47

CHAPTER 3

TESTING METHODS

3.1 MATERIAL PROPERTIES

3.1.1 Cement

OPC-43 Grade was used as per IS 8112 with specific gravity 3.15.
The percentage of water required for standard consistency is 29.57%. The
initial and final setting times for cement were 30 minutes and 320 minutes.
The percentage of cement particles passing through IS 90 micron sieve is
96.4%. Chemical compositions and physical properties of OPC are given in
Table 3.1(a) & (b).

Table 3.1(a) Chemical composition of OPC

Compound Percentage
Silicon-di-Oxide (SiO2) 21
Aluminium Oxide (Al2O3) 5.6
Ferric Oxide (Fe2O3) 4.8
Calcium Oxide (CaO) 63
Magnesium Oxide (MgO) 0.7
Sulphur tri Oxide (SO3) 2.8
Loss on ignition 2.1
Bogue’s compound Composition
Tricalcium Silicate (C3S) 43.5
Dicalcium Silicate (C2S) 25
Tricalcium Aluminate (C3A) 8
Tetra Calcium Alumino Ferrite (C4AF) 12
 48

Table 3.1(b) Physical Properties of OPC

Physical Properties
28 days compressive strength (N/mm2) 62
Fineness (m2 / Kg) 295

3.1.2 Aggregate

The Fine Aggregate used was river sand passing through 4.75 mm
sieve, falling under zone III as specified in IS 383-1978 and with specific
gravity 2.60. Coarse aggregates used were crushed angular aggregates of
nominal size 20mm, with specific gravity 2.60 and bulk density 1636Kg/m3.
Locally available water conforming to IS456-2000 was used for concreting
and curing. Rebars of size 12mm dia. and 70mm length was used.

The mix proportion for M30 concrete arrived by IS code method is

given in Table 3.2.

Table 3.2 Mix proportion for M30 concrete arrived by IS code method

Materials / m3
Water Cement Fine aggregate Coarse Aggregate
of concrete
(Kg) 191.6 399 540 1175
Mix 0.48 1 1.353 2.944

3.1.3 Fly ash

Fly ash was taken from Tuticorin thermal power plant. The fly ash
obtained was Class F with specific gravity of 2.12 with Blaine’s fineness of
305 m2/Kg.
 49

3.1.4 RHA

Processed RHA was obtained from NK.Enterprises, Singhania

House, Jharsuguda, Orissa, India. It was supplied in the brand name, Silpozz.
The RHA was grey in colour with mean particle size of 25 microns and
specific gravity 2.3 and Blaine’s fineness of 315 m2/Kg. The chemical
composition of RHA is given in Table 3.3.

Table 3.3 Chemical composition of RHA

SiO2 (91.79%)
Composition Al2O3 Fe2O3 CaO MgO Na2O K2O
R* NR*
% 90.21 1.58 2.12 0.80 1.27 0.67 0.14 0.76
R* - Reactive; NR* - Non-reactive

Table 3.3 (Continued)

Composition
Others LOI Total
[Contd.]
% 0.89 1.56 100

The XRD picture of RHA given in Figure 3.1 shows its amorphous
property, which confirms that RHA is reactive in nature.
 50

Figure 3.1 X-Ray Diffraction pattern of RHA

3.1.5 LP

LP was obtained from limestone kiln at Madurai, Tamilnadu, India.

LP used had a specific gravity of 2.80 with Blaine fineness as 480m2/Kg.

The X-Ray Diffraction of LP is given in Figure 3.2.

Figure 3.2 X-Ray Diffraction of LP

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From a mineralogical point of view, lime is composed mainly of

portlandite [Ca(OH)2]. Low quantities of calcite (~10%) were detected. This
was probably due to a partial recarbonation of portlandite during storage,
handling or other manufacturing processes. Mineralogical analysis was
carried out using X-ray diffraction (XRD) with PAN analytical make, Model -
X’per PRO with source CuK radiation (2.2KW Max.), Graphite crystal
diffraction beam side with sample spinner and zero background sample
holder. Particle size analysis of LP was done to see the particle size
distribution.

Figure 3.3 Particle size distribution for LP

From Figure 3.3, the particle size distribution of LP lies

between 0.1 to 100 m, with about 10% less than 1 m. This fineness of
LP makes it readily react to give early strength to concrete. The major
frequency lies within particle sizes of 40 m to 50 m. From the figures it
is obvious that, LP is found to be finer, similar to PPC and RHA.
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3.2 TESTS CARRIED OUT

3.2.1 Compression Test

The compressive strength of concrete was carried out as per IS516-

1959. Concrete specimens of 150 x 150 x150 mm cubes were cast with
different types of blended cement concrete. After 24 hours the specimens
were demoulded and subjected to curing for 28 days in ordinary tap water.
After the curing period was over, the cubes were tested in the Compression
Testing Machine (CTM) of capacity 2000kN, at the rate of loading of 140
kN/minute. Figure 3.14 shows the compression test setup on concrete cube
specimen. The ultimate load at which the cube failed was taken. Tests were
carried out on triplicate specimens and average compressive strength values
were recorded.

Figure 3.4 Compression test on concrete cube

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3.2.2 Split tensile test

Split tensile test was carried out as per ASTM C496-90. Concrete
cylinders of size 150 mm diameters and 300 mm height were cast. During
casting, the cylinders were mechanically vibrated using a table vibrator. After
24 hours, the specimens were removed from the mould and subjected to water
curing for 28 days. After the specified curing period was over, the concrete
cylinders were subjected to split tensile test by using universal testing
machine. Tests were carried out on triplicate specimens and the average split
tensile strength values were recorded, as shown in Figure 3.5.

Figure 3.5 Split tensile test on concrete cylinder

3.2.3 Flexural strength test

Flexural strength test was carried out as per IS516-1959 by

casting concrete beams of size 150 x 150 x 700mm size. After 24 hours,
the specimens were removed from the mould and subjected to water
curing for 28 days. After the specified curing period was over, the
 54

concrete specimens were subjected to flexural test by applying four point

loading using UTM, as shown in Figure 3.6.

Figure 3.6 Flexure beam test

3.2.4 Bond strength of concrete

Bond strength of concrete was carried out as per IS 2770 – 1967 –

Part-1. The aim of this experiment is to determine the bond between steel and
concrete in Reinforced concrete structures under static loading. Cold twisted
deformed bars of 12 mm diameter and 600 mm long were used for steel-
concrete bond strength determination. The rod was placed centrally along
with helical reinforcement provided in the centre of the concrete cube of size
100 × 100 × 100 mm. The rebar is projected down for a distance of about 10
mm from the bottom face of the cube as cast and projected upward from the
top up to 300 mm height in order to provide an adequate length to be gripped
for application of load. During casting of concrete cubes, the moulds were
mechanically vibrated.

The cubes were removed from the mould after 24 h and then cured
for 28 days with complete immersion in distilled water. After the curing
 55

period was over the steel-concrete bond strength was determined using
Universal Testing Machine (Model: UTM-60) of capacity 60t. The bond
strength was calculated from the load at which the slip was 0.25 mm. Tests
were carried out in triplicate specimens and average bond strength values
were obtained. The pull out load is then converted into bond stress on the
surface area of contact of the reinforcement as given in Equation 3.1.

P
Bond stress, (3.1)
DL

where,

P, D and L refer to the applied load, diameter and embedment length

of the bar, respectively.

3.2.5 Test for density, permeable voids and water absorption

The permeability of concrete is a measure of the rate at which a

liquid pass through it. The permeability of concrete depends upon its pore
network, which arises from the excess water used during mixing and
during initial hardening process. The overall porosity includes closed or
logged pores in addition to a network of inter connected pores. Pore size
ranges from a few angstroms to about 100 A for the so called ‘gel pores’,
from 100 to 100000 A in ‘capillary pores’ and a few millimeter in ‘air or
large pores’. Inter connected pores endow the concrete permeability. All
the hydrated cement products are subjected to attack by sulphates,
chlorides, and acids and less by water. This is because of low equilibrium
solubility of the hydrated components and low mass transfer of well-
cured concrete. It is a usual practice to assess the water permeability
characteristics when assessing the durability characteristics. Permeability
can be measured by conducting standard test methods. In the present
 56

investigation, percentage of water absorption, percentage of permeable

voids and percentage of total voids have been determined as per ASTM C
642-06.

This test was done as per procedure given in ASTM C 642-06

by oven-drying method. For this test 50mm diameter and 50mm height
cubes were cast. After 24 hours of demoulding, the specimens were kept
immersed in water. At the end of 28 days, the specimens were taken from
the curing tank and air-dried to remove the surface moisture. Then, the
specimens were dried in an oven at a temperature of 100+10o C for 48
hours, and allowed to cool at room temperature. At the end of 48 hours,
the weights of the specimens were measured to an accuracy of 1 gram
using a standard weighing balance. Then the specimens were kept
immersed in water continuously for 48 hours. Initially up to 30 minutes,
1hour, 2, 3, 4, 6, 24 and 48 hours the increase in weight was measured
after wiping out the initial surface water using dry cloth. After 48 hours of
immersion in water the specimens were heated continuously for a period
of 5 hours. Then the weights of the specimens were taken after a time gap
of 14 hours. The specimens were suspended in water and its submerged
weight was determined.

To determine the percentage of total voids the apparent specific

gravity of the specimen has to be determined. From the above data
percentage of water absorption, percentage of permeable voids,
percentage of total voids, and co-efficient of water absorption were
determined based on Equations 3.2, 3.3 and 3.4.

Percentage of Water absorption

B A
% of water absorption = x100 (3.2)
A
 57

where,

A = weight of oven dried sample in air.

B = weight of surface dry sample in air after immersion in water.

Percentage of Permeability

Volume of permeable Voids=[(C –A)/(C-D)] x 100 (3.3)

where,

C = weight, after 5 hours heating

D = submerged weight in water

Percentage of Total Voids

% of Total Voids = [(g1 – g3)/g3 ] x 100 (3.4)

where, g1 = A / (C-D)

g3 = apparent specific gravity of the specimens.

3.2.6 Rapid Chloride ion Penetration Test (RCPT)

This test was conducted as per ASTM C1202-10. Concrete disc of

size 100 mm diameters and 50 mm thickness were cast and allowed to cure
for 28 days. After 28 days of curing, the concrete specimens were subjected to
RCPT test by impressing a voltage of 60 V. Two halves of the specimens
were sealed with plastic container of diameter 100 mm.

The Rapid Chloride ion Permeability Test (RCPT) was conducted in

accordance with ASTM C1202-10 using concrete disc of size 100 mm
diameters and 50 mm thickness. After 28 days of curing, the concrete
specimens were subjected to RCPT test by impressing a voltage of 60 V
between two containers filled with 3% NaCl solution and 0.3 N NaOH
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solution. Current was measured at every 30 minutes up to 6 hours, based on

Equation 3.5.

Q = 900 (I0 + 2I30 + 2I60 +………+ 2I300 + 2I330 + I360) (3.5)

Where,

Q = Charge passed (Coulombs),

I0 = Current (amperes) immediately after voltage is applied, and

It = Current (amperes) at t min after voltage is applied.

Figure 3.7 Rapid chloride ion penetration test setup

One side of the container is filled with 3% NaCl solution (that side
of the cell was connected to the negative terminal of the power supply), the
other side was filled with 0.3 N NaOH solution (which was connected to the
positive terminal of the power supply). Current was measured at every 30
minutes up to 6 hours. Chloride contamination and temperature at every
30 minutes was also monitored. The experimental setup is shown in Figure
3.7. From the results using current and time, chloride permeability was
calculated in terms of Coulombs at the end of 6 hours.
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3.2.7 Chloride diffusion coefficient

The amount of chloride ion migrating through different types of

concrete specimens after 28 days of moisture curing was monitored
periodically by removing small aquilot and determining the chloride
concentration of these samples, until steady state was reached (120 hours).
Chloride diffusion coefficient was calculated using Nernst–Einstein equation
(Song, 2009) given in Equation 3.6.

JRTL
D (3.6)
ZFC 0 E

where, D is the chloride diffusion coefficient at steady state

condition (cm2/s), J is the flux of chloride ions (mol/cm2s), R is the gas
constant (8.314 J/K mol), T is the absolute temperature (300K), L is the
thickness of the specimen (cm), Z is the valency of chloride ion (Z = 1), F is
the Faradays constant (9.648 × 104 J/Vmol), C0 is the initial chloride ion
concentration (mol/l), E is the potential applied (60 V).

3.2.8 Impressed voltage test

This test has been conducted as an accelerated corrosion testing

technique for comparing different characteristics of concrete (Song, 2009).
Cylindrical concrete specimens of size 50 mm diameter and 100 mm height
were cast with LP and RHA at various percentages of replacement with
centrally embedded rebar of 12 mm diameter and 70 mm height. During
casting, the moulds were mechanically vibrated. After 24 hours, the
cylindrical specimens were demoulded and subjected to water curing for 28
days. After curing, the specimens were subjected to impressed voltage test. In
this technique, the concrete specimens were immersed in 5% NaCl solution
and embedded steel in concrete is made anode with respect to an external
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stainless steel electrode serving as cathode by applying a constant positive

potential of 12 V to the system from a DC source, as shown in Figure 3.8 and
Figure 3.9.

Figure 3.8 Schematic representation of impressed voltage test

The variation of current is recorded with time. For each specimen, the
time taken for initial crack and the corresponding maximum anodic current
flow was recorded. Three specimens were used for this technique.

Figure 3.9 Impressed voltage test

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3.2.9 Anodic polarization Technique (Harmlessness test)

Mild steel rods were embedded in concrete specimens of size 50

mm diameter and 100 mm height. The concrete specimens were subjected to
anodic polarization studies using a three electrode system which consists of
embedded steel in concrete as anode, stainless steel ring electrode as cathode
and saturated calomel electrode as reference electrode. Anodic polarization
study was carried out in 3% NaCl solution. The current flowing at +260 mV
was recorded for all the specimens upto 72 hours.

3.2.10 Linear Polarisation Resistance(LPR) Technique

Linear polarization measurements were conducted using ACM field

machine (UK). Reinforced (12mm diameter and 40mm length TMT rebar)
cylindrical concrete specimens of size 50mm diameter and 60mm height
admixed with 3% chloride were cast with various systems. The experimental
setup consists of three electrode cell assembly in which rebar acts as a
working electrode, perforated stainless steel cylindrical sheet as a counter
electrode and Saturated Calomel Electrode (SCE) as a reference electrode and
the whole assembly was immersed in a beaker containing distilled water as
electrolyte.

In this investigation, the rebar was polarized to the potential range

of -20 to +20mV from OCP at a scan rate of 0.1mVs-1 and a current response
was measured. The polarization resistance Rp of the embedded steel in
concrete was obtained from the slope of the potential current curve. From the
Rp values, the corrosion current Icorr (µA cm-2) and corrosion rate were
determined using the relationship given in Equation 3.7.

B
I corr (3.7)
Rp
 62

where,

B is a Stern-Geary constant = 26 mV

From the Icorr value, the corrosion rate (mm/year) was calculated
from Equation 3.8.

Corrosion rate = 0.0116 x Icorr (3.8)

All the experiments were carried out at room temperature of 35 ± 1oC.

3.2.11 A.C. Impedance measurements

Impedance measurements were carried out using steel in various

quaternary cement mixes using an ACM Instrument (UK). The real part (Z’)
and the imaginary part (-Z”) of the cell impedance were measured for various
frequencies (10 mHz to 30kHz). Plots of Z’ vs Z” were made.

3.2.12 Open Circuit Potential (OCP) measurements

Cylindrical concrete specimens of size 50mm diameter and 100mm

height were cast with 12mm diameter and 70mm length rebars which were
embedded in the centre of the concrete specimen with a bottom cover of
20mm. The rebars were cleaned with pickling acid and degreased before
being embedded in concrete. After 24 hours, the concrete specimens were
demoulded and cured for 28 days in distilled water. The specimens were kept
under alternate wetting and drying condition upto 60 days in 3% NaCl
solutions. One cycle consists of 3 days wetting and 3 days drying. The
process was continued upto 10 cycles.

Measurements of OCP were made using a voltmeter with a high

input impedance of 10 M.ohms. The positive terminal of the voltmeter was
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connected to the working electrode i.e., reinforced steel. The common

terminal was connected to the external reference electrode (SCE). The
corresponding potentials were recorded. OCP for all the specimens were
monitored over an exposure period of 120 days as per ASTM C -876-2010.

3.2.13 Gravimetric weight loss determination

100mm height and 60 mm diameter concrete cylinders were cast and

12mm diameter rebar of 70mm length were embedded at the centre of the
specimen. The initial weight of the rebar was taken before embedment in the
concrete. After casting, the specimens were cured for 28 days. Then all the
specimens were subjected to alternate wetting and drying cycle mentioned
above. The process was continued for 120 days. After 120 days the specimens
were broken open and the specimens were visually examined for its rust
initiation. Then all the rebars were pickled in inhibited hydrochloric acid as
per method prescribed in ASTM G1-1995 to remove the rust. Final weights of
the rebars were measured. From the initial and final weight, loss in weight due
to corrosion was determined.

From this, Corrosion rate was calculated as per Equation 3.9.

87.6 xW
Corrosion rate (in mmpy) = (3.9)
DxAxT

where,

W =loss in weight, mg, D = density of iron, g/cm3,

A = area of the bar, cm2, T = time, hours

3.2.14 pH measurement

The pH of all the quaternary concrete extracts was determined using

a portable Roy instrument (model pH 300) pH meter which was calibrated
 64

using a buffer solution of pH 9. pH values were measured at the end of an

exposure period of 120 days. At the end of the exposure period, concrete
specimens were split open and the concrete core sample very near to the rebar
was taken, powdered and the fine powder was taken for pH measurements.

3.2.15 Scanning Electron Microscope (SEM) - EDAX

At the end of the exposure period, core samples were cut from the
steel-concrete interface and subjected to scanning electron microscopy and
EDAX analysis for identification of elements present in the concrete samples.
SEM scans a focused beam of electrons across the specimen and measures
any of several signals resulting from the electron beam interaction with the
specimen. Images of topography can be used to study particle size, shape,
surface roughness and fracture surfaces, while polished surfaces are used for
determination of phase distribution and chemical composition. A concrete
prism was cut into cubes approximately 10mm square, one side of which was
ground flat. The hydrated samples were flooded with acetone to stop
hydration reactions. After drying, the specimens were subjected to gold
sputtering to make it conductive. A micrograph was recorded using the
scanning electron microscope (SEM-Hitachi Model, S-3000H, Japan).

3.2.16 X-Ray Diffraction (XRD) Studies

The samples were crushed mechanically and subjected to x-ray

diffraction studies. XRD is a technique which can be used for identification
of rock or mineral content of powder samples, or determination of the
chemical structure of crystalline materials. An X-ray beam is directed to a
powder sample; diffracted x-rays from the crystalline constituents are then
collected as planar reflections, characteristic of crystalline phases present in
the sample. Once the phases present in the fines have been identified, they
 65

can be correlated with the chemical composition obtained from chemical

analysis.

For XRD analysis, raw materials were ground to a fine powder of

less than 63 m. X-Mineralogical analysis was carried out using XRD with
Analytical make, Model - X’per PRO with source CuK radiation (2.2KW
Max.), Graphite crystal diffraction beam side with sample spinner and zero
background sample holder. XRD gives optimal results in terms of
characterization when crystalline components are analysed. In the case of
glassy, where atoms adopt a much less organized structure, the XRD diagram
presents the shape of a broad hump (halo) which displays a maximum peak
corresponding to the most probable spacing between atoms. When a
component is partly crystalline, partly glassy, the diagram is made of a halo
surmounted by a set of peaks.

3.2.17 Thermo Gravimetric/Differential Thermal Analysis (TG/DTA)

TG/DTA was used for the study of thermal behaviour and to

characterize the various compounds in the specimens. TG/DTA were carried
out using a simultaneous TGAsDTA 851 Mettler Toledo thermoanalyser
(Schwerzenbach, Switzerland) using alumina crucibles, with holed lids, at 20º
C/min heating rate, under static air atmosphere, from ambient temperature to
1000º C.

3.3 METHODOLOGY

3.3.1 Binary blending of OPC with fly ash

To characterize the amount of fly ash in the binary blending of

cement (PPC), four mixes of concrete OPC, OPC + 10% fly ash, OPC + 20%
fly ash and OPC + 30% fly ash were adopted. Three sets of cubes were cast
 66

for the above mixes, for which the compressive strength, density variation and
water sorptivity were found after 28, 60, 90, 120, 300 and 450 days.

3.3.1.1 Tests on Binary blending of OPC with fly ash

Compressive strength was determined as the first step to ascertain

the basic strength development of the binary mix specimens. Water sorptivity
measured was the unidirectional movement of fluids, due to the capillary
forces exerted by the pore structure, to be drawn into the body of the material.
The sides of the specimen were sealed with transparent epoxy coating so as to
allow the water to penetrate along one side of the specimen. The samples
were dipped in the fluid in a vertical position with one surface in partially
immersed to a depth of 5mm and the other open to the atmosphere, as shown
in Figure 3.10.

Figure 3.10 Water sorptivity test

The density variations of the specimens arrived by taking the cubes

from the solution, wiping the wet surface and finding out the weight of the
specimen. The variation in the ratio between weight and volume of the
specimen gives the density variation of the concrete specimens.
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Figure 3.11 Curing of Specimens in Water, Na2SO4 and MgSO4 solution

The above sets of cubes were cast in triplicate for each mix and kept
in ordinary potable water, 5% Na2SO4 solution and 5% MgSO4, as shown in
Figure 3.11. The MgSO4 and Na2SO4 solution were replaced every three
months.

3.3.2 Ternary and Quaternary blending of OPC with fly ash

Based on the compressive strength, density variation and absorption

tests, the binary mix which performs well is selected for quaternary blending
with RHA and LP. Since there is a synergy between fly ash and LP in ternary
blending, which is well established by Weerdt et al (2011) and the improved
performance of quaternary blended cements as reported by Pipilikaki et al
(2009), the blending procedure adopted in this work is given in Table 3.4.

Table 3.4 SCMs in Ternary and Quaternary mixes

S.No. Blending Type SCMs added

1 Ternary OPC + RHA + LP
2 Quaternary OPC + fly ash + RHA + LP