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Tests on Cement

Chemical Evaluation –
• Determine the composition of various oxides
Physical Evaluation –
• Specific Gravity - ratio of the weight of an equal volume of water
• Fineness – measure of size of cement particles
• Standard Consistency – Determination of quantity of water to be mixed
to produce standard paste
• Initial and Final setting time - Measure the rate of solidification of
standard cement paste
• Soundness – Change in volume upon setting
• Strength – Failure stress of mortar specimens
• Heat of Hydration
• Transverse strength

Dr. Sahil Bansal, IIT Delhi 1


Physical Requirements for Ordinary Portland
Cement (IS:269-2015) OPC 53

2
Specific Gravity – IS:4031 (Part 11)
Relevance:
• Specific gravity is determined by measuring the weight of a cement sample and its
volume by measuring the liquid displaced by the cement sample.
• The specific gravity of OPC is generally around 3.15. if a given sample of cement
exhibits a value of specific gravity significantly different from 3.15, the quality of the
sample may be suspect.
• If clay, ground sand, fly ash and such impurities (or adulterants) had been added to
the cement the lower values of specific gravity will be obtained.
• Likewise, partly hydrated cement (which can occur due to prolonged storage under
moist environment) will also lead to lower values of specific gravity.

Dr. Sahil Bansal, IIT Delhi 3


Specific Gravity – IS:4031 (Part 11)
Precautions:
• The liquid which is to be used
should be such that it does not have
any chemical reaction/ physical
interaction with cement.
• The cement should not have any
agglomerated particle with internal
voids otherwise only average
apparent density will be measured.

Le-Chatelier Flask
Dr. Sahil Bansal, IIT Delhi 4
Specific Gravity – IS:4031 (Part 11)
1. Dry the flask carefully and fill with kerosene or naphtha to a point on the stem between
zero and 1 ml.
2. Record the level of the liquid in the flask as initial reading (V1) *.
3. Put a weighted quantity of cement (about 64 g) W into the flask so that level of
kerosene rises to about 22 ml mark, care being taken to avoid splashing and to see that
cement does not adhere to the sides of the above the liquid.
4. After putting all the cement to the flask, roll the flask gently in an inclined position to
expel air until no further air bubble rises to the surface of the liquid.
5. Note down the new liquid level as final reading (V2) *.
6. The density of cement is given by: W / ( V2 - V1).
✓ The flask shall be immersed in a constant temperature water bath, maintained at
about room temperature, for a sufficient interval of time before making either of the
readings.
✓ Two tests shall be carried out and the average shall be reported. If the difference
between the two values differs by more than 0.03, the test shall be repeated.
✓ Determined to an accuracy of 0.01 g/cm3.

Dr. Sahil Bansal, IIT Delhi 5


Fineness - IS:4031(Part 1, Part 2, Part 15)
Relevance:
■ Cement is obtained by grinding various raw materials after calcination.
■ Fineness is a measure of the size of the cement particles.
■ The fineness of cement has an important role on the rate of hydration and
hence on the rate of gain of strength and on the rate of evolution of heat.
■ Finer cement offers a greater surface area for hydration and hence the faster
development of strength although the ultimate strength is not affected.
■ Fineness also provides more cohesiveness to concrete and avoid separation of
water at the top of concrete (called bleeding).
■ However, disadvantages of high fineness are: cost of grinding is high, finer
particles deteriorates on exposure to the atmosphere during bad storage, high
heat of hydration, increase in drying shrinkage and hence cracking of the
concrete, and increase in requirement of gypsum because C3A is available for
early hydration.

Dr. Sahil Bansal, IIT Delhi 6


Fineness by Dry Sieving - IS:4031 (Part 1)
1. Agitate the sample of cement to be tested by shaking for 2 minutes in a stoppered jar to
disperse lumps. Stir the resulting powder gently using a clean dry rod in order to distribute
the fines throughout the cement.

2. Weigh approximately 10 g of cement to the nearest 0.01 g and place it on the sieve (W). Fit
the lid over and pan under the sieve. Air set lumps in the cement sample must be crushed
using fingers and not by pressing with the sieve.

3. Shake the sieve by swirling, planetary and linear movement until no more fine material
passes through it. More or less continuous rotation of the sieve shall be carried out
throughout sieving.

4. Remove and weigh the residue (R). Express its mass as a percentage of the quantity first
placed in the sieve.

Obtain R1 and R2 using two samples to nearest


0.1%. If the results differ by more than 1
percent absolute, carry out a third sieving and
report the mean of the three values else report
the mean of the two values.

Dr. Sahil Bansal, IIT Delhi 7


Fineness - IS:4031(Part 1, Part 2, Part 15)
Fineness is a measure of the size of the cement particles

■ Part 1: Fineness by dry sieving

■ Part 2: Fineness by Blain Air Permeability Apparatus

■ Part 15: Fineness by wet sieving

Air Permeability Apparatus


(Blaine type)

Dr. Sahil Bansal, IIT Delhi 8


Fineness by Blain Air Permeability Apparatus
Working Principle:
■ In this experiment measure of fineness of
cement is obtained by determination of specific
surface using air-permeability apparatus.
■ The specific surface is defined as the total
surface area of all the particles in sq. cm per one
gram of cement.
■ The principle of this method is in observing the
time taken to draw a fixed quantity of air
through a prepared bed of cement of definite
dimensions and porosity.
■ Finer the cement, larger will be its specific
surface. Larger specific surface means the air
faces higher resistance to pass through the
cement bed on the account of larger frictional
forces, resulting in increased time taken.
Dr. Sahil Bansal, IIT Delhi 9
Fineness by Blain Air Permeability Apparatus
1. Determine the density of cement sample as described in IS:4031 (Part 11).

■ Determination of the Bed Volume:

1. Apply a very thin film of light mineral oil to the cell interior. Place the perforated
disc on the ledge in the cell. Place two new filter paper discs on the perforated disc
and ensure that each covered the base of the cell whilst lying flat by pressing with
a rod.

2. Fill the cell with mercury. Remove any air bubbles with a clear dry rod. Ensure
that the cell is full by pressing a glass plate on the mercury surface until it is flush
with the cell top.

3. Empty the cell, weigh the mercury to the nearest 0.01 g, (m2), and record the
temperature.

4. Remove one filter paper disc. Form a compacted cement bed by the method
described in the next section and place on it a new filter paper disc. Refill the cell
with mercury, removing air bubbles and levelling the top as before. Remove the
mercury, weigh it to the nearest g, (m3), and check the temperature.

5. The bed volume is given by: V= (m2 - m3) / D where D is the density of mercury
at the test temperature taken from Table.

6. Repeat the procedure with fresh cement beds until two values of V are obtained
differing by less than 0.005 cm3. Record the mean of these two values as V.

Dr. Sahil Bansal, IIT Delhi 10


Fineness by Blain Air Permeability Apparatus
■ Formation of cement Bed
1. Agitate the sample of cement to be tested by shaking for 2 min in a stoppered jar to disperse
agglomerates. Wait for 2 min. Stir the resulting powder gently using a clean dry rod in order
to distribute the fines throughout the cement.
2. To give a cement bed of porosity e = 0.500 weigh a quantity of cement, m1, calculated from:
m1 = 0.500 pV (g)
p is the density of the cement (g/cm3)
V is the volume of the cement bed (cm3)
1. Place the perforated disc on the ledge at the bottom of the cell and place on it a new filter
paper disc.
2. Place the weighed quantity of cement, m1, in the cell taking care to avoid loss.
3. Tap the cell to level the cement. Place a second new filter paper disc on the levelled cement.
4. Insert the plunger to make contact with the filter paper disc. Press the plunger gently but
firmly until the lower face of the cap is in contact with the cell. Slowly withdraw the plunger
about 5 mm, rotate it through 90” and gently but firmly press the bed once again until the
plunger cap is in contact with the cell.
5. The bed is now compacted and ready for the permeability test. Slowly withdraw the plunger.

Dr. Sahil Bansal, IIT Delhi 11


Fineness by Blain Air Permeability Apparatus
1. Manometer is filled to the level of the lowest etched line.

2. Attach the permeability cell with the manometer (use, if


necessary, a little light grease to ensure an airtight joint).

3. Open the stopcock and with gentle aspiration raise the level
of the manometer liquid to that of the highest etched line by
sucking the air.

4. Close the stopcock and the manometer liquid will begins to


flow. Start the timer as the liquid reaches the second etched
line and stop it when the liquid reaches the third etched line.
Record the time t, to the nearest 0.2 s and the temperature to
the nearest 1°C.

5. Repeat the procedure on the same bed and record the


additional, values of time and temperature.

6. Prepare a fresh cement bed and carry out the permeability


test twice on the second bed, recording the values of time
and temperature as before.

Dr. Sahil Bansal, IIT Delhi 12


Fineness by Blain Air Permeability Apparatus

Dr. Sahil Bansal, IIT Delhi 13


Fineness by Blain Air Permeability Apparatus

Dr. Sahil Bansal, IIT Delhi 14


Fineness: Standard Specifications
Indian Standard Min Finenees Value
Type of cement
Reference (m2/kg)
OPC (33) 269 225
OPC (43) 269 225
OPC (53) 269 225
PPC 1489 300

Dr. Sahil Bansal, IIT Delhi 15


Standard Consistency - IS 4031(Part 4)
Relevance:
■ The water requirement for making specimens for
finding out setting times, soundness and strength
of cement depends upon the normal consistency
of cement to be used.
■ Since different batches of cement differ in
compound compositions and fineness, pastes with
some fixed water content may differ in
consistency when first mixed.
■ For this reason, the consistency of the paste is
standardized by varying the water content until
the paste has a given resistance to consistency.
Vicat’s Apparatus

Dr. Sahil Bansal, IIT Delhi 16


Standard Consistency - IS 4031(Part 4)

The standard
consistency is that
consistency, which
will permit the vicat
plunger to
penetrate to a point
5 to 7mm from the
bottom of the vicat
mould when tested
as described below.

Vicat’s Apparatus
Dr. Sahil Bansal, IIT Delhi 17
Standard Consistency - IS 4031(Part 4)
1. Take 400 g of cement sieved and add 120 ml of water (i.e. 30% by weight of cement) to
the cement and mix thoroughly with two trowels for 3 to 5 (not less than three and
more than five) minutes till a uniform cement paste is achieved. The gauging time shall
be counted from the time of adding water to the dry cement until commencing to fill
the mould.
2. Fill the past in mould and level with trowel. Shake or tap to remove air bubbles.
3. Place the nonporous plate and the mould under the plunger. Release the plunger gently
to touch the surface of paste. Record the initial reading. Release the plunger quickly
and allow penetrating into the paste. When the plunger comes to rest, note the final
reading. This operation shah be carried out immediately after filling the mould.
4. Repeat the procedure with fresh paste varying the water percentage until the plunger
penetrates to a depth 5 to 7 mm from the bottom of the Vicat mould.

Dr. Sahil Bansal, IIT Delhi 18


Standard Consistency - IS 4031(Part 4)

Dr. Sahil Bansal, IIT Delhi 19


Setting or Hardening …..
■ Setting/stiffening : Solidification of the plastic cement paste (in few hours). It is
essential that it remain plastic long enough to permit being transported, placed,
consolidated, and finished.

■ Hardening : Strength gain with time (over several weeks). After completion of
mixing, concrete gradually stiffens until it becomes rigid.

20
Setting Times - IS 4031(Part 5)
Relevance:

■ Initial set represents approximately the time at which fresh cement can no longer be
properly mixed, placed, and compacted. Generally occurs in 2-4 hrs.

■ Final set represents approximately the time after which strength begins to develop at
a significant rate. Generally occurs in 5-8 hrs.

■ The initial and the final setting times of cement are the points arbitrarily defined by
the method of test. Do not mark a specific change in the physical-chemical
characteristics of the cement paste.

■ The initial setting time and the final setting time, as measured by penetration
resistance methods (Vicat’s Apparatus)

■ Setting time of cement does not correlate with setting time of concrete.

Dr. Sahil Bansal, IIT Delhi 21


Setting Times - IS 4031(Part 5)
■ Preparation of Test Block
1. Prepare a uniform cement paste by gauging 400 g of cement with 0.85 times the water required to give a paste of
standard consistency (Standard consistency of cement is determined as described in IS:4031 (Part 4)). The procedure
of mixing and filling the mould is same as standard consistency.

2. Start the stopwatch or note down the time when water is added to the cement.
■ Determination of initial setting time:
3. Place the test block confined in the mould and resting on the non-porous plate, under the rod bearing the initial
setting needle (C); lower the needle gently until it comes in contact with the surface of the test block and quickly
release, allowing it to penetrate into the test block.

4. Repeat this procedure until the needle, when brought in contact with the test block and released as described
above, fails to pierce the block beyond 5.0 ± 0.5 mm measured from the bottom of the mould. Note the time.

5. The difference of time between operations (2) and (4) provides the initial setting time of cement.
■ Determination of final setting time:
6. Replace needle (C) of the Vicat apparatus by the needle with an annular attachment (F).

7. The cement shall be considered as finally set when, upon applying the needle gently to the surface of the test
block, the needle makes an impression thereon, while the attachment fails to do so.

8. The interval of time between operation (2) and (7) provides the final setting time of cement.

Dr. Sahil Bansal, IIT Delhi 22


Setting Times - IS 4031(Part 5)

Dr. Sahil Bansal, IIT Delhi 23


Setting times: Standard Specifications
Type/name of cement Referenced indian Initial setting Final setting
stanadard time, mints time, mints
(min.) (max.)
OPC(33) IS:269 30 600
OPC(43) IS:269 30 600
OPC(53) IS:269 30 600
PPC IS:1489 30 600

Dr. Sahil Bansal, IIT Delhi 24


Soundness - IS 4031(Part 3)
Background:

■ Hardened cement paste may undergo an undesirable large expansion due to delayed
hydration of some oxides which had not combined at the time of formation of clinker.

■ The ability of cement to retain its volume after it gets hardened is known as soundness
of the cement. It is essential that the cement concrete shall not undergo appreciable
change in volume after setting.

■ Unsoundness produces cracks, distortion and disintegration there by giving passage to


water and atmospheric gases which may have injurious effects on concrete and
reinforcement.

Dr. Sahil Bansal, IIT Delhi 25


Soundness - IS 4031(Part 3)
■ Unsoundness in cement does not come to surface for a considerable period of time.

■ This test is designed to accelerate the hydration of free lime by the application of heat
thus discovering the defects in a short time. Further, to minimize the shrinkage of
cement paste, the test setup is kept immersed in water bath.

Le-chatelier apparatus

Measurement of expansion of cement after being kept at 100°C for 3 hours

Dr. Sahil Bansal, IIT Delhi 26


Soundness - IS 4031(Part 3)
1. Take 200 g amount of cement and prepare a cement paste by adding 0.78 times the water
required for standard consistency. (Standard consistency of cement is determined as
described in IS:4031 (Part 4))
2. Now place the lightly oiled Le-Chatelier mould on the glass panel and fill the mould with
the prepared cement paste up to the top. While placing the cement hold the mould edges
gently together.
3. Now place another lightly oiled glass plate on the top and put weight on it.
4. Submerge the whole assembly into the water pot at a room temperature and keep it
undisturbed for 24 hours at a temperature of 27±2° C.
5. Now remove the whole assembly from water and measure the distance between the mould
edges. Note that distance as L1. The measuring pointers should indicate to the nearest 0.5
mm
6. Submerge the mould again in water at the temperature prescribed above. Bring the water to
boiling, with the mould kept submerged, in 25 to 30 minutes, and keep it boiling for three
hours.
7. Remove the mould from the water, allow it to cool and measure the distance between the
indicator points. Note that distance as L2.
8. Soundness of Cement is given by L1 – L2.

Dr. Sahil Bansal, IIT Delhi 27


Soundness - IS 4031(Part 3)

Dr. Sahil Bansal, IIT Delhi 28


Soundness: Standard Specifications
Type/Name of cement Reference Indian standard Expansion (max.)
OPC (33) IS:269 10 mm
OPC (43) IS:269 10 mm
OPC (53) IS:269 10 mm
PPC IS:1489 10 mm

Dr. Sahil Bansal, IIT Delhi 29


Compressive Strength - IS 4031(Part 6)
Background:
■ Among physical properties of cement, compressive
strength is the most important property.
■ All the other factors remaining constant, the strength of
concrete or mortar depends upon the type and nature of
cement.
■ Strength test is not made on plain cement due to excess
shrinkage and cracking of plain cement paste. The test is
therefore carried out on blocks of mortar made of cement,
sand and water.
■ As the quality of sand from different sources varies, it is
necessary to use sand of standard quality for this test.

Dr. Sahil Bansal, IIT Delhi 30


Compressive Strength - IS 4031(Part 6)

Preparation of cement mortar cubes


200gms of cement
600 g of standard sand
Water 𝑃/4 + 3.0 %

Curing of cement mortar cubes


In moist closet or moist room for 24 ± 1 hours.
Submerge in clean fresh water (27 ± 2°C) until testing.

Testing of cement mortar cubes


At least 3 cubes.
Load uniformly at the rate of 35 N/mm2 per minute.

Dr. Sahil Bansal, IIT Delhi 31


Compressive Strength - IS 4031(Part 6)

Dr. Sahil Bansal, IIT Delhi 32


Compressive Strength - IS 4031(Part 6)
■ Preparation of cement mortar cubes:
1. Take 200gms of cement and 600 g of standard sand (i.e. ratio of cement to sand is 1:3) in a non-porous enamel tray and mix them
with a trowel for one minute.
2. Add water quantity 𝑃/4 + 3.0 % of combined weight of cement and sand and mix the three ingredients thoroughly until the
mixture is of uniform colour. The time of mixing should be less than three minutes and not more than four minutes.
3. Immediately after mixing fill the mortar into greased cube moulds of sizes 70.6 mm.
4. Compact the mortar by
a. Place the assembled mould on the table of the vibration machine and hold it firmly in position by means of a suitable
clamp.
b. Place the mortar in the cube mould and prod with the rod. The mortar shall be prodded 20 times in about 8 s to ensure
elimination of entrained air and honeycombing.
c. Place the remaining quantity of mortar in the hopper of the cube mould and prod again as specified for the first layer and
then compact the mortar by vibration.
d. The period of vibration shall be two minutes at the specified speed of 12 000 ± 400 vibration per minute.
e. At the end of vibration, remove the mould together with the base plate from the machine and finish the top surface of the
cube in the mould by smoothing the surface with the blade of a trowel.
■ Curing of cement mortar cubes:
1. Keep the filled moulds in moist closet or moist room for 24 ± 1 hours after completion of vibration.
2. At the end of that period, remove them from the moulds and immediately submerge in clean fresh water and keep there until
taken out just prior to breaking. The water in which the cubes are submerged shall be renewed every 7 days and shall be
maintained at a temperature of 27 ± 2°C.
3. After they have been taken out and until they are broken, the cubes shall not be allowed to become dry.
■ Testing of cement mortar cubes:
1. Take the cube out of water at the end of seven days. Measure the dimensions of the surface in which the load is to be applied. Let
them be ‘L’ and ‘B’ respectively.
2. Place the cube in compressive testing machine (without any packing between the cube and the steel plattens of the testing
machine) and apply the load uniformly at the rate of 35 N/mm2 per minute.
3. Note the load at which the cube fails.
4. Repeat the same procedure (steps 8 to 10) for other two cubes.
5. Repeat the whole procedure (Step 7 to 11) to find the compressive strength of the cube at the end of 28 days.

Dr. Sahil Bansal, IIT Delhi 33


Compressive Strength - IS 4031(Part 6)

Dr. Sahil Bansal, IIT Delhi 34


Compressive strength: Standard Specifications

Cement type Compressive strength (MPa)


1 Day 3 Days 7 Days 28 Days
OPC(33) — 16 22 33
OPC(43) — 23 33 43
OPC(53) — 27 27 53
PPC — 16 22 33

Dr. Sahil Bansal, IIT Delhi 35

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