33

CHAPTER 3
MATERIALS AND METHODS

3.1

MATERIALS
The materials such as cement, fine aggregate, coarse aggregate,

water, fly ash and fly ash aggregates were used in the present work. The
methodology adopted for the formation of fly ash aggregates is also presented
in this chapter.
3.1.1

Cement
Ordinary Portland Cement of 43 grade confirming to IS: 8112-1989

was used for the present experimental investigation. Its specific gravity is
3.15. The cement was tested as per the procedure given in Indian Standards.
The physical properties and chemical composition are given in Table 3.1 and
Table 3.2, respectively.
Table 3.1 Physical Properties of 43 Grade Cement
S.No

Test Particulars

1
2
3
4
5
6
7
8

Fineness (m2/kg)
Initial setting time (min)
Final setting time (min)
Standard consistency(%)
Soundness (mm)
Compressive strength (MPa)3-days
Compressive strength (MPa)7-days
Compressive strength (MPa)28days
Specific gravity

Results
Obtained
310
35
360
28.0
1.0
27.0
37.0
48.0

Requirements of IS
8112-1989
Minimum 225
Minimum 30
Maximum 600
Maximum 10
Minimum 23
Minimum 33
Minimum 43

3.15

34

Table 3.2 Chemical Composition of 43 Grade Cement

S.No

Compound

Results %

Requirements of IS
8112-1989

CaO

63.00

SiO2

21.10

Al2O3

6.00

Fe2O3

3.50

MgO

1.50

Maximum 6

Na2O

0.20

K2 O

0.35

SO3

2.00

Loss of ignition

2.00

Maximum 5

10

Insoluble residue

0.30

Maximum 2

3.1.2

Fine Aggregate
Natural river sand with fraction passing through 4.74 mm sieve and

retained on 600 sieve was used and tested as per IS:2386. The fineness
modulus of sand is 2.68 with a specific gravity of 2.66. The physical
properties are presented in Table 3.3. River sand confirms to grading zone II
of IS: 383-1970.
Table 3.3 Physical Properties of Fine Aggregate
S.No

Test Particulars

Results Obtained

Specific gravity

2.66

Bulk density (Kg/m3)

1808

Size (mm)

Fineness Modulus

Below 4.75
2.68

35

3.1.3

Coarse Aggregate
Hard broken granite stone (HBG) coarse aggregates confirming to

graded aggregate of size 20 mm as per IS:383-1970. Its specific gravity is

2.71. The coarse aggregates were tested as per the procedure given in
IS: 2386-1963 and the physical properties are given in Table 3.4 (Eco housing
2009).
Table 3.4 Physical Properties of Coarse Aggregate
S.No

3.1.4

Test Particulars

Results Obtained

Shape

Angular

Specific gravity

2.71

Bulk density (Kg/m3)

1685

Size (mm)

Crushing value (%)

24.94

IMPact Value (%)

23.86

4.75 to 20

Water
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 for mixing
concrete and curing the specimens as well.
3.1.5

Fly Ash
Fly ash (Class F) obtained from Mettur Thermal Power Station

(MTPS) was used in the experimental work. The comparison of chemical

composition of fly ash produced at MTPS to that of worlds standard is given
in Table 3.5.

36

Table 3.5 Comparison of Chemical Composition of Fly Ash

Chemical Composition
Constituent

World

Fly ash used in

Std. (%)

Thesis work (%)

Silica

SiO2

62.57

54.92

Alumina

Al2O3

31.45

23.04

Ferric Oxide

Fe2O3

1.87

Titanium Dioxide

TiO2

1.45

Manganese Oxide

MnO

0.005

Calcium Oxide

CaO

0.40

3.84

Magnesium Oxide

MgO

0.38

2.82

Sodium Oxide

Na2O

0.05

Potassium Oxide

K2 O

0.82

Iron

Fe2O

6.62

Phosphorus

P2 O 5

0.30

2.70

Alkali metals Oxide

Sulphur Trioxide

SO3

0.76

Magnesium oxide

MgO

2.82

Loss on Ignition

LOI

1.00

2.88

3.1.6

Fly ash Aggregates

The class F fly ash was used in the formation of fly ash aggregates.

The details are presented in this chapter.

3.1.6.1

Formation of fly ash aggregates

The constituents like cement, fly ash and water produce the fly ash

aggregates. Water is the binding material that paves the way for the function
of the aggregate with good bonding (Khaled Ramadan et al 2007).

37

3.1.6.2

Proportions for fly ash aggregates

Cement and fly ash are constituents for preparation of the

aggregates. Also water is the binder which is added to increase the

workability. Six different proportions of cement and fly ash such as 10:90,
12.5:87.5, 15:85, 17.5:82.5, 20:80 and 22.5:77.5 were tried. (Somnuk Tang
Term Sirkal et al 2000).
3.1.6.3

Preparation of fly ash aggregates

Cement and fly ash were mixed in above six proportions in a

concrete mixer. Water was added to the mix by adopting the water cement
ratio of 0.3. The contents were thoroughly mixed in the drum until the
complete formation of fly ash aggregates. This method of formation of fly ash
aggregates is called pelletisation. The fly ash aggregates are shown in Figure 3.1.

Figure 3.1 Fly Ash Aggregates

3.1.6.4

Drying and curing of fly ash aggregates

The fly ash aggregates were taken out from the mixer and allowed

to dry for a day. Then the aggregates were cured in a water tank for 7 days.
3.1.6.5

Segregation of fly ash aggregates

After curing, they were segregated into fine and coarse aggregates

based on size of pellets as shown in Figure 3.2. The aggregates having size

38

less than 4.75 mm were sieved as fine aggregates and size more than 4.75 mm
were sieved as coarse aggregate. From them 20 mm size coarse aggregates
were sieved separately to use them as coarse aggregates. The physical
properties of fly ash fine aggregate (FFA) and fly ash coarse aggregate (FCA)
are given in Tables 3.6 and 3.7, respectively. The grading curves for
conventional fine aggregate (CFA) and fly ash fine aggregate are shown in
Figure 3.3. The grading curves for conventional coarse aggregate (CCA) and
fly ash coarse aggregate are shown in Figure 3.4.

Figure 3.2 Segregation of Fly Ash Aggregates

Table 3.6 Physical Properties of Fly Ash Fine Aggregate

S. No
1.
2.
3.
4.

Test Particulars
Specific gravity
Bulk density (Kg/m3)
Size (mm)
Fineness Modulus

Results
Obtained
1.28
838
Below 4.75
2.70

Table 3.7 Physical Properties of Fly Ash Coarse Aggregate

S. No
1.
2.
3.
4.
5.
6.

Test Particulars
Shape
Specific gravity
Bulk density (Kg/m3)
Size (mm)
Crushing value (%)
IMPact Value (%)

Results
Obtained
Spherical
1.3
913
4.75 to 20
25.6
21.6

39

Figure 3.3

Grading Curves for Conventional Fine Aggregate and Fly

Ash Fine Aggregate

Figure 3.4

Grading Curves for Conventional Coarse Aggregate and Fly

Ash Coarse Aggregate

40

3.2

MIX PROPORTIONING
The procedure for mix proportioning is to combine different

concrete ingredients based on their properties to obtain the required properties

of the fresh as well as the hardened concrete. The properties for the concrete
are chosen from the structural design and the requirements of safe and
functional structures. The requirements are consistency, workability,
compressive strength, density, freeze-thaw resistance, water permeability,
thermal conductivity and service life of the structure (Andrew Short 1963).
The stability against segregation of aggregate, insignificant internal water
bleeding, homogeneity after transportation and coMPaction are the
requirements which are implicit and expected of good quality concrete.
3.2.1

Mix Proportioning of Control Concrete

Control concrete having 28 days of compressive strength of

20 MPa was developed. The mix design was carried out based on IS 10262 1982. The mix design procedure and the mix design are presented in
Appendix 1. The mix proportion and quantity of materials taken for one cubic
meter are given in Table 3.8.
3.2.2

Mix Proportioning of Fly Ash Aggregate Concrete

The fly ash aggregate concrete mix design was done based on the

experimental investigations at the building research station UK which has

developed empirical graphs relating the important parameters like type of
aggregate, cement content, water/ cement ratio, workability, strength and
relative density. The mix design procedure and the mix proportioning of fly
ash aggregate concrete are presented in Appendix 2.

41

The trial mixes have been made and the quantity of materials taken
for one cubic metre have been presented in Table 3.8.
Table 3.8 Materials Required Per m3 of Concrete

S.No

Mix Details

Cement
(Kg)

FA
(Kg)

FFA
(Kg)

CA
(Kg)

FCA
(Kg)

WATER
(Kg)

M1

Control

416

636.95

1112.97

208

M2

10:90

257

396

691

123

M3 12.5:87.5

257

396

691

123

M4

257

396

691

123

M5 17.5:82.5

257

396

691

123

M6

257

396

691

123

M7 22.5:77.5

257

396

691

123

3.2.3

15:85
20:80

Workability Tests on Fly Ash Aggregate Concrete

The workability tests such as Slump test, Compaction factor test

and Vee bee Time test were conducted on fresh concrete as per IS
specification and presented in Table 3.9.
3.2.4

Slump Test
The slump test was conducted as per Indian Standards. A mould of

300 mm high frustum of a cone was placed with levelled surface. The
concrete was filled with three layers, each layer was tamped 25 times with a
16 mm diameter steel rod with a rounded nose. The top was struck off
level and the mould held firmly against the slab base. The mould was
lifted gently, the decrease in height of the concrete was measured.
(Gao Li-Xiong et al 2004).

42

3.2.5

CoMPaction Factor Test

The coMPaction factor was carried out as per standards with

coMPacting factor test apparatus. The top hopper was gently filled with
concrete and the bottom hopper was kept closed. The top hopper was opened
and the concrete fell from the upper hopper into the lower one. Then the
lower hopper was opened and the concrete fell from the lower hopper into the
mould (Aggarwal et al 2007).
The degree of coMPaction was calculated using the following
formula:

Compaction Factor CF

3.2.6

Density of partial compacted concrete

Density of fully compacted concrete

Vee-Bee Time Test

The workability of concrete was measured by Vee-Bee time

apparatus with standard specification. The time required for the complete
remoulding of concrete was measured.
Table 3.9 Workability of Fly Ash Aggregate Concrete Mixtures and
Control Concrete

S.No

Mix details

1
2
3
4
5
6
7

M1 Control
M2
10:90
M3 12.5:87.5
M4
15:85
M5 17.5:82.5
M6
20:80
M7 22.5:77.5

Slump (mm)
60
70
76
80
84
87
90

Workability
Compaction
Factor
0.80
0.86
0.88
0.90
0.91
0.91
0.93

Vee-Bee Time
(Sec)
25
18
16
14
13
12
11

43

3.3

STRENGTH OF FLY ASH AGGREGATE CONCRETE

The mechanical properties of fly ash aggregate concrete such as

compressive strength, split tensile strength and Flexural strength have been
studied in this chapter.
3.3.1

Compressive Strength Test

150 mm x 150 mm x 150 mm concrete cubes were tested as per IS

516-1959. All the specimens were tested in saturated surface dry condition,
after wiping out the surface moisture. For each mix, six identical specimens
were tested at the age of 1 day, 3 days, 7 days, 14 days, 28 days, 56 days and
90 days. The test was conducted in 120 tonne compression testing machine.
The load was applied at the rate of 140kg/cm2/min until the failure of the
specimen. The maximum load applied to the specimen until failure was
recorded. The ultimate load divided by the cross sectional area of the
specimen is equal to the ultimate cube compressive strength.
3.3.2

Cylinder Compressive Strength Test

The cylinder compressive test was carried out at the age of 1 day, 3

days, 7 days, 14 days, 28 days, 56 days and 90 days for the 150 mm diameter
and 300 mm high cylinder specimen using 120 tonne compression testing
machine according to Indian Standard specifications.
3.3.3

Split Tensile Strength Test

This is an indirect test to determine the tensile strength of

cylindrical specimens. Splitting tensile strength tests were carried out at the
age of 7 and 28 days for the concrete cylinder specimens of size 150 mm
diameter and 300 mm height in 1200 kN compression testing machine as per
IS: 5816-1970. To avoid the direct load on the specimen, the cylindrical

44

specimens were kept in between the wooden strips. The load was applied
gradually till the specimen fails and the readings were noted. The splitting
tensile strength has been calculated using the relationship

ft =

2P
DL

Where,
ft = Splitting tensile strength of concrete in MPa
P = Load at failure in Newton
D = Diameter of the cylinder = 150 mm
L = Length of cylinder = 300 mm
3.3.4

Flexural Strength Test

Flexural strength test was carried out at the age of 7 days and 28

days on the 100 mm x 100 mm x 500 mm prism specimen using 120 tonne
capacity Flexural Strength Testing Machine by subjecting the specimen to
two point loading to determine the flexural strength as per IS: 516-1959. The
flexural strength has been calculated using the formula
fr = PL/BD2
Where,
fr

= Flexural strength of the specimen in MPa

= Maximum load in Newton applied to the specimen

= Measured depth of the specimen in mm at the point of failure

= Span in mm

= Measured width of the specimen in mm

45

3.3.5

Modulus of Elasticity Test

The modulus of elasticity test was carried out at the age of 28 days

for the 150 mm diameter and 300 mm high cylinder specimen using 1200 kN
compression testing machine as per standards. The modulus of elasticity has
been calculated from stress strain graph of various fly ash aggregate concrete
mixtures.
3.3.6

Relationship between the Mechanical Properties of Fly ash

Aggregate Concrete
The relationship between the mechanical properties of fly ash

aggregate concrete have been studied as below by the regression analysis.

Equations showing the relationship were also derived.
a) Relationship between compressive strength and Flexural
strength
b) Relationship between compressive strength and Split tensile
strength
c) Relationship between compressive strength and Elastic Modulus
3.4

DURABILITY OF FLY ASH AGGREGATE CONCRETE

A concrete is said to be durable if it withstands the conditions for

which it has been designed over a period of years without any deterioration.
Hence the production of fly ash aggregate concrete involves appropriate
selection and proportioning of the constituents to produce a composite mainly
characterised by its low porosity and pore structure.

46

The durability characteristics of fly ash aggregate concrete have

been studied by conducting the tests such as saturated Water absorption,
Sorptivity, Corrosion, Rapid chloride Permeability, Acid resistance and
Carbonation. The durability tests are presented in this chapter.
3.4.1

Saturated Water Absorption Test

The water absorption was determined on 150 mm x 150 mm x 150

mm cubes as per ASTMC-6420-81 by drying the specimens in an oven at the

temperature of 105 C to constant mass and immersing in water after cooling
to room temperature. The specimens were taken out of water at regular
interval of time and weighed. The process was continued till the weights
became constant (fully saturated).
The difference between the water saturated mass and oven dry mass
expressed as a percentage of oven dry mass gives the saturated water
absorption.
Percentage of saturated water absorption

Percentage of water absorption (%)

Saturated weight Dry weight

x100
Dry weight

W2 W1
x100
W1

Where,
W1 = Weight of specimen after drying at oven temperature of 105 C
W2 = Weight of specimen at saturated condition (saturated weight).
The test is shown in Figures 3.5 and 3.6

47

Figure 3.5 Saturated Water Absorption Test

Figure 3.6 Saturated Water Absorption Test

3.4.2

Sorptivity Test
The sorptivity test was conducted on 150 mm x 150 mm x150 mm

cubes. The sorptivity measures the rate of penetration of water into the pores
in the concrete by capillary suction. Taken that the cumulative volume of
water that has penetrated per unit surface area of exposure is plotted against

48

the square root of time t, the resulting graph that could be approximated by a
straight line is considered as a measure of rate of movement of water through
the capillary pores and is called sorptivity. The sorptivity test was conducted
on cubes by immersing them in water and measuring the gain in mass at
regular interval of 30 minutes duration over a period of 2 hours.
The test is shown in Figures 3.7 to 3.12

Figure 3.7 Schematic Arrangement for Sorptivity Test

Figure 3.8 Curing of Specimens

49

Figure 3.9 Test Specimens after Demoulding

Figure 3.10 Specimens before Applying Epoxy Resin

50

Figure 3.11 Specimens after Applying Epoxy Resin

Figure 3.12 Sorptivity Test

51

3.4.3

Accelerated Corrosion Test

The cylindrical specimens of 150 mm diameter x 300 mm height

were cast with 8 mm diameter steel rod embedded concentrically in the

cylinder for accelerated corrosion test of fly ash aggregate concrete mixtures.
The corrosion test set up is shown in Figure 3.13. The specimens were
partially immersed in 3.5% sodium chloride solution (NaCl) and 3v direct
current (DC) was impressed on the rebar act as the cathode. The
electrochemical cell was found by connecting to a DC voltage source. The
impressed current was supplied for 150 hours continuously and also
monitored for corrosion. The rate of corrosion was measured by half-cell
potential as per ASTMC 376-80 at the intervals of 2 hours until failure of the
specimen. The differences between weight losses of rebar before and after
corrosion are used to calculate the percentage of weight loss of rebar due to
corrosion.

Figure 3.13 Half Cell Potential Measurement Setup

52

3.4.4

Rapid Chloride Ion Penetration Test

The Rapid Chloride Ion Penetration Test (RCPT) was performed as

per ASTMC 1202. The test method consists of monitoring the amount of
electrical current passed through 51 mm thick slices of 102 mm nominal
diameter of cylindrical specimens for duration of 6 hours. The total charge
passed during this period was calculated in terms of coulombs using the
trapezoidal rule as given in ASTMC 1202. The charge passed (Q) was
calculated by the following formula.
Q = 900 (I0 + 2I30 + 2I60 + . +2I330 + I360)
Where,
Q = Charge passed (Coulombs)
I0 = Current (amperes) at t minutes after voltage is applied.
The RCPT test set up is shown in Figure 3.14 and 3.15.

Figure 3.14 Schematic of RCPT Setup

53

Figure 3.15 Rapid Chloride Permeability Test

3.4.5

Acid Resistance Test

Standard 150 mm x 150 mm x 150 mm cubes were used for acid

resistance test. The cubes were cast, demoulded after 24 hours and immersed
in water for curing till the time of testing. After the end of the curing period
the cubes were weighed (W1) and immersed in 1% diluted sulphuric acid
solution and 3% sodium chloride solution for acid resistance test. The cubes
were taken outside and weighed (W2) after 45 days. The percentage loss in
weight was calculated.
Percentage of losses = W1 W2 x 100
W1
Where,
W1 = Weight of cubes before immersion in solution
W2 = Weight of cubes after immersion in solution.
The test is shown in Figures 3.16 and 3.17

54

Figure 3.16 Immersing of Specimens in Acid

Figure 3.17 Weighing of Cube Specimen

3.4.6

Carbonation Test
The carbonation test was carried out on 100 mm x 100mmx100 mm

cubes. The cubes were cast, demoulded and cured. After curing the cubes
were air dried. Then they were kept in air tightened box. The CO 2 gas was
passed into the box continuously for 10 hours and 20 hours. The depth of

55

carbonation and pH values were determined after 10 hours and 20 hours. This
test was conducted to evaluate depth upto which the concrete has become
virtually acidic. The following method was adopted.
A pH indicator solution of phenolphthalein in dilute alcohol was
sprayed on a fresh concrete surface.
The pH indicator changes color according to the alkalinity of
concrete.
As pH value decreases from 10.0 to 8.2 and below, the indicator
changes from dark pink to colorless.
The test is shown in Figures 3.18 and 3.19.

Figure 3.18 Carbonation Chamber

Figure 3.19 Cube Specimens in

Carbonation Chamber

56

3.4.7

Pull Out Test

Bond strength between cement paste and steel reinforcement is of

considerable importance. The bond strength arises primarily from the friction
and adhesion between concrete and steel. The bond strength of concrete is a
function of compressive strength and is approximately proportional to the
compressive strength upto about 20 MPa. Debonding of concrete cover may
lead to loss of confinement and reduction of bond strength at interfacial zone
between the two materials.
Pull out measures the force required to pull out from the concrete, a
rod which has been cast into that concrete. The stronger the concrete, the
more is the force required to pull out. (Yun Bai et al 2004).
The concrete cubes of size 150 mm were cast with an 8 mm
diameter steel rod inserted for a height of 75 mm inside the concrete and
projecting above the concrete.
Pull out test was conducted in a Universal Testing Machine (UTM)
of 600 KN capacity, as per IS: 2770 (Part I -1967). Test specimens consist of
concrete cubes of size 150 mm with an 8 mm diameter steel bar embedded
vertically along a central axis in each specimen. The bar projected down for
distance of about 75mm from the bottom face the cube as cast. The concrete
specimen was mounted in Universal Testing Machine (UTM) in such a
manner that the bar was pulled axially from the cube. The load was applied to
the reinforcing bar at a rate not greater than 2250 kg/min. The slip at the
loaded end of the bar and the maximum pull was noted.
The test is shown in Figure 3.20

57

Figure 3.20 Pull Out Test Setup

3.4.8

Relation between the Strength and Durability Characteristics

The Relationship between strength and durability characteristics

have been studied by regression analysis. The equations showing the

following relations were derived.
a) Relationship between Compressive strength and Saturated
Water Absorption.
b) Relationship between Compressive strength and Weight Loss
of Rebar due to Corrosion.
c) Relationship between Compressive strength and Weight
Losses due to Acid attack.
d) Relationship between Compressive Strength and Chloride Ion
Penetration.

58

e) Relationship between Saturated Water Absorption and Weight

Loss of Rebar due to Corrosion.
f) Relationship between Saturated Water Absorption and
Sorptivity.
g) Relationship between Sorptivity and Weight Loss due to Acid
Attack.
h) Relationship between Sorptivity and Weight Loss of Rebar
due to Corrosion.
3.5

MICROSTRUCTURE

OF

FLY

ASH

AGGREGATE

CONCRETE
Microstructure of fly ash aggregate concrete was studied by using
scanning electron microscopy (SEM) and XRF analysis for the specimen
mixes corresponding to compressive strength, corrosion, acid resistance and
carbonation.
3.6

ECONOMY OF FLY ASH AGGREAGTE CONCRETE

The cost of fly ash aggregate concrete with various cement fly ash

proportions has been worked out following the prevailing schedule of rates
and compared with control concrete. The cost details are presented in
Appendix 3.