plastic shrinkage. It increases the
packing density of the cementitious system, thus creating a less permeable
structure (Malek et al 2005).

Geopolymer concrete in this study was made from low calcium fly ash
with a combination of sodium hydroxide (NaOH) and sodium silicate solution
(Na2SiO3). Fly ash used in this study was low-calcium (ASTM Class F) dry fly
ash from Ennore thermal power station, Chennai as shown in Table 3.1. The
chemical compositions of the fly ash from all batches as determined by X-Ray
Fluorescence (XRF) analysis are given in Table 3.2.

Table 3.1 Type of Fly ash Used for the Study

Material Class Source


Fly ash F Ennore thermal power station,
Chennai, Tamil Nadu, India.
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Table 3.2 Test Report on Fly ash Analysis (ASTM Class F)

%
S.No Constituents
Composition
1. Silica (as SiO2) 48
2. Alumina (as Al2O3) 29
3. Ferric Oxide (as Fe2O3) 12.7
4. Calcium Oxide (as CaO) 1.76
5. Magnesium Oxide(MgO) 0.89
6. Sodium (as Na2O) 0.39
7. Potassium (as K2O) 0.55
8. Sulphur (as SO3) 0.5
9. Loss On Ignition 1.61

3.2.2 Alkaline Activators

The alkaline liquid used was a combination of sodium silicate solution


and sodium hydroxide solution. The NaOH solids were dissolved in water to
make the solution. The mass of NaOH solids in a solution depends on the
concentration of the solution and is expressed in terms of Molar (M). NaOH
solution with a concentration of 8 M consisted of 8 x 40 = 320 grams of NaOH
solids (in flake or pellet form) per litre of the solution, where 40 is the
molecular weight of NaOH. The mass of NaOH solids was measured as 262
grams per kg of NaOH solution of 8M concentration. Similarly the mass of
NaOH solids per kg of the solution for 14M concentration was measured as
404 grams and for 16M mass of NaOH solid is 444 grams. Chindaprasirt et al
(2007) found that, to produce a higher strength geopolymer the optimum
sodium silicate to sodium hydroxide ratio was in range of 0.67 to 1.00.
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Alternatively the concentration of NaOH between 10M and 20M give small
effect on the strength. Test result of sodium silicate is shown in Table 3.3.

Table 3.3 Test Result of Sodium Silicate

Percentage
S.No Constituents
Composition
1. Na2O 13.7
2. SiO2 29.4
3. Water 55.9

3.2.3 Aggregates

In the absence of the usage of proper alternative aggregates becoming


possible in the near future, the concrete industry globally will consume 8-12
billion tons annually of natural aggregates after the year 2010 (Tsung et al
2006). Aggregates are inert granular materials such as sand, gravel or crushed
stone which, along with water and Portland cement, constitute an essential
ingredient in concrete. Good concrete mix aggregates need to be clean, hard,
strong particles free of absorbed chemicals or coatings of clay and other fine
materials that could cause the deterioration of the concrete. Aggregates which
account for 60 to 75 percent of the total volume of concrete are divided into
two distinct categories fine and coarse. Fine aggregates generally consist of
natural sand or crushed stone with most particles passing through a 4.75 mm
sieve. Coarse aggregates are particles retained in 4.75 mm sieve. Gravels
constitute the majority of coarse aggregate used in concrete with crushed stone
making up most of the remainder.
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3.2.3.1 Fine Aggregate

River sand available in Chennai was used as a fine aggregate and tested
as per IS: 2386 (part III). Sieve analysis results of fine aggregate are shown in
Table 3.4.

Table 3.4 Sieve Analysis Result of Fine Aggregate

Mass Cumulative Cumulative % Cumulative


IS Sieve
Retained on Mass
size Mass Retained % Passing
Sieve (gm) Retained (gm)
4.75mm - - - -
2.36mm 70 70 3.5 96.5
1.18mm 98 168 8.4 91.6
600µ 985.5 1153.5 57.68 42.33
300µ 726.5 1880 94 6
150µ 95 1975 98.75 1.25
Pan 25 2000 100 0

3.2.3.2 Coarse Aggregate

The coarse aggregate comprises the portion of the aggregate which has
large particle size. It may be either crushed or uncrushed. They generally
posses all the essential qualities of a good building stone showing very high
crushing strength, low absorption value, least porosity, interlocking textures
variety of appealing colors and susceptibility to perfect polish. In the present
study granite has been used as a coarse aggregate in concrete. Sieve analysis
of the coarse aggregate has been done and the percentage passing at different
sieves is presented in Table 3.5. Figure 3.1 shows the materials used in
preparing geopolymer concrete. The method of preparation of geopolymer
concrete is shown in Figure 3.2.
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Table 3.5 Sieve Analysis Result of Coarse Aggregate

Mass retained Cumulative Cumulative


IS sieve Cumulative
on each sieve mass % mass
Size % Passing
(gm) Retained (gm) retained
12.5mm 181.0 181.0 9.05 90.95
10mm 714.3 895.5 44.7 55.2
4.75mm 55.5 1987 99.3 0.6

Figure 3.1 Materials used in Geopolymer Concrete

3.3 Preliminary Laboratory Work

The preliminary laboratory work revealed the following:


The main objectives of the preliminary laboratory work were:

To familiarize with the making of fly ash-based geopolymer concrete.

To understand the effect of the sequence of adding the alkaline


activator to the solids constituents in the mixer.

To observe the behaviour of the fresh fly ash-based geopolymer


concrete and its workability.

To develop the process of mixing.


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3.3.1 Mixing

Davidovits (2002) has suggested that the preference of a mixture of


sodium silicate solution and sodium hydroxide solution together at least one
day before adding the liquid to the solid constituents. The fly ash and the
aggregates are first mixed together in a mixing pan for about 5 minutes
manually as shown in Figure 3.3. After the dry mix is made, the prepared
alkaline solution is thoroughly mixed with the dry mix for another 5 minutes
to make fresh geopolymer concrete which is shown in Figure 3.4. The fresh
concrete was placed in the mould. The specimens were compacted with three –
layer placing and tamping using a rod. This was followed by an additional
vibration of 10 seconds using a vibrating table. Specimens such as cubes,
cylinders and beams were cast and tested. After casting the concrete mix was
allowed to settle down in the moulds for 30 minutes. Different batches were
adopted for 7 days, 14 days and 28 days of testing. The preparation of
geopolymer concrete is shown in Figure 3.2.

Alkaline Activator
Aggregate Fly ash (Sodium Hydroxide +
Sodium Silicate)

Geopolymerisation
(Open to atmosphere and
elevated temperature)

Storage open to
atmosphere

Figure 3.2 Preparation of Geopolymer Concrete


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Figure 3.3 Dry Mixing of Materials

Figure 3.4 Fresh Geopolymer Concrete

3.3.2 Curing

There are two types of curing used in this study viz., Curing at room
temperature and curing at an elevated temperature of 60ºC in laboratory oven.
After casting, the concrete mix is allowed to settle in the mould for 30
minutes. For air curing the specimens were allowed to cool in air, demoulded
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and kept open until the day of testing as shown in Figure 3.5. The specimens
were kept in the hot air oven for curing at 60oC as shown in Figure 3.6. During
the curing process, the geopolymer concrete experiences polymerization
process. Due to the increase in temperature, polymerization become more
rapid and the concrete gain 70% of its strength within 3 to 4 hrs of curing
(Kong and Sanjayan, 2008). Heat curing of GPC is generally recommended,
both curing time and curing temperature influence the compressive strength of
GPC (Mustafa Al Bakri, 2011). With curing temperature in range of 60 oC to
90oC within time in 24 to 72 hrs, the compressive strength of concrete can be
obtained about 400 to 500 kg/cm2 (Chanh et al, 2008 ).

Figure 3.5 Specimen After Curing


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Figure 3.6 Oven Curing

3.4 Mix Proportion

3.4.1 Mix Proportion for Geopolymer Concrete Block

The laboratory program conducted in this investigation focused on four


basic mixes and these were designated with the molarity of NaOH. The
concentration of NaOH used in the experimentation was based on the review
of previous research (Hardjito and Rangan 2005). Accordingly the
performances of geopolymer concrete block specimens made with 8M, 10M,
12M and 14M of NaOH were evaluated. The ratio of sodium silicate solution-
to-sodium hydroxide solution was fixed as 2.5. The ratio of fly ash: sand:
coarse aggregate was 1:1.1:2.6 with ratio of activator solution to fly ash as 0.4.
The geopolymer concrete mixes were designated as GP1, GP2, GP3 and GP4
respectively. Table 3.6 shows the mix proportion for GPC.
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Table 3.6 Mix Proportions for GPC for 1 m3 of Concrete

Aggregate Fly NaOH Solution Sodium


Designation Curing
Specimen C.A Sand ash Mass Molarity Silicate
of Mix Condition
(kg) (kg) (kg) (kg) (M) (kg)
30ºC and
GP1 1274 539 490 41 8M 103
60ºC
GPC Solid 30ºC and
GP2 1274 539 490 41 10M 103
Block (150 60ºC
x150 x 150 30ºC and
mm) GP3 1274 539 490 41 12M 103
60ºC
30ºC and
GP4 1274 539 490 41 14M 103
60ºC

30ºC and
GP1 1274 539 490 41 8M 103
GPC 60ºC
Hollow
Block (100 30ºC and
GP2 1274 539 490 41 10M 103
x 100 x 250 60ºC
mm) with
30ºC and
one hollows GP3 1274 539 490 41 12M 103
60ºC
of size 45x
75 x125mm 30ºC and
GP4 1274 539 490 41 14M 103
60ºC

3.4.2 Mix Proportion for Geopolymer Brick

The behaviour of unreinforced geopolymer brick masonry prism is


compared with clay brick masonry prism. English bond unreinforced Clay
Brick Prism (CBP) and Geopolymer Brick Prism GBP (M1) and GBP (M2) of
brick size 225 x 105 x 70 mm were cast using 10M and 12M NaOH
concentration with prism dimension of 609 x 220 x 609 mm (h/t = 2.77) and
609 x 220 x 914 mm (h/t = 4.3). Table 3.7 shows the mix proportion for
preparing GPC bricks.
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Table 3.7 Mix Proportion for Geopolymer Brick

Mix
Mix
Proportion of
Designation Type of Mix Proportion Proportion
mortar
of Prism Brick of Brick of Fly ash :
(Cement :
Binder)
Sand)
CBP Clay Brick Burnt Clay - 1: 4
Moulded
GBP (M1) Geopolymer 1:3 (Fly ash: 1: 0.54 1: 4
Brick Quarry Dust)
GBP (M2) Geopolymer 1: 1.1: 2.6 1:0.54 1: 4
Brick (Fly ash :sand:
Coarse
Aggregate)

3.5 Summary

This chapter enlists the materials used for making geopolymer concrete,
mixture proportions, manufacturing and curing of the test specimens. Fly ash
used in this study was low-calcium (ASTM Class F) dry fly ash from Ennore
thermal power station, Chennai. The alkaline liquid comprises a combination
of sodium silicate solution and sodium hydroxide solids. Coarse and fine
aggregates used in the local concrete industry were used. The coarse
aggregates were crushed granite-type aggregates comprising 20 mm, 14 mm
and 7 mm and the fine aggregate was fine sand. The mixture proportions used
in this study were developed based on previous study on fly ash-based
geopolymer concrete (Hardjito and Rangan, 2005). Molarity of sodium
hydroxide (NaOH) solution was chosen in the range of 8M to 14M. Ratio of
activator solution-to-fly ash by mass was fixed to be 0.40. Curing at elevated
temperatures was done in two different ways, i.e. curing at room temperature
and in the laboratory oven at 60ºC. Mix proportion used for geopolymer brick
to construct geopolymer prism and clay brick prism is also presented.

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