Portland Cement

Part 2
 BASIC TESTS OF PORTLAND CEMENT

 All developed countries have their own national standards for cements. These standards
place limits on the cement composition and its physical properties. They also describe
the test procedures to be used to determine cement composition and cement
properties. An understanding of the significance of some of these properties is helpful
in interpreting results of cement tests.

These properties include:
Consistency
Fineness Compressive strength
Setting time
Soundness

Heat of hydration Specific gravity Loss on ignition

Each one of these properties has an influence on the performance of cement in concrete. 
 1.  FINENESS
 Approximately 95% of cement particles are smaller than 45 micrometers, with the
average particle around 15 µm. Cement particles >45 μm are slow to hydrate and those
>75 μm may never hydrate completely. An estimate of the relative rates of reactivity of
cements with similar compound composition cannot be made without knowing the
complete particle size distribution.

Fineness (= surface area/weight): The fineness of Portland cement is an important

quality index. It represents the average size of the cement grains. The fineness controls
the rate and completeness of hydration due to the exposure surface of cement particles
to the water. The finer the cement particles, the more rapid the reaction, the higher the
rate of heat evolution, and the higher the early strength. However, finer cement
particles can lead to high hydration heat, high possibility of early age cracking, and
possible reduced durability.

 The fineness is usually measured by the Blaine air‐permeability test (ASTM C 204 or
AASHTO T 153) . In this method, cement particles are placed on a porous bed and then
a given volume of fluid (air) is passed through the bed at a steady diminishing rate. After
all the air is passed, the time (t) for the process is recorded. The specific surface of the
cement can be calculated using:
S = K √t , where K is a constant.
 1.  FINENESS

 Cements with finer particles have more surface area in square meters per kilogram of
cement (Average Blaine fineness of modern cement ranges from 300‐500 m2/kg).

 Approximately for quality control purposes in the cement industry, the fineness is easily
determined as the residue on standard sieves such as No. 200 mesh (75 μm) and No.
325 mesh (45 μm).

Washing cement over  45‐micrometer sieve (helps 
Particle size distribution of Portland cement
monitor cement fineness during production).
 1.  FINENESS

Relation between specific surface area and compressive strength of concrete
 2.  SOUNDNESS
Certain cements undergo a large expansion after setting causing disruption of the hardened
mass. This will cause serious difficulties for the durability of structures when such cement is
used. The expansion is measured using the autoclave‐expansion test (ASTM C 151).

Soundness: Unsoundness in cement paste results from excessive volume change after
setting. Unsoundness in cement is caused by the slow hydration of excessive amounts of
MgO (magnesia) or free lime (hard‐burnt CaO)1, 2. The reactions are:
MgO + H2O → Mg(OH)2
CaO + H2O → Ca (OH)2

Hydration of magnesia to magnesium hydroxide is a slow and expansive reaction that can
cause unsoundness (cracking and pop‐outs in cement‐based products).

1) Another factor that can cause unsoundness is the later formation of ettringite.

2) The source of MgO in cement is usually dolomite (MgO.CaCO3), which is present as an impurity in most
limestones. A part of the total MgO in PC clinker (up to 2%) may enter into solid solution with the various
clinker compounds; the rest occurs as crystalline MgO (periclase). Uncombined or free calcium oxide is rarely
present in significant amounts in modern PC. Improper proportioning of raw materials, inadequate grinding
and homogenization of the raw mix, and insufficient temperature or hold time in the kiln burning zone are
among the principal factors that account for the presence of free or crystalline calcium oxide in PC clinker.
 2.  SOUNDNESS

Most specifications for PC limit the magnesia (Periclase) content to 5%* . This limit of MgO
ensures that unsoundness (expansion) will not occur as a result of the delayed hydration of
free MgO.

*The expansive effect of high MgO in cement was first recognized in 1884 when a number of concrete
bridges and viaducts in France failed two years after the construction. About the same time, the town hall
of Kassel in Germany had to be rebuilt as a result of expansion and cracking attributed to crystalline MgO in
cement. The French and the German cements contained 16‐30% and 27% MgO, respectively. This led to
restrictions on the maximum permissible MgO in cement. The current ASTM Standard Specification for
Portland Cement (ASTM C 150‐83) requires that the MgO content in cement shall not exceed 6%.

The deleterious effect associated with the expansion due to hydration of crystalline CaO was recognized in
the 1930s when certain 2‐5‐year‐old concrete pavements cracked. Initially suspected to be due to MgO, the
expansion and cracking were attributed later to the presence of hard‐burnt CaO in the cement used for the
construction of the pavements. Laboratory tests showed that the cement pastes made with a low‐MgO
Portland cement, which contained 2.8% hard‐burnt CaO, showed considerable expansion. However, with
concrete mixtures, due to the restraining effect of the aggregate, relatively large amounts of hard‐burnt
CaO are needed to obtain a significant expansion. The phenomenon is virtually unknown with modern
concrete because better manufacturing controls on the quality of Portland‐cement clinker have assured
that the content of uncombined or free CaO in clinker seldom exceeds 1%.
 2.  SOUNDNESS: Le Chatelier test BS 4550
Since these reactions are very slow processes, taking several months and even years to
finish, and their hydration products are very aggressive, their crystal growth pressure will
crack and damage the already hardened cement paste and concrete.

The soundness of the cement must be tested by an accelerated method due to the slow
process. One test is called the Le Chatelier test (BS 4550), and is used to measure the
potential for the volumetric change of the cement paste*. The Le Chatelier test is used
mainly for free lime detection**.

Procedure (Le Chatelier test, BS 4550):

1. Fill the cylinder‐shaped container with cement paste of normal consistency.
2. Cover the container with glass plates.
3. Immerse in water (20◦C) and measure the distance of the indicator at the top of the apparatus.
4. Boil the specimen for 1 h and measure the distance again after cooling.
5. Expansion should be less than 10mm for acceptable cement quality.

*The so‐called boiling method includes also the Pat test. Pat test is to make the cement paste of normal
consistency into cement cake, boil it for 3h, and then observe it by naked eyes. If there is no crack and no
bending by ruler inspection, it is called qualified soundness. If there is contradictory between the results
measured by Pat test and Le Chatelier test, Le Chatelier test should prevail.

**The hydration of free magnesium oxide is slower than that of free calcium oxide. Therefore, its
harm can be inspected only by autoclave test.
 2.  SOUNDNESS: Le Chatelier test BS 4550

Le Chatelier test apparatus

 III.7.2.  SOUNDNESS: the autoclave expansion test ASTM C151

Another method is the autoclave expansion test (ASTM C151), which uses an autoclave to
increase the temperature to accelerate the process.

Procedure (the autoclave expansion test ASTM C151):

Mold a cement paste with normal consistency into a container and cure normally for 14 h. Then remove from
the mold, measure the size of the specimen, and place the specimen into autoclave. Raise the temperature in
the autoclave so that the stem pressure inside can reach 2MPa in 45 to 75 min.
Maintain the pressure of 2MPa for 3h. Cool the autoclave down so that the pressure is released in 1.5h. Cool
the specimen in water to 23◦C in 15 min. After another 15 min, measure the size of the specimen again; the
expansion must be less than 0.80% to be acceptable. Autoclave testing can test both excess free lime and
excess MgO.

In the soundness test, 25‐mm square bars are exposed to high

temperature and pressure in the autoclave to determine the volume
stability of the cement paste.
 3. CONSISTENCY
Consistency refers to the relative mobility of a freshly mixed cement paste or mortar or to
its ability to flow. During cement testing, pastes are mixed to normal consistency as defined
by a penetration of 10 ± 1 mm of the Vicat plunger below the original surface in 30 s after
being released (ASTM C 187). Make trial pastes with varying percentages of water until the
normal consistency is obtained. Make each trial with fresh cement (w/c about 0.26).
Mortars are mixed to obtain either a fixed water‐cement ratio or to yield a flow within a
prescribed range. The flow is determined on a flow table as described in ASTM C 230. Both
the normal consistency method and the flow test are used to regulate water contents of

Fig. 18:Consistency test for mortar using the

removed and the table undergoes a succession

flow table: The mortar is placed in a small brass
mold centered on the table. After the mold is

of drops, the diameter of the pat is measured to

Fig. 17: Normal consistency test for paste 

pastes and mortars, respectively.

using the Vicat plunger.

determine consistency.
Consistency test for mortar using the flow table: The
mortar is placed in a small brass mold centered on the
table. After the mold is removed and the table undergoes a
Normal consistency test for paste 
succession of drops, the diameter of the pat is measured to
using the Vicat plunger. determine consistency.
 4. SETTING TIME
The object of the setting time test is to determine:
1. The  time  that  elapses  from  the  moment  water  is  added  until  the  paste  ceases  to  be 
fluid and plastic (called initial set) and 
2. The time required for the paste to acquire a certain degree of hardness (called final set). 

 Setting time is measured using the Vicat apparatus (ASTM C 191 or AASHTO T 131).
The setting times indicate that a paste is or is not undergoing normal hydration reactions.
Equipment and Materials
1.2‐kgs scale accurate to 0.1 grams.
2.Vicat Apparatus (see figure), which consists of a movable rod, B, weighing 300g; one end, C, the
plunger end, being 10 mm in diameter for a distance of at least 5 cm; and the other end having a
movable steel needle, D, 1 mm in diameter and 5 cm in length. The rod, B, is reversible and can be
raised or lowered by the set screw, E, which has an adjustable indicator, F. The latter moves over a
graduated scale, attached to the frame, A. The cement paste is held in a conical ring, G, which has
an inside diameter of 7 cm at the bottom and 6 cm at the top, and has a height of 4 cm. The
truncated cone rests on a glass plate, H, which is 10 cm square.
3.An electrically driven mixer with a 4.73‐liter bowl and a removable stainless steel paddle that
conforms to within 0.8 mm to the shape of the bowl.
4.For a scraper, use a kitchen tool known as a plate and bowl scraper.
5.At least 3 kg of Portland cement and a supply of water.
 7.4. SETTING TIME

Vicat Apparatus
 Time of Set of Hydraulic Cement by Vicat Needle (ASTM: C 191)

Consistency Determination
1. Place the rod, C, at the bottom of the Vicat Apparatus with the needle, D, at the top.
2. The plunger end, C, should now be brought into contact with the top of the cement
paste in the ring; tighten the set screw, E.
3. Set the movable indicator, F, to the zero mark on the scale and release the rod
immediately.
4. The paste will be considered to have normal consistency if C settles 10 ± 1 mm into the
paste in 30 seconds.
5. Repeat the procedure with fresh cement batches, varying the amount of water until a
paste of normal consistency is obtained.
6. The amount of water required to obtain a cement paste of normal consistency should
be determined to the nearest gram.
 Time of Set of Hydraulic Cement by Vicat Needle (ASTM: C 191)

Time of Setting Determination

1. Begin the time of setting determination immediately after the normal consistency
specimen in the ring has been undisturbed in a moist cabinet for 30 minutes.
2. Determine the penetration of the 1‐mm needle, D, in 30 seconds and every 15 (10 for
Type III cement) minutes thereafter, until a penetration of 25 mm or less is obtained.
For this test lower the needle, D, until it just touches the cement paste, tighten the set
screw, E, and set the movable indicator, F, to the zero mark on the scale and release the
rod. Allow the needle to settle for 30 seconds and take the reading to determine the
penetration.
3. Record the results of all penetration readings (see table).
4. Determine the time of initial set by interpolating the results to find the time for a
penetration of 25 mm*.
5. The final setting time is recorded when the needle, D, does not visibly sink into the
paste.
*The only computation required in the Test Procedure outlined previously is the interpolation of the
time of set unless a test value of exactly 25 mm of penetration of needle, D, is obtained. Normally
there will be a prior period value greater than 25 mm and a succeeding one of less than 25 mm, from
which the time to the nearest minute will be determined for the time of setting determination. With
each succeeding rest period of 10 or 15 minutes, depending upon the type of cement in the test
specimen, the depth of penetration will decrease.
Time of Set of Hydraulic Cement by Vicat Needle (ASTM: C 191)22
 4. SETTING TIME
 Initial setting time is the time from the instant at which water is added to the cement to
the instant at which the Vicat’s initial set needle penetrate to a point 25 mm. ASTM C 150
prescribes a minimum initial setting time of 60 minutes for Portland cements.

 Final setting time corresponds to the time at which the Vicat's final set needle makes an
impression on the paste surface but the cutting edge fails to do so. ASTM C 150 prescribes
a maximum final setting time of 10 hours for Portland cements

 Gypsum in the cement regulates setting time. Setting time is also affected by: cement
fineness, w/c ratio, and admixtures
 5. COMPRESSIVE STRENGTH
 Compressive strength as specified by ASTM cement standards is that obtained from tests of
50‐mm (2‐in.) mortar cubes tested in accordance with ASTM C 109 (AASHTO T 106). These
cubes are made and cured in a prescribed manner using a standard sand.

 Compressive strength is influenced by the cement type, or more precisely, the compound
composition and fineness of the cement.

 In general, cement strengths (based on mortar‐cube tests) cannot be used to predict

concrete strengths with a great degree of accuracy because of the many variables in
aggregate characteristics, concrete mixtures, and environmental conditions in the field.

50‐mm (2‐in.) mortar cubes are cast (left) and crushed (right) to determine strength characteristics of
cement.
 5. COMPRESSIVE STRENGTH

Relative strength development of PC mortar cubes as a percentage of 28‐

day strength. Mean values adapted from Gebhardt 1995.
 6. SPECIFIC GRAVITY AND BULK DENSITY

 The particle density of PC ranges from 3.10 to 3.25, averaging

3.15 g/cm3. Portland blast‐furnace‐slag and Portland‐
pozzolan cements have densities ranging from 2.90 to 3.15,
averaging 3.05 g/cm3. The density of a cement, determined
by ASTM C 188 (using the Le Chatelier flask), is not an
indication of the cement’s quality; its principal use is in
mixture proportioning calculations.

 Relative density (also called specific gravity) is a dimensionless number determined by

dividing the cement density by the density of water at 4°C. The density of water at 4°C
is 1.0 g/cm3.

 The bulk density of cement can vary considerably depending on how it is handled and
stored. PC that is fluffed up may weigh only 830 kg/m3, whereas when consolidated by
vibration, the same cement can weigh as much as 1650 kg/m3 . For this reason, good
practice dictates that cement must be weighed for each batch of concrete produced, as
opposed to use of a volumetric measure.
 7. LOSS ON IGNITION

 Loss on ignition (LOI) of PC is determined by heating a cement sample of known weight

to between 900°C and 1000°C until a constant weight is obtained. The weight loss of the
sample is then determined. Normally, a high loss on ignition is an indication of pre‐
hydration and carbonation, which may be caused by improper or prolonged storage. The
test for loss on ignition is performed in accordance with ASTM C 114. LOI values range
from 0 to 3%.

Loss on ignition test of cement.