CE 772 Pavement Materials

Module 7-8: Cementitious Materials

Dr. Solomon Debbarma Email: sdebbarma@iitb.ac.in Phone: 8837237899 (M); 7131 (O)
 Referred Books

• Concrete Microstructure, Properties and Materials by Mehta and Monteiro

• Properties of Concrete by A.M. Neville,
• Concrete Technology, M.S. Shetty
• Integrated Materials and Construction Practices for Concrete Pavement: A State-
of-the-Practice Manual, FHWA HIF - 07 – 004,
https://intrans.iastate.edu/app/uploads/2019/05/IMCP_manual.pdf
 Materials for Concrete Structures

Coarse Aggregates Fine Aggregates Cement Water

Chemical Accelerators Plasticizers Retarders Air entraining

Admixtures

Mineral
Common Terminology
 Challenge
Coarse Aggregate Fine Aggregate

Already selected in the previous module

Cement Type???

Technical parameters Economic & Environmental parameters

• Strength (compressive or flexural) • Economical
• Early age strength • Less green house gas emissions
• Less shrinkage • Higher storage life
• Marine water Resistance
• Durability….
 Interesting Facts about Cement

• Current consumption of concrete is more than 30 billion tons every year

• Second highest used material after water
• Why concrete?

➢ Can be molded into any shape and size

➢ Water resistant

➢ Cheapest and most readily available material

• Cost of 1 kg of concrete?

• 1 m3 = 6000 Rs
• Density of concrete = 2400 kg/m3
• 2400 kg/m3 = 6000 Rs
• 1 kg = 2.50 Rs • Much Cheaper than 300 ml water
 Common Terminology

• Cement is the glue that binds concrete together, and its chemical composition
influences concrete behavior
• Hydraulic cement is a material that sets and hardens when it comes in contact with
water through a chemical reaction called hydration, and is capable of doing so under
water (ASTM C 125-03) i.e. cements that only hardens by reacting with water but also
form a water-resistant product are called Hydraulic Cements. Whereas, nonhydraulic
cements are the cements that hydrates but the final product is not water-resistant

• Hydraulic cements include Portland cement and blended cements

• The inventor of the first Portland cement thought its color was similar to that of rock
found near Portland, England; thus, the name

• Pozzolan: Material that reacts with cement & water to improve its microstructure

• Supplementary cementitious materials: cements and pozzolans other than Portland

cement
 Cement Production
• What do we need from cement ?
• Binding Strength: Cement react with water (hydration process) to produce Calcium Silicate
Hydrate (C-S-H) gel that provides strength.

C-S-H

calcareous Siliceous Mixing Water

materials Materials

• Clay apart from silica could

contains alumina (Al2O3) and iron
oxide (Fe2O3) and alkalies (Na2O
• Limestone (CaCO3) • Clay is used for silica and K2O)
Mostly Used • Alumina and Iron oxide helps in
Why clay is preferred?
• Chalk reducing the fusion temperature i.e.
• Sea-Shells • Quartz (which are highly siliceous) are formation of calcium silicates at
difficult to grind lower temp. Fluxing Agents
• Clay is available in finely grounded • If not present in clay, intentionally
state; saves energy could be added (Bauxite & Iron
• It also contains Al & Fe oxides which ore)
lowers fusion temperature • Alkalies are not desirable since
leads to alkali-silica reaction
 Cement Production
• Stages
Step 1: Mining of Aggregates:
• Limestone & Clay (silty clay, Zafarana clay, and Kaolin.)

Step 2: Crushing, stacking, and reclaiming of raw

materials
• Aggregates are crushed by crushers (jaw & then
impact) to reduce size less than 50 mm
Step 3: Raw meal drying, grinding, and homogenization
• The raw mix, limestone, clay and additives (iron &
bauxite ore) are fed from their bins to raw mills for
drying and fine grinding
• Materials are blended in powdered form (size < 75
µm)
Step 4: Clinkerization
• Blended materials are heated together in a rotatory
kiln (temperature above 1400° C); clinkers of size
~25 mm are formed
Step 5:Cement grinding and storage
• Clinker and 5% gypsum (to avoid flash set) are
extracted from their respective hoppers and fed to
the cement mills which reduces the cement clinkers
sizes between 10-15 µm.
 Cement Production

Two Process are used: DRY & WET Production. In wet production grinding and homogenization of
the raw mix is carried out in the form of slurry (30-40% water). Modern cement plants favors the
dry process, which is more energy efficient because water in the slurry must be evaporated before
clinkering.
09-02-2023 10
 Process Map for a Typical Cement Plant in India – Ordinary
Portland Cement (OPC)

Major raw materials: Limestone, Coal, Pet coke, Lignite, Clay

Other significant inputs: Electricity (from the grid), Alternative fuels, Gypsum,
Water, Plant and equipment
Important sub-processes: Limestone extraction, Raw meal preparation,
Clinkerization, Blending, Packing and dispatch,
Power generation
Products: Bulk cement, Cement bags, Clinker
 Cement Production

Virtual tour of cement plant

http://www.cement.org
Mindess & Young, 1981
 Cement Production
• Chemical Reactions in Rotary Kiln
Limestone CaO + CO2

Clay SiO2 + Al2O3 + Fe2O3

Gypsum CaSO4· 2H2O

• Main Compounds: Bogue’s Compounds • Abbreviation

3Cao. SiO2 Tri-Calcium Silicate C3S

Limestone + Clay 2Cao. SiO2 Di-Calcium Silicate C2S

3Cao. Al2O3 Di-Calcium Aluminate C3A

4CaO. Al2O3. Fe2O3 Tetra-Calcium Aluminoferrite C4AF

Proportion Significance
C3S Since due to impurity Al, Fe, S (gypsum) in ~55-60% Early Age Strength
production, these compounds are impure and
C2S ~15-20% Later Age Strength
hence known as alite (C3S) & belite (C2S)
C3A Aluminate ~5-10% Setting Time
C4AF Ferrite ~5-8% Color
CSH2 Gypsum (S = sulphate) ~2-6% C3A retardation
 Cement Composition of Cement

Chemical formula Notation Name Typical

weight %
CaO C Lime, calcium oxide 60-67
SiO2 S Silica, silicon dioxide 17-25
H2O H Water --
Al2O3 A Alumina, aluminum oxide 3-8
Fe2O3 F Iron or ferric oxide 1-6
MgO M Magnesia, magnesium oxide 1-4
K2O, Na2O K, N Alkalis, Potassium & sodium oxides 0.5-1.2
SO3 S Sulphur trioxide 2-3.5
CO2 C Carbon dioxide --

• This (MgO)is due to impurtity in limestone. This is not good for

concrete since leads to expansive reaction & breaking of concrete. Shall
< 5%
• From Clay, may lead to alkali silica reaction;
• Na2O + 0.658K2O should not exceed 0.60%
09-02-2023 M. Santhanam and G. Sivakumar 14
 Cement Production
• IS 8112 for OPC 43 grade requirement

• Insoluble residue: is a measure of adulteration of cement largely arising from impurities in

gypsum; determined by treating with HCl

• Loss on ignition: extent of carbonation and hydration of free lime and free magnesia due to
exposure of cement to atmosphere
 Cement Production
• How to perform the chemical composition of cement? X-Ray Fluorescence (XRF)

Pellets XRF Machine Output

• How to estimate the compounds proportion for a particular grade of cement? X-Ray Defraction
(XRD)/Rietveld Analysis
 Cement Production
• How to estimate the compounds proportion without having XRD machine?

• Bogue equations could be used:

%C3S = 4.071C – 7.600S – 6.718A – 1.430F – 2.85S

%C2S = 2.867S – 0.7544C3S

%C3A = 2.650A – 1.692F

%C4AF = 3.043F

C= CaO S = Sio2 A = Al2O3 F = Fe2O3 S = SO3

Home activity: The chemical analysis of a clinker was: O = {C, S, A, F, S } = {64.80, 21.08, 5.25, 2.71,
2.88} %. Using the above analysis, calculate the amounts of the four main clinker minerals (C3S, C2S,
C3A & C4AF)

Check it with the literature value in the previous slides…

 Cement Hydration
• Anhydrous (substance that contains no water) cement does not bind aggregates. It
requires water for achieving adhesive property. The chemical reaction that take
place between cement and water is referred as hydration of cement.

• Cement compounds + water = Hydrated products + heat

❑ Hydration Mechanisms: a) Through Solution b) Direct Contact/solid state/topochemical

a) Through Solution: In this, cement compounds (C2S,C3S

etc) dissolves in water to produce a supersaturated
solution followed by precipitation of hydrated products

b) Direct Attack: In this, reaction takes place directly at

the surface of anhydrous cement compounds without the
compounds going into the solution

Through solution mechanism is dominant in the early

stages of cement hydration. At later stage, when the ionic
mobility in the solution becomes restricted, the hydration
of residual cement particles may occur by direct attack
reactions
 Hydrated Products

Hydration of Aluminate to Ettringite (AFt): This reaction is immediate and leads to flash set of cement.
Unless this is lowered down by some method, its not possible to use cement. This is done by adding gypsum.
C3A + 3CSH2 + 26H = C6AS3H32, Δ H = 207 cal/g or -1672 J/g

• The tricalcium aluminate reacts with the gypsum in the presence of water to produce calcium aluminate
tri sulphate hydrate i.e. ettringite (AFt)
• Large amount of heat is generated due to this reaction
• The compound does not contribute to the strength of the cement glue
• Ettringite consists of long crystals that are only stable in a solution with gypsum

Hydration of Ettringite to Monosulphate (AFm):

• This happens in cement having C3A more than 5% only

• Since more gypsum cannot be added (5-6%; expansive reaction), after depletion of gypsum, the
aluminate concentration goes up due to renewed hydration of C3A and C4AF. At this stage, ettringite
becomes unstable and is gradually converted into mono-suplhate.
• Calcium monosulphate is not good for concrete as is an expansive reaction

C6AS3H32 + 2C3A + 4H → 3C4ASH12

Overall reaction:
C3A + CSH2 + 10H → C4ASH12 (ΔH = -1144 J/g)
 Hydrated Products
Hydration of Ferrite:
• From hydration point of view, it is convenient to discuss the hydration reaction of C3A and C4AF together since both
results in formation of products similar in structure
• Depending on sulfate concentration: C4AF forms C6AFS3H32 (similar to ettringite but different chemical
composition) or C4AFSH18 (similar to calcium monosulphate)
• The reactivity of C4AF is slower than C3A
Then why to take risk and add Al & Fe in cement? They act as fluxing agent
Hydration of Calcium Silicates

Calcium silicates (C3S + C2S) + water → C-S-H + Ca(OH)2

provides strength • Does not contribute to strength

• Leads to durability issues in
sulphate environment
• However, being alkaline maintain
pH value around 13: good for
reinforced concrete (protective
layer)

09-02-2023 20
 Hydrated Products
Hydration of Calcium Silicates
2C3S + 6H → C3S2H3 + 3CH (ΔH = -500 J/g)
Moderate reaction rate, gives high strength and heat liberation

2C2S + 4H → C3S2H3 + CH (ΔH = -260 J/g)

Slow reaction rate, gives low initial but high later strength, and low heat liberation

C3S produces round 61% CSH & 39% CH C2S produces round 82% CSH & 18% CH

C3S requires 24% water for complete hydration & C2S requires only 21%

What do you think, which is better?

Obliviously cement rich in C2S will give higher ultimate strength with lesser heat and lower
quantity of CH (more durable)
However, we need higher strength at initial days. Fine particles of C3S in presence of gypsum
starts to hydrate within an hour of addition of water
What to do now???
Addition of SCM will reduce CH content and increases the CSH product along with higher initial
strength
09-02-2023 21
 Hydrated Products

Ettringite - 15 to 20%
Calcium silicate hydrates, CSH - 50 to 60%
Calcium hydroxide (lime) - 20 to 25%
Voids (capillary voids and entrapped and entrained air) - 5 to 6%

Development of Strength of pure Compounds

09-02-2023 22
 Morphology of Hydration Products

Scanning electron micrograph of 7-day old hardened cement paste (×3500).

Bottom left: cement particle coated with C-S-H surrounded by ettringite needles;
Upper left: platelets of monosulfoaluminate; Right: large crystal of calcium hydroxide
Young et al., 1998
 Microstructure of Hydrated Cement Paste

C-S-H

C-S-H

C-S-H: Agglomerations of C-S-H particles of 1-100 nm.

H: Hexagonal crystals of calcium hydroxide, monosulfoaluminate and calcium
aluminohydrate of about 1 μm.
C: Capillary pores and voids of 10 nm to 1 μm.
Mehta and Monteiro
 Cement Hydration
• Heat of Hydration Significance
• The heat evolved during hydration reaction (exothermic) is known as heat of hydration
• Sometimes Hindrance: Mass concrete (high heat more thermal shrinkage & cracking)
• Beneficial: Concreting in winters (T< 5°C; ambient temp is too low to kick start hydration
process)
• Beneficial: Indicative of cement reactivity

• Ascending Peak A: last for few minutes and indicates the

sulphate and aluminates are resolving in water

• Descending Peak A: Initial heat evolution ceases quickly

when the solubility of aluminates is depressed in the
presence of sulfates in the solution
• Peak B: Happens about 4-8 hrs. Formation of Ettringite.
Also includes some heat due to heat of solution of C3S and
heat of formation of CSH gel.
• Ascending Peak B: Cement loses its plasticity (initial set)

• Descending Peak B: Beginning of hardening (final set)

Heat Liberation
• 50% heat is evolved in first 3 days & 70% in 7 days
 Rate of Heat Evolution During Hydration

Stage I: Rapid evolution of heat, lasts about 15 minutes.

Stage II: Dormant period, lasts until initial set occurs in 2 to 4 hours
Stage III: Rapid reaction of C3S during the acceleration period, with the peak being reached at
about 8-10 hours, much after final set at 4-8 hours and hardening has begun
Stage IV: Rate of reaction slows down until steady state is reached in 12-24 hours
Stage V: Steady state

09-02-2023 • What is the significance of above relation? 26

Mindess & Young
 Rate of Heat Evolution During Hydration

09-02-2023 FHWA HIF - 07 - 004

 Rate of Heat Evolution During Hydration

❑ Mixing

• In general, during hydration the reactions between

silicates and water produce the primary compounds
that make concrete strong and durable. But silicates
dissolve very slowly and do not have an immediate
effect.
• Aluminates and gypsum, on the other hand, dissolve
and react within minutes of being mixed with water,
with immediate effect. Together with water, the
dissolved aluminate begins developing new
compounds, generating significant heat. Unchecked,
these reactions would cause irreversible, flash set or
stiffening of the concrete.
• Fortunately, the fast-dissolving gypsum reacts with
the dissolved aluminate and water to create a gel-like
substance that coats the cement compounds. The
coating slows the aluminate reactions almost as soon
as they start, reducing the amount of heat generated
and the potential for flash set

09-02-2023 FHWA HIF -2807 - 004

 Hydration Stages

❑ Dormancy

• Aluminate reactions are generally controlled for about

two to four hours by sulphates: the dormant period.
• During this time, the concrete is plastic and does not
generate heat. The dormant stage gives the
construction crew time to transport, place, and finish
the concrete while it is workable.
• During dormancy, it looks as though nothing is
happening in the mixture. However, the cement
compounds are continuing to dissolve, and the water
is becoming saturated with dissolved calcium and OH
(hydroxyl) ions

09-02-2023
FHWA HIF - 29
07 - 004
 Hydration Stages

❑ Hardening

• When the water becomes supersaturated with

dissolved calcium ions, new compounds begin
forming, heat is generated, and the mixture begins
stiffening. This is the beginning of the hardening stage
• During the hardening stage, new compounds
(products of hydration) continue growing and heat
continues to be generated. Some of the compounds
are finger-like, fibrous growths; others are more
crystalline .
• These compounds interweave and mesh together
around the aggregates, causing the concrete to
become stiffer and eventually become a solid. At final
set, the concrete has become strong enough to walk
on. Still, the concrete cannot carry traffic.

09-02-2023 FHWA HIF -3007 - 004

 Hydration Stages

❑ Cooling

• Due to changes in temperature and moisture content, the

concrete shrinks. Friction between the shrinking
concrete and the base layer under the pavement causes
stress that will eventually cause the concrete to separate
or crack. To relieve the stress and prevent concrete from
cracking randomly, workers must saw joints. (Joints
simply control the crack locations.)
• Occurs two to four hours, to saw joints successfully
(Pavements). This period is called the sawing window.
The sawing window begins when the concrete can be
sawed without excessive raveling, and ends before the
concrete begins to crack randomly.
• Approximately four to six hours after initial set,
hydration slows and the amount of heat generated begins
to drop
• This slowdown is caused by the buildup of hydration
products, which have begun to interfere with contact
between the remaining water and cement in the concrete

09-02-2023 FHWA HIF -3107 - 004

 Hydration Stages

❑ Densification

• During the final stage of hydration, the reactions

continue slowly, generating little heat
• Continued growth and meshing of hydration products
results in a strong, solid mass . Long after the concrete is
strong enough to carry load, this process will continue—
as long as cement and water are present in the
concrete—increasing the concrete’s strength and
reducing its permeability.

09-02-2023 FHWA HIF -3207 - 004

 Hydration Stages

09-02-2023 FHWA HIF - 33

07 - 004
 Hydration Stages

❑ Upto when cement will continue to hydrate??

09-02-2023 FHWA HIF - 34

07 - 004
 Cement Hydration
❑ Upto when cement will continue to hydrate??

• Generally cement hydration is a never-ending process

• It can be mapped through cumulative heat of hydration

Curing Age Cumulative Heat Strength of

of Hydration Ultimate strength
3 days ~40-50% ~40-50%
7 days ~60-70% ~60-70%
28 days ~80-90% ~80-90%

❖ As per IRC:58-2015,
• 90 days compressive strength = 20% higher than 28 days
• 90 days flexural strength = 10% higher than 28 days strength
 Cement Hydration
Apart from chemical/compound composition, which other factor will
affect the reactivity of cement?
❑ Fineness of Cement

Low surface Area High surface Area

• Fineness of cement has a great effect on the rate of hydration

• High fineness, more surface area to hydrate
• Beneficial for early development of strength, ultimate strength will be mostly similar

❑ What will be the drawbacks???

 Cement Hydration
❑Fineness of Cement
❑ Drawbacks
• Higher initial heat of hydration
• More shrinkage and thus more chances of cracks
• Ultimate strength is mostly same, cost of grinding is considerable high
• Finer cement has more chances to deteriorate on exposure to atmosphere
(air setting if humidity present)
• More gypsum is required to retard the C3A reaction (fine cement more surface
area of C3A)
• Finer cement leads to stronger reaction with alkali reactive aggregate
❑ What should we do, more surface fineness or less fineness?
We need more initial strength for opening to traffic. We can address other by
proper curing and others….
Finely grounded C3S cements are mostly used for high early strength concretes
 Cement Hydration
❑Fineness of Cement

• Particles larger than 45 µm are slow to hydrate

• Particles size more than 75 µm may never hydrate completely

• Minimum specific surface area = 225 m2/kg

 Structure of Hydrated Cement
❑ Interfacial Transition Zone (ITZ)
• Concrete is generally considered as two-phase material: paste & aggregate
• Aggregate phase has little impact on overall strength
• Transition zone can be considered as third phase due to difference in properties

• It is the weakest link in concrete matrix due to:

a) Poor quality: due to internal bleeding at
aggregate surface (large piece, elongated, flaky
particles; wall effect), the W/C at ITZ is higher
by about 0.1 and cement content is lesser by
about 100 kg/m3
b) Size and concentration of Calcium hydroxide and
ettringite are also larger in the ITZ
c) Due to shrinkage /temperature variation, micro
cracks develops even before the structure is
loaded
 Structure of Hydrated Cement
❑ Gel pores & capillary pores
• Porosity keeps on decreasing with
hydration of compounds
• The volume of hydrated products is
approximately twice that of anhydrous
cement grains

Lets understand with a simple example:

1 hour: paste contains anhydrous cement, hydrated
products and water
Further lapse: quantity of products increases, and others
decreases. At this stage, some of the water is used for
hydration, some remains within gel pores and remaining in
the paste
1 month: 85-90% hydrated products, 10-15% unhydrated
cement. At this stage, some of the water (after hydration),
occupies gel-pores and remaining water causes capillary
cavities
1 year: capillary porosity further decreases (depending
upon temp/humidity)
 Water Required for Complete Hydration
Water within Cement Paste

• Bound water: This is chemically bound to the hydration product, and can only be removed
on ignition. Also called ‘non evaporable’ water. Water required for hydration
• Interlayer water: Water held in between layers of C S H. The drying of this water leads to a
lot of shrinkage due to the collapse of the C S H structure.
• Adsorbed water: Water adsorbed on the surface of hydration products, primarily C S H.
Water can be physically adsorbed in many layers, but the drying of farther surfaces can
occur at about 30 % relative humidity. Drying of this water is responsible for a lot of
shrinkage.
• Capillary water: Present in voids larger than 50 Å. Further classified into: (a) free water,
the removal of which does not cause any shrinkage strains, and (b) water held by capillary
tension in small pores, which causes shrinkage strains on drying.

Absorbed water and interlayer water = Gel Water

= 15% water is required to fill gelpores, else shrinkage
Bound water = 23% water is required for completed hydration
total water required = 38% by weight of cement i.e. W/C (min) = 0.38
Some Important Relationship
 Some Rereferred Codes
• IS: 269 for OPC: (classified as 33, 43 and 53 grade; the grade implies the strength
achieved by the cement mortar at 28 days)
• IS:1489 Part 1 for PPC
• IS:455 for Slag Cement
• IS:16415 for Composite Cements
• IS:12600: Portland Cement, Low Heat (Low C3A and C3S contents)
• IS:8041-1978: Rapid Hardening Portland Cement
• ASTM C150
• AASHTO M 85

▪ Sulphate-resisting cement: Low C3A content

▪ White cement: Very low iron oxide content (clay without impurities is used in the manufacture;
contamination during grinding has to be avoided; higher fineness increases brightness of the colour)
 Basic tests for cements

How to check the fineness of cement at field?

❖ Determination of fineness by dry sieving

• Weight 100 g of cement in the 90µm sieve

• Break down the air-set lumps with finger
• Keep the sieve in sieve shaker for 2 mins or sieve
manually for ~15 minutes
90 µ mesh sieve

• Weight the mass of particles collected in pan IS 4031 (Part 1) : 1996

Reaffirmed in 2005

Recommenced value: 90% particles by weight particles should be <90µm

09-02-2023 44
 Basic tests for cements
❖ Determination of finesses by Blaine air permeability test (1/2)
Specific Surface Area in m2/kg

Principle: Flow of air has a relation with the specific surface area of cement

• Calculate the volume of the compacted bed of cement (V)

V=(WA -WB)/ρ
where,
WA = mass of the mercury required to fill the permeability cell
WB = mass of the mercury to fill the portion of the cell not occupied by he bed of cement formed by 2.8 gm of
standard cement sample.
ρ = Density of mercury at the temperature of test
• Determine the mass of sample W required to produce a bed having porosity of (e =
0.5) as follows
W = SG x V x (1 - e)
• Evacuate the air until the fluid moves above the upper line without pulling if
over the top of the side outlet close the valve and note the time Ts taken by manometer
liquid to fall from 2nd mark (from top) to the 3rd mark on the manometer when the
air allowed to permeate though the compacted bed of standard cement sample.
IS 4031 (Part 11) : 1998
09-02-2023 45
 Basic tests for cements

❖ Determination of finesses by Blaine air permeability test (2/2)

• Weigh an amount of cement sample equal to that determined in previous step and
perform calibration
• Place the perforated disc in the permeability cell, and then add a filter paper, followed
by the sample and another filter paper
• Evacuate the air until the fluid moves above the upper line without pulling it over the
top of side tube. Close the valve of manometer and note the time T it takes for the fluid
to drop from the 2nd mark to the 3rd mark on the manometer when the air is allowed
to permeate through the compacted bed of cement
• Calculate the specific surface S in sq. cm/gm of the tested cement by using the following
formula with the temperature at the calibration and at the time of test are within ±3%
of each other.
S = (Ss x √T) / √Ts
where,
Ss = Specific surface of standard cement used in calibration;
Ts= Measured time (seconds) required for the fluid to fall the middle interval for standard
sample;
T = Measured time (seconds) required for the fluid to drop over the middle interval.

Recommenced value: 225 m2/kg

IS 4031 (Part 11) : 1998
09-02-2023 46
 Basic tests for cements

❖ Determination of Specific Gravity of cement

• Fill the flask with Kerosene

• Keep the flask in the water bath at a constant
temperature to avoid flask temperature variations.
• Note the final reading on the flask.
• Fill the flask with a known weight of cement
• Put the flask in the water bath again
• Take the final reading and calculate specific gravity
using this formula Le-Chatelier flask
Specific gravity = mass of cement (g)/ Displaced
volume

Recommenced value: 3.15

IS 4031 (Part 11) : 1998
09-02-2023 47
 Basic tests for cements
❖ Determination of soundness of cement

• Place the mould on a glass sheet and fill it with cement paste
having standard consistency with 0.78 times the water
• Cover the mould with another piece of glass sheet and
Le-Chatelier apparatus
immediately submerge in water at 27 ± 2 ºC for 24 hours
• Measure the distance separating the indicator points. (L1)
• Submerge the mould again in boiling water for 3 hours
• Remove the mould from the water, allow it to cool and
measure the distance between the indicator points (L2)

Recommenced value: L1-L2 < 10 mm

IS 4031 (Part 3) : 1988
Reaffirmed in 2005
09-02-2023 48
 Basic tests for cements
❖ Determination of consistency and setting time
• 500 grams of cement is taken on a glass plate and 25 % by weight (of cement)
of water is added
• The Vicat mould is filled with this paste by keeping the mould over a
non- porous plate and the top is levelled and placed under the Vicat
plunger (10 mm diameter) VICAT apparatus
• The settlement of the plunger is read directly from the graduated scale. If it is between 5 and
7 mm from the bottom, then the water added is correct. Otherwise, test is to be repeated as
above by preparing pastes with varying percentages of water, until the amount of water
necessary to produce the required penetration of 5 to 7 mm
• 500 grams of cement is taken and to it 85% (by weight) of water required for normal
consistency, as determined earlier is added
• Initial setting time is defined as the period of time elapsing between the time when water is
added to the cement and the time at which the 1 mm square Vicat needle fails to pierce the
paste by about 5 ±0.5 mm from the bottom of the mould
• The final setting time is the time interval between the time when water is added to the
cement and the time at which the annular attachment of the particular needle fails to make
an impression on the surface of the test block of cement paste
Recommenced value: IS 4031 (Part 4) : 1988
Reaffirmed in 2005
Initial setting time - 30 mins
IS 4031 (Part 4) : 1988
Final setting time - 600 mins Reaffirmed in 2005
09-02-2023 49
 Isothermal calorimetry

I-Cal 4000 HPC Isothermal Calorimeter from

Calmetrix can be used to monitor 4 samples (upto
125 ml) simultaneously. The equipment facilitates
the testing of cement past, mortar and concrete.

The calorimeter is used to measure the heat of

hydration and the applications can be extended to
compatibility of admixtures, sulfate optimization, the
hydration kinetics and their sensitivity to
temperature.

An example of the heat rate from the cement

hydration is shown here.

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 Basic tests for cements
❖ Determination of Compressive Strength of cement
• Weigh 300 gm of cement and prepare the corresponding weights of standard sand
and water
• Follow the mix procedure as follows:
Place all the mixing water in the bowl
Add the cement to the water, mix at the low speed (140±5 rpm) for 30 seconds
Add the entire quantity of sand slowly over a (30 s) period , while mixing at slow speed
• Stop the mixer and let the mortar stand for 1.5 min and scrape down the mortar
collected on the side of the bowl
• Again run the mixer for 1 min at medium speed
• Keep the cubes in the curing under water (preferably in mist room), take the
specimen and clean it with cloth and test for compressive strength.

IS 4031 (Part 3) : 1988

Reaffirmed in 2005
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