CHAPTER - I

INTRODUCTION
1.0 General
Concrete is one of the most widely used man-made construction material in the
world. Metakaolin is the cementetious material used as an admixture to produce high
strength concrete. Optimal quality of metakaolin for M70 grade of concrete has been
worked out, which can replace the cement in order to get better strength and durability.
Also identification of the drying shrinkage and permeability characteristics of blended
cement has been done. Jipingbai studied that when metakaolin is used as a partial
replacement for Portland cement, tends to improve both the mechanical properties and
durability of concrete. Friars and Cabrera investigated the relation between the pore size
distribution and degree of hydration of metakaolin based cement pastes. It was reported
that metakaolin showed the best improvement on the mechanical properties of concrete.
Palomo investigated the chemical stability as metakaolin based cement composites. Not
until the 1900s did engineers and materials technologists become involved in optimizing
the strength of concrete, though concrete has been used throughout history as a building
material. With each successive development and corresponding strength increase, the
definition of high strength was revised. Of course, there is no exact point of separation
between normal-strength concrete. According to the American Concrete Institute, high
strength is defined as that over 6000psi (41 MPa) compressive strength. This value was
adopted by ACI in 1984, but is not yet hard and fast, because ACI recognizes that the
definition of high-strength varies on a geographical basis. J.Francis Young of the
University of Illinois at Champaign-Urbana has developed a strength classification
system that, though not yet adopted by a recognized authority, is a helpful tool for
describing high strength concretes.
A versatile material, high strength concrete (HSC) possesses desirable properties
other than high strength. The most dramatic and memorable applications stem from this
aspect, however, as high-rise buildings like 311 South Wackier Drive create striking
visual impressions. This structure, at 969 ft (295 m), was the worlds tallest concrete
building when completed in 1989, utilizing concrete with compressive strengths of up to
12,000 psi (83 MPa).

1.1 Metakaolin
Metakaolin is the white powder of A
l 2 O3

.2Si

O3

.2

H2

l 2 O3

.2Si

O2

by dehydrating kaolin (A

O) at an appropriate temperature (700-900oC). Kaolin is in a

layered silicate structure, with the layers binding with each other via the Van Der Weals

bond, among which O H

is bound firmly. Kaolin, when being heated in air, may

experience several structural changes, and when being heated to around 600 oC, the
layered structure of kaolin is damaged due to dehydration to form a transient phase with a
poor crystallinity, i.e. metakaolin. As the molecular arrangement of metakaolin is
irregular in a thermodynamic metastable condition, it is cementetious under an adequate
excitation. With a high activity, metakaolin can be used to manufacture cementetious
materials and mix high-strength high-performance concrete.
1.1.1 Uses of Metakaolin
MK finds usage in many aspects of concrete:

1.1.2

High performance, high strength and lightweight concrete

Precast concrete for architectural, civil, industrial and structural purposes
In tall and heavy structures where high strengths are required
Fibre cement and Ferro cement products
Glass fibre reinforced concrete
Mortars, stuccos, repair material, pool plasters.
Advantages of Metakaolin
Increased compressive and flexural strengths
Reduced permeability (including chloride permeability)
Reduced potential for efflorescence, which occurs when calcium is transported by
water to the surface where it combines with carbon dioxide from the atmosphere

to make calcium carbonate, which precipitates on the surface as a white residue.

Increased resistance to chemical attack
Increased durability
Reduced effects of alkali-silica reactivity (ASR)
Enhanced workability and finishing of concrete
Reduced shrinkage, due to "particle packing" making concrete denser
Improved color by lightening the color of concrete making it possible to tint
lighter integral color.

1.1.3 Applications of Metakaolin Concrete

2

 Metakaolin is used in colors industrial floorings.

Fiber cement &Ferro cement products, glass fiber reinforced concrete, stuccoes,
repair materials, pool plasters etc.
In pre-cast concrete works.
In tall and heavy structures where high strengths are required.
In combination with other chemical admixtures and steel fibers, it is suitable for
repair works,
In the manufacture of concrete pipes, Metakaolin addition has shown to increase
the external load bearing capacity of the pipes and increased resistance against
chemical attack,
Concrete containing Metakaolin is known to have improved resistance to
freezing, thawing, chloride penetration and deeper scaling making it useful for
road construction,
The low permeability and absorption of the Metakaolin mixed cement concrete as
well as its enhanced resistance to deterioration in a variety of chemically
aggressive environments, found a gainful use in shortcrete applications in
chemical, mining, paper and pulp industries.
1.1.4 Forming Metakaolin
The T-O clay mineral kaolinite does not contain interlayer cations or interlayer
water. The temperature of dehydrolxylation depends on the structure layer stacking order.
Disordered kaolinite dehydroxylates between 530 and 570 C, ordered kaolinite between
570 and 630C. Dehdydroxylated disordered kaolinite shows higher pozzolanic
activity than ordered. The dehydroxylation of kaolin to metakaolin is an endothermic
procees due to the large amount of energy required to remove the chemically bonded
hydroxyl ions. Above temperature range of dehydroxylation, kaolinite transforms into
metakaolin, a complex amorphous structure which retains some long-range order due to
layer stacking. Much of the aluminum of the octahedral layer becomes tetrahedrally and
pentahedrally coordinated. In order to produce a pozzolan (supplementary cementitious
material) nearly complete dehydroxylation must be reached without overheating, i.e
thoroughly roasted but not burnt. This produces an amorphous, highly pozzolanic state
whereas overheating can cause sintering, to form a dead burnt, nonreactive refractory,
containing mullite and a defect Al-Si spinel. Reported optimum activation temperatures
vary between 550 and 850 C for varying durations, however the range 650-750 C is
most commonly quoted. In comparison with other clay minerals kaolinite shows a broad
temperature interval between dehydroxylation and recrystallization, much favouring the
3

formation of metakaolin and the use of thermally activated kaolin clays as pozzolans.
Also, because the octahedral layer is directly exposed to the interlayer (in comparison to
for instance T-O-T clay minerals such as smectites), structural disorder is attained more
easily upon heating.
1.2 Fire resistance of concrete
In the structural design of buildings, in addition to the normal gravity and lateral
loads, it is in many cases necessary to design the structure to safely resist exposure to fire.
Several investigations have shown that the deterioration in the compressive strength
of concrete under high temperature exposure. There are indeed rare researches about
temperature gradient and exposure time of the concrete indirect contact with the fire
flames. In this study there is an attempt to investigate the effect of temperature gradient
and exposure of high strength concrete to fire flames on compressive strength, tensile
strength and flexural strength and Stress-strain curve of high strength concrete.
In common with other structural members, performance assessment of concrete
elements is normally carried out with respect to a standard heating curve developed in a
fire resistance test furnace. This heating regime is defined purely in terms of a
temperature-time curve, originally conceived as being representative of the development
of a fire in a standard living room, and expressed in essentially identical form in a
number of standards, both nationally, i.e. the ISO-834 fire curve, and internationally, i.e.
the BS-476 curve in the UK, ASTM E-119 in the US. Other standard fire curves exist
which is intended to replicate the temperature developments in other assumed scenarios.
For example, the hydrocarbon curve is commonly used in the chemical processing
industry to represent the development of a fire involving liquid fuels. This curve has a
much more rapid growth phase and high temperatures (over 1000C) are attained within
the first 20 minutes of the fire. This curve has a very fast temperature development and
attains a peak value of 1350C after about an hour. It has also been used in testing of nontunnel structural members. Firstly, though temperature development is standardised via
furnace control, the actual heating impact on the structure is dependent on other variable
factors, including the optical properties of the furnace gases and the thermal response of
the structure. Secondly, the test results provide very little information on the likely
performance of structural elements in situ, i.e. taking into account the interaction between
different parts of a structure, the effects of restraint, etc. Thirdly, whilst there may be
gradients in thermal exposures even within the uniform heating environment of fire
4

resistance furnaces, even steeper gradients are common in fully-developed compartment

fires. The effects on structural performance of spatial non-uniformities in heating are
poorly known, though it has long been recognised that spalling can be linked to these
conditions. Finally, standard curves make no attempt to account for the important postfire cooling stage of a fire. The potential significance of cooling on concrete performance
was demonstrated during a test of some concrete structural elements at Hagerbach test
gallery, Switzerland. During the test a concrete sample resisted temperatures of up to
1600C for two hours without failure, but half an hour into the cooling phase the sample
collapsed explosively. It is not currently known, in the majority of cases, how much
spalling exhibited in a real building fire takes place as a result of cooling rather than
heating. Although considerable research has been conducted to understand the behaviour
of steel structures during cooling, no equivalent effort has so far been made for concrete.
As is clear from the above, standard fire tests can only simulate a very limited range of
heating conditions. Recently there has been some discussion on the different response to
fire behaviours of concrete in short hot fires compared to long cool ones. While many
of these scenarios are covered by the so called parametric curves, most testing is still
conducted with the standard furnace. Methods to establish equivalency between standard
testing and real fire behavior are very crude and mostly designed for steel members and
not for concrete or thermal insulation. Short hot fires provide severe thermal stresses to
structures but are of limited duration. During long cool fires, peak temperatures are
lower, but due to the longer fire duration the concrete member may be heated to a much
greater depth. Debate on which of these conditions is more harmful to concrete is
ongoing.
1.2.1 Fire Effect on the Mechanical Properties of Concrete
Several mechanisms have been identified for the deterioration of concrete due to
high temperature. These include decomposition of the calcium hydroxide with time and
water, expansion of lime on re-hydration, destruction of gel structure, phase
transformation in some types of aggregate, and development of micro-cracks due to
thermal incompatibility between cement paste matrix and aggregate phase.
High strength concrete, in comparison with medium strength concrete, is more
brittle; contains less water; and the solid particles are more compact. Hence, the effects of
high temperature on high strength concrete will be different to those with the medium
strength concrete.
5

1.3 Need for Present Study

The behavior of high strength concrete in strength and temperature has been known
earlier where as partially replaced cement by Metakaolin has not been known. Hence this
study is emphasised on mechanical properties of M70 grade of concrete with partially
replaced cement when exposed to various temperature effects.
1.4 Objective of Study
To evaluate Split tensile strength and Stress-strain curve of MKC at 15%
replacement by exposing to temperature of 100oC, 200oC, 300oC, 400oC and 500oC.
1.5 Scope of Study
The results of this experimental study are applicable, only to
a) The effect on Split tensile strength and Stress-strain curve of concrete, caused by
the replacement of cement by Metakaolin to the extent of 0% and 15% in respect
of OPC.
b) With the use of Super plasticiser (Conplast sp430) at a dosage of 500ml per 50 kg
of cement as a step to reduce the higher water demand for the same workability of
concrete mix.
c) Variation of Stress-strain curve and Split tensile strength of cylinders curing for a
period of 28 days.
d) Variation of mechanical properties for

temperature effect on cylinders for

different temperature such as 100C, 200C, 300C, 400C and 500C

duration of 1,2 and 3 hours in furnace.

for

CHAPTER-II
THEORY AND LITERATURE REVIEW
2.0 General
This chapter deals with the theoretical particulars and test particulars of materials
used in the investigation. The materials used, design details and various tests in fresh and
hardened properties of concrete are dealt in detail.
2.1 Materials
The properties and specifications of various materials used in the preparation of
test specimens are as follows.
2.1.1 Cement
The main raw material for the production of cement is clinker. Clinker is an
artificial rock made by heating limestone and other raw materials in specified quantities
to a very high temperature in a specially made kiln. Portland cement is hydraulic cement
made by finely pulverizing the clinker produced by calcining to incipient fusion a
mixture of argillaceous and calcareous materials. It is the fine grey powder that is the
most important ingredient of concrete; hence the name Cement concrete. Cement
undergoes a chemical reaction with water and sets and hardens when in contact with air
or underwater. The global production of cement is approximately 1.5 billion tons per
year.
Portland cement is a general term used to describe hydraulic cement. The typical
raw materials used for making cement are limestone (CaCo3), sand (SiO2), stale clay
(SiO2, Al2O3, orFe2O3), and iron ore (Fe2O3). Thus the chemical components of cement
are calcium (Ca), silicon (Si), aluminum (Al), and iron (Fe). The calcareous component,
lime, (CaO), is derived from one of the following: limestone, chalk, marble, lime sand
shell deposit, lime sludge. The argillaceous component (SiO2, Al2O3, or Fe2O3) is derived
from one of the following: clay, shale, tuff ash, slate, glass. Different brands of cement
have been found to possess different strength development characteristics and rheological
behavior due to the variations in the compound compositions and fineness. Hence it was
decided to use cement from a single supplier. Ordinary Portland Cement (OPC) is now
available in three grades namely 33, 43 and 53 grades, the number indicating the
compressive strength of standard cement sand mortar cubes in MPa at 28 days curing.
7

Table 2.1.1 Physical Properties of cement

Permissible limit as per

Properties

Results

Fineness of grinding

270 M2/kg

Shall not be less than 225 m2/kg

Normal consistency

33%

Specific gravity

3.15

Initial

120min

Should not be less than 30min

Final

240min

Should not be more than 600min

3 days

31N/mm2

Should not be less than 23 N/mm2

7 days

42.74 N/mm2

Should not be less than 33 N/mm2

28 days

53.23 N/mm2

Should not be less than 43 N/mm2

IS: 12269-1987

Setting Time

Compressive strength
of mortar cubes for

Table 2.1.2 Chemical Properties of cement

Component
SiO2
AL2O3
Fe2O3
CaO
MgO
K2O
Na2O
Ti02
P2O5
SO3

Amount (% by mass)
21.89
5.6
3.75
62.33
1.04
0.92
0.11
0.30
0.17
2.88

The cement used for this present study was PARASAKTI (OPC) 43 grade
conforming to IS: 8112 1989. It was fresh, was of uniform color, consistency, and free
from lumps and foreign matter. Mortar cube strengths corresponding to 3, 7 and 28 days
were 31 N/mm, 42.74 N/mm and 53.23 N/mm respectively. Physical and chemical
properties of cement are tabulated in Table 2.1.1 and 2.1.2 respectively.

2.1.2 Fine aggregate

Fine aggregate used for HSC should be properly graded to give minimum void
ratio and free from deleterious materials like clay, silt content and chloride contamination
8

etc. The optimum gradation of fine aggregate for HSC is determined more by its effect on
water requirement than on physical packing. American Concrete Institute (ACI)
committee reports that sand with fineness modulus below 2.5 gives concrete a sticky
consistency, making it difficult to compact and sand with fineness modulus about 3 gives
the best workability and compressive strength. Properties such as void ratio, gradation,
Specific gravity, Fineness modulus, free moisture content, Specific surface and bulk
density have to be assessed to design a dense HSC mix with optimum cement content and
reduced mixing water.
The fine aggregate used in the present experimental programme is river sand
conforming to Zone III as per IS 383:1970.It is clean, free from organic matter, silt and
clay. The physical properties of fine aggregates are as tabulated in Table 2.1.3.
Table 2.1.3 Properties of fine aggregate
Properties
Specific gravity
Bulk density (gm/cc)
Fineness modulus

Test values
2.60
1.68
2.66

Fig 2.1.2 Fine aggregate

2.1.3 Coarse aggregate
The coarse aggregate is the strongest and the least porous component of concrete. It
is also chemically stable material. Presence of Coarse aggregate reduces the drying
shrinkage and other dimensional changes occurring on account of movement of moisture.
Coarse aggregate contributes to impermeability of concrete, provided that it is properly
graded and the mix is suitably designed. Coarse aggregate in cement concrete contributes
9

to the heterogeneity of the cement concrete and there is a weak interface between cement
matrix and aggregate surface in cement concrete. These two factors result in lower
strength of cement concrete. But in HSC, by restricting the maximum size of aggregate
and also by making the transition zone stronger by usage of mineral admixtures, the
cement becomes more homogeneous and there is a marked enhancement in the strength
properties as well as durability characteristics of concrete.
Properties such as crushing strength, durability, Stress-strain curve, maximum size,
gradation, shape and surface texture characteristics, percentage of deleterious particles as
well as flakiness and elongation indices need special consideration while selecting the
coarse aggregate for HSC. The aggregate should be sound, free from deleterious material
and must have crushing strength at least 1.5 times of concrete.
Grading of concrete plays crucial role in HSC and it becomes even more important
if placement is by pump. Flaky and elongated particles are to be restricted to a minimum
to reduce the weaker zones in the concrete. This is important for tensile strength.
Although Indian code does not specify any limit on flakiness and elongation indices, it is
preferable to limit these indices individually to 15 percent and their combined value to 25
percent for good quality of concrete.
Width of section and spacing of reinforcement usually govern selection of
maximum size of aggregate. In case of normal strength concrete, it may be desirable to
use larger size of aggregates as possible, to reduce the volume of cement paste resulting
in an economic mix design. However, one of the important factors that determine the
maximum size of aggregate is the bond between mortar and aggregate. Bigger size
particles cause concentration of stresses around the particles due to differences between
the elastic modulus of the paste and the aggregate and results in lower strength of
concrete.
When smaller sizes of aggregates are used, the increase in strength is due to the
reduction in the average bond stress, due to the increased surface area of the aggregates.
As far as the shape of the aggregate is concerned, crushed granite coarse aggregate
provides better interlocking and hence higher than rounded gravel aggregate. The coarse
aggregate meeting the requirements of BIS: 383-1970 is suitable for making HSC.
The coarse aggregate used is from well-established quarry, satisfying the code IS
383:1970. The mixture of coarse aggregates is used; mix proportion used is 100% of
20mm only. The material is of uniform colour and has good angularity. The physical
properties of coarse aggregate are tabulated in Table 2.1.4.
10

Table 2.1.4 Properties of coarse aggregate

Properties

Test values

Specific gravity

2.64

Bulk density (Loose) (gm/cc)

1.38

Bulk density (compacted) (gm/cc)

1.53

A machine crushed granite stone aggregate of maximum size 20 mm was used.

Tests on aggregates were conducted as per IS 2386 (Part III) of 1963.

F
ig 2.1.3 Coarse aggregate
2.1.4 Water
Water is an important ingredient of concrete as it actively participates in the
chemical reactions with cement to form the hydration product, calcium-silicate-hydrate
(C-S-H) gel. The strength of cement concrete depends mainly from the binding action of
the hydrated cement paste gel. A higher water-binder (w/b) ratio will decrease the
strength, durability, water-tightness and other related properties of the concrete. As per
Neville (2000), the quantity of water added should be the minimum requirement for
chemical reaction of unhydrated cement, as the excess water would end up only in the
formation of undesirable voids (capillary pores) in the hardened cement paste of concrete.
The strength of cement paste is inversely proportional to the dilution of the paste. Hence,
it is essential to use as little paste as possible, consistent with the requirements of
workability and chemical combination with cement.
From HSC mix design considerations, it is important to have the compatibility
between the given cement and the chemical and mineral admixtures along with the water
used for mixing. The water used for making concrete should be free from undesirable
11

salts that may react with cement and admixtures and reduce their efficiency. Silts and
suspended particles are undesirable as they interface with setting, hardening and bond
characteristics. Algae in mixing water may cause marked reduction in strength of
concrete either by combining with cement to reduce the bond or by causing large amount
of air entrainment in concrete.
Water conforming to the requirements of BIS: 456-2000 is found to be suitable for
making HSC. It is generally stated that water fit for drinking is fit for making concrete.
The water used is potable water collected from laboratory taps and satisfies the code IS
3025:1984. Water cement ratio of 0.31 for M70 grade of concrete was adapted in the
experimental programme.
2.1.5 Metakaolin
Metakaolin is a calcined product of the clay mineral kaolinite. The particle size of
metakaolin is smaller than cement particles, but not as fine as silica fume.
When kaolinite, a layered silicate mineral with a distance of 7, 13 between the layer of
SiO2 and Al2O3 is heated, the water contained between the layers is evaporated and
the kaolinite is activated for exaction with cement.
Metakaolin is refined kaolin clay that is fired (calcined) under carefully controlled
conditions to create an amorphous aluminosilicate that is reactive in concrete. Like other
pozzolans (fly ash and silica fume are two common pozzolans), metakaolin reacts with
the calcium hydroxide (lime) byproducts produced during cement hydration. Calcium
hydroxide accounts for up to 25% of the hydrated Portland cement, and calcium
hydroxide does not contribute to the concretes strength or durability. Metakaolin
combines with the calcium hydroxide to produce additional cementing compounds, the
material responsible for holding concrete together. Less calcium hydroxide and more
cementing compounds means stronger concrete. Metakaolin, it is very fine and highly
reactive, gives fresh concrete a creamy, non sticky texture that makes finishing easier.
Alkali-silica reaction is a reaction between calcium hydroxide (the alkali) and glass
(the silica) which can cause decorative glass embedment in concrete to pop out. Because
metakaolin consumes calcium hydroxide, it takes away the alkali and the reaction does
not occur.
Table 2.1.5 Physical Properties of Metakaolin
Average particle size, m

1.5

12

Specific Gravity

2.65

Bulk density (kg/m3)

710 kg/m3

Physical form

Off White Powder

Table 2.1.6 Chemical Properties of Metakaolin

SI.NO
1
2
3
4
5
6

Characteristics

Result Metakaolin (%wt)

Loss of Ignition
4.52
Silica(as SiO2)
60.45
Alumina(as Al2O3)
16.23
Iron(as Fe2O3)
8.56
Calcium(as Cao)
3.73
Magnesium(as MgO)
2.14
*Source- koat manufacturing company, Gujarat, India.

2.1.6 Chemical Admixtures

HSC has low water-binder (w/b) ratio and has ultra fine particles in the form of
mineral admixtures such as fly ash. Hence, effective dispersion of cement and fly ah is
necessary to achieve proper microstructure of the hardened concrete as well as
workability of the concrete without increasing the unit water content and cement content
of a mix. This is achieved with the use of chemical admixtures. Hence, chemical
admixtures are essential ingredients in the HSC mix, as they increase the efficiency of
cement paste by improving the workability of the mix and thereby resulting in
considerable decrease of water requirement. Thus, with w/b ratio as low as 0.3 or less, the
concrete mix can be produced with the use of chemical admixtures. The water content
could be reduced; thereby effective control on the w/b ratio could be maintained to
achieve the desired strength and durability.
The commonly used chemical admixtures are plasticizers and super plasticizers,
retarders and air entraining agents. Plasticizers and super plasticizers, being surfactant in
nature, help to disperse the cementations particles in the mix, thus fluidity of the concrete
mix is increased. Retarders reduce the initial rate of hydration of cement so that the fresh
concrete retains its workability for a longer time. Air entraining agents artificially
introduce (entrain) Air bubbles which increase the workability of the mix of their ballbearing and also enhance the resistance to deterioration of hardened concrete.
2.1.6.1 Super Plasticizer
13

For producing HSC, the most important chemical admixture is the super plasticizer,
which is a High-Range Water-Reducing Admixture (HRWRA).There are four types of
super plasticizers.

Sulphonated formaldehyde melamine(MSF) condensates with a chloride content

of 0.005 percent(Type A)

Sulphonated naphthalene formaldehyde (NSF) condensates with negligible

chloride content (Type B).

Modified lingo sulphonates which contain no chlorides (Type C).

Carboxyl acrylic ester copolymer (Type D).

Super plasticizers are water reducers which are capable of reducing water content

by about 30 percent. However it is noted that full efficiency of super plasticizer can be
got only when it is added to mix that has an initial slump of 20 to 30 mm. Addition of
super plasticizer to stiff concrete mix reduces its water reducing efficiency. Depending on
the solid content of the mixture, a dosage of 1 to 3 percent by weight of content is
advisable.
In order to improve the workability of high strength concrete, super plasticizer
Conplast 430 was used. This had 40% active solids in solution.
2.1.6.2 Properties of Conplast SP430
Commercial Name: Conplast sp 430
Basic ingredient: Sulphonated naphthalene formaldehyde
Specific gravity: 1.22
Appearance: liquid brown colour optimization
2.1.6.3 Mechanism of Action of Super Plasticizer
The mechanism by which super plasticizer produces their effect can be explained
as follows .It consists of very large molecules (colloidal size) which dissolve in water to
produce ions with high negative charge (anions).These anions are attracted to the surface
of cement grains and at the normal levels of admixture usage are absorbed in sufficient
numbers to form a complete monolayer around them. The combination of electrostatic
repulsion and ionic size brings about a rapid dispersion of the individual cement grains.
2.2 Workability
Workability is the ability of a fresh (plastic) concrete mix to fill the form/mould
properly with the desired work (vibration) and without reducing the concrete quality.
14

Workability depends on water content, aggregate (shape and size distribution),

cementations content and age (level of hydration) and can be modified by adding
chemical admixtures, like super plasticizer. Raising the water content or adding chemical
admixtures will increase concrete workability. Excessive water will lead to increased
bleeding (surface water) and segregation of aggregates (when the cement and aggregates
start to separate), with the resulting concrete having reduced quality. The use of an
aggregate with an undesirable gradation can result in a very harsh mix design with a very
low slump, which cannot be readily made more workable by addition of reasonable
amounts of water.
Workability of fresh concrete is determined by following methods:
1. Slump cone Test.
2. Compacting Factor.
2.2.1 Slump Cone Test
Slump test is the most commonly used method of measuring consistency of
concrete which can be employed either in laboratory or at site of work. It is not suitable
method for very wet or very dry concrete. It does not measure all factors contributing to
workability, nor is it always representative of the place ability of the concrete. However,
it is used conveniently as a control test and gives an indication of the uniformity of
concrete from batch to batch.
This test is used to determine the workability of concrete. The apparatus is a cone
of 10 cm top diameter, 20 cm bottom diameter, and 30 cm height.It has two handles for
lifting purposes. Initially the cone is cleaned and oil is applied on the inner surface. Then
the concrete to be tested is placed into the cone in three layers. Each layer is compacted
20 times by a standard tamping rod. After filling the cone, it is lifted slowly and carefully
in the vertical direction. Concrete is allowed to subside and this subsidence is called
slump.
If the slump is even, then it is termed as true slump. If one half of cone slides, it is
called shear. If entire concrete slides, it is called collapse. Shear slump indicates that
concrete is non-cohesive and shows a tendency for segregation. Generally, the slump
value is measured as the difference between the height of the mould and the average
height after subsidence. Slump test is a simple test and is widely used.

15

Fig 2.2.1 Slump test apparatus

2.2.2 Compaction Factor Test
Compaction factor test was developed by Road Research Laboratory U.K. and is
one of the most efficient tests for measuring workability. A standard amount of concrete
is allowed to fall from a standard height and the compaction factor is measured. It has
two hoppers and a cylinder. The first hopper has a top diameter of 25.4 cm, bottom
diameter of 12.7 cm, and an internal height of 27.9 cm. the second hopper has a top
diameter of 22.9 cm, bottom diameter of 12.7 cm, and an internal height of 22.9 cm. The
cylinder has an internal diameter of 15.2 cm and height of 30.5 cm. the distance between
the two hoppers and between the lower hopper and the cylinder is 20 cm.
The concrete sample to be tested is first placed in the top hopper. The trap door is
opened and concrete is allowed to fall to the lower hopper. Similarly, from the lower
hopper, concrete is allowed to fall into the cylinder below. Now the cylinder is weighed
and the weight is called as weight of partially compacted concrete. Now the cylinder is
emptied and refilled with concrete from the same sample. It is rammed or vibrated
heavily and its weight is taken. This weight is known as weight of fully compacted
concrete. These values are used to calculate the compaction factor by using the following
relation:
Compaction factor =

weightofpartiallycompactedconcrete
weightoffullycompactedconcrete

16

Fig.2.2.2 Compacting factor apparatus

17

LITERATURE REVIEW
The study of behavior of Portland cement concrete had been taken up extensively
by many authors since good olden days. The existing literature on the behavior of HSC
under elevated temperature conditions with consideration of parameters like compressive,
flexural and Split tensile strength, stress-strain behavior are reviewed briefly and the
details are as presented below.
Khatib et al.(11) (1996) investigated the porosity and pore size distribution of cured
Ordinary Portland Cement-Metakaolin paste. Pastes containing 0, 5, 10 and 15
Metakaolin were prepared at a constant water / binder (w/b) ratio of 0.55. Specimens
were moist cured for period from 3 days to 365 days. The intruded pore volume and the
pore structure were determined by mercury intrusion porosimetry. The proportion of large
pores in the paste decreases with both increase in Metakaolin content and increase in
curing time. Although the total intruded pore volume generally decreases with increase in
curing time it is found to increase with increase in Metakaolin content. Also an increase
in pore volume is observed between the curing times of 14 and 28 days for pastes
containing Metakaolin.
Rama Rao et al.(15) (1997) concluded that the durability of concrete using rice husk ash
as an admixture is better in terms of permeability, abrasion and chemical resistance to
sulphate attack.
Khatib et al.

(12)

(1998) in their research said that the partial substitution of cement with

Metakaolin is investigated in terms of resistance of Metakaolin mortar to Sodium

Sulphate (Na2So4) Solution and some specimens are cured in water. Results on strength,
pore size distribution, porosity, are reported.
Five different mixes were prepared starting from M5, M10, M15, M20, and M25
with Metakaolin content varying from 5,10,15,20 and 25% respectively .specimens of all
these different mixes were prepared, cured in 5%(Na2So4) solution and then tested . The
test results concluded that the increasing levels of Metakaolin in PC mortars exposed to
(Na2So4) solution produce reduced the levels of expansion and increased the resistance to
cracking. Mortars exposed to (Na2So4) solution and containing Metakaolin levels of up to
10% exhibit a loss in strength, and those containing Metakaolin levels of 15% exhibit a
gain in strength, relative to equivalent water-cured specimens.

18

Long T.Phan et al.

(13)

(2000) A compilation of fire test data which shows distinct

behavioral differences between high-strength concrete (HSC) and normal strength

concrete (NSC) at elevated temperature is presented. The differences are most
pronounced in the temperature range of 20 C to 400 C. What is more important is the
observed explosive spalling of HSC specimens during fire tests.. A comparison of test
results with current code provisions on the effects of elevated temperatures on concrete
strength shows that the CEN Euro codes and the CEB provisions are unconservative.
Aspects of analytical modeling for predicting the buildup of internal pressure during
heating are discussed.
Frais.M et al.(8) (2000) The authors show the results of an investigation focusing on the
effect of Metakaolin (MK) on the micro-structure of MK-blended pastes. Pastes
containing 0%, 10%, 15%, 20% and 25% of MK were prepared at a constant
water/binder ratio of 0.55 and cured at 200C for hydration periods from 1 to 360 days.
They investigated total capillary and gel porosity evolution with the curing period and
also estimated the degree of hydration in the ordinary Portland cement and Metakaolin
blended pastes. The values of the degree of hydration are calculated from the amount of
Ca (OH) 2 present in the paste and from the data of differential thermal analysis (DTA)
thermogravimetry (TG). A good association between porosity and degree of hydration
has been established. The total porosity decreases up to 28-56 days of curing time. They
observed that, up to 28 to 56 days of curing the porosity is same for all the mixes.
Beyond 56 days the porosity of all the Metakaolin mixes increasing when compared with
OPC mix. Similar phenomenon is observed for capillary porosity. The best evidence of
the influence of MK on the refineness of the pore structure was detected in pores with
radius smaller than 100A. Between 7-90 days, the gel porosity of MK mixes increase,
while the OPC mix remains practically constant. The results show the necessity of
obtaining important improvement in the porosity reducing the average pore diameter and
gel porosity. Measured lime contents show the total consumption of MK (10% to 15%) at
90 days of hydration time. A good statistical relationship has been found between the
degree of hydration and the porosity.
Xia Oquian and Zongjinli(20) (2001) studied the stressstrain relationships of concrete
containing 0% to 15% of Metakaolin at an incremental rate of 5%. They concluded that
incorporation of Metakaolin up to 15% has increased the tensile and compressive strength

19

and also peak strain is increased at increasing rate of Metakaolin up to 15%.

Incorporation of Metakaolin has slightly increased the compressive elasticity modulus.
Bo wu, Xiao - Ping Su and Huili(3) (2002) studied the effect of high temperature on
residual mechanical properties of confined and unconfined high strength concrete. They
varied the temperature from 100C to 900C. Also elastic modulus decreases sharply at
the higher temperatures.
Chi-Sun Poon et al.(5) (2003) an experimental investigation was conducted to evaluate
the performance of metakaolin (MK) concrete at elevated temperatures up to 800 C.
Eight normal and high strength concrete (HSC) mixes incorporating 0%, 5%, 10% and
20% MK were prepared. The residual compressive strength, chloride-ion penetration,
porosity and average pore sizes were measured and compared with silica fume (SF), fly
ash (FA) and pure ordinary Portland cement (OPC) concretes. It was found that after an
increase in compressive strength at 200 C, the MK concrete suffered a more severe loss
of compressive strength and permeability-related durability than the corresponding SF,
FA and OPC concretes at higher temperatures. Explosive spalling was observed in both
normal and high strength MK concretes and the frequency increased with higher MK
contents.
Srinivasa Rao et al.(18) (2004) investigated the effect of elevated temperatures ranging
from 50 to 250o C on the tensile strength (splitting and flexural) of High-Strength
Concrete (HSC) made with Portland Cement (PC) and Pozzolana Portland Cement
(PPC), for application in the chemical and metallurgical industries or thermal shielding of
nuclear power plants. Tests were conducted on 150 mm diameter cylindrical specimens
and 100 mm x 100 mm x 500 mm beam specimens. The specimens were heated to
different temperatures of 50, 100, 150, 200 and 250 o C for three different durations of 1, 2
and 3 hours at each temperature. After the heat treatment, the specimens were tested for
both splitting and flexural tensile strengths. Test results were analysed and the effects of
elevated temperatures on PPC concrete were compared with PC concrete. Results
concluded that PPC concrete exhibited better performance than PC concrete.

Abdul Razak et al.(1) (2005) in this study, metakaolin (MK) and silica fume (SF) were
used as cement replacement materials at 5%, 10%, and 15% by mass. Water/cementitious
materials (w/cm) ratios varied from 0.27 to 0.33, and strength testing was conducted up
20

to an age of 180 days. It was found that the strength of a pozzolanic mixture could be
related to the strength of its equivalent control by a linear function. Key parameters
involved in the model are the pozzolanic and dilution factors, which can be correlated to
the pozzolan content in the mixture. The study concludes that the accuracy of the model
increases with concrete age. At ages 28 days and above, 97% of the estimated strengths
are within 5% of the actual value.
Chi-Sun Poon et al.(6) (2006) this study is to relate the mechanical and durability
properties of high performance metakaolin (MK) and silica fume concretes to their
microstructure characteristics. The compressive strength and chloride penetrability of the
control and the concretes incorporated with MK or silica fume (SF) at water-to-binder
(w/b) ratios of 0.3 and 0.5 are determined. The pore size distribution and porosity of the
concretes are also measured. The effect of MK and SF on the interfacial porosity is
discussed based on test results. It is found that MK concrete has superior strength
development and similar chloride resistance to SF concrete and the MK concrete at a w/b
of 0.3 has a lower porosity and smaller pore sizes than the control (plain) concrete. The
resistance of the concretes to chloride ion penetration correlates better with the measured
concrete porosity than with the paste porosity. The differences between the measured and
calculated concrete porosity is smaller for MK and SF incorporated concrete than for the
control concrete, indicating an improvement in the interfacial microstructure with the
incorporation of the pozzolanas. This difference is found to be related to the strength and
chloride penetrability of concrete to some degree.
Nabil M. Al-Akhras(14) (2006) this study investigates the effect of metakaolin (MK)
replacement of cement on the durability of concrete to sulfate attack. Three MK
replacement levels were considered in the study: 5%, 10%, and 15% by weight of
cement. The other experimental parameters investigated in the study were: water to
binder ratio (0.5 and 0.6), initial moist curing period (3, 7, and 28 days), curing type
(moist and autoclaving), and air content (1.5% and 5%). After the specified initial moist
curing period, concrete specimens were immersed in 5% sodium sulfate solution for a
total period of 18 month. The degree of sulfate attack was evaluated by measuring
expansion of concrete prisms, compressive strength reduction of concrete cubes, and
visual inspection of concrete specimens to cracks. The study showed that MK
replacement of cement increased the sulfate resistance of concrete. The sulfate resistance
of MK concrete increased with increasing the MK replacement level. The sulfate
21

resistance of MK concrete at w/b ratio of 0.5 was found higher than that at w/b ratio of
0.6. Autoclaved MK concrete specimens showed superior sulfate resistance compared to
moist cured ones. The pore volume of autoclaved MK concrete was found less than that
of moist cured MK concrete. The air entrained MK concrete showed higher improvement
in the sulfate resistance than the non-air entrained MK concrete.
Bamonte et al.(2) (2010) the present investigation deals with high temperature, in order
to evaluate the thermal diffusivity and the mechanical decay as a function of the
temperature, since there is still scanty information in the literature on the hightemperature behavior of this family of materials. The very high-strength concrete
(VHSC) investigated turned out to be very efficient, since (1) its compressive strength
exhibits a decay very close to that of normal-strength concrete, with no sizable
differences between the hot and residual properties (250750C); (2) its specific
fracture energy increases very much indeed with the temperature; and (3) its rather low
thermal diffusivity guarantees good insulation properties. As an application of this
material, the parking apron of an airport and its two-layered pavement subjected to a hot
spot (T400C) have been considered, in order to investigate whether delamination at the
interface between the top VHSC layer and the bottom normal strength concrete layer
and/or cracking in the bottom layer may occur. The performance of the pavement was
analyzed for different values of the thickness of the top VHSC layer and also for different
values of its thermal properties, and proved to be very satisfactory in terms of tensile
behavior. However, the critical factor remains the initial heating rate.
Rafat Siddique et al.(16) (2010) an investigation dealing with the effect of metakaolin
(MK) on the near surface characteristics of concrete are presented in this paper. A control
concrete having cement content 450 kg/m3 and w/c of 0.45 was designed. Cement was
replaced with three percentages (5, 10, and 15%) of metakaolin weight. Tests were
conducted for initial surface absorption, sorptivity, water absorption and compressive
strength at the ages of 35, 56, and 84 days. Test results indicated that with the increase in
MK content from 5 to 15%, there was a decrease in the initial surface absorption,
decrease in the sorptivity till 10% metakaolin replacement. But at 15% MK replacement
an increase in sorptivity was observed. All mixtures showed low water absorption
characteristic i.e. less than 10%. Compressive strength shared an inverse relation with
sorptivity. Higher MK replacements of 15% are not helpful in improving inner core
durability, even though it helps in improving surface durability characteristics.
22

Dinakar et al.(7) (2011) examined High Reactive Metakaolin (HRM) for high strength
and high performance concrete. According to him supplementary cementing materials
(SCMs) such as fly ash, silica fume and GGBS are increasingly used in recent years as
cement replacement material. They help obtain both higher performance and economy.
These materials increase the long term performance of the concrete through reduced
permeability resulting in improved durability. Metakaolin, which is a relatively new
material in the concrete industry, is effective in increasing the compressive strength,
reducing the sulphate attack and improving air-void network. Metakaolin differs from the
more commonly used mineral admixtures, such as fly ash and silica fume, in that it is not
a by-product. It is manufactured under conditions by thermally activating purified
kaolinite clay within a specific temperature range (650800C). The resulting anhydrous
alumino-silicate (Al2Si 2O7) also represented as AS2 is mainly amorphous in nature and
behaves as a highly reactive artificial pozzolan. He also explained Behaviour of
metakaolin in concrete composites such that the strength of metakaolin concrete may not
be same as that of the normal plain cement concrete. Comparing the mixtures containing
5 and 10 percent HRM and silica fume, it was observed that the compressive and flexural
strength in HRM mixtures were significantly greater than those of non-pozzolanic control
mixture and slightly higher than the silica fume mixtures. In conclusion, it was also
reported that HRM has high reactivity and that the strength and performance of 10
percent HRM concrete was similar to, or even better than the 10 percent silica fume
concrete.
Beulah et al.(4) (2012) this paper presents an experimental investigation on the effect of
partial replacement of cement by metakalion by various percentages viz 0%, 10%, 20%,
and 30% on the properties of high performance concrete, when it is subjected to
hydrochloric acid attack. An aggregate binder ratio of 2 and different water binder ratios
viz 0.3, 0.35, 0.40 and 0.45 was used in this investigation. Concrete specimens of size
150 x 150 x 150 mm were casted to find residual compressive strength and specimens of
size 100 x 100 x 100mm were casted to find percentage weight loss; both the sizes of
specimens were casted and cured as per IS specification. After 28 days water curing, the
concrete specimens were kept immersed in 5% concentrated hydrochloric acid solution
for 30, 60 and 90 days for observation. Before immersion, they were weighed accurately
and after required days of immersion and observation, the specimens were removed from
hydrochloric acid media, weighed accurately and tested for their compressive strength;
23

weight loss and hardness of concrete were studied. The various results which indicate the
effect of replacement of cement by metakalion on HPC are presented in this paper to
draw useful conclusions.
Vikas Srivastava et al.(19) (2012) this study deals with the addition of some pozzolanic
materials, the various properties of concrete viz, workability, durability, strength,
resistance to cracks and permeability can be improved. Silica fume is a byproduct
resulting from the reduction of high purity quartz with coal or coke and wood chips in
an electric arc furnace during the production of silicon metal or silicon alloys. The
principle physical effect of silica fume in concrete is that of filler, which because of its
fineness can fit into space between cement grains in the same way that sand fills the
space between particles of coarse aggregates and cement grains fill the space between
sand grains. Metakaolin is also one of such waste/ non - conventional material which can
be utilized beneficially in the construction industry. This paper presents the results of an
experimental investigations carried out to find the suitability of silica fume and
metakaolin combination in production of concrete. The optimum doses of silica fume and
metakaolin in combination were found to be 6% and 15% (by weight) respectively, when
used as part replacement of ordinary portland cement.

24

CHAPTER - III
METHODOLOGY
3.1 Introduction
Based on the preliminary investigations carried out, the experimental
investigation is planned as under.
1. To obtain the mix proportions of OPC concrete for M70 by Erntroy and
Shacklocks Empirical graphs
2. Preparation of Testing Specimens
To prepare the concrete cylinders (150 x 300mm) for Split tensile and
Stress-strain curve with 0% and 15% replacement of OPC with
Metakaolin for M70 grade concrete for temperature study i.e., for 100 oC,
200oC, 300oC, 400oC and 500oC.
To cure the specimens for 28 days.
3. To evaluate the mechanical characteristics of concrete such as Split tensile and
Stress-strain curve.
4. To evaluate the temperature studies of M70 grade MKC at an exposure of 100 oC,
200oC, 300oC, 400oC and 500oC for 1hr, 2hr and 3hr duration.
5. To evaluate and compare the results.
3.2 Method of Mix Design
Design of HSC mixes involves determination of the proportion of the constituents,
cement, coarse and fine aggregates, metakaolin, water and chemical admixture such
as Super plasticizer, so that resultant composition produces a mix which will possess
specified properties in fresh and hardened state. Mix design of HSC is a more critical
process than the design of normal strength concrete (NSC), due to the presence of
mineral and chemical admixtures and attainment of low water-binder material ratio.
In case of low and medium strength concretes, the strength is mainly influenced
by the water/cement ratio, and is almost independent of the other parameters. The
properties of high strength concretes with a compressive strength above 400 kg/cm 2 are
influenced by the properties of the aggregate in addition to that of water/cement ratio. To
obtain high strengths, it is necessary to use the lowest possible water/cement ratios which
affects the workability of the mix and necessitates the use of normal vibration techniques
for proper compaction. In this context, it is to be noted high strengths have to be achieved
by suitable proportioning and not by steam curing or application of pressure. In the
25

present state of the art, concrete which has a desired 28 days compressive strength up to
700 kg/cm2 can be made by suitable proportioning of the ingredients using normal
vibration methods for compaction of the mixes. The highest strengths reported by Collins
are in the vicinity of 1100 kg/cm2. Recent report by PAROTT outlines the experimental
investigations on the production and properties of high strength concrete, pursued at the
Cement and Concrete Association, London.
3.2.1Erntroy and Shacklocks Empirical Graphs
Erntroy and Shacklock have suggested empirical graphs relating the compressive
strength to an arbitrary reference number for concrete made with crushed granite, coarse
aggregates and irregular gravel. These graphs are shown in fig 3.2.1 and fig 3.2.2 for
mixes with ordinary Portland cement and in fig 3.2.3 and fig 3.2.4 for mixes with rapid
hardening Portland cement. The relation between water cement ratio and the reference
number for 20mm and 10mm maximum size aggregates is shown in fig 3.2.5, in which
four different degrees of workability are considered. The range of the degrees of
workability varying from extremely low to high corresponds to the compacting factor
values of 0.65 and 0.95 respectively.
The relation between the aggregate-cement and water-cement ratios, to achieve
the desired degree of workability with a given type and maximum size of aggregate are
compiled in table 3.2.1 and 3.2.2 for two different types of cements.

26

Table 3.2.1: Aggregate cement ratio (by weight) required to give four degrees of
workability with different water-cement ratios using ordinary Portland cement

Type of coarse aggregate*

Irregular grave

Maximum size of aggregate

Degree of workability

20 mm

EL VL

EL

Crushed granite

10mm
VL

20mm
EL

VL

10mm

EL

VL

Water/cement ratio
by weight
0.30

3.0

2.4

0.32

3.8

2.5

3.2

0.34

4.5

3.0

2.5

3.9

3.3

2.9

3.6

2.3

4.2

2.8

2.3 -

4.0

2.6

2.6 -

4.6

3.2 2.6

0.36

5.2

3.5

3.0

2.5

4.6

3.1 2.6

0.38

4.0

3.4

2.9

5.2

0.40

4.4

3.8

3.2

0.42

4.9

0.44

5.2

3.6 3.1 2.6 4.7

3.2

2.7 2.3

3.5 3.0 2.5

4.1 3.5 2.9 5.2

3.6

3.0 2.6

3.9 3.3 2.7

4.5 3.8

3.2

4.0

3.3 2.9

4.1 3.5

4.3 3.6 3.0

4.9 4.2

3.5

4.4

3.6 3.1

5.3

4.5 3.8

4.7 3.9

3.3

5.3 4.5

3.7

4.8

3.9 3.3

0.46

4.8 4.0

5.1 4.2

3.6

4.8

4.0

5.1

4.2 3.6

0.48

5.2 4.4

5.4 4.5

3.8

5.1

4.2

5.5

4.5 3.8

0.50

5.5 4.7

4.0

5.4

4.5

4.8

*Natural sand used in combination with both types of coarse aggregate

EL = Extremely Low

VL = Very Low

L= Low

27

M = Medium

4.7

4.0

Table 3.2.2: Aggregate cement ratio (by weight) required to give four degrees of
workability with different water-cement ratios using rapid hardening cement
Type of coarse aggregate*

Irregular gravel

Maximum size of aggregate

20 mm

Degree of workability EL VL

Crushed granite
10mm

EL

VL

2.4 -

20mm
EL

VL

10mm

EL

VL

Water/cement ratio
by weight
0.32

2.6

0.34

3.4

2.2

2.8

0.36

4.1

2.7

2.3

3.5

0.38

4.8

3.2

2.8

2.3

4.2

2.9 2.4

0.40

5.5

3.7

3.2

2.7

4.9

0.42

4.2

3.6

3.0

0.44

4.6

0.46

0.48

0.50

2.9

3.5

3.6

2.4

2.2

4.3

2.9 2.4

3.9

2.5

4.9

3.4 2.9 2.6 4.5

3.0

2.5

3.3 2.8 2.3 5.5

3.9 3.3 2.9 5.0

3.4

2.9 2.4

3.7 3.0 2.6

4.2 3.6

3.2 5.5 3.8

3.2 2.7

4.0 3.4

4.1 3.5 2.9

4.7 4.0

3.5

4.2

3.5 3.0

5.0

4.3 3.7

4.5 3.8 3.2

5.1 4.3

3.7

4.6

3.8 3.2

5.5

4.7 4.0

4.9 4.1 3.5

5.5 4.6

4.0

5.0

4.1 3.4

5.0 4.3

5.2 4.4 3.7

4.2

5.3

4.4 3.7

4.9

*Natural sand used in combination with both types of coarse aggregate

EL = Extremely Low

VL = Very Low

L= Low

M = Medium

The limitations of these design tables being that they were obtained with
aggregates containing 30 percent of the material passing the 4.75 mm IS sieve. Thus, if
other ingredients are used suitable adjustments have to be made. Aggregates available at
site may be suitably combined by the graphical method to satisfy the above requirement.
In view of the considerable variations in the properties of aggregates, it is generally
recommended that trial mixes must first be made and suitable adjustments in grading and
mix proportions effected to achieve the desired.

28

3.3 Mix Design Procedure

The mean design strength is obtained by applying suitable control factors to the specified
minimum strength.

1. For a given type of cement and aggregates used, the reference number
corresponding to the design strength at a particular age is interpolated from graph
3.3.1 to 3.3.4.
2. The water-cement ratio to achieve the required workability and corresponding to
the reference number is obtained from graph 3.3.5 for aggregates with maximum
sizes of 20mm and 10mm.
3. The aggregate-cement ratio to give the desired workability with the known water
cement is obtained by absolute volume method.
4. Batch quantities are worked out after adjustments for moisture content in the
aggregates.

Graph-3.3.1: Relation between compressive strength and reference number

(Erntroy and shacklock)

29

Graph-3.3.2: Relation between compressive strength and reference number

(Erntroy and shacklock)

Graph-3.3.3: Relation between compressive strength and reference number

(Erntroy and shacklock)

30

Graph-3.3.4: Relation between compressive strength and reference number

(Erntroy and shacklock)

Graph-3.3.5: Relation between water-cement ratio and Reference Number

31

Graph-

3.3.6:
Relation
waterratio and
Reference
Number

between
cement

Graph-3.3.7: Combining of Fine aggregates and Coarse aggregates

TABLE 3.3.1 DESIGN MIX PROPORTIONS (M70 Grade)
Design Method

Maximum

Mix Proportions (By Weight)

ERNTROY

Size Of C.A
20 mm

Cement
1

&

F.A
1.155

C.A
2.145

SHACKLOCK

3.4 Preparation of Testing Specimens

The specimens of standard cylinders (150mm x 300mm) are casted.
32

W/C Ratio
0.30

In specimens 192(cylinders) the cement was replaced by MK (0% and 15%) with
M70 grade concrete mix were casted and cured for 28 days for temperature studies.
3.4.1 Mixing
In the present work, the machine mixing process is employed. In the individual
mix, ingredients are weighed with their proportions exactly and then the materials are
thoroughly mixed in their dry condition before water is added. The prepared mix was
then immediately used for testing workability of fresh concrete mix. In case of
replacement cement with MK, the MK is first thoroughly mixed with cement in dry state
and then this was mixed with aggregate.
3.4.2 Casting of the Specimens
The cast iron moulds are cleaned to avoid dust particles and applied with oil on all
sides before concrete is poured in to the moulds. The moulds are placed on a level
platform. The well mixed green concrete is filled in to the moulds by vibration with table
vibrator. Excess concrete was removed with trowel and top surface is finished level and
smooth as per IS 516-1959.

Fig. 3.1Casting of the specimens

3.4.3 Compaction of Concrete
33

Compaction of concrete is the process adopted for expelling the entrapped air
from the concrete. In the process of placing and mixing of concrete, air is likely to get
entrapped in the concrete. If air is not removed fully, the concrete loses strength
considerably.
In order to achieve full compaction and maximum density, Table vibrator is used
in this experiment.
3.4.4 Curing of test specimens
After casting, the moulded specimens are stored in laboratory in room
temperature for 24 hours. After these periods the specimens were removed from the
moulds and immediately submerged in clean, fresh water curing tank for required period
as per IS 516-1969. The specimens are cured for 28 days.

Fig. 3.2 Specimens in curing tank

3.5 Tests for Workability

34

3.5.1 Slump Cone Test

Slump cone test is a very common test for determination of workability of
concrete. This test was carried out for M70 grade concrete mix, before casting the
specimens.
3.5.2 Compaction Factor Test
This test is more accurate than slump cone test and this test is used to determine
the workability of low water cement ratio concrete more accurately. This test is
conducted as per IS 1199-1959.
Table3.5.1 Slump and Compaction Factor Values for M70
Sl.No.
1
3

Description for M70

Plain Concrete
Metakaolin 15%

Compaction Factor
0.85
0.82

Slump (mm)
25
21

3.6 Testing of specimens

A time schedule for testing of specimens is maintained to ensure their proper
testing on the due date and time. The cast specimens are tested as per standard
procedures, immediately after they are removed from curing pond and wiped off the
surface water, as per IS 516-1959. The test results are tabulated.
3.6.1 Test for Split tensile strength
The specimen cylinders of 150 mm in diameter and 300 mm long after subjected
to temperature exposure for specified duration were released from the furnace and tested
for Split tensile strength after the specimens were cooled down to the normal room
temperature condition. Before placing the cylinder specimens in the compressive testing
machine, diametrical lines were marked at the two ends of the specimen. Plywood strip
was arranged in the machine to place the specimen by aligning in such a way that the
lines marked on the end of specimen are truly vertical and centred over the plywood strip.
Another plywood strip was then placed on the cylinder length wise in such a way that it is
centred on the lines marked at the ends of the cylinder as shown in fig3.4. The failure
load applied on the specimen was recorded. Finally the Split tensile strength of the
specimen was computed as mentioned below.
Split tensile strength=

2P
ld

Where d = dia of the cylinder measured.

35

l = length of cylinder measured.

P = maximum load recorded.
The average value of the three specimens was considered as the Split tensile
strength after satisfactory compliance of the condition that individual variation shall not
be more than 15 % of the average strength observed.

Fig.3.4 Testing of cylinder in C.T.M

3.6.2 Stress-Strain behavior
In order to ascertain the stress-strain relationship of concrete, as many as 96
numbers of cylinders were cast at 0%, 15% metakaolin and cured in the water tank for 28
days period. After the completion of the said period of curing, the samples were removed
from the tank and exposed to normal room temperature condition to wipe out the
moisture film on the specimen. 3 specimens of 0% and 3 specimens of 15% metakaolin
are marked to be kept under room temperature condition among the total 96 samples.
Balance 90 samples were placed in the furnace for heating under different temperatures
i.e., starting from 100 to 500oC at an interval of 100oC for 1, 2, and 3 hours exposure.
After heating the specimens for required time period, the specimens were removed from
the furnace and allowed to cool down to normal condition. Initially the cylinders marked
as S1, S2, S3 were tested for the behavior of stress-strain in C.T.M (as shown in Fig.3.6).

36

Fig.3.6 Testing of cylinder for stress-strain behavior in C.T.M

The surfaces of the cylinders were wiped off to make it free from any dust. The
bearing surfaces of the testing machine were wiped clean which are to be in contact with
the specimen. The loading frame with two circles one at top and other at bottom was
fitted to the cylinders and after placing the specimen into the machine steel supports were
removed. The top of the dial gauge attached to the loading frame was adjusted to touch
the cylinder outer surface by adjusting the initial reading to coincide with zero reading.
The cylinder specimen was gently placed on the bearing plate and the axis of the
specimen was carefully aligned with the centre of the spherically seated platen. No
packing was allowed between the faces of the test specimen and the steel platen of the
testing machine.
The machine was operated by increasing the load and the dial gauge readings
were noted down at intermittent dial gauge values. The procedure was continued for all
the specimens and readings were noted down. The stress was calculated from the applied
load divided by area of cylinder. The corresponding strain values were computed by
adopting decrease in length/original length of cylinder.

3.7 Description of Furnace

The purpose of the electric furnace is to heat the concrete specimens under study.
The heating arrangement in the furnace is as per International Standard ISO
834specifications. The furnace can be separated into two parts. The separated part can be
pulled out after loosening the screws provided for tightening the two parts. It consists of

37

wheels at the bottom on rails and can be moved to required location. It also consists of a
bed of refractory bricks of 110mm size, on which the specimen is to be placed.
The unseparated part is the heating chamber. This chamber measures 650mm in
height, 500mm in width and 1800mm in length, with the sides and top lined with
electrical heating coils embedded in refractory bricks. In this furnace, all the four faces of
the specimens can be exposed to high temperature. Temperature in the furnace is
controlled by means of a dedicated control panel which houses the power supply and
circuit switches for the furnace. The control panel also has an over temperature controller
to prevent the damage to the furnace by tripping out, if the temperature inside the furnace
exceeds specified temperature. The maximum operating temperature of the furnace is
1050C. Air vents are also provided in the unseparated part, at the top, to allow vapour to
escape from the heating chamber and to allow any thermocouple leads, if provided, to be
connected to a digital temperature logger. Concrete specimens are placed in the furnace
and exposed to the temperature for the required time. Then the required tests are
conducted for compression and flexure.
3.7.1 Heating and testing of specimens
After completion of curing of cylinder specimens, the same were removed from the
curing tank and transfer into open air condition to allow the same for drying without any
moisture filming on the surface. The specimens cylinders were transferred into furnace
where they were subjected to elevated temperatures i.e. 100, 200, 300, 400 and 500 oC for
1h, 2h and 3h exposure respectively as shown in Fig.3.8

38

Fig.3.8 Furnace with specimens

39

CHAPTER-IV
RESULTS AND DISCUSSION
The tests were carried out to obtain Split tensile strength and Stress-strain curve
of M70 grade concrete. The specimens are tested for 28 days for 0% and 15%
replacement of MK for Stress-strain curve and Split tensile strength. These are presented
in tables and graphs were plotted correspondingly.
It is also observed that the factors considerably influenced the strength of MKC
when exposed to temperature of 100oC, 200oC, 300oC, 400oC and 500oC.
In the present experimental work the specimens exposed to temperature undergo
physical changes and weight loss. The free moisture content is lost initially, followed by
physical adsorption of water.

4.1 Effect of Temperature on Split tensile Strength of Metakaolin Concrete

(Temperature Studies)
Table 4.1.1 28 Days Split tensile Strength exposed to different Temperatures

Sl.No.
1
2
3
4
5
6

28 days Split tensile strength for

28 days Split tensile strength for

Temperature

duration of exposure of 0% MKC

duration of exposure of 15%

(Mpa)
1 hour
5.59
5.66
4.88
4.31
3.82
3.32

MKC (Mpa)
1 hour
2 hour
6.37
6.37
6.50
6.58
6.15
6.01
5.59
5.23
4.67
4.46
3.82
3.61

27
100
200
300
400
500

2 hour
5.59
5.73
4.67
4.10
3.68
3.11

3 hour
5.59
5.45
4.53
3.89
3.54
2.97

40

3 hour
6.37
6.44
5.80
5.16
4.17
3.32

6
5.5
5
4.5
4

Split Tensile Strength (Mpa)

0% meta 1H Duration

3.5

0% meta 2H Duration
0% meta 3H Duration

3
2.5
2
0

200 400 600

Temperature in C

Graph 4.1.1 28 Days Split tensile Strength of concrete (%) vs. Exposed
Temperature (C) of 0% MKC

7
6.5
6
5.5
5
Split Tensile Strength (Mpa)

4.5

15% meta 1H Duration

15% meta 2H Duration

3.5

15% meta 3H Duration

3
2.5
2
0 200 400 600

Temperature in C

Graph 4.1.2 28 Days Split tensile Strength of concrete (%) vs. Exposed Temperature
(C) of 15% MKC

41

7
6.5
6
5.5

Split Tensile Strength (Mpa)

0% meta 1H Duration

4.5

0% meta 2H Duration

0% meta 3H Duration
15% meta 1H Duration

3.5

15% meta 2H Duration

15% meta 3H Duration

2.5
2
0

500 1000

Temperature in C

Graph 4.1.3 28 Days Split tensile Strength of concrete (%) vs. Exposed Temperature
(C) of 0% and 15% MKC
From the above graphs 4.1.1, 4.1.2, it is observed that the Split tensile strength
increases at 100oC temperature when compared to the strength obtained at normal room
temperature for 0% and 15% replacement of MK. The increase in Split tensile strength
associated with the increase in temperature is attributed to the increase in the surface
forces between gel particles (Vander wall forces) due to the removal of moisture content.

4.2 Effect of Temperature on Stress-strain curve of Metakaolin Concrete

The stress-strain behavior of cylinder specimens for 0% and 15% of metakaolin

cured for 28 days age and subjected to elevated temperature from 100 to 500 oC apart
from room temperature were as shown below. The various graphs plotted are as shown in
Fig.4.2.1 to 4.2.6.

42

40
35
30
25

Stress (Mpa) 20

0% meta

15

15% meta

10
5
0
0

Strain

Graph 4.2.1 Stress-strain curve of concrete at room temperature

40
35
30
25

0% meta 1H Duration
0% meta 2H Duration

Stress (Mpa) 20

0% meta 3H Duration

15

15% meta 1H Duration

15% meta 2H Duration

10

15% meta 3H Duration

5
0
0

Strain

Graph 4.2.2 Stress-strain curve of concrete exposed to 100oC for different exposure
durations

43

40
35
30
25

0% meta 1H Duration

Stress (Mpa) 20

0% meta 2H Duration
0% meta 3H Duration

15

15% meta 1H Duration

10

15% meta 2H Duration

15% meta 3H Duration

0
0

Strain

Graph 4.2.3 Stress-strain curve of concrete exposed to 200oC for different exposure
durations

44

35
30
25
0% meta 1H Duration

20

Stress (Mpa)

0% meta 2H Duration
0% meta 3 H Duration

15

15% meta 1H Duration

10

15% meta 2H Duration

15% meta 3H Duration

5
0
0

Strain

Graph 4.2.4 Stress-strain curve of concrete exposed to 300oC for different exposure
durations
30
25
0% meta 1H Duration

20

0% meta 2H Duration
0% meta 3H Duration

Stress (Mpa) 15

15% meta 1 H
Duration

10

15% meta 2H
Duration
15% meta 3H
Duration

5
0
0

Strain

Graph 4.2.5 Stress-strain curve of concrete exposed to 400oC for different exposure
durations

45

25
20
0% meta 1H Duration

Stress (Mpa)

15

0% meta 2H Duration

10

15% meta 1H
Duration

0% meta 3H Duration

15% meta 2H
Duration

5
0
0 0 0 0 0 0 0 0 0

Strain

46

15% meta 3H
Duration

Graph 4.2.6 Stress-strain curve of concrete exposed to 500oC for different exposure
durationsCHAPTER - V

CONCLUSIONS AND RECOMMENDATIONS

5.1 Conclusions
Based on the experimental investigation carried out, the following conclusions are made.
1. Workability of concrete decreases with the increase in Metakaolin
replacement level.
2. The Split tensile strength of conventional concrete and concrete with MK as
partial replacements are compared and observed and concluded that the
strength of the conventional concrete is slightly lower than the MKC.
3. At room temperature and 100oC exposure, the stress-strain relationship is
similar to the conventional concrete & MKC behavior. However the trend is
different for temperature exposure of 200oC to 500oC.
4. The strength increases at 100oC temperature and thereafter it starts losing its
strength as the temperature increases.
5.2 Scope for Further Study
1.

The study may be extended to know the behavior of concrete at elevated

temperatures up to 800o C.

2.

MKC exposed to duration of heating from 4 hours to 8 hours at different

temperatures can be carried out.

3.

Studies on replacement levels for higher grade concretes can be carried out.

4.

Beams with different shear span to effective depth ratios, varying

percentage of tensile reinforcement and varying percentage of MK, may be
investigated.

5.

Combination of Metakaolin with different other mineral admixtures like fly

ash and Rise Husk Ash can be carried out.

6.

For use of MKC as a structural material, it is necessary to investigate the

behavior of reinforced MKC under flexure, shear, torsion and compression
and the same exposed to an elevated temperature.

7.

Some tests relating to durability aspects such as water permeability,

resistance to penetration of chloride ions, corrosion of steel reinforcement,
durability in marine environment etc. need investigation.

47

8.

The study may further be extended to know the behavior of concrete

whether it is suitable for pumping purpose or not as present day technology
is involved in ready mix concrete where pumping of concrete is being done
to greater heights.

9.

To develop new design guide lines for making MKC suitable to withstand
high temperatures, acids, alkali and seawater attack.

48

REFERENCES
1) Abdul Razak (2005) Strength estimation model for high-strength concrete
incorporating metakaolin and silica fume, Cement & Concrete Research 35, pp
688-695.
2) Bamonte p (2010) Thermal and Mechanical Properties at High Temperature of
a Very High-Strength Durable Concrete Journal of Materials in Civil
Engineering ASCE, pp 545-555.
3) Bo Wu,Xiao-Ping Su. Hui Li and Jie Yuan (2002) Effect of High Temperature
on Residual mechanical properties of Confined and Unconfined high strength
concrete, ACI-Materials journals, Vol.99, No.4, pp 231-239.
4) Beulah M (2012) Effect of Replacement of Cement by Metakalion on the
Properties of High Performance Concrete Subjected to Hydrochloric Acid
Attack, IJERA, Vol.2, Issue 6, pp.033-038.
5) Chi-Sun Poon (2003) Performance of metakaolin concrete at elevated
temperatures, Cement & Concrete Research 25, pp 83-89.
6) Chi-Sun Poon (2006) Compressive strength, chloride diffusivity and pore
structure of high performance metakaolin and silica fume concrete, Cement &
Concrete Research 20 pp 858-865.
7) Dinakar P (2011) High reactive metakaolin for high strength and high
performance concrete The Indian Concrete Journal, pp 28-34.
8) Frias M (2000) Pore size distribution and degree of hydration of Metakaolincement pastes, Cement & Concrete Research Vol.30, pp 561-569.
9) IS 516: 1959, Method of test for strength of concrete, Bureau of Indian
Standards, New Delhi.
10) IS 12269: 1987, Specification for 43 Grade Ordinary Portland Cement,
Bureau of Indian Standards, New Delhi.
11) Khatib and S.Wild (1996) Pore size distribution of Metakaolin paste in
cement and concrete research, ICJ Vol. 26 No. 10, pp 1545-1553.
12) Khatib and Wild (1998). Sulphate Resistance of Metakaolin Mortar, Cement
and Concrete Research, ICJ Vol .28. No. 1, pp 83-92.
13) Long T. Phan (2000) Fire Performance of High Strength Concrete Journal of
Materials in Civil Engineering ASCE, May 8-10.
14) Nabil M. Al-Akhras (2006) Durability of metakaolin concrete to sulfate attack,
Cement and Concrete Research 36, pp- 17271734.
15) Rama Rao G.V, Seshagiri Rao M.V. (1997), Improvement in Durability
Characteristics of concrete using Pozzolanic Material as Admixture,
49

Proceedings of International Conference on maintenance & Durability of

Concrete Structures, Mar 4-6.
16) Rafat Siddique (2010) Effect of metakaolin on the near surface characteristic
of concrete, Materials and Structures 44, pp 77-88.
17) Shetty, M.S. Concrete Technology, S.Chand& company ltd, New Delhi.
18) Srinivasa Rao K, Potha Raju.M & Raju.P.S.N (2004) Effect of Age on HSC
on Reswidual Compressive Strength under Elevated temperatures, International
Conference on Advances in Concrete and Construction, pp 733-741.
19) Vikas Srivastava (2012) Effect of Silica Fume and Metakaolin combination on
concrete, IJCSE, Vol.2, Issue 3, PP 893-898.
20) Xia oquian and Zongjinli (2001). The relationships between stress and strain
for high performance concrete with Metakaolin, Cement & concrete research 31,
pp 1607-1611.

50

APPENDIX
Design of M70 Grade Concrete by Erntroy and Shacklocks Method
Specified 28 day cube strength = 70MPa.
Very good degree of control:
Control factor =0.85.
Degree of workability = very low.
Type of cement = Ordinary Portland cement (43 grade)
Type of coarse aggregate = crushed granite (angular) maximum size-20mm
Type of fine aggregate natural sand
Specific gravity of cement

= 3.15

Specific gravity of sand

= 2.60

Specific gravity of Coarse aggregate

= 2.64

The fine and coarse aggregate contains 5 and 1 percent moisture respectively and
by assuming aggregate is 100% passing through 20mm IS sieve and 96% through 10mm
IS sieve.
Average strength = 70/0.85 = 82.35MPa.
Reference number = 0.
With reference number, the water/ cement ratio is = 0.30.
For 20mm maximum size aggregate and very low workability, aggregate / cement ratio
for the desired workability = 3.3
The aggregate are combined so that 30percent of the material passes through the 4.75mm
I.S. sieve.
Ratio of fine to total aggregate = 35%.
Required proportions by weight of dry material are
Cement

: F.A

C.A.

35
100 ) X 3.3

: (

: 1.155

65
: ( 100

: Water.
) X 3.3

: 2.145

: 0.30

: 0.30.

If C= weight of cement required per m3 of concrete.

Then

C
3.15 +

1.155 C
2.60

2.145 C
2.64

C [0.317 + 0.444+0.812 + 0.30] =1000

C=533.9 kg/m3 of concrete
51

0.30C
1

= 1000

=534 kg/m3
Design MIX Proportion:
Ratio of mix proportion by weight:
Mix Grade

Cement

Fine Aggregate

M 70

1.155

Coarse

Water/

Aggregate

Cement

2.145

0.30

Material requirement (M70)

Mix design ratio

1: 1.155: 2.145: 0.30

S.NO

Material required

Quantity in kg/m3

Cement

534

Fine Aggregate

616.77

Coarse Aggregate

1145.43

Water

160.2 liters

The compressive Strength of OPC concrete after the trials mixes is 79.55 Mpa at 28 days.
Trail mix proportion:
Ratio of mix proportion by weight:
Mix Grade

Cement

Fine Aggregate

M 70

1.225

Coarse

Water/

Aggregate

Cement

2.275

0.31

Material requirement (M70)

Mix design ratio

1: 1.225: 2.275: 0.31

S.NO

Material required

Quantity in kg/m3

Cement

520

Fine Aggregate

637

Coarse Aggregate

1153

Water

161.2 liters

The compressive Strength of OPC concrete after the trials mixes is 68.78 Mpa at 28 days.

52