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COMPREHENSIVE TRAINING ON MATERIALS

TESTING TECHNOLOGY

MODULE II- SAMPLING AND TESTING CEMENT AND CONCRETE MIX

Prepared by:

JULIETA C. RABOT
DPWH-BRS
Module II- SAMPLING AND TESTING CEMENT AND CONCRETE MIX

OUTLINE:
I. Introduction: Cement
II. Definition: Portland Cement
Hydraulic Cement
Hydration
Heat of Hydration
III. Basic Composition of Portland Cement
IV. Raw Materials Used in the Manufacture of Cement
V. Manufacture of Portland Cement
A. Basic Processes
B. Steps
VI. Principal Compounds Present in the Finished Cement
VII. Types of Portland Cement/ Uses
VIII. Pozzolan
A. Types
B. Uses
IX. Blended Hydraulic Cement (Portland-Pozzolan Cement)
A. Kinds
B. Types
C. Uses
X. Sampling/Minimum Testing Requirements
XI. Different Tests on Portland Cement
A. Physical Tests
B. Chemical Tests
XII. Significance of Tests
XIII. Specifications
What is Cement?

The term cement, in its broader

meaning, applies to any materials
that will bind two or more non-
adhesive substances together. The
cements to be considered here are
those which have a limestone,
oyster-shell, coquina shell or similar
lime base and are used to form
concrete.
Composition of Concrete
By Weight: By Volume:

1. Cement – 14% CA - 50% 1. Cement – 10%

2. Aggregates – 80% FA - 30% 2. Aggregates – 70%

3. Water – 6% 3. Water – 15%

4. Air – 5%

Composition of Concrete is Classified

into Two Groups:
1. Active Group – Cement and Water
2. Inactive Group – Coarse and Fine Aggregates

Functions of Cement:
1. To bind CA and FA together.
2. To fill the voids in between CA and FA to form a compact mass.
Cement + water = cement paste fill small voids in FA fill large voids in CA
What is Portland Cement?

Portland Cement is defined as the

product obtained by burning
(calcining) to incipient fusion a
properly proportioned mixture of
argillaceous and calcareous
materials and the burnt product
which is called clinker is then mixed
with Gypsum (CaSO4.2H2O), and
pulverized to form Portland Cement.
INCIPIENT FUSION

Burning the materials to make it

liquid by heating it into a very high
temperature, at about 14800C. At
this temperature, the initial melting
stage of the materials is reached
known as the point of incipient
fusion. Here sintering takes place
and a clinker is formed.
What is Hydraulic Cement?
Portland Cement is a hydraulic cement, that is,
it reacts or combined chemically with water
(hydrates), one that will harden under water.
The process is known as Hydration.

The heat generated in the reaction of cement

and water is called Heat of Hydration.
The reaction produce a substance that is
durable, resists the effects of water, and
continues to gain strength as long as moisture is
present. It will continue to gain strength even
when completely submerged in water.
HYDRATION:
The process in which the cement reacts or
combined chemically with water

HEAT OF HYDRATION:
 The heat produced by the chemical reaction
between cement and water.

 The amount of heat generated depends on the

chemical composition of the cement.

 The rate of heat generation is affected by: the

fineness of the cement, the chemical
composition and the temperature during
hydration.

.
Portland Cement has the Following Basic
Composition

1. Lime (CaO) = 60 – 65%

2. Silica (SiO2) = 10 – 25%

3. Iron Oxide (Fe2O3) = 2 – 4%

4. Alumina (Al2O3) = 5 – 10%

Raw Materials Used in the Manufacture of Portland
Cement

Most of the ingredients in Portland Cement are found in

nature, but they cannot always be used in their natural
form. Limestone, shale, clay, chalk, marl, oyster
shells, silica sand, iron ore and blast furnace slag may
be used as raw materials. Each cement plant may use
a different combination of raw materials which when
ground, blended, and tested under rigid control, produce a
cement that is uniform in strength and quality. Depending
on the location of the cement manufacturing plant,
available raw materials are pulverized and mixed in
proportions such that the resulting mixture will have the
desired chemical composition.
Argillaceous Raw Materials
Those materials which contributes Silica (SiO2),
Alumina (Al2O3) and Iron Oxide (Fe2O3) to the
clinker, it includes clay, shale, blast furnace slag,
iron ore, sand,etc.

Calcareous Raw Materials

Those material which contributes Lime (CaO) and
Magnesia (MgO) to the clinker, it includes
limestone, chalk, marls, marine (oyster shells),
etc.
Typical Sources of Raw Material Used in the Manufacture of Portland Cement

COMPONENTS
Lime Silica Alumina Iron
Cement Rock Sand Clay Iron Ore
Limestone Traprock Shale Iron Calcine
Marl Calcium Slag Iron Dust
Alkali Waste Silicate Fly Ash Iron Pyrite
Oyster Shell Quartzite Copper Slag Iron Sinters
Coquina Shell Fuller’s Earth Aluminum Ore Refuse Iron Oxide
Chalk Staurolite Blast Furnace Flue Dust
Marble Diaspore Clay
Granodiorite
Kaolin

Source: Portland Cement Association

GYPSUM (CaSO42H2O)

A predetermined percentage of gypsum is added to

regulate the setting time that will be required for a
particular cement. The addition of small quantity of
gypsum is of great importance because it can stabilize
and control the rate of hydration. Although small in
quantity, the addition of gypsum must be done with
some care, as its prime purpose is to react with the
tricalcium aluminate, the quantity added must
correspond to the amount of tricalcium aluminate
available. Small amount added will often increase the
strength, too much amount leads to slow expansion of
the set cement and may result in crumbling.
Portland Cement is Manufactured by Two (2) Basic Processes:

1. Wet Process

In the wet process proper proportions of raw materials are mixed

with enough water to form a slurry, which is 30 to 35 % water.

In this form the materials are further proportioned, mixed, ground and
pulverized and then pumped to a furnace called a kiln.

It is use for a very friable materials such as chalk and clay, wet
process are preferred because of more accurate control of the raw
mix.

2. Dry Process

The dry process is similar, except that the materials are proportioned,
stored, ground, mixed, pulverized and fed into the kiln in a dry state.

Preferred when raw materials are hard rocks, less fuel is required for
burning than in the wet process.
Steps in the Manufacture of Portland Cement

1. Raw materials is first reduced to 5 in. size (primary

crusher), then 3/4 in. size in secondary crusher, and
stored separately and conveyed to grinding mill.

2. Raw materials are ground to powder and blended

(incorporation of raw materials to form a homogeneous
mixture).

3. The burning of the raw mix in a kiln to form a clinker

(burning changes raw mix chemically into cement clinker).

4. The grinding or pulverizing the clinker with the addition of

a small proportion of gypsum to a fine powder (Portland
Cement).
Three heating stages occurring in a Rotary Kiln:
1. @ 425oC - Drying – excess water is driven off
2. @ 875oC - Calcining – heating to a high temperature but
below the melting or fusing point, causing decomposition
of carbonates and other compounds (limestone
breaksdown into CaO and CO2).
CaCO3 CaO + CO2 Calcium Carbonate (limestone)
MgCO3 MgO + CO2 Magnesium Carbonate
Al2Si2O7 Al2O3 + 2SiO2 Aluminum Silicate (clay)
Fe2O3 Hematite (Iron Ore)
3. @1400oC – 1480oC – Clinkering – initial melting stage of
material, known as the point of incipient fusion, is reached
sintering takes place and a clinker is formed. Oxides
recombine to form cement compounds.
Cement Compounds: C3S, C2S, C3A, C3AF
where: C =CaO, S = SiO2, A = Al2O3, F = Fe2O3
C3S = 3CaO.SiO2, C2S = 2CaO.SiO2
C3A = 3CaO.Al2O3, C3AF = 3CaO.Al2O3.Fe2O3
Principal Compounds which are Present in the Finished
Cement
When lime and silica are heated to the sintering
temperature in the presence of alumina and ferric oxide, four
basic components of cement are formed. These clinker
compounds that are formed by sintering are responsible for
the hydration process:

1. Tricalcium Silicate, 3CaO.SiO2 (C3S)

2. Dicalcium Silicate, 2CaO.SiO2 (C2S)

3. Tricalcium Aluminate, 3CaO.Al2O3 (C3A)

4. Tetracalcium Alumino Ferrite, 4CaO.Al2O3.Fe2O3 (C4AF)

1. Tricalcium Silicate (C3S) = 3CaO.SiO2

 Responsible for the initial set and of the early strength development of the
cement, high percent will give high strength, faster strength development.

 It has all the essential properties of portland cement, it undergoes an

initial and final set within an hour after mixing and when properly prepared
shows no unsoundness.

 Mixes of tricalcium silicate and water are less plastic, more water are
required to obtained a workable paste, addition of gypsum to the mass
render it more plastic and has some effect on setting time.

 Can be calculated as follows:

C3S = 4.07(CaO) - 7.60(SiO2) - 6.72(Al2O3) - 1.43(Fe2O3) - 2.85(SO3)

2. Dicalcium Silicate (C2S) = 2CaO.SiO2

 Also responsible for the strength development, high percent will give high
strength but slow in development.

 Exhibits no definite setting time and mixed mass sets only slowly over a
period of some days, addition of gypsum produces little change.

 It produces little strength at early ages but gains steadily in strength at

later ages until it approaches equality with tricalcium silicate. Tricalcium
silicate attains the greater part of its strength in seven (7) days.

 Added strength in the final hardening which may be prolonged over many
months (slow), hardens the slowest, releases the least heat, and has a
low shrinkage.

 Can be calculated as follows:

C2S = 2.87(SiO2) - 0.754(3CaO.SiO2)

3. Tricalcium Aluminate (C3A) = 3CaO.Al2O3

 Control the volume change of cement, aid in development of early

strength of cement. Facilitate combination of lime and silica.

 It reacts the most rapidly, gaining an appreciable amount of its maximum

strength at first day after mixing, it liberates the most heat, and undergoes
the most shrinkage.

 Gives a flash set on mixing with water and this is accompanied by the
evolution of so much heat as to lead to violent steaming, as cement,
become finer, the setting rate is accelerated making the problem of flash
set more prevalent, addition of small quantity of gypsum counteract this
detrimental reaction.

 Weak resistance against sulfate attack.

 Can be calculated as follows:

C3A = 2.65(Al2O3) - 1.69(Fe2O3)

4. Tetracalcium AluminoFerrite (C4AF) =
4CaO.Al2O3.Fe2O3

 Must not be present in excess amount because it will

displace the silicate which is responsible in strength
development.
 Hydrates rapidly
 More stable than C3A
 Contribution to overall strength is insignificant
 Accelerate the hydration of silicates

 Can be calculated as follows:

C4AF = 3.04(Fe2O3)
Typical Average Values of Compound of Portland Cements of Different Types

Compound Composition, %

Cement
Free Loss on
C3S C2S C3A C4AF CaSO4 MgO
CaO Ignition

Type I 59 15 12 8 2.9 0.8 2.4 1.2

6
Type II 46 29 12 2.8 0.6 3 1
(8 max.)

12
Type III 60 12 8 3.9 1.3 2.6 1.9
(15 max.)

30 46 5
Type IV 13 2.9 0.3 2.7 1
(35 max.) (40 min.) (7 max.)

4
Type V 43 36 12 2.7 0.4 1.6 1
(5 max.)

The numbers in parenthesis are the maximum or minimum values specified by ASTM C 150-84
Schematic Representation of the Formation and
Hydration of Portland Cement

Component
elements O2 Si Ca Al Fe

Component
oxides CaO SiO2 Al2O3 Fe2O3

Cement
Compounds C 3S C2S C3A C4AF

Portland
Cements Various Types

Hydration
products C-S-H gel Ca(OH)2
HYDRATION OF CEMENT

At any stage of hydration, the cement paste consists of gel (a finely-grained

product of hydration having large surface area collectively called gel), the
remnant of unreacted cement, calcium hydroxide Ca(OH)2, and water, besides
some other minor compounds.

The reactions of compounds and their products may be symbolically

represented as:
2C3S + 6H C3S2H3 + 3Ca(OH)2 Silicate phase
2C2S + 4H C3S2H3 + Ca(OH)2
C3A + 6H C3AH6
C4AF + 7H C3AH6 + CFH

The product C – S – H represents the calcium silicate hydrate which is the

gel structure. The above equations only refer to the processes in which
the cement compounds (C3S and C2S, etc.) react with water to form a
strong hydrated mass. The hydrated crystals are extremely small, varying
from colloidal dimensions(less than 2um) to 10 um or more. The Ca(OH)2
liberated during the reaction of silicate phase crystallizes in the available free
space.
Types of Portland Cement

For most construction purposes a standard type of Portland Cement is used.

However, special types are manufactured for specific uses. The amount of
the four (4) basic ingredients can be varied to produce different types of
portland cement, each with some unique characteristics:
1. Type I (Normal Type)
This is a standard portland cement used for general construction work when
the special properties of the other types are not required.
Uses
It is normally used for reinforced concrete buildings, bridges, pavement and
sidewalks where the soil conditions are normal, for most concrete masonry
units, and for all uses where the concrete is not subject to special sulfate
hazard or where the heat generated by the hydration of the cement is not
objectionable.
2. Type II (Moderate-Sulfate Resistant)
This cement has a lower heat of hydration than Type I and generally sets
more slowly. It has a better resistance to the action of sulfate than Normal
Portland and is used where sulfate concentrations in ground waters are
higher than normal but not unusually severe It also generates heat at a
slower rate than Normal Portland and is used in mass concrete works. Its
use will minimize temperature rise, a property which is particularly important
when concrete is being placed in hot weather.
Uses
It is used in drainage structures, foundations and floor slabs, where the soil
contains a moderate amount of sulfates.

3. Type III (Highly-Early Strength)

This type develops approximately 190% of the strength of Type I at three
(3)days and 90% to 130% at 28 days. It develops considerable heat during
setting.
Uses
It is used where higher strengths are required at early periods usually of a
week or less. It is particularly useful where it is required to remove forms as
soon as possible or when the structure must be brought into service quickly.
High-early strength makes it possible to reduce the period of protection for
concrete during cold weather.
4. Type IV (Low-Heat of Hydration)
This is a special cement for use where the amount and rate of heat
generated must be minimized. Strength is also developed at a slower rate.
Low-heat portland cement was first developed for use in the construction of
the Hoover Dam. Its slow setting time is an advantage in large structures,
where solid one-piece construction is desire..
Uses
It is intended for use in massive concrete structures, such as large dams,
where the temperature rise resulting from heat generated during hydration is
a critical factor.
5. Type V (Sulfate - Resistant)
A special cement intended to be used in structures to prevent damage from
severe sulfate action of soils or high alkali content of waters.
Uses
Intended for use in structures subject to attack by sulfate concentrations in
some waters, such as may be found in certain manufacturing plants or in the
ground water in some areas. It is also resistant to the action of seawater.
Approximate Relative Strength of Concrete As Affected by Type of Cement

Compressive Strength – Percent of Strength of

Normal (Type I) Portland – Cement Concrete
Type of Portland
Cement
1 Day 7 Days 28 Days 3 Months

I. Normal 100 100 100 100

II. Moderate 75 85 90 100

III. High-Early Strength 190 120 110 100

IV. Low-Heat 55 55 75 100

V. Sulfate-Resistant 65 75 85 100
Approximate Composition Limits of Portland Cement

CaO ------------------ 60 – 70

SiO2 ------------------ 17 – 25

Al2O3 ------------------ 3–8

FeO3 ------------------ 0.5 – 6.0

MgO ------------------ 0.1 – 5.5

Na2O + K2O ------------------ 0.2 – 1.3

SO3 ------------------ 1.0 – 3.0

Oxide Composition of Type I or Normal Portland Cement

Oxide Ingredient Range, %

Lime, CaO 60 – 66

Silica, SiO2 19 – 25

Alumina, Al2O3 3–8

Iron Oxide, Fe2O3 1–5

Magnesia, MgO 0–5

Sulfur Trioxide, SO3 1-3

Source: Portland Cement Association

Oxide and Compound Compositions of a Typical Portland Cement

Typical Oxide Composition, percent

CaO 63
SiO2 20
Al2O2 6
Fe2O2 3
MgO 1 – 1/2
SO3 2
K2O
1
Na2O
Other 1
Loss on ignition 2
Insoluble Residue 1/2

Hence, Calculated Compound Composition, percent

C 3A 10.8
C 3S 54.1
C 2S 16.6
C4AF 9.1
Minor compounds -
POZZOLAN AND POZZOLANIC
CEMENT
POZZOLAN:

A siliceous or siliceous and aluminous

material, which in itself possesses little or
no cementitious value but which will, in
finely divided form and in the presence of
moisture, chemically react with calcium
hydroxide (lime at ordinary temperature to
form compounds possessing cementitious
properties.
Two (2) Kinds of Pozzolan

1. Natural Pozzolan

Materials of volcanic origin (volcanic ash), it

includes a number of natural materials such as
diatomaceous earth, opaline cherts and shales,
tuffs and pumicites, which is composed of a
mixture silicates and contain both glass and
crystalline particles.

2. Artificial Pozzolan

Product obtain by heat treatment of natural

materials such as clays and shales and certain
siliceous rocks and pulverized fuel ash.
Pulverized Fuel Ash (Fly Ash)

• The most common artificial pozzolan, obtained

by electrostatic or mechanical means form the
flue gases of furnace in coal-fired power plant
stations. The fly ash particles are spherical
and of at least the same fineness as cement
so that silica is readily available for reaction.

• A fly ash is a fine residue which results from

the combustion of powdered coal and may
contain various amounts of carbon, silica,
sulfur, alkalis and other ingredients.
Uses of Pozzolan

• Use as a substitute for a proportion of the

portland cement in concrete, but in some
cases it is preferable to use it as an addition
(admixture).

• These pozzolanic materials are generally

substitute for 10 to 35 percent of the cement.

• This substitute produces concrete that is more

permeable but much more resistance to the
action of salt, sulfate or and water.
Blended Hydraulic Cement

Hydraulic cement used for general

construction and or some special
application containing pozzolan ,
blast – furnace slag, limestone, or
some combination of these with
portland cement clinker or slag with
lime in different porportions.
Blended Hydraulic Cement
Kinds of Blended Hydraulic Cements for
General Concrete Construction

1. Type IS - Portland - blast-furnace slag cement

2. Type IP - Portland - pozzolan cement
3. Type IL - Portland - limestone cement
4. Type IT -Ternary blended cement (consist of
portland cement with either a combination of two
different pozzolans, slag and pozzolan, a
pozzolan and limestone, or a slag and a
limestone.
Portland – Pozzolan Cement
• Defined as a blend of ordinary portland cement and
pozzolan.

• These cements are made by intergrinding or blending

pozzolans with portland cement

• A hydraulic cement consisting of an intimate and

uniform blend of portland cement and fine pozzolan
produced by intergrinding portland cement clinker and
finely divided pozzolan, or a combination of
intergrinding and blending, in which the amount of the
pozzolan constituent is within specified limits, usually
between 15 and 40 weight percent of the portland-
pozzolan cement.
Types of Portland - Pozzolan Cement

1. Type IP

Portland-Pozzolan cement for use in

general concrete construction.

2. Type P

Portland-Pozzolan cement for use in

concrete construction where high
strengths at early ages are not required.
Uses of Portland-Pozzolan Cement

• Particular useful in marine and hydraulic constructions and other

mass concrete structures.

• Use in large mass concrete works because of reduction in heat

evolution, examples are the constructions of dams and bridges.
Portland-pozzolan cement produces less heat of hydration and
offers greater resistance to the attack of impurities in water than
Normal Portland Cement.

• The original reason for the use of pozzolanic portland cement

was the improved durability combined with some economy
obtained in marine, hydraulic and underground structures.

• The portland-pozzolan cement can generally be used wherever

ordinary portland cement is usable under normal condition.

• Use in concrete with low-heat characteristics and in concrete

requiring good chemical resistance.
DPWH STANDARD SPECIFICATION ( BLUE BOOK)
Item 311 – Portland Cement Concrete Pavement and
Item 405 – Structural Concrete

Section 311.2 – Material Requirements

Subsection 311.2.1 Portland Cement

It shall conform to the applicable requirements of Item

700, Hydraulic Cement. Only Type I Portland Cement
shall be used unless otherwise provided for in the
Special Provisions. Different brands or the same
brands from different mills shall not be mixed nor shall
they be used alternately unless the mix is approved by
the Engineer.
Section 311.2 – Material Requirements
Subsection 311.2.1 Portland Cement

However, the use of Portland-Pozzolan Cement Type IP

meeting the requirements of AASHTO M 240/ ASTM C
595, Specifications for Blended Hydraulic Cement shall
allowed, provided that trial mixes shall be done and that
the mixes meet the concrete strength requirements, the
AASHTO/ASTM provisions pertinent to the use of
Portland Pozzolan Cement Type IP shall be adopted.
Sampling/Testing Requirements
ASTM C183-SAMPLING AND THE AMOUNT OF TESTING
OF HYDRAULIC CEMENT
The cement may be sampled by any of the applicable methods:

1.1 From the Conveyor Delivering to Bulk Storage – Take one grab
sample, having a mass of at least 5 kg (10 lb) at approximately 6-h intervals.

“Grab Sample” – A cement sample secured from a conveyor, from bulk

storage, or from bulk shipment in one operation, shall be termed a “grab
sample.” A sample obtained during a 10-min interval using an automatic
sampling device that continuously samples a cement stream may also be
termed a grab sample.

“Composite Sample”- Grab samples taken at prescribed intervals over a

period of time may be combined to form a “composite sample” representative of
the cement produced during that period of time.

All samples, whether grab or composite, shall have a mass of at least 5 kg (10
lb).
Sampling/Testing Requirements

1.2 Transfer Sampling – Sample cement in storage while the cement is being
transferred from one bin to another. Take one grab sample from the transfer
stream for each 360 Mg (400 tons) of cement, or fraction thereof, but take no
less than two grab samples and combine them to produce a composite
sample.

1.3 Other Sampling Methods – When neither of the above sampling methods is
applicable, samples may, when authorized by the purchaser, be taken by one
of the following methods:

1.3.1 From Bulk Storage at Point of Discharge – Withdraw cement from

the discharge openings in a steady stream until sampling is completed. In
sampling bulk storage at points of discharge , while the cement is flowing
through the openings, take samples as such intervals so that at least two
grab samples shall be secured for each 360 Mg (400 tons) in the bin or silo.

1.3.2 From Bulk Storage and Bulk Shipment by Means of a Slotted

Tube Sampler –When the depth of the cement to be sampled does not
exceed 2.1 m (7 ft), obtain samples using a slotted tube sampler . Take
samples from well-distributed points and various depths of the cement so
that the samples taken will represent the cement involved.
Sampling/Testing Requirements

Sampling

1.3.3 From Packaged Cement by Means of Tube Sampler – Insert the

sampler diagonally into the valve of the bag and place the thumb over the air
hole. Then withdraw the sampler. Take one sample from a bag in each 4.5
Mg (5 tons) or fraction thereof.

1.3.4 From Bulk Shipment of Car or Truck:

(a). Single Shipment – If only one car or truck is being loaded and the
loading is continuous and all from the same source, take a 5-kg (10 lb)
sample. If not continuous or unknown, combine five or more portions from
different points in the load to form the test sample.

(b) Multiple Shipment – When the shipment consists of several cars

or trucks loaded from the same source and on the same day, sample the
shipment at the rate of one sample for each 90 Mg (100 tons) of cement or
fraction thereof, but take not less than two samples.
Sampling/Testing Requirements
STORAGE OF CEMENT

Cement, in bulk, can best be stored in bins of depth 2 m or more, usually

a crust about 5 cm thick forms, and this must be removed before cement is
taken for use. The bagged cement may also be kept safely for many months if
stored in waterproofed shed with nonporous walls and floors, the wind being
tightly shut. Once the cement has been properly stored it should not be
disturbed until it is to be used. The practice of moving and restacking the bags
to reduce warehouse pack only exposes fresh cement to air.

DPWH STANDARD SPECIFICATION (BLUE BOOK)

Item 311 : PORTLAND CEMENT CONCRETE PAVEMENT
Item 405 – STRUCTURAL CONCRETE

Subsection 311.2.11 – Storage of Cement and Aggregates

All cement shall be stored, immediately upon delivery at the Site, in

weatherproof building which will protect the cement from dampness. The floor
shall be raised from the ground. The buildings shall be placed in locations
approved by the Engineer. Provisions for storage shall be ample, and the
shipments of cement as received shall be separately stored in such a manner
as to allow the earliest deliveries to be used first and to provide easy access of
each shipment for identification and inspection
Sampling/Testing Requirements

Subsection 311.2.11 –Storage of Cement and Aggregates

Storage buildings shall have capacity for storage of a sufficient quantity of

cement to allow sampling at least (12) days before the cement is to be used.
Bulk cement, if used, shall be transferred to elevated air tight and
weatherproof bins. Stored cement shall meet the test requirements at any
time after storage when retest is ordered by the Engineer. At the time of use,
all cement shall be free-flowing and free of lumps.

REJECTION

Cement which for any reason, has become partially set or which contains
lumps of caked cement shall be rejected. Cement salvaged from discarded or
used bags shall not be used. Samples of cement shall be obtained in
accordance with AASHTO T 127/ASTM C 183.

Due to defective storage for long periods, cement is adversely affected. The
cement remaining in bulk storage with the manufactures for more than six(6)
months or cement in jute bags in local storage in the hands of dealers for more
than three (3) months after completion of tests may be retested before use and
rejected if they fail to conform to any of the requirements of the specification.
Sampling/Testing Requirements

PROTECTION OF SAMPLES

As samples are taken, place them directly in moisture-proof airtight

containers to avoid moisture absorption and aeration of the sample. If the
samples are placed in cans, fill the can completely and immediately seal.
Use moisture-proof multiple-wall paper bags or plastic bags if they are strong
enough to avoid breakage, and if they can be sealed immediately after filling
in such a manner as to eliminate excess air in the sample and avoid moisture
absorption and aeration of the sample. Samples shall be treated as
described in the Preparation of Sample.

PREPARATION OF SAMPLE (PHYSICAL TESTING)

Before testing, pass each sample through an 850-um(No. 20) sieve, or

any other sieve having approximately the same size openings, in order to mix
the sample, break up lumps, and remove foreign material. Discard the
foreign materials and hardened lumps that do not break up on sieving or
brushing. Store the cement in airtight moisture-proof containers to prevent
aeration or absorption of moisture prior to test.
Sampling/Testing Requirements

SAMPLE PREPARATION (CHEMICAL ANALYSIS):

1. Before testing, pass representative portions of each sample through a No.

20 (0.850 mm) sieve, or any other sieve having approximately 20 openings/1
in., in order to mix the sample, break up lumps, and foreign materials.
Discard the foreign materials and hardened lumps that do not break up on
sieving or brushing.

2. By means of a sample splitter or by quartering, the representative sample

shall be reduced to a laboratory sample of at least 50 g. Where the larger
quantities are required for additional determinations such as water-soluble
alkali, chloride, duplicate testing, etc., prepare a sample of at least 100 g.

3. Pass the laboratory sample through a U.S. No. 100 sieve (sieve opening of
0.150 mm). Further grind the sieve residue so that it also passes the No. 100
sieve. Homogenize the entire sample by again passing it through the sieve.

4. Transfer the sample to a clean, dry, glass container with an airtight lid and
further mix the sample thoroughly.

5. Expedite the above procedure so that the sample is exposed to the

atmosphere for a minimum time.
Sampling/Testing Requirements

REQUIREMENTS FOR CEMENT MIXING ROOMS

The temperature of the air in the vicinity of the mixing slab, molds, and
base plates shall be maintained at 23+/-4.0 oC and at a relative humidity of
not less than 50 %.
The temperature of the mixing water used to prepare cement paste and
mortar specimens shall be 23.0 +/- 2.0 oC.

REQUIREMENTS FOR MOIST CABINETS AND MOIST ROOMS

Maintain the atmosphere in the moist cabinet or moist room at a

temperature of 23.0 +/- 2.0 oC and a relative humidity of not less than 95 %.
Maintain atmospheric conditions within a moist cabinet or moist room
such that test specimens in storage are saturated with moisture to the degree
needed to ensure that the exposed surfaces of all specimens in storage both
look moist and feel moist.
Equip all moist cabinets and moist rooms with a temperature recorder.
The use of humidity recording devices is optional.

.
Sampling/Testing Requirements

TEMPERATURE MEASURING DEVICES

Reference Temperature Measuring Device – used to verify the

temperature recorder, must be accurate and readable to 0.05 o C .
A copy of the certificate or report which verifies the accuracy shall be
available in the laboratory.

Temperature Recorder – shall record temperatures every 15 min or

less and shall be accurate and readable to 1 o C . The data from the
recorder shall be evaluated at a minimum once each week.

.
Sampling/Testing Requirements

QUANTITY REPRESENTED :

One ( 1 ) Quality Test for every 2000 bags or

fraction thereof.

TESTING REQUIREMENTS :

At least 10 kg of sample shall be submitted

in an airtight container.
Different Tests on Portland Cement ASTM Standards

Physical Tests

1. Density/Specific Gravity (ASTM C – 188)

2. Fineness by: No. 200 Sieve (ASTM C – 184)

Air Permeability Test (ASTM C – 204)

3. Normal Consistency (ASTM C - 187)

4. Time of Setting by : Vicat Needle (ASTM C – 191)

Gillmore Needle (ASTM C – 266)

5. Autoclave Expansion (ASTM C – 151)

6. Compressive Strength (ASTM C -109)

Different Tests on Portland Cement ASTM Standards

CHEMICAL ANALYSIS OF HYDRAULIC CEMENT

(ASTM C-114)

1. LOSS ON IGNITION (LOI)

2. INSOLUBLE RESIDUE (IR)

3. SULFUR TRIOXIDE (SO3)

4. MAGNESIUM OXIDE (MgO)

Significance of Tests
DENSITY/SPECIFIC GRAVITY :

The test method covers the determination of the

density of hydraulic cement. The density of
hydraulic cement is defined as the mass of a unit
volume of the solids. Its particular usefulness is in
connection with the design and control of concrete
mix. The specific gravity of portland cement is
generally about 3.15. Specific gravity is not an
indication of the quality of the cement. It is used
in calculating mix designs.
Significance of Tests

FINENESS:
The test method covers the determination of the
fineness of hydraulic cement. One of the
important physical properties of cement is its
fineness. Fineness affects the rate of hydration:
the finer the cement, the faster strength
development takes place. The effects of greater
fineness on strength are particularly noticeable
during the first 7 days. Also as fineness increases,
the amount of water required for a constant slump
concrete decreases, to the limits reached by the
higher ranges of fineness in high-early-strength
cement. Greater fineness not only improves the
strength but also watertightness, workability,
appearance and durability of concrete.
Significance of Tests

NORMAL CONSISTENCY:

The test method is intended to be used to determine the

amount of water to prepare hydraulic cement pastes for
testing. It determines the volume of water to be added in
cement paste in order to reduce its in a certain state of
plasticity. If insufficient amount of water is added in the
mix, some particles of cement will not be chemically
changed, if much water is used the excess water may be
trapped in the cement paste, the resulting concrete will be
weaker. The quality of the cement paste is determined by
the proportion of water to cement, too much water prevents
proper setting, too little water prevents complete chemical
combination. At low water-cement ratio, cement pastes
has a consistency of a thick cream (0.25 – 0.35), at high
water cement ratio, the mix become increasingly fluid in its
characteristics.
Significance of Tests

TIME OF SETTING:
The purpose of the test method is to establish whether a
cement complies with a specification limit on setting time.
A method of determining the time occupied in the process
of setting, the time interval in which the cement must
remain in plastic state. Setting time is an important
characteristics of cement which must be regulated. It is
necessary for concrete to remain plastic long enough for
finishing operations to be carried out. A knowledge of the
time of setting is of value since crystallization begins with
the initial set and molding and placing of mortar should be
complete before the cement begins to set. In practical
circumstances, the length of time that a concrete mixture
will remain plastic is usually more dependent on the
amount of mixing water used and the atmospheric
temperature than on the setting time of the cement.
Significance of Tests

INITIAL SET :

The time which elapses before the paste ceases to be

fluid and plastic. Interval between the gauging and
partial of plasticity.

FINAL SET:

The time required for the paste to harden to a certain

degree. The time required for the gauged cement to
acquire sufficient firmness to resist a certain definite
pressure.
Significance of Tests

FALSE SET :

Grab Set, Premature Stiffening, Hesitation Set, is the rapid

development of rigidity (hardness) in a mixed cement
paste, mortar or concrete without the evolution of much
heat which rigidity can be dispelled and plasticity regained
by further mixing without the addition of water.

QUICK OR FLASH SET:

The rapid development of rigidity in a mixed cement paste,

mortar or concrete, usually with the evolution of
considerable heat, which rigidity cannot be dispelled nor
can the plasticity be regained by further addition of water.
Significance of Tests

AUTOCLAVE EXPANSION:

The test method covers the determination of the

autoclave expansion of Portland cement by means of
a test on a neat cement specimen. This method of
test is for determining the soundness of Portland
cement, soundness is a physical property tested by
determining the ability of a hardened cement paste to
retain its volume after setting. Lack of soundness or a
delayed destructive expansion is caused by too much
hard-burned free lime or magnesia in the cement.
Autoclave expansion test provided an index of
potential delayed expansion caused by the hydration
of CaO and MgO or both.
Significance of Tests

AIR CONTENT:

Air content of freshly mixed mortar is the

volume of air (or other gas) voids in a freshly
mixed cement mortar, usually expressed as
a percentage of total volume of the mortar.
The purpose of the test method is to
determine whether or not the hydraulic
cement under test meets the air-entraining
or non-air-entraining requirements of the
applicable hydraulic cement specification for
which the test is being made.
Significance of Tests

COMPRESSIVE STRENGTH:

The test method provides a means of determining the

compressive strength of hydraulic cement and other
mortars and result may be used to determine
compliance with specification. Compressive strength
is the maximum load sustained by standard specimen
when subjected to a crushing force. The ability of
cement to develop compressive strength in a concrete
mixture is one of its most important characteristics.
Strength tests at various ages indicate the strength-
producing characteristics of cement but should not be
used to try to predict strengths accurately because of
the great number of variable that may occur in a
number of concrete mixtures.
Factors that Affects the Strength of Cement
1. Grading of the sand or aggregate

2. Proportion of water used

3. Degree of mixing

4. Temperature and humidity of the atmosphere in which

it is conducted

5. Method in which the materials is placed in the moulds

and the specimen made

6. Curing condition

7. Methods of testing and the age at which tests are

carried out
Chemical Analysis of Portland Cement

MAJOR COMPONENTS :
SiO2 (Silicon Dioxide)
Al2O3 (Aluminum Oxide)
Fe2O3 (Ferric Oxide)
CaO (Calcium Oxide)
MgO (Magnesium Oxide)
SO3 (Sulfur Trioxide)
Loss on Ignition

MINOR COMPONENTS :
Na2O (Sodium Oxide)
K2O (Potassium Oxide)
TiO2 (Titanium Dioxide)
P2O5 (Phosphorus Pentoxide)
ZnO (Zinc Oxide)
Mn2O3 (Manganic Oxide)
Sulfide Sulfur

SEPARATE DETERMINATIONS:
Insoluble residue
Chloroform-soluble organic substances
Free calcium oxide
Water-soluble alkali
LOSS ON IGNITION (LOI) : A test carried out on Portland
cement to determine how much weight a sample will lose
when heated to 900 to 10000C. It determines the
freshness of cement and the moisture content
accumulated and present in the cement cause by free
hydration and carbonation of cement.

INSOLUBLE RESIDUE (IR) : To determine the acid-

insoluble materials (inert) present in cement.

SULFUR TRIOXIDE (SO3) : Oxide form from Gypsum

(CaSO4.2H2O), it affects the strength and setting time of
cement.

MAGNESIUM OXIDE (MgO) : It causes unsoundness

(volume change) on cement.
SPECIFICATIONS:

ASTM C 150 (AASHTO M 85) : Standard

Specification for Portland Cement

ASTM C 595 (AASHTO M 240):

Standard Specification for Blended
Hydraulic Cement
ASTM C151

Standard Test Method for

Autoclave Expansion of Hydraulic
Cement
Significance and Use
The autoclave expansion test provides an index of
potential delayed expansion caused by the hydration of
CaO (Calcium Oxide) or MgO (Magnesium Oxide) , or
both, when present in hydraulic cement.

This method of test is for determining the soundness

of Portland cement. Soundness is a physical property
tested by determining the ability of a hardened cement
paste to retain its volume after setting
Specification Requirement

- 0.8 % max. (-Shrink or +Expand)

Apparatus/Equipment
Molds
- conforming to the requirements of Practice C490 for test specimens
used in the determination of length change of cement paste.

Gauge Length = 250 mm

Moist Cabinet or Room

- conforming to the
requirements of Specification
C511

Temperature : 23.0 ± 2.0°C

Relative Humidity : not less than 95%
Length Comparator

- The comparator used for

measuring length change of
specimens shall conform to
the requirements of Practice
C490.
Autoclave Machine
consisting of a high-pressure steam
vessel provided with a thermometer
well. The autoclave shall be equipped
with automatic controls and either a
rupture disk with a bursting pressure
of 2.4 MPa [350 psi] ± 5 % or a
safety valve that actuates at this
pressure. In addition, the autoclave
shall be equipped with a vent valve
to allow the escape of air during the
early part of the heating period and
to release any steam pressure
remaining at the end of the cooling
period.
Sample Worksheet

DPWH-QMSF-43 Rev00 Worksheet on Physical Test of Cement-Normal

Consitency,Time of Setting, Autoclave Expansion.docx
Reporting of Results

Report as percent of effective gauge length to the

nearest 0.01 %.
Computation of Autoclave Expansion

AUTOCLAVE EXPANSION :

La - Length comparator reading of specimen before

Autoclaving, mm ----------------
Lb - Length comparator reading of specimen after
Autoclaving, mm ----------------
G - Gauge length, mm ----------------- 250
Lb - La
Autoclave Expansion, % = x 100 =
G
Sample Computation
The comparator reading before and after autoclaving are 3.861
mm and 4.867, respectively, compute for the autoclave
expansion.
AUTOCLAVE EXPANSION :

La - Length comparator reading of specimen before

Autoclaving, mm ---------------- 3.861
Lb - Length comparator reading of specimen after
Autoclaving, mm ---------------- 4.867
G - Gauge length, mm ----------------- 250
Lb - La
Autoclave Expansion, % = x 100 = + (0.40%)
G
Sample Computation
The comparator reading before and after autoclaving are 1.023
mm and 0.821, respectively, compute for the autoclave
expansion.
AUTOCLAVE EXPANSION :

La - Length comparator reading of specimen before

Autoclaving, mm ---------------- 1.023
Lb - Length comparator reading of specimen after
Autoclaving, mm ---------------- 0.821
G - Gauge length, mm ----------------- 250
Lb - La
Autoclave Expansion, % = x 100 = - (0.08%)
G
COMPREHENSIVE TRAINING ON
MATERIALS TESTING TECHNOLOGY
MODULE II- SAMPLING AND TESTING CEMENT AND CONCRETE MIX
(PHYSICAL TEST OF CEMENT)
Different Tests on Portland Cement ASTM Standards

Physical Tests

1. Density/Specific Gravity (ASTM C – 188)

2. Fineness by: No. 200 Sieve (ASTM C – 184)

Air Permeability Test (ASTM C – 204)

3. Normal Consistency (ASTM C - 187)

4. Time of Setting by : Vicat Needle (ASTM C – 191)

5. Autoclave Expansion (ASTM C – 151)

6. Compressive Strength (ASTM C – 109)

7. Air Content (ASTM C – 185)

Different Tests on Portland Cement ASTM Standards

CHEMICAL ANALYSIS OF HYDRAULIC CEMENT

(ASTM C-114)

1. LOSS ON IGNITION (LOI)

2. INSOLUBLE RESIDUE (IR)

3. SULFUR TRIOXIDE (SO3)

4. MAGNESIUM OXIDE (MgO)

ASTM C187-16
Standard Test Method for Amount of
Water Required for Normal Consistency
of Hydraulic Cement Paste
Significance and Use

This test method is intended to be used to determine

the amount of water required to prepare hydraulic
cement pastes with normal consistency, as required
for Time of Setting and Autoclave Expansions Tests.
Requirements:

25% - 35% Normal Consistency

Consistency Determination - 10 ± 1 mm Penetration

Apparatus/Equipment
Reference Masses
and Devices for
Determining Mass

-conforming to the
requirements of
Specification C1005
Glass Graduates

- 200 or 250-mL
capacity, and
conforming to the
requirements of
Specification C1005
Vicat Apparatus
The Vicat apparatus shall consist of a frame A
bearing a movable rod B, weighing 300 g, one
end C, the plunger end, being 10 mm in diameter
for a distance of at least 50 mm, and the other
end having a removable needle D, 1 mm in
diameter and 50 mm in length. The rod B is
reversible, and can be held in any desired position
by a set screw E, and has an adjustable indicator
F, which moves over a scale (graduated in
millimetres) attached to the frame A. The paste is
held in a rigid conical ring G, resting on a plane
nonabsorptive square base plate H, about 100
mm on each side. The rod B shall be made of
stainless steel and shall be straight with the
plunger end which is perpendicular to the rod
axis. The ring shall be made of a
noncorroding, nonabsorbent material, and
shall have an inside diameter of 70 mm at the
base and 60 mm at the top, and a height of
40 mm.
Mixer, Bowl, and
Paddle

- shall conform to the

apparatus section of
Practice C305

Slow Speed: 140±5rpm

Medium Speed: 285±10rpm
Flat Trowel

- having a sharpened
straight-edged steel
blade 100 to 150 mm
in length
Procedures:
I. Preparation of Cement Paste
Step 1: Prepare the Apparatus and Sample.
Cement: 650g
Water: ? ; try 25% - 35% Normal Consistency (trial and error)
Step 2: Place all the mixing water in the bowl.
Step 3: Add cement to the bowl for 30 Seconds for the absorption of the water.
Step 4: Start the mixer at slow speed for 30 Seconds.
Step 5: Stop the mixer 15 Seconds during this time scrape down into the batch any
paste that may have collected on the side of the bowl.
Step 6: Start the mixer at medium speed for 60 Seconds.
Sample Worksheet

DPWH-QMSF-43 Rev00 Worksheet on Physical Test of Cement-Normal

Consitency,Time of Setting, Autoclave Expansion.docx
Reporting of Results
Calculate the amount of water required for
normal consistency as the mass of water divided
by the mass of dry cement, expressed as a
percentage. Calculate the mass ratio to the
nearest 0.1 % and report the mass ratio to the
nearest 0.5 %.
Computation of Normal Consistency