Cement

Manufacture, Properties, Testing Methods and

Types

S P Singh
PhD (Roorkee); Post Doc (Scotland)

Professor of Civil Engineering

Dr B R Ambedkar National Institute of Technology
Jalandhar – 144 011
e [email protected]
m 98140 88475
www.nitj.ac.in/ce/spsingh
Portland Cement
• Cement is a well known building material and has occupied an
indispensable place in construction.
• There are variety of Cements available in the market and each
type is used under certain conditions due to its properties.
• The cement commonly used is Portland Cement and the fine and
coarse aggregates used are those that are obtained from nearby
sand, gravel or rock deposits.
• The ingredients of Concrete can be classified into two groups –
active and inactive. Active – Cement and Water. Inactive – Fine
and Coarse Aggregates. Inactive group is also called sometimes
– Inert Matrix.
Portland Cement
Portland Cement is a pulverized material that develops binding
forces due to a reaction with water.
 Hydraulic Cement → Stable under water
 Non-hydraulic Cement → Products of hydration are not resistant
to water (i.e. limestone)
Hydraulic Cements
Cements that harden by reaction with water and form a water-
resistant product.

Portland cement is a Hydraulic Cement capable of setting,

Portland cement is a Hydraulic Cement capable of setting, hardening and
hardening and
remains stable remains
under water. Itstable underofwater.
is composed calciumItsilicates
is composed of
and some
calcium
amount of silicates
gypsum. and some amount of gypsum.
Portland Cement
• Portland Cement is an extremely ground material having adhesive
and cohesive properties, which provide binding medium for the discrete
ingredient's.
• It is obtained by burning together, in a definite proportion, a mixture of
naturally occurring argillaceous (containing alumina) and calcareous
(containing calcium carbonate or lime) materials at a high temperature of
about 14500 C.
• The product obtained is called clinker, is cooled and ground to the
required fineness to produce the material known as Cement.
• Its inventor, Joseph Aspdin, called it Portland Cement because when it
hardens it resembles stone found in Portland in England.
• During grinding of clinker, gypsum (CaSo4) is added to adjust the setting
time.
Portland Cement
 Portland Cement →
Gypsum+Portland Cement Clinker
(pulverizing)

 Portland Cement Clinker →

Calcareous & Clayey Materials
(burning)

 Paste → P.C. + Water

Pulverizing:
 Mortar → P.C. + Water + Sand
To reduce (a substance) to
 Concrete → P.C. + Water + Sand + fine particles, as by
Gravel crushing or grinding.
Raw Materials for Portland Cement
1) Calcareous Rocks (CaCO3 > 75%)
 Limestone
 Marl
 Chalk
 Marine shell deposits
2) Argillocalcareous Rocks (40%<CaCO3<75%)
 Cement rock
 Clayey limestone
 Clayey marl
 Clayey chalk
 Raw Materials for Portland Cement
3) Argillaceous Rocks (CaCO3 < 40%)
 Clays
 Shales
 Slates

 Portland Cement is made by mixing

substances containing CaCO3 with
Clinker
substances containing SiO2, Al2O3,
Fe2O3 and heating them to a Clinker
which is subsequently ground to
powder and mixed with 2-6% of
gypsum.
Gypsum
Portland Cement
Mixing
materials
Raw
materials Clinker Portland Cement

 Portland cement is formed by grinding together materials such as clay

Gypsum and limestone and is heated to about 1450℃. At 650℃ the limestone
separates into CO2 and CaO. When the silica reaches the point of
fusion, the atoms are able to move about and the CaO combines with
SiO2 and a small amount of Al2O3 and Fe2O3, forming Portland
Cement Clinker.
 The clinker is then ground to a fine powder, and a small amount of
gypsum is added.
 Production and Composition
of Portland Cement

Limestone

Blending 1450℃
Grinding
Clay Raw material Clinker

Cement
Iron ore Gypsum
powder
Mixing
materials

Process to Produce Portland Cement

Production of Portland Cement
• There are two processes known as ‘wet’ and ‘dry’ depending upon whether the
mixing and grinding is done in wet or dry conditions.
• With a little change, there can be semi-dry process where the raw materials are
ground dry and then mixed with 10-15% water and further burnt to clinkering
temperature.
• For many years, the wet process remained popular because of the possibility of
more accurate control in the mixing of raw materials. The technique of mixing of
raw materials in powder form was not available then.
• Later, the dry process gained momentum with the modern development of
technique of dry mixing of powdered materials using compressed air. The dry
process requires much less fuel as materials are already in a dry state, whereas, in
the wet process the slurry contains 30-50% water. Thus to dry the slurry, more fuel
consumption is there.
Production Steps
1) Raw materials are crushed, screemed & stockpiled.
2) Raw materials are mixed with definite proportions to obtain “raw
mix”. They are mixed either dry (dry mixing) or by water (wet
mixing).
3) Prepared raw mix is fed into the rotary kiln.
4) As the materials pass through the kiln their temperature is rased
upto 1300-1600 °C. The process of heating is named as “burning”.
The output is known as “clinker” which is 0.15-5 cm in diameter.
5) Clinker is cooled & stored.
6) Clinker is ground with gypsum (3-6%) to adjust setting time.
7) Packing & marketting.
Portland Cement – Oxide Composition
• When lime stone and clay are the two basic components, the proportions will be
4 parts lime stone to one part of clay. Depending upon the wide variety of raw
materials used in the manufacture of Cement, the oxide composition of Ordinary
Portland Cement (OPC) may be as follows:

• These oxides interact

with each other to form
more complex
products during fusion.
The difference in the
various types of OPCs
arise due to the
variation of relative
proportions of these
compounds.
Mineral Compounds and Properties

 Main Mineral Compounds of Portland

Cement Clinker include:
 Tricalcium silicate
 Dicalcium silicate
 Tricalcium aluminate
 Tetracalcium aluminoferrite
 Properties of the compounds are shown
in the next slide.
Mineral Compounds of Portland Cement
Chemical
Compounds Abbreviation
structural formula

Tricalcium silicate 3CaO·SiO2 C3S

Dicalcium silicate 2CaO·SiO2 C2S

Tricalcium
3CaO·Al2O3 C3A
aluminate

Tetracalcium
4CaO·Al2O3·Fe2O3 C4AF
aluminoferrite
Mineral Compounds and Properties
• As mentioned earlier, the oxides present in the raw materials when subjected
to high clinkering temperature combine with each other to form complex
compounds.
• The identification of the these compounds is largely based upon the research
work of ‘R H Bouge’ and some times called Bouge’s Compounds.
Properties of Mineral Compounds
Tricalcium Dicalcium Tricalcium Tetracalcium
Mineral type
silicate silicate aluminate aluminoferrite
Abbreviation C3S C2S C3A C4AF

Content (%) 37-60 15-37 7-15 10-18

Hydration
fast slow fastest fast
speed
Hydration
much little most more
heat
early low
Strength high low low
later high
Anti-
good fine poor excellent
corrosion
Shrinkage middle better big small
Hydration of Cement
• Anhydorus cement does not bind fine and coarse
aggregates. It acquires adhesive property only
when mixed with water.
• The Chemical reactions which take place between
cement and water are referred as hydration of
cement.
• The reaction of cement with water is exothermic
and liberates considerable amount of heat.
Hydration Mechanism
When mixed with water,
Portland cement hydrates
and forms heat.
3CaO·SiO2+H2O CaO·2SiO2·3H2O+Ca(OH)2

Tricalcium silicate hydrates rapidly and gives

earlier strength and earlier heat of hydration.
Tricalcium silicate is formed in a kiln when the charge
contains an abundance of lime, and hence the greater
amount of CaO in the reaction.
Hydration Mechanism

2CaO·SiO2+H2O 3CaO·2SiO2·3H2O+Ca(OH)2

Dicalcium silicate hydrates slowly and is

responsible for strength increase in concrete at later
ages. The heat of hydration is liberated slowly.
More dicalcium silicate is formed when the raw
materials contain less lime.
Hydration Mechanism
Tricalcium aluminate hydrates rapidly and
liberates a large amount of heat.
If this reaction were not controlled,
concrete would set so rapidly (flash set) that
it could not be used in construction.

3CaO·Al2O3+H2O 3CaO·Al2O3·6H2O
Hydration Mechanism

4CaO·Al2O3·Fe2O3+H2O
3CaO·Al2O3·6H2O+CaO·Fe2O3·H2O
The addition of iron or iron ore to the raw materials
lowers the percentage of tricalcium aluminate. The iron
reacts with the tricalcium aluminate, forming the tetra
calcium aluminoferrite.
This compound does not add significantly to the
properties of concrete, but does cause the charge in the
cement kiln to liquefy at lower temperature (lowers the
point of fusion), thus reducing the energy required in
cement manufacture.
To avoid flash set

 A small amount of gypsum (CaSO4·2H2O)

intergrounding with the cement clinker
retards the hydration reaction of
tricalcium aluminate.
 Mechanism of Modifying Setting
Time by Gypsum
 The protecting layer is formed by wrapping up
the clinker by Calcium sulfoaluminate hydrate
needle crystal, hinders the entry of water, slows
down hydration and stops flash setting. Thus
the gypsum can modify the setting time.

3CaO·Al2O3·6H2O+ H2O+CaSO4·2H2O
3CaO·Al2O3·3CaSO4·31H2O
 Factors Influencing Setting and
Hardening of Portland Cement
Factors such as: fineness and type of cement, blend of gypsum,
age, temperature and humidity which influence setting and hardening of
Portland cement.

Fineness

Age Types

Factors
Blend of
Temperature
Gypsum
Humidity
Factors influencing Setting and Hardening of Portland Cement
 Hydration of Cement
• Anhydrous cement does not bind fine and coarse aggregates.

• It acquires adhesive property only when mixed with water.

•The chemical reaction that takes place between cement and water is
called hydration of cement.

• The chemistry of concrete is essentially the chemistry of reactions

between cement and water.

• Le Chatlier was the first to observe that the products of hydration of

cement are chemically the same as the products of hydration of the
individual compounds under similar conditions.

• The two calcium silicates are the main compounds in cement and the
physical behaviour of cement during hydration is similar to that of these
two compounds alone.
 Hydration of Cement
•The products of hydration of cement have a very low solubility in water as
shown by the stability of hydrated cement paste in contact with water.

• The hydrated cement bonds firmly to the un-reacted cement, but the
exact way in which this happens is not known.

• The rate of hydration decreases continuously and even after a long time,
there remains an appreciable amount of unhydrated cement.

• It is believed that the product consisting of CaO.SiO2.H2O and Ca(OH)2

are formed during the hydration of silicates. Ca(OH)2 is an unimportant
product and CaO.SiO2.H2O is the significant product. This product is
called tobermorite gel. But commonly the product of hydration is called
C-S-H gel. The gel consists of crystals and is porous in nature. Its porosity
is to the extent of 28%.
 Heat of Hydration
• The reaction of cement with water is exothermic
and liberates a considerable amount of heat – heat
of hydration.

• This can be demonstrated if a freshly mixed mass

of cement with water is put in flask and the
temperature is measured at regular intervals.

• The study and control of heat of hydration is very

important particularly in the construction of dams
and other mass concrete structures.

• Refer to Fig. 1.2 – On mixing cement with water, a

rapid heat evolution, lasting for few minutes
occurs.

• This is due to reaction of solution of aluminates

and sulphates. This heat evolution ceases quickly
due to the suppression of aluminates by gypsum.

• The next peak formation is due to ettringite and

due the reaction of C3S.

• The hydration product of C3A is Calcium

Aluminate Trisulphate – ettringite.
 Basic Properties of Cement Compounds
• Different compounds hydrate at different rates and
liberate different quantities of heat.

• Since retarders are added to control the flash

setting of C3A, the early heat of hydration is mainly
attributed to C3S.

• The two silicates, namely, C3S and C2S, which

together constitute about 70 to 80% of the cement,
control the most of the strength giving properties.

• Upon hydration, both C3S and C2S form the same

product called calcium silicate hydrate i.e. C3S2H3
and calcium hydroxide – Ca(OH)2.

• C3S readily reacts with water and produces more

heat of hydration and early strength. A cement with
more C3S content, is better suited for cold weather
concreting.

• C2S hydrates rather slowly and is responsible for the later strength of concrete. It produces less heat of hydration.
C3S and C2S need approximately 24 and 21% of water by weight respectively, for chemical reaction but C 3S liberates
nearly three times as much calcium hydroxide on hydration as C2S.

• C2S provides more resistance to chemical attack.

 Basic Properties of Cement Compounds
• The amount of C3A present in most cements is
comparatively small but its behaviour and structural
relationship with other phases of cement make it of
interest.

• The reaction of C3A with water is very violent and leads to

immediate stiffening of the paste known as flash set. To
prevent this, gypsum is added to the cement during
manufacturing stage.

• The hydrated aluminates do not contribute any thing to

the strength. On the other hand, their presence is harmful
to the durability of concrete, particularly where concrete is
likely to be attacked by sulphates.

• Hydration of C4AF is believed to form CaO-Fe2O3-H2O. A

hydrated calcium ferrite of the form C3FH6 is comparatively
more stable.

• In the presence of gypsum, depending upon the concentrations of aluminate and sulphates in the solution, the
precipitating crystalline product is calcium aluminate trisulphate hydrate (C6S3H32) – which is called ettringite.

• Gypsum not only reacts with C3A, with C4AF it forms calcium sulphoferrite as well as calcium sulphoaluminate,
and its presence may accelerate hydration of silicates.
 Transition Zone, Hydrated Cement
• It is important to study the structure of hydrated cement
paste.

• Concrete is considered a two phase material – paste

phase and aggregate phase.

• Paste phase – more important as it influences the various

properties of concrete as compared to aggregate phase.

• Strength, permeability, durability, shrinkage, elastic

properties and creep are more influenced by the properties
of paste phase rather than aggregate phase.

• At macro level – the aggregate particles are dispersed in

cement paste matrix. However, at micro level – the area in
the vicinity of large aggregate particles is called the
Transition Zone. This area represents the interfacial region
between the particles of coarse aggregates and hardened
cement paste.
• The Transition Zone is generally a plane of weakness and has greater influence on the mechanical properties of
concrete.

• Though Transition Zone is composed of same cement paste, the quality of paste there is poor as due to
bleeding, water accumulate below elongated and flaky aggregates. This reduces the bond between paste and
aggregates.
Specifications and Testing of Ordinary
Portland Cement
Specifications
• Ordinary Portland Cement 33 Grade: IS 269 1989 (Reaffirmed 1998)

• Ordinary Portland Cement 43 Grade: IS 8112 1989

• Ordinary Portland Cement 53 Grade: IS 12269 1987 (Reaffirmed 1999)

• OPC: IS 269 2015 for 33, 43 and 53 Grade (All in one)

Testing
• IS 4031-1: Fineness by dry sieving
• IS 5513 –1996: Vicat
• IS 4031-3: Soundness Apparatus
• IS 4031-4: Standard Consistency • IS – 650: Standard
• IS 4031-5: Initial Setting Time Sand
• IS 4031-6: Compressive Strength of Cement
Types of Cement
Types of Cement
Types of Cements
Types of Cements
Types of Cements
Types of Cement –
Ordinary Portland Cement
• Commonly used Portland Cement in India is 33 grade (IS 269 – 1989), 43 grade (IS 8112 – 1989) and 53
grade (IS 12269 – 1987) having 28 days average compressive strength of 33 MPa, 43 MPa and 53 MPa
respectively.

• All the three grade of cements are produced from the same materials and the higher strength is
achieved by increasing the content of C3S and by fine grinding of the clinker.

• The fineness of 53 Grade cement determined by Blaine’s Air Permeability test is of the order of
350000 mm2/gm, the initial and final setting time being the same for all the grades.

• It has been seen that the greater fineness of 43 and 53 grade cements increase workability of
concrete due to reduction of friction between aggregates.

• In these days, the higher grade cements have become more popular and 33 grade cement is more or
less is obsolete.

• The manufacture of OPC is decreasing day by day with the increase in the use of blended cements on
account of lower energy consumption, environmental pollution, economic and other aspects.

• In western countries, the use of OPC has come down to about 40% of the total cement production.

• In years to come, the production of OPC is going to further reduce, but it will remain an important
type for general construction.
Types of Cement –
Rapid Hardening Cement (IS 8041 – 1990)
• This cement is similar to OPC but with higher C3S content (lower C2S content) and finer grinding.
Higher fineness of cement provides greater surface area for action with water.

• It gains strength more quickly than OPC though the final strength is only slightly higher.

• Rapid hardening cement which develops higher rate of strength – not to be confused with quick
setting cement – which sets quickly.

• Rapid hardening cement develops at the age of 3 days approximately same strength as by OPC at the
age of 7 days. It generate much higher heat of hydration during early period. Therefore, rapid
hardening cement should not be used in mass concrete.

Applications
• In pre-fabricated concrete construction.

• Where form work is required to be removed early for re-use elsewhere.

• Road repair work.

• In cold weather concrete the rapid rate of development of strength reduce the vulnerability of
concrete to frost damage.
Types of Cement –
Sulphate Resisting Cement (IS 12330 – 1988)
• OPC is susceptible to the attack of sulphates, in particular to the action of magnesium sulphate.

• Sulphates react with free calcium hydroxide in set cement to form calcium sulphate and with calcium
aluminate, to form calcium sulphoaluminate – the volume of which is about more than 200% of the
volume of the original aluminates. Therefore, the expansion within cement results in cracks and
disruption.

• Solid sulphates do not attack the cement. However, sulphates in solution, permeate though the
hardened concrete and attack the calcium hydroxide and hydrated calcium aluminates.

• Portland cement with low C3A (< 5%) and C4AF contents is very effective against Sulphate attack.
Such a cement having high silicate content is called Sulphate Resisting Cement. IS Code limits the
total content of C4AF and C3A not more than 25%.

Applications
• Concrete to be used in marine conditions.

• Concrete to be used in foundations and basement, where soil is infested with sulphates.

• Concrete to be used in the construction of sewage treatment works.

• Concrete to be used for fabrication of pipes which are to buried sulphate bearing soils.
Types of Cement –
Low Heat Cement (IS 12600 – 1989)
• Formation of cracks in large body of concrete due to heat of hydration focused the attention to
produce this kind of cement which produces less heat or the same amount of heat at lower rate during
hydration process.

• Cement having this property was developed in the USA during 1930 for use in mass concrete
applications such as dams, where temperature rise by heat of hydration can be excessively large.

• Low heat cement is less reactive than OPC and is obtained by increasing the content of C2S and
reducing C3S and C3A. This results in slow development of strength and but the ultimate strength is
the same.

• In any case, to ensure sufficient development of strength, the specific surface of cement must not be
less than 320000 mm2/gm. The initial setting time is greater than OPC.

• As per Indian Standard, the heat of hydration of low het cement should be

7 Days – not more than 65 calories per gm

28 Days – not more than 75 calories per gm

Types of Cement –
Portland Pozzolana Cement (IS 1489 – 1991)
• Portland Pozzolana Cement is obtained by
intergrinding of OPC clinker with about 15 to 30%
of pozzolanic material.

• A pozzolanic material is silicious or aluminious

material which in itself does not possess
cementitious property, but which in finely divided
form in the presence of water reacts with calcium
hydroxide to form compounds possessing
cementitious properties.

• The pozzolanic materials generally use for the

manufacture of PPC are clay (IS 1489 Part 2 of
1991), fly ash (IS 1489 Part 1 of 1991).

• The pozzolanic action is

Calcium Hydroxide + Fly Ash + Water =

C-S-H gel
Testing of Ordinary Portland Cement
Fineness by Sieving through 90 micron Sieve

Apparatus
Test Sieve
It comprises a firm, durable, non-corrodible, cylindrical frame
of 150 mm to 200 mm nominal
diameter and 40 mm to 100 mm depth, fitted with 90
pm mesh sieve cloth of woven stainless steel, or other
abrasion-resisting and non-corrodible metal wire.
The sieve cloth shall comply with the requirements
of IS 460 ( Part 1) : 1985 and IS 460 ( Part 3 ) : 1985
and shall be free of visible irregularities in mesh size
when inspected optically by the methods of IS 460
( Part 3 ) : 1985. A tray fitting beneath the sieve frame
and a lid fitting above it shall be provided to avoid
loss of material during sieving.
Testing of Ordinary Portland Cement
Fineness by Sieving through 90 micron Sieve
Procedure to obtain 5. Then calculate the residue of the cement
Determination of the Cement Residue R as the mean of R, and R, as a percentage,
Agitate the sample of cement to be tested by shaking expressed to the nearest 0.1 percent.
for 2 min in a stoppered jar to disperse agglomerates. When the results differ by more than 1 percent
Wait 2 min. Stir the resulting powder gently using a absolute, carry out a third sieving and calculate the
clean dry rod in order to distribute the fines mean of the three values. The sieving process is
throughout carried out manually by a skilled
the cement. and experienced operator.
Fit the tray under the sieve, weigh approximately 10 g
of cement to the nearest 0.01 g and place it on the
sieve, being careful to avoid loss. Disperse any
agglomerates. Fit the lid over the sieve. Agitate the
sieve by swirling, planetary and linear movement until
no more fine material passes through it. Remove and
weigh the residue. Express its mass as a percentage,
R,, of the quantity first placed in the sieve to the
nearest 0.1 percent. Gently brush all the fine material
off the base of the sieve into the tray.
Repeat the whole procedure using a fresh 10 g
sample
Testing of Ordinary Portland Cement
Standard Consistency
Testing of Ordinary Portland Cement
Standard Consistency
Testing of Ordinary Portland Cement
Standard Consistency
Testing of Ordinary Portland Cement
Initial Setting Time
Testing of Ordinary Portland Cement
Final Setting Time Needle
Testing of Ordinary Portland Cement
Final Setting Time
Testing of Ordinary Portland Cement
Compressive Strength
Testing of Ordinary Portland Cement
Soundness
Testing of Ordinary Portland Cement
Soundness

• It is very important that the cement after setting shall not undergo any
appreciable change of volume. This will cause serious difficulties for the
durability of structures when such cements are used.
• The unsoundness of cement is due to the presence of excess lime, excess
of magnesia or excessive proportions of sulphates.
• This is also due to inadequate burning of or insufficiency in grinding or
thorough mixing of raw materials.
• Unsoundness of cement does not come to the surface for a considerable
period of time and therefore, accelerated tests are required to be
conducted to detect unsoundness of cement.
Testing of Ordinary Portland Cement
Soundness

Le-Chatelier Water Bath Le-Chatelier Mould

Testing of Ordinary Portland Cement
Soundness
Testing of Ordinary Portland Cement
Soundness
Testing of Ordinary Portland Cement
Compressive Strength
Concrete – let 's make the best of it.

57