Cement Testing PDF

Short Notes of Cement Chemistry
NARENDRA KUMAR KANCHKAR

Quality Controller(Cement)
nk.kanchkar@gmail.com
Cement History:
Joseph Aspdin took out a patent in 1824 for "Portland Cement," a material he produced
by firing finely-ground clay and limestone until the limestone was calcined. He called it Portland
Cement because the concrete made from it looked like Portland stone, a widely-used building
stone in England.
In 1845, Isaac Johnson made the first modern Portland Cement by firing a mixture of
chalk and clay at much higher temperatures, similar to those used today. At these temperatures
(1400C-1500C), clinkering occurs and minerals form which are very reactive and more strongly
cementitious.
-Development of rotary kilns
- Addition of gypsum to control setting
- Use of ball mills to grind clinker and raw materials
Rotary kilns gradually replaced the original vertical shaft kilns used for making lime from
the 1890s. Rotary kilns heat the clinker mainly by radiative heat transfer and this is more
efficient at higher temperatures, enabling higher burning temperatures to be achieved. Also,
because the clinker is constantly moving within the kiln, a fairly uniform clinkering temperature
is achieved in the hottest part of the kiln, the burning zone.
The two other principal technical developments, gypsum addition to control setting and
the use of ball mills to grind the clinker, were also introduced at around the end of the 19th
century.
In india first cement plant installation at Porbandar (Gujrat) in 1914
Cement Definition:
Cement is a binder, a substance that sets and hardens independently, and can bind
other materials together such as sand, bricks (civil material).
Cement is defined as a hydraulic binder which when mixed with water forms a paste
which sets and hardens by mass of hydration reaction and processes and which after hardening,
retains its strength and hardening even under water,
Cement used in construction is characterized as hydraulic or non-hydraulic. Hydraulic
cements (Portland cement) harden because of hydration chemical reactions that occur
independently of the mixture's water content; they can harden even underwater or when
constantly exposed to wet weather. The chemical reaction that results when the anhydrous
cement powder is mixed with water produces hydrates that are not water-soluble.
Material made by heating a mixture of limestone and clay in a kiln at about 1450 C, then
grinding to a fine powder with a small addition of gypsum.
Combination of C3A, C3S, C2S, C4AF and mix gypsum in few quantity is called cement.
Cement Manufacturing Technologies:
Wet Process
Dry Suspension (SP) Process
Dry Pre calciner (PC) Process (Present time use)
Wet Process: These plant are characterized by low technology, low capacity, high man power and
high energy consumption.the maximum capacity of the wet process plant operating in India is only
300 TPD.
Dry Suspension (SP) Process: In SP plant, the ground raw meal is feed to a four stage Pre-heater
system.the hot air coming out of kiln is used for pre heating the could feed entering the system.
The material as it comes out of pre heater enters the kiln partial calcined (about 40%) at a
temperature of 800OC. the kiln is used only for carrying out the remaining calcinations and sintering.
The cooling of clinker is done in the cooler and cooler air is used back in the kiln for combustion.
Generally ball mill used for grinding limestone.
Dry Pre Calciner (PC) Process:the dry Pre-calciner plant is advancement over the dry SP plant.
An additional vessel called the Precalciner is provided. The ground raw meal after getting preheated
in the pre heater system (6 stage pre-heater) enters the calciner. The fuel is partly (extant of 60%)
fired in the calciner. The additional heated is used for completing the calcinations reaction before
the material enters the kiln. the kiln is used only for carrying out the sintering reaction. Generally
VRM and roll press used for grinding limestone.
6 stage pre-heater:
S.No.
Cyclone name
Temperature
(Approx)
Getting sample loss
Degree ofcalcinations
1.
2.
3.
4.
5.
6.
1F& 2F
1E& 2E
1D & 2D
1C & 2C
1B & 2B
1A & 2A
280-332OC
370-420OC
540-600OC
630-710OC
770-850OC
857-890OC
30-33 %
25-30 %
20-25 %
15-20 %
10-15 %
2-5 %
10 %
23 %
40 %
55 %
24 %
90-95 %
4 Zone occurs in kiln: -1.Dehydration Zone(1100OC) 2. Calcinations Zone(1250OC)3. Clinkersition Zone

(1400OC) 4. Cooling Zone.(1000OC)
2
*Examples of raw materials for portland cement manufacture.

Calcium
Silicon
Aluminum
Iron
Coal
Limestone
Clay
Clay/Bauxite
Clay
Anthracite
Marl
Marl
Shale
Iron ore
Bituminous
Calcite
Sand
Fly ash
Mill scale
Lignite
Aragonite
Shale
Aluminium ore refuse Shale
Pith
Shale
Fly ash
Blast furnace dust Pet Cock
Sea Shells
Rice hull ash
Cement kiln dust
Slag
*Summary of the different ways to represent some cement minerals and products.
Chemical Name
Chemical Formula Oxide Formula
Cement
Notation
Mineral
Name
Tricalcium Silicate
Dicalcium Silicate
Tricalcium Aluminate
Tetracalcium
Aluminoferrite
Calcium hydroxide
Calcium sulfate dihydrate
Ca3SiO5
Ca2SiO4
Ca3Al2O6
Ca2AlFeO5
3CaO.SiO2
2CaO.SiO2
3CaO.Al2O3
4CaO.Al2O3.Fe2O3
C3S
C2S
C3A
C4AF
Alite
Belite
Aluminate
Ferrite
Ca(OH)2
CaSO4.2H2O
CaO.H2O
CaO.SO3.2H2O
CH
Portlandite
Gypsum
Calcium oxide
CaO
CaO
C
C
H2
Lime
Reaction Occurring in Pre heater to kiln:

1.
2.
3.
4.
5.
6.
7.
Evaporation of free water

Release of combine water from clay
Dissociation of magnesium carbonate
Dissociation of Calcium carbonate
Dissociation of lime and clay
Commencement of liquid formation
Further formation of liquid and completion
Of clinker compound
- 100oC
- 500oC
- 900oC
- above900oC
- 900oC-1200oC
- 1200oC-1280oC
- above1280oC
Phase of Clinker formation:

It is know that fuel economy or improved burn ability in the formation of clinker can be effected
through the following stage of clinker burning.
:- 800oC
:-900oC
:-1000oC
= Formation of 2CaO.Fe2O3
= Formation of 2CaO.Fe2O3.CaO.Fe2O3
= Formation of 2CaO.SiO2+2CaO.Al2O3
SiO2+Ferrite Phase
= Formation of 2CaO.SiO2, 5CaO.3(Al2O3)
5CaO.Al2O3, 3CaO.SiO2, Ferrite Phase
= Formation of 2CaO.SiO2, 3CaO.SiO2
:-1100oC
:-1200oC
3
12CaO.7Al2O3, SiO2+2CaO.Fe2O3, 3CaO.SiO2,

= Formation of 3CaO.Al2O3, 3CaO.SiO2
2CaO.SiO2 + Ferrite Phase
= Formation of 3CaO.Al2O3, 3CaO.SiO2
2CaO.SiO2+ Ferrite Phase
:-1300oC
:-1400oC
Effects of Various Factors on Raw mix Burnability:

Characteristic
/Modulus
Limiting
range
Preferable
range
Silica modulus
(SM)
1.9-3.2
2.3-2.7
Alumina
modulus (AM)
1.5-2.5
1.3-1.6
Lime
saturation
factor (LSF)
0.661.02
0.92-0.96
Free silica
0-3
As low as
possible
MgO
0-5
0-3
Alkalies
0-1
0.2-0.3%
Sulphur
compound
0-4
0.5-2%
Fluorides
0-0.6
0.030.08%
Chlorides
0.06
Up to
0.015%
Effects
If SM High
Result in hard burning, high fuel consumption,
difficulty in coating formation, radiation from shell
is high, deteriorates the kiln lining
If AM High
Impacts harder burning, high fuel consumption,
Increases C3A decreases C4AF, reduces liquid phase
& kiln output, if AM is too low and raw mix is
without free silica, clinker sticking and balling is too
high.
A higher LSF
Make it difficult to burn raw mix, increases C3S,
reduces C2S, deteriorates refractory lining, increases
radiation from shell, increases kiln exit gas
temperature.
A higher silica
Increases fuel and power consumption, causes
difficulty in coating formation, deteriorates
refractory, increases radiation of heat kiln shell,
A higher MgO
Favours dissociation of C2S and CaO and lets C3S
form quickly, tends the balling easy in the burning
zone and affects kiln operation.
A high alkali
Improves burnability at lower temperature &
deteriorates at higher, increase liquid content and
coating formation, lowers the solubility of CaO in
melt, breaks down alite & belite phases, creates
operational problem due to external & internal cycle.
A higher Sulphur compound
Acts as an effective mineraliser and modifier of
alkali cycle by forming less volatiles,
A higher fluorides
Leads to modify the kinetic of all burning reaction ,
lowers the temperature of C3S formation by 150-200
A higher chlorides
Higher Cl forms more volatiles % causes operational
problem due to its complete volatilization in burning
zone, increases liquid formation & melting point of
the absorbed phase is drastically change.
4
Phase data for a Type I OPC paste made with a w/c of 0.45.
Phase
C3S
C2S
C3A
C4AF
Gypsum (CH2)
C-S-H (solid)a
C-S-H (with gel pores)b
Portlandite (CH)
Ettringite (AFt)
Monosulfoaluminate (AFm)
Water
Gel porosity
Capillary porosity
Density (g/cm )
3.15
3.28
3.03
3.73
2.32
2.65
1.90
2.24
1.78
2.02
1.00
---
Volume %
At Mixing
Mature Paste
23.40
7.35
4.42
2.87
3.47
0
0
0
0
0
58.49
0
58.49
1.17
0.78
0.00
1.39
0.00
29.03
49.99
13.96
6.87
15.12
31.69
20.96
10.73
Bulk Density:(RAW & FINAL PRODUCT)

Cilnker = 1360 Kg/M3,Gypsum = 1.38 Mt/M3, Iron = 2700 Kg/M3,Lime stone = 1400 Kg/M3
Fly ash = 550 Kg/M3,Coal = 850 Kg/M3, Sand = 1600 Kg/M3,Cock = 480-640 Kg/M3,
Cement = 1500 Kg/M3,Raw meal = 1250 Kg/M3,
Properties of the major cement minerals:

About 90-95% of a Portland cement is comprised of the four main cement minerals, which are C3S,
C2S, C3A, and C4AF, with the remainder consisting of calcium sulfate, alkali sulfates, unreacted
(free) CaO, MgO, and other minor constituents left over from the clinkering and grinding steps. The
four cement minerals play very different roles in the hydration process that converts the dry cement
into hardened cement paste. The C3S and the C2S contribute virtually all of the beneficial properties
by generating the main hydration product, C-S-H gel. However, the C3S hydrates much more quickly
than the C2S and thus is responsible for the early strength development. The C3A and C4AF minerals
also hydrate, but the products that are formed contribute little to the properties of the cement paste.
As was discussed in the previous section, these minerals are present because pure calcium silicate
cements would be virtually impossible to produce economically.
The crystal structures of the cement minerals are quite complex, and since these structures do not
play an important role in the properties of cement paste and concrete we will only present the most
important features here. More detailed information can be found in the book by Taylor. The
hydration reactions of the cement minerals are covered in Section5.3.
Tricalcium Silicate (C3S)
C3S is the most abundant mineral in Portland cement, occupying 4070 wt% of the cement, and it is
also the most important. The hydration of C3S gives cement pastes most of its strength, particularly at
early times.
Pure C3S can form with three different crystal structures. At temperatures below 980C the
equilibrium structure is triclinic. At temperatures between 980C 1070C the structure is
monoclinic, and above 1070C it is rhombohedral. In addition, the triclinic and monoclinic structures
each have three polymorphs, so there are a total of seven possible structures. However, all of these
structures are rather similar and there are no significant differences in the reactivity. The most
important feature of the structure is an awkward and asymmetric packing of the calcium and oxygen
5
ions that leaves large holes in the crystal lattice. Essentially, the ions do not fit together very well,
causing the crystal structure to have a high internal energy. As a result, C3S is highly reactive.
The C3S that forms in a cement clinker contains about 3-4% of oxides other than CaO and SiO2.
Strictly speaking, this mineral should therefore be called alite rather than C3S. However, as discussed
in Section 3.2, we will avoid using mineral names in this monograph. In a typical clinker the C3S
would contain about 1 wt% each of MgO, Al2O3, and Fe2O3, along with much smaller amounts of
Na2O, K2O, P2O5, and SO3.These amounts can vary considerably with the composition of the raw
materials used to make the cement, however. Of the three major impurities, Mg and Fe replace Ca,
while Al replaces Si.
One effect of the impurities is to stabilize the monoclinic structure, meaning that the structural
transformation from monoclinic to triclinic that would normally occur on cooling is prevented. Most
cements thus contain one of the monoclinic polymorphs of C3S.
There exist seven known polymorphs between room temperature and 1070 oC: three triclinic (denoted
with T), three monoclinic (M) and one rhombohedral (R) polymorph. Due to incorporations in the alite
crystal lattice, M1 and M3 polymorphs are present mostly in industrial clinker. Cooling clinker from
1450oC, inversion of the R polymorph to M3 and further more to M1 occurs, forming small crystals (M3)
rich in substituents or large crystals, poor in substituted ions (M1). Especially, high MgO- concentrations
promote high nucleation, resulting in formation of small automorphic M3- crystals.The different
polymorphs do not show significant differences in the hydraulic properties.
Dicalcium Silicate (C2S)

As with C3S, C2S can form with a variety of different structures. There is a high temperature
structure with three polymorphs, a structure in that is in equilibrium at intermediate temperatures,
and a low temperature structure. An important aspect of C2S is that -C2S has a very stable crystal
structure that is completely uncreative in water. Fortunately, the structure is easily stabilized by the
other oxide components of the clinker and thus the form is never present in portland cement. The
crystal structure of C2S is irregular, but considerably less so than that of C3S, and this accounts for
the lower reactivity of C2S. The C2S in cement contains slightly higher levels of impurities than C3S.
According to Taylor, the overall substitution of oxides is 4-6%, with significant amounts of Al2O3,
Fe2O3, and K2O.
The second largest clinker phase in Portland cement is belite. Its hydration product develops similar
strength in cement as alite, only much more slowly. Belite makes up between 15 and 30 wt.% of
Portland cement clinker and consists of 60-65 wt.% CaO, 29-35 wt.% SiO2 and 4-6 wt.% substituted
oxides, mainly Al2O3 and Fe2O3, but also K2O, Na2O, MgO, SO3 and P2O5.7 Belite crystallizes in
five polymorphs: -belite, H-belite, L-belite, -belite (H = high and L = low symmetry) and
-belite (Fig. 2-7), which differ in structural and hydraulic properties. The - polymorphs are the
most hydraulic forms of belite, whereas -belite is a non-hydraulic polymorph and does not account
for the setting and hardening of cement. -belite is also a hydraulic polymorph, but less hydraulic
than the - polymorphs. It is the most common polymorph in industrial Portland cement clinker. A
phenomenon, that needs to be prevented by trace compounds inclusions, is disintegration (dusting) of
clinker, which happens if -C2S is not stabilized during cooling and/or by inclusions affording a part
--C2S inversion. -C2S crystals are less dense (more voluminous) than -C2S crystals, which
causes cracking of other -C2S crystals, forming a voluminous powder and dust
Tricalcium Aluminate (C3A)

Tricalcium aluminate (C3A) comprises anywhere from zero to 14% of a portland cement. Like C3S, it
is highly reactive, releasing a significant amount of exothermic heat during the early hydration
period. Unfortunately, the hydration products of formed from C3A contribute little to the strength or
other engineering properties of cement paste. In certain environmental conditions (i.e., the presence
of sulfate ions), C3A and its products can actually harm the concrete by participating in expansive
reactions that lead to stress and cracking.
Pure C3A forms only with a cubic crystal structure. The structure is characterized by Ca+2 atoms and
rings of six AlO4 tetrahedra. As with C3S, the bonds are distorted from their equilibrium positions,
leading to a high internal energy and thus a high reactivity. Significant amounts of CaO and the
Al2O3 in the C3A structure can be replaced by other oxides, and at high levels of substitution this can
lead to other crystal structures. The C3A in portland cement clinker, which typically contains about
13% oxide substitution, is primarily cubic, with smaller amounts of orthorhombic C3A. The C3A and
C4AF minerals form by simultaneous precipitation as the liquid phase formed during the clinkering
process cools, and thus they are closely intermixed. This makes it difficult to ascertain the exact
compositions of the two phases. The cubic form generally contains ~4% substitution of SiO2, ~5%
substitution of Fe2O3, and about 1% each of Na2O, K2O, and MgO. The orthorhombic form has
similar levels, but with a greater (~5%) substitution of K2O.
Tetracalcium Aluminoferrite (C4AF)
A stable compound with any composition between C2A and C2F can be formed, and the cement
mineral termed C4AF is an approximation that simply the represents the midpoint of this
compositional series. The crystal structure is complex, and is believed to be related to that of the
mineral perovskite. The actual composition of C4AF in cement clinker is generally higher in
aluminum than in iron, and there is considerable substitution of SiO2 and MgO. Taylor. reports a
typical composition (in normal chemical notation) to be Ca2AlFe0.6Mg0.2Si0.15Ti0.5O5. However, the
composition will vary somewhat depending on the overall composition of the cement clinker.
*Set up and solve a system of four equations and four unknowns to find the mineral
composition of the cement.
Once the total amount of C, S, A, and F residing in the cement minerals has been calculated by
adjusting the total oxide composition of the cement or clinker (steps 1 and 2) and the ratio of the
oxides within each of the main cement minerals has been estimated (step 3), a system of four
equations in four unknowns can be set up and solved for the amount (in wt%) of each cement
mineral. Using the cement oxide composition for proficiency cement #135 given in Table 3.4 and the
mineral oxide compositions given in Table 3.5 results in the following set of equations:
0.716C3S + 0.635C2S + 0.566C3A + 0.475C4AF = 62.52 (C)
0.252C3S + 0.315C2S + 0.037C3A + 0.036C4AF = 21.34 (S)
0.010C3S + 0.021C2S + 0.313C3A + 0.219C4AF = 4.40 (A)
0.007C3S + 0.009C2S + 0.051C3A + 0.214C4AF = 3.07 (F)
a
Formula =1.7C-S-4H. b Formula =1.7C-S-1.6H.
Rate of Clinker Phase on Properties of Cement:

C3A
C3S
C2S
C4AF
Rapid
Quick
Slow
Setting time
Rapid
Fast
Slow
Rapid
Hydration
High-1day
High-14 day
Low
Early strength
Less
High
Late strength
207
120
62
100
Heat of
Hydration(cal/g)
Poor
Moderate
High
High
Resistance to
Chemical attack
low
Dying Shrinkage
Alite C3S
= Responsible for early Strength.
Belite C2S
= Give ultimate (late) Strength along with alite.
Aluminate C3A
= Contributes to early strength, Help faster setting, Liberates more heat in
concrete
= Not contribution to Strength, Requited to reduce the burning Temperature
C4AF
for clinkerisationMostly occurs as a glassy interstitial phase.
Specification of Various Type of Cement:

TYPE OF
CEMENT
LOI
MgO
5%Mx
6%Mx
5%
Mx
6%Mx
4%Mx
6%Mx
Low heat
cement
Rapid
hardening
Sulphate
Resisting
Masonary
Cement
Hydrophobic
cement
Super
sulphate
White cement
5%
Mx
6%Mx
6%Mx
5%
Mx
6%Mx
6%Mx
5%
Mx
6%Mx
10%M
x
6%Mx
PSC
5%
Mx
5%
Mx
33 G
43 G
53 G
PPC
8%Mx
6%Mx
IR
4%
Mx
3%
Mx
3%
Mx
4%
Mx
4%
Mx
4%
Mx
4%
Mx
4%
Mx
2%
Mx
5%
Mx
FORM
ULA
SO3
Finenes
s
2
(M /Kg)
3%Mx
>225
3%Mx
>225
3%Mx
>225
3%Mx
>320
3%Mx
>325
2.5%
Mx
>225
3%Mx
15%Mx
in 45M
3%Mx
Soundnes
s
LechateAuto
Clave
10mm0.8%
10mm0.8%
10mm0.8%
10mm0.8%
10mm0.8%
10mm0.8%
Setting
Time
IST- FST
Compressive
Strength
3 7 28
2
Days(N/mm )
30-600
16
22
33
30-600
23
33
43
30-600
27
37
53
60-600
10
16
35
30-600
27
30-600
10
16
33
10mm -1%
90m-24H
>350
10mm0.8%
30-600
16
22
31
1.5%
Mx
>400
5mm - ---
30-600
15
22
30
>225
30-600
15
20
30
3%Mx
>225
30-600
16
22
33
3%Mx
>300
30-600
16
22
33
Special Test:PPC Drying Shrinkage 0.15%max,
10mm0.8%
10mm0.8%
10mm0.8%
Important Formula Use in Cement Analysis.

Hydraulic Modulus: HM =
Silica Ratio:
Alumina Ratio:
Or Iron Modulus
SM =
AM =
CaO
SiO2 + Al2O3 +Fe2O3
(Typical Range: 1.7 to 2.3)
SiO2
Al2O3 +Fe2O3
Al2O3
Fe2O3
Lime saturation Factor: (For OPC Cement)

LSF =
CaO- 0.7 SO3
2.8 SiO2 + 1.2Al2O3 +0.65Fe2O3
Lime saturation Factor :( Lime stone)

LSF =
CaO X 100
2.8 SiO2 + 1.2Al2O3 +0.65Fe2O3
(Typical Range: 95 to 110)
Lime saturation Factor: (if Alumina modulus >0.64) LSF =

CaO
2.8 SiO2 + 1.65Al2O3 +0.35Fe2O3
Lime saturation Factor: (if Alumina modulus <0.64)

LSF =
CaO
2.8 SiO2 + 1.1Al2O3 +0.7Fe2O3
Bogus formula for Clinker Constituent

(if Alumina modulus >0.64)
C3S = 4.071 CaO (7.602 SiO2+ 6.718 Al2O3 +1.43Fe2O3+2.8SO3)Note: CaO = CaO - F/CaO
C2S = 2.867 SiO2 - 0.7544 C3S
C3A = 2.65 Al2O3 - 1.692 Fe2O3
C4AF = 3.043 Fe2O3
C3S = Tri Calcium Silicate. (Molecular weight = 228 g/g mol)
C2S = Di Calcium Silicate. (Molecular weight = 172 g/g mol)
C3A = Tri Calcium Aluminate. (Molecular weight =270 g/g mol)
C4AF = Tetra Calcium Aluminate Ferate. (Molecular weight = 486 g/g mol)
(if Alumina modulus <0.64)
C3S = 4.071 CaO (7.602 SiO2 + 4.479 Al2O3 +2.86Fe2O3)
C2S = 2.867 SiO2 - 0.7544 C3S
C3 A = 0
C4AF+ C2F =2.1 Al2O3 +1.702Fe2O3
Note: CaO = CaO - F/CaO
Bogus formula for Cement Constituent

(if Alumina modulus >0.64)
Note: CaO = CaO - F/CaO
C3S = 4.071 CaO (7.602 SiO2+ 6.718 Al2O3 +1.43Fe2O3+2.85 SO3)
C2S = 2.867 SiO2 - 0.7544 C3S
C3A = 2.65 Al2O3 - 1.692 Fe2O3
C4AF = 3.043 Fe2O3
9
Bogus Factor :as per duda book

C4AF = C4AF/ Fe2O3 = 486/160=3.043,
C3A = C3A / Al2O3 = 270/102= 2.65, C3A/ Fe2O3 = 270/160= 1.69,
C2S = C2S /SiO2= 172/60=2.87,C2S /C3S= 172/228=0.75,
C3S = C3S/ CaO = 228/56= 4.07,
LSF =
Liquid Value:
LV= 1.13C3A +1.35C4AF + MgO +Alkalies
Burnability Index:
BI =
C3 S
C4AF + C3A
Burnability Factor:
BF = LSF + 10 SM 3(MgO + Alkalies)
Coal Analysis:
NCV = 8455 114 (M% + Ash %) Cal/gm
UHV = 8900 138 (M % + Ash %) Cal/gm
GCV = PC X 86.5 (60*M %)
PC = 100- (1.1*Ash + M %)
CV = % C*8000 + % H*32000
100
100
Coal Consumption: =
Coal feed X 100

Clinker Production
Ash absorption:
% of ash in fuel X coal consumption

100
Raw meal to clinker factor: =
Specific Heat:
V=
100-ash absorption
100-LOI
NCV X % of coal Consumption

100
Insoluble Residue:
IR (max %) = X+4 (100-X)
100
Blain :
Blain = Time X Factor
Factor = STD Blain
Time
(Note: X= % of Fly ash)
10
CYCLONE LOSS:
100(KF loss Cyclone loss)

(100 Cyclone loss) X KF loss
=
Clinker to cement factor:
X 100
Clink.+Flyash/Slag+additives(kg)
Clinker consumed (kg)
Chemical Composition (General):

LOI
SiO2
Al2O3
Fe2O3
CaO
MgO
PPC
5.0
31.0
4.5
3.5
43.0
5.0
Clinker
0.5
21-22
5-6
3-5
62-65
3-6
Limestone
34
12
2.4
1.6
43.0
3.8
Iron Ore
10
13
14
71
1.5
16
14
34
5mx
50-60
20-33
2-7
2-10
Na2O
SO3
+K2O
F/
CaO
1.4
.5-1.0
.2-1.0
.5-2
.5
42
5 Mx
1.5mx
2.75mx
C3S
C2S
C3A
C4AF
48
28
12
Letrite
Gypsum
Mni Gyps
Fly ash
Physical Analysis of PPC:

TEST- Residue (sieve), Blain, Normal consistence, Setting time, Compressive strength,
Soundness-(AC&LC)
Blain (IS -4031 part-2) = 300 M2/kg minimum
NC/SC
Setting time
Strength
Auto clave
Le-chate
Part-4
270C 20C
Part-5
270C 20C
Part-6
270C 20C
Part-3
270C 20C
Part-3
270C 20C
65% 5,
Not less than
90%
300/400 gm
65% 5,
Not
less than 90%
65% 5,
Not less than 90%
300/400 gm
65% 5,
Not less than
90%
100 gm
Req.waterX100
sample weight
Vicat
apparatus
NC*0.85*S.Wt
100
Vicat apparatus
200gm-cm,
600gm-1s+2s+3s
(NC+3) *800
4
100
Vibrating & CSTm
65% 5,
Not less than
90%
300/400 gm
=NC
NC*0.78*S.wt
100
Water Bath
100oC
Expend Time
As possible
vicat Reading
5-7 cm
As possible
vicat Reading 57 cm
Other
Use needle
10mm
60-70mm
Use needle
2&5mm
60-70mm
Initial 30 min
minimum
Final-600 min
maximum
IS- 4031
Lab
Tempture
Lab/Chamber
R-Humidity
Sample
weight
Water
Requirement
Apparatus
Cube size
IS
Requirement
72 1hour- 16mpa
168 2hour-22mpa
672 4hour- 33mpa
(MPa=N/Kg*0.2032)
Gauging
1min dry, 4 min wet
70mm
3 day- 16mpa
7 day- 22mpa
28 day- 33mpa
11
AC machine
2150C,
21 kg/cm2
RH-C-24hour
ACM-3 Hour
Gauging
5 min
25,250mm
0.8 % max
WB-24hour
H.WB-3 Hour
35mm
10 mm max
FLY ASH Analysis (IS-1727)

TEST- BLAIN (Minimum 320),Lime Reactivity(min. 4.5 MPa), Dry Shrinkage (max .15), Comparative
Strength (Not less than 80%)
Lab Temp.
/RH
Test
Specimen
Lime Reactivity
Dry Shrinkage
Comparative Strength
27OC 2 / 65% 5
27OC 2 / 65% 5
27OC 2 / 65% 5
50mm
25/250mm
50mm
0.2N :0.8 :3
Pozz : Ce
1: 2M: 9
H. Lime: Pozz: Sand
150:300M:1350gm
Require
Sample
Require
Water (Table
Flow)
Age of
Testing
ment : Sand
60N:240:900gm
70 5% with 10
drop in 06 Second
100-115% with 25
drop in 15 Second
105 5% with 25
drop in 15 Second
10 Day
35 Day
7,28,90 Day
3,7,28, Day
24 hour RH chamber
(272OC&>90%)
24 hour RH
chamber
(27OC&>90%)
24 hour RH chamber
(272OC&>90%)
6day water tank-I
(272OC
28day Environment
Chamber
(272OC& 50%)-II
2day RH chamber
(272OC&>90%)
Testing
Condition
0.2N :0.8 :3
Pozz : Cement : Sand
100N:400:1500gm
0.8 :3
Cement : Sand
400:1500gm
8day Environment
Cmb.
(502OC&>90%)
Dry shrinkage= II-I

M=Specific gravity of Pozz.
Specific gravity of H. lime
N=Specific gravity of Pozz.

Specific gravity of cement
7,28,90day water
tank
(272OC)
28 dya not less than
80% to blank
strength
N=Specific gravity of Pozz.
7,28,90day
water tank
(272OC)
Blank Strength
Specific gravity of cement
STI (Scheme of testing & inspection)

Form-1:FORMAT FOR MAINTENANCE OF TEST RECORDS WEIGHMENT CONTROL AT PACKING STAGE (Clause 6.2)
Date
Shift
No. Of Bag
Net mass of bags from nozzles No.1, No. 2,
Remark
Form-2:RAW MATERIAL TESTING (CL.7 of STI)

Date of receipt of
material
Date of testing
Name of the
Material
Source of supply and

consignment No.
Details of analysis for

Specified requirements
Form-3:PRODUCTION DATA (POST GRINDING DETAILS OF PRODUCTION ACCEPTED & REJECTEDFOR ISI MARK)
Shift
Quantity
Passed for ISI Marking
Rejected
Remarks
Form-4-A:POZZOLANA (One sample per week) Column 6 of Table 1A (A) Calcined clay pozzolana
Date
Fitness
Lime Reactivity
CompressiveStrength at 28 Days
Drying ShrinkageMax
Form-4-B :FLY ASH POZZOLANA (See Column 6 of Table 1 A)

SO2+A1203
SiO2
MgO
SO3
Na2O
LOI
Fineness
12
Lime
Compressive
Drying
Soundness
+Fe203
sulphur
reactivity
Strength
Shrikage
Auto clave
Form-5:CLINKER (DAILY COMPOSITE SAMPLE) (See Column 6 of Table 1A)

Laboratory Ball-Mill Testing is required to be done when there is change in the source of Raw Material or change in design
Date of
Total
Insoluble SiO2
CaO AlO
FeO
SO MgO LSFLime Alunin
Sample
Disposa
manuacture loss of
Residue
Saturation a
Pass/Fails l/
Ignition
Factor
Factor
Action
-6-A:CLINKER GROUND WITH GYPSUM (Daily composite sample) (Note under Column 6 of Table 1 A)
Date of
Grinding
Fineness
Soundness
Setting time
Compressive Strength
AC
IST
3day-
LC
- FST
7day-
Sample
Pass//fail
28day
Disposal/Actio
n taken if sample
fails
Form-6-B:CLINKER GROUND WITH GYPSUM & POZZOLANA (Column 6 of Table I A)

Date of
Grinding
Fineness
Soundness
Setting time
Compressive Strength
AC
IST
3day-
LC
- FST
7day-
28day
Dry
shrinkage
(Weekly)
Sample
Pass/fail
Disposal/Ac
tio
Form-7: PORTLAND POZZOLANA CEMENT GRINDING/ BLENDING (Daily/Weekly Composite sample) (Column 5 of Table 1B)
Date of
Grinding
Loss on
Ignition
MgO
Insoluble
Material
SO3
Fineness
Soundness
Le-ch
Auto
Clave
Setting
Time
IST
/FST
Compressive
Strength
3 7 28
days
Drying
Shrinkage
(Weekly)
Sample
Pass/Fail
Acti
on
take
Form-8:PORTLAND POZZOLANA CEMENT CRINDING (For Alternate hourly Samples) (Column 5 of Table 1B)
Date of
Grinding
Time at
Fineness
Setting Time
(IST)-(FST)
Sample
fail/pass
Mode of disposal/Action
taken if sample fails
Form-9:PORTLAND POZZOLANA CEMENT PACKING STAGE (Daily/Weekly Composite Samples) (Column 6 of Table 1B)
Date
of
Pcking
Loss
On
Igniti
on
MgO
Insoluble
Materia
SO3
Chloride
Content
(Weekly
Fine
ness
Soundness
Le Auto
Ch Clav
Setting
time
ISTFST
Compressive
Strength
3
7
28
days
Drying
Shrinkage
(Weekly)
Sample
Pass
/Fail
Mode of
disposal/Ac
tion taken if
sample fails
Form-10:(See Clause 3 of STI)

S.No.
Date Calibration
Result of Calibration (Test records indicating

details of standard values and observed values for
each equipment to be kept in proforma for which
various columns be devised; as required)
Name of Equipment
Action taken if equipment
found
defective
Sl. No. (If any)

Remarks
FREQUENCY OF CALIBRATION:
Blaines apparatus- Daily with licensee sown Standard cement sampleand once in a month with standard
cement samples supplied by NCCBM.
Compressive strength -Once in a month with licensees own proving ring and the proving ring shall be calibrated once
Testing machine
in two years from the recognized calibrating agency like NPL/NABL accredited Lab or
Proving ring manufacturer having NPL certified calibrator.
Apply Load
5,10,15,20
Reading-1
R-2
R-3
Average
True Load
Error %
1+2+3/ 3
=app. load*avg. load

/Std. difference
=true.Load-app.Load)*100
/applied load
Std.
Differ.
Autoclave pressure gauge - Once in a six months either by licensees own dead weight Pressure gauge or from
Approved independent agency /NABL accredited Lab or manufacturer of such
gauge having NPL certified calibrator.(dead weight Pressure gauge in 4year)
13
Vibration machine - Once in a month by licensees own tachometer. The tachometer shall be calibrated once
in three Years from approved out Side agency /NABL accredited Lab having NPL
certified calibrator. (12000 400 RPM)
Chemical analysis
Type of analysis: 1 Gravimetric- IR, SO3, SiO2, R2O3 (Residual Oxide/3rd group)
2 Volumetric- CaO, MgO (Fe2O3, Al2O3)
3 Spectroscopy 1.Flame Photo metter-K2O, Na2O (Uncoloured element)
2. UV-Spectro metter TiO2, P2O5, MnO2, (Coloured & miner)
4 X-ray Method
Solution Prepare:
Normality:
Equivalent weight
Volume in letter.
(Equivalent weight = In acid from:-
In Basic from:-
Molaritiey:
Molecular weight
Removal H+ ion
Molecular weight
Removal OH- ion
Gram mole number

Volume in letter.
(1000ppm=1gm chemical dissolved in 1000ml or1 Litter)

(1ppm= 1gm chemical dissolved in 100000ml or 1000 Litter)
Soiled chemical to solution (formula) = ENV
1000
(E=equivalent weight, N= Require Normality, V= Require volume)
Liquid chemical to solution formula =
Density =
Mass
Volume
N1V1 =N2V2
Important Molecular weight.

O-16,
Na-23,
Mg-24,
Al-27, Si-28, S-32, Cl-34,
CaCO3 =100,
SiO2=60,
Al2O3=102,
C3S=228,
C2S= 172,
C3A= 270,
Fe2O3 =160,
C4AF= 486,
14
K-39, Ca-40, Fe-55.8,

MgO= 40,
Na2O= 62,
CaSO4.2H2O =145
Zn-65.39
K2O = 94
Lime Stone- TC&MC

Take 50 ml HCL (0.4N)
in conical Flask
Add 1.0 gm lime stone

sample
Solution use:
= NaOH (0.2N)
40(Mwt)*0.2(N)*1000(ml)/1000= 8gm/L
= HCL(0.4N)
36.46(Mwt)*100/35.4(Purity)=87.28ml/L-1N
=87.28ml/L-1N* 0.4 (Req.N)=34.91 ml/L
= Indicator dissolved in Alcohol
Boil minimum 2min
Add IndicatorPhynopthleen C20H14O4

Mwt-318.33,pH-8.2-9.8
Cool
Titrate with NaOH
(0.2N) slow titration
End point white to
pink colour
Take NaOH Burette

reading
TC = 100-Burette reading
Add excess10/20ml
NaOH (0.2N)
Boil about 1min.
Add IndicatorThymopthleen
Calculation:
CC
= TC MC
CaO = CC / 1.786
MgO = MC / 2.09
Cool
Titrate with HCL (0.4N)
Fast titration
End point purple
to white- pink
Take HCL Burette

reading
MC = [Ex.NaOH-{2*HCL-BR}] X0.84
Q.1 why multiply 1.786 for CaO? = CaO/CaCo3

Q.2 why multiply 2.09 for MgO? = MgO/MgCo3
Q.3 why multiply 0.84 for MC?
15
Cement- IR & SO3

1.0 gm cement sample
Dissolved 1:1 HCL
For Acid
reaction
Solution use:
= 2N- Na2CO3= 10.6 gm sodium carbonate
dissolved in 100 ml distilled water
(Eq.wt = 53, Mwt 105.99 g/mol)
= 1:1 HCL = 50 ml HCL dissolved in 50 ml
Distil water.(Mwt 36.46 g/mol)
= BaCl2 = 10 gm BaCl2 dissolved in 100 ml
distilled water.
Heat below boils

Temp. 15 minute
Filter- 40 N. paper
Wash Hot water
Filtrate
Residue
Boil + add hot BaCl2

10 ml
React with Na2CO3 -30

ml
For Base
reaction
Slowly Cool for ppt

form (4 hour)
Heat 10 minute below

boil temp.
Filter- 40 N. paper
For Alkali
remove
Filter 42 N paper
Wash with 1:99 HCl &

Hot water
Wash Hot water
Dryad in Oven
Dryad in Oven
Ignited at 1000oC
Minimum 30 min
Ignited at 1000oC
Weight
Weight IR
Weight X 34.3 = SO3
IR=
Final weight-Initial weight
Q.1 what is IR?
Material which is not reacts (dissolved) with Acid and basis.
Q.2 why multiply 34.3 for SO3?
Because So3 is found in BaSO4 Form
= (SO3/BaSO4)*100 = (80/137+32+64)*100 = (80/233)100 =0.3433*100 = 34.33
IR (max %) =
X+4 (100-X)
(Note: X= % of Fly ash)
100
=methyl Orange use checking for alkali removes.
16
Clinker, Cement & Raw material (SiO2, R2O3)

All Raw materials & Cement
Clinker Sample
0.5 gm sample + Fusion mix.

In Platinum crucible
0.5 gm sample in beaker

Add NH4Cl 2-3gm (mix well)
Fuse 1000oC for 1 hour
Add Con. HCL- 5ml,

Bake on Hot plate & cool it
Add HCL (1:1), 20-30 ml
Add HCL (1:1), 10-20 ml

+Distilled water + Heat
Wash Crucible with H2O

add NH4Cl + Bake on Hot
plate & cool it
Filter with 40N paper
Add HCL (1:1), 20-30 ml

+Heat
Isolate
R2O3
Oxidizing
agent
Filtrate
Heat it +Add NH4Cl 2-3gm
Residue
Wash with hot Distilled water

Dry (oven) + Ignite at 1000oC
Boil it + Add HNO3 (1:1), 0.5ml

SiO2= (F wt I wt)*200
Add NH4OH (1:1)
ppt
form
2 drop H2SO4 + 2 drop H2O

Add 20 ml HF
Filtrate in 500ml
flask
Put on Hot plate & dry
Residue
Dry (oven) + Ignite at 1000oC
CaO & MgO Process

next page
Use Solution:
NH4OH(1:1)
250 ml NH3 + 250 ml H2O
HNO3 (1:1)Fusion mix.= (Na2CO3+K2CO3)
SiO2= (F wt I wt)*200
R2O3= (F wt I wt)*200
Reaction:
= M SiO3 + 2HCl
M Cl2 + H2SiO3
= H2SiO3+ Evaporation
SiO2 +(H2O)
= SiO2 + Impu. + 4HF
SiF4 +2H2O
H2SiO3 + 2H2 SiF6
= (FeCl3 + AlCl3) + 3NH4OH
{Fe(OH)3 + Al(OH)3} + 3NH4Cl
={Fe(OH)3 + Al(OH)3} + Ignition
Fe2O3 + Al2O3
17
Clinker, Cement & Raw material (CaO, MgO)-EDTA method

After filtrate R2O3 solution make up 500 ml
For-CaO
For- MgO
Take 20 ml aliquot solution
Take 20 ml aliquot solution
Add Tri ethanol amine (TEA)

5 ml (For Isolation), C6H15NO3,
Mwt-149.19 g/m
Add Tri ethanol amine (TEA)

5 ml (For Isolation), C6H15NO3,
Mwt-149.19 g/m
Add Glycerol 5 ml
(For Isolation), C3H8O3,
Mwt-92.10 g/m
Add Eriochrome black T (EBT)

Indicator, C20H2N3NaO7S
Mwt-461.38 g/m
Add Patton & Reader (P&R)

Indicator, C21H14N2O7S
Mwt-438.42 g/m
Add 10-20 ml Buffer Solution

(For pH-10)
Mwt-000 g/m
Add 10-20 ml Sodium (4.0N)

Hydroxide NaOH (For pH-12)
Mwt-40 g/m
Titrate with EDTA

(ethylene di amine tetra
acetate) Mwt-372.34 g/m
(end colour red- pink to blue)
Titrate with EDTA

(ethylene di amine tetra
acetate) Mwt-372.34 g/m
(end colour red- pink to purple)
{0.05608 X mol. EDTA(0.01)X V1 X Vmu X100} D.F.
Volume taken X Sample weight
= V1- EDTA Burette reading
= Vmu- Volume make up
= Difference Factor - as per EDTA standard
{0.04032 X mol. EDTA(0.01)X (V2- V1)X Vmu X 100} D.F.

= V2- Cao titration BR
= DF as per EDTA standard
Solution Use:
= Buffer solution- 70 gm NH4Cl dissolved in 570
ml NH4OH.
= 4.0N NaOH- 160 gm dissolved in 1000 ml H2O.
=EDTA- 3.7224 gm dissolved in H2O 100 ml and
make up 1000 ml solution.
= Zn solution (0.01N)-0.6537 gm diss. In 0.1N HCL
Reaction:
= Ca2++ EDTA.2Na+
Di Sodium Salt
E.D.T.A STANDARDISATION (Difference Factor)

= 10 ml Zn sol (0.1N).+ EBT +Buffer sol. Titrate
with EDTA (end colour pink to blue)
M1V1=M2V2, M2=0.01 X 10ml /B.R.
18
2Na++ EDTA.Ca2+
Ferric Oxide (Fe2O3) Testing by EDTA method in Cement (In OPC)

Make the solution to 250 ml in a standard volumetric
flask after removal of silica. Measure 25 ml of acid
solution of the sample through pipette in a flask. Add
very dilute ammonium hydroxide (1:6)
1:6) till turbidity
appears.
clear the turbidity with a minimum amount of dilute

hydrochloric acid(1:10) and a few drops in excess to
adjust the pH 1 to 1.5. Shake well.
Add 100 mg of sulphosalicylic acid and titrate with

0.01M EDTA solution carefully to a colouress or pale
yellow solution.
CALCULATION:
CALCULATION:1 ml of 0.01M EDTA = 0.7985 mg Fe2O3
Fe2O3(%) = 0.07985 X V X M X 250 X 100
W X 25
Where,V= volume of EDTA used and
W= weight of sample
M = Molarity of EDTA
19
Alumina (Al2O3) Testing by EDTA method in Cement

After testing of Fe2O3 add 15 ml of standard
EDTA to the same flask add 1ml H3PO4(1:3)
and 5 ml of H2SO4(1:3) and one drop of thymol
blue into a flask
add ammonium acetate solution by stirring until

the colour changes from red to yellow add 25 ml
of ammonium acetate in excess to attain a pH of
5.5 -6.0
Heat the solution to boiling for one minute and

then cool.Add 0.5 mg solid xylenol orange
indicator and bismuth nitrate solution slowly with
constant stirring.
Add 2-3
3 ml of bismuth nitrate solution in excess.
Titrate with EDTA to a sharp yellow endpoint
CALCULATION:1 ml of 0.01M EDTA = 0.5098 mg Al2O3
Al2O3(%) = 0.05098 X V1 X M X 250 X 100

W X 25
V1= V2-V3-(V4
(V4 X factor of Bi(NO3)3
Where,V1= volume of EDTA for alumina
V2 = total volume of EDTA used in titration
V3 = volume of EDTA used for iron
V4 = total volume of bismuth nitrate solution
used in the titration.
W= weight of sample
M = Molarity of EDTA
20
RapidCaoof Clinker/PPCby KMnO4 method (ASTM)

PPC Cement
0.2 gm sample + Fusion mix.
In Platinum crucible
Fuse 1000oC for 1 hour
Clinker Sample /OPC

0.2 gm sample + Add 1:1 Hcl
Just Boil+ Continue in Hot Plate

Add methyl Orange- few
drop
Add HCL (1:1), 20-30 ml

Wash Crucible with H2O
Add NH4OH (1:1)

until Colour yellow
Just Boil
Add lump sum 0.2 gm
OXALIC Acid (until Colour
lightly pink)
Add 20ml hot Ammonium
Oxalate (50%) (White)
Filter with 40 No. Paper

Wash with hot water
Take Residue in beaker
Add H2SO4 (1:1)
Titrate with KMnO4

(0.01772 N)
B.R. X 0.5 X Factor / Sample
wt.
KMnO4 STANDARDISATION
*5.6 gm KMnO4 dissolved in
1000ml H2O for 0.1772N
Solution.
*0.67 gm OXALIC Acid + H2O+
1:1 H2So4 titrate with KMno4.
Factor = 56/BR
21
Aliquot
solution
OUT
Fast CaO
Take 0.5gm sample
Add 1:1 Hcl (20 ml Approx)
Just Boil
Filter With 41 No Paper in 500 ml round bottom
flask& make up 500 ml
Cool & shake well
Take 20 ml aliquot sample in Conical Flask
Add approx 5 ml glycerol

Add Approx 1 ml TEA
Add NaOH ( 2 pellet)
Wine Red Color
Sky Blue
Add P&R Indicator 0.05gm (Approx)

Titrate With 0.01N EDTA
(until No Color Change)
Calculate
{0.05608 X mol. EDTA(0.01)X V1 X Vmu X100} D.F.

= Difference Factor - as per EDTA standard
OR
BR X 2.804 = CaO%
(For 20 ml Volume taken)
22
Filter
Out
Iron (Raw material) -Dichromate method:(ASTM)

0.5 gm sample + Fusion mix. In
Platinum crucible
Fuse in 1000oC minimum 30 min
Cool and wash Pt. crucible with

1:1 HCl
Wash crucible with Distilled
water
Clinker sample
0.5 gm clinker sample dissolved
in HCl -1:1
Boil & add SnCl2 Drop wise till

colourless solution
Completely cool (Room Temp.)
Add Barium di phenol Salfonate

(BDS) Indicator
K2Cr2O7calibration to FAS
= take 20 ml H2O + 0.5 gm FAS +

Acid mixture +BDS Ind. + titrate with
Potassium dichromate
Add 5-10 ml HgCl2 and Acid

mixture Masking agent
Titrate with K2Cr2O7Potassium
dichromate
Factor= 20/BR
Iron= B.R X Factor (K2Cr2O7)
Solution Preparation:
=Acid mix.- 15% H2SO4+ 15%H3PO4 +70% H2O
=K2Cr2O7(N/16) 3.07 gm dissolved in 1000ml
H2O
=BDS 1gm dissolved in 100 ml dil. HCL (10%)
=SnCl2 5 gm dissolved in 100 ml dil. HCL (10%)
=Fusion mix Na2CO3+K2CO3
= HgCl2- 56 gm dissolved in 1000ml H2O
Reaction:
= 2Fe3+ + Sn2+
= 2Fe2+ + K2Cr2O7
23
2Fe2+ + Sn4+
2Fe3+
Free Lime Test:(Clinker)
Take 1 gm Clinker sample in

beaker
= 1 Glycerol : 5 Ethanol
Add 10 ml Ethylene Glycol

Put for 45 min in water bath
Residue out
Filtrate
Add Bromocrsol Grate Green
Indicator
Titrate with 0.1N HCL
Reaction:
Ca(OH)2 + 2HCl
CaCl2 + H2O
Factor= CaO / 2 HCL
End Colour Green to golden

Yellow
F/CaO= B.R X 0.28 (HCL Factor)
= Normality of HCL =. Purity *1000*Specific Gravity / 100 * Equivalent wt

= Normality of HCL =. (36 * 1000 * 1.18)/100*36.5 = 11.64 N.(N1)
= So 0.1N HCL=N1V1 = N2V2, =11.64*V2 = 0.1*1000, =V2= 0.1*1000/11.64 = 8.59ml
24
Cloride Test (Cl):-0.1% max
Take 1 gm sample in beaker
Dissolved 1:3 HNO3

Filter 41N paper in Conical
Take aliquot sample
Add 10 ml AgNO3 (0.1N)
Residue out
Add 2ml Nitro Benzene

Add 4 Drop Ferric Indicator
NH4.Fe (SO4)2.12H2O
Titrate with Ammonia thyo
saynte (.01N) NH4SCN
End Colour white to
0.3546 X 100 X (10-BR)

Sample weight
25
Reaction:
M Cl2 + 2 HNO3
M(NO3)2+2HCl
HCl + AgNO3
AgCl + HNO3
AgNO3 + NH4SCN
AgSCN + NH4NO3
Alkali Test (Na2O+K2O):-( PPC=0.8% max)

Take 0.25 gm sample in
Platinum crucible
10 ml HF and backing
Add 2ml HNO3
Blank Solution: 2.5 ml HNO3 + 2.5 ml
Alumina sulphate + 250 ml H2O.
Standard Solution:
NaCl: 1.885 NaCl Dissolved In 1000ml
H2O (for 1000ppm).
KCl: 1.583 KCl Dissolved In 1000ml H2O
(for 1000ppm).
Add 10 ml HClO4
(Per Choleric acid)
Put Hot plate & up to Syrupy

Extract dissolved to 1:1 HNO3
in bicker
Filter 41N paper in 250 ml
Volumetric Flack
Make up 250 ml with H2O
Volume makeup X 100 X ppm reading

Sample weight X 106
*Pre heater Coating sample in (about) Na2O= 1-2% & K2O=12-16%.
26
Residue out
Reactiv Silica Test: (Fly ash) (IS-3812)

Take 0.5 gm sample in beaker
Add 50 ml HCl (1:1)

Boil and Cool
Add 16 gm KOH
4 hour Put on Hot plate &
Volume maintain 60 ml by
H2O
Filter 40N Paper
Residue out
Aliquot Solution bake

Dissolved with 1:1 HCl + Heat
Filter 40N paper

Residue dry in oven
Residue Ignite 1000OC
RS= Initial Wt. Final Wt.
*200
27
Sulpher Test: (Coal), ESCHKA Method (IS 1350-P3)

Take 0.1 gm sample platinum
crucible
Add 1-2 gm ESCHKA mixture
= 0.1374 = S /BaSO4
= ESCHKA mixture = (2:1) Mgo+ Na2CO3
(Light Calcined magnesia oxide
+Anhydrous Sodium carbonate)
Fuse at 800OC
Dissolved to 1:1 HCl
Filter 41N paper
Residue out
Aliquot Solution Boil
Add 20 ml BaCl2
Cool
Filter 42N Paper
Residue Ignite at 900OC
Ash X 0.1374 X100
Coal Grading: Coal is the combination of Organic (Carbon) and Inorganic (Si02, R2O3 etc) material. It is use for
heating purpose.
Grade
A
B
C
D
E
F
G
Un-grade
Type of Coal:
A+M %
UHV cal/g
<19.5
>6200
19.5-24.0
6200-5600
24.0-28.7
5600-4940
28.7-34.1
4940-4200
34.1-40.2
4200-3360
40.2-47.1
3360-2400
47.1-55.1
2400-1300
>55.1
<1300
1. Anthracite 2.Buteminus 3. Lignite 4. Pith
28
Indian Standard ReferenceUse in Cement Chemistry

Cement
IS 269:1989 Specification for ordinary Portland cement, 33 grade
IS 455:1989- Specification for Portland slag cement
IS 1489(Part 1):1991 Specification for Portland pozzolana cement Part 1 Flyash based
IS 1489(Part 2):1991 Specification for Portland-pozzolana cement: Part 2 Calcined clay based
IS 3466:1988 Specification for masonry cement
IS 6452:1989- Specification for high alumina cement for structural use.
IS 6909:1990 Specification for super sulphated cement
IS 8041:1990 Specification for rapid hardening Portland cement
IS 8042:1989 Specification for white Portland cement
IS 8043:1991 Specification for hydrophobic Portland cement
IS 8112:1989 Specification for 43 grade ordinary Portland (43-S)
IS 8229:1986 Specification for oil-well cement.
IS 12269:1987 Specification for 53 grade ordinary Portland
IS 12269:535 Specification for TRS-T40 grade ordinary Portland
IS 12330:1988 Specification for sulphate resisting Portland
IS 12600:1989 Specification for low heat Portland cement
Instrument use in cement analysis

IS 12803:1989 Methods of analysis of hydraulic cement by X-ray fluorescence spectrometer.
IS 12813:1989 Method of analysis of hydraulic cement by atomic absorption spectrophotometer
Apparatus use in cement analysis

IS 5512:1983 Specification for flow table for use in tests of hydraulic cements and pozzolanic
materials
IS 5513:1996 Specification for vicat apparatus.
IS 5514:1996 Specification for apparatus used in Le-Chatelier test
IS 5515:1983 Specification for compaction factor apparatus
IS 5516:1996 Specification for variable flow type air-permeability apparatus (Blaine type)
IS 14345:1996 Specification for autoclave apparatus
Physical & Chemical Analysis of Cement

IS 4031(Part 1):1996 Methods of physical tests for hydraulic cement: Part 1 Determination of
fineness by dry sieving
fineness by specific surface by Blaine air permeability method
soundness
consistency of standard cement paste
IS 4031(Part 5):1988 Methods of physical tests for hydraulic cement: Part 5 Determination of initial
and final setting times
compressive strength of hydraulic cement (other than masonry cement)
compressive strength of masonry cement
transverse and compressive strength of plastic mortar using prism
IS 4031(Part 9):1988 Methods of physical tests for hydraulic cement: Part 9 Determination of heat of
hydration
drying shrinkage
29
density
IS 4031(Part 12):1988 Methods of physical tests for hydraulic cement: Part 12 Determination of air
content of hydraulic cement mortar
IS 4031(Part 13):1988 Methods of physical tests for hydraulic cement: Part 13 Measurement of
water retentively of masonry cement
false set
IS 4031(Part 15):1991 Methods of physical test for hydraulic cement: Part 15 Determination of
fineness by wet sieving
IS 4032:1985 Method of chemical analysis of hydraulic cement
IS 3535:1986 Methods of sampling hydraulic cement
IS 12423:1988 Method for colorimetric analysis of hydraulic
IS 4845:1968 Definitions and terminology relating to hydraulic cement.
IS 5305:1969 Methods of test for P2O5.
Pozzolana material
IS 1727:1967 Methods of test for pozzolana materials.
IS 12870:1989 Methods of sampling calcined clay pozzolana.
IS 3812(Part 1):2003 Specification for pulverized fuel ash Part 1 For use as pozzolana in cement,
cement mortar and concrete
IS 3812(Part 2):2003 Specification for pulverized fuel ash Part 2 For use as admixture in cement
mortar and concrete
IS 6491:1972 Method of sampling fly ash
IS 12089:1987 Specification for granulated slag for manufacture of Portland slag cement.
Coal
IS 1350:1984 (Part-I) Methods of test Proximate analysis
IS 1350:1970 (Part-II) Methods of test Calorific value.
IS 1350:1969 (Part-III) Methods of test Sulphur analysis
IS 1350:1974 (Part-IV) Methods of test Ultimate analysis.
IS 1350:1979 (Part-V) Methods of test Special Impurity.
Lime stone
IS 1760:1991 (Part- I to V) Methods of Chemical Analysis of Limestone.
IS 1760 (Part 3):1992 Methods of chemical analysis of limestone, dolomite and alliedmaterials:
Part 3 Determination of iron oxide, alumina, calcium oxideand magnesia
Gypsum
IS 1288:1982 Methods of test mineral gypsum.
IS 1289:1960 Methods of sampling mineral gypsum
IS 1290:1982 Mineral gypsum.
Bag
IS11652:1986 High density polyethylene (HDPE) woven sacks for packing cement
IS 11653:1986 Polypropylene (PP) woven sacks for packing cement
IS 12154:1987 Methods of Light weight jute bags for packing cement
IS 12174:1987 Jute synthetic union bags for packing cement
IS 2580:1995 Methods of Jute sacking bags for packing cement
Sand and Other

IS 169:1966Specification for atmospheric condition for testing. (for Physical Test)
IS 397:2003 Statistical Quality Control.
IS 460:1962Specification for test sieves.
IS 650:1991 Specification for standard sand for testing of cement.
IS 456:2000 Code of practice plain and reinforced concrete
30
IS 712:1964 Hydrated Limes.

IS No.
IS- 4032
IS- 4031-P1
IS- 4031-P2
Important Point
*The difference between check determinations by EDTA method

shall not exceed 0.2 percent for calcium oxide and magnesia, 0.15, 0.2 percent for
silicaand alumina, and 0.1 percent for other constituents.
*The maximum acceptable difference in the percentage of each alkali
Between the lowest and highest value obtained shall be 0.04.
* Check the sieve after every 100 sieving
* EXPRESSION OF RESULTS
Report the value of R, to the nearest 0. I percent, as the residue on the 90 pm
sieve for the cement tested.
The standard deviation of the repeatability is about 0.2 percent and of the
reproducibility is about 0.3 percent.
The cement bed volume and the apparatus constant shall be recalibrated with
the reference cement: a) after 1 000 tests, b) In the case of using:-another type of
manometer fluid, another type of filter paper, anda new manometer tube; and c)
at systematic deviations of the secondaryreference cement.
IS- 4031-P3
IS- 4031-P4
IS- 4031-P5
31
Bag Testing:
Mass
75
Leng
th
74
Widt
h
48
Stitc
hes
14
Ends
40
Picks
40
(Gms
)
(Cm)
(Cm)
Per
Dm
Per
Dm
Per
Dm
69.0
74.0
48.5
14
39.00
39.0
Effective
valve Size
(10 x 22)
Seepage
of
Cement
(Cm)
MAX-100
(Gms/Ba
g)
Warp
Way
87
Warp
Elongations
%
Weft
Way
87
Weft
Elongations
%
Top/
Bottom
40
55.0
89.1
21.0
86.1
21.0
42.0
11.0
22.50
Strength in KGF
Fabric
Seam
= CaCO3 Maximum = 8.00% + 1.00%
Important Note.
= In PPC Cement Fly ash use not less than 15% and not more than 35%
=In PSC Cement Slag use not less than 25% and not more than 70%
= Endothermic reaction occurs in kiln & Pre heater.
= Exothermic reaction occurs in bomb calorimeter.
= Coal analysis sample size is (pass 212) -212 micron.
= 3.14 density of Portland cement.
= Di butyl thylate use in manometer (Blain apparatus) due to low density &viscosity, non volatile,
non hygroscopic liquid. (Air Permeability test).
= In CST, Cube Breaking Speed 35 N/mm2 or 2.9 Kn/s (only For Cube Size 70.5mm)
= During the calibration of CST/Balance maintain 272 or slandered equipment calibrated
temperature, otherwise use factor K= 0.027% with obtained value.
= Cement Expired as per BIS,in Bag 3 month and in bulk 6 months. (IS-8112)
= purity of gypsum = CaSO4/ SO3 = 172/80 = 2.15(factor)
= 1.6 ton CO2 generate in 1 ton clinker Production.
= 1.8 GJ/t Energy consumed for 1 ton clinker production in 6 stage Pre heater.
= Chromic Acid use forwashing glass ware. (10gm K2Cr2O7 + 200 ml H2SO4)
K2Cr2O7 + 4 H2SO4
K2SO4+ Cr2(SO4)3+4 H2O + 3O
X-ray: =
n= 2d sin
(n= number of wave, = wave length, d= distance two layer, sin= angle of wave)
When bombarding of cathode ray on high melting point metal than reflected ray is called X ray.
= C3S + H2O
CSH + Ca (OH)2 + Fly ash
CSH
References:-(http://iti.northwestern.edu/cement/monograph/Monograph1_4.html)
(http://www.understanding-cement.com/parameters.html)
*Cement_Data_Book_Duda_III edition.
* IS book 1727,3812,4031,4032,1350.
* jaypee cement testing manual.
* Taylor cement chemistry.
Note: writer not responsible for any mistake.
32
Thank you.............
33

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Short Notes of Cement Chemistry

NARENDRA KUMAR KANCHKAR

Cement Manufacturing Technologies:

Getting sample loss

4 Zone occurs in kiln: -1.Dehydration Zone(1100OC) 2. Calcinations Zone(1250OC)3. Clinkersition Zone

*Examples of raw materials for portland cement manufacture.

Rice hull ash

Cement kiln dust

Chemical Formula Oxide Formula

Reaction Occurring in Pre heater to kiln:

Evaporation of free water

Phase of Clinker formation:

12CaO.7Al2O3, SiO2+2CaO.Fe2O3, 3CaO.SiO2,

Effects of Various Factors on Raw mix Burnability:

Bulk Density:(RAW & FINAL PRODUCT)

Properties of the major cement minerals:

Dicalcium Silicate (C2S)

Tricalcium Aluminate (C3A)

Formula =1.7C-S-4H. b Formula =1.7C-S-1.6H.

Rate of Clinker Phase on Properties of Cement:

Specification of Various Type of Cement:

Special Test:PPC Drying Shrinkage 0.15%max,

Important Formula Use in Cement Analysis.

(Typical Range: 1.7 to 2.3)

(Typical Range: 1.8 to 2.7)

(Typical Range: 1.0 to 1.7)

Lime saturation Factor: (For OPC Cement)

(Typical Range: 0.66 to 1.02)

Lime saturation Factor :( Lime stone)

(Typical Range: 95 to 110)

Lime saturation Factor: (if Alumina modulus >0.64) LSF =

(Typical Range: 92 to 108)

Lime saturation Factor: (if Alumina modulus <0.64)

(Typical Range: 92 to 108)

Bogus formula for Clinker Constituent

Note: CaO = CaO - F/CaO

Bogus formula for Cement Constituent

Bogus Factor :as per duda book

Coal feed X 100

% of ash in fuel X coal consumption

Raw meal to clinker factor: =

NCV X % of coal Consumption

(Note: X= % of Fly ash)

100(KF loss Cyclone loss)

Clinker to cement factor:

Chemical Composition (General):

Physical Analysis of PPC:

FLY ASH Analysis (IS-1727)

Dry shrinkage= II-I

N=Specific gravity of Pozz.

Specific gravity of cement

STI (Scheme of testing & inspection)

Net mass of bags from nozzles No.1, No. 2,

Form-2:RAW MATERIAL TESTING (CL.7 of STI)

Source of supply and

Details of analysis for

Passed for ISI Marking

Form-4-B :FLY ASH POZZOLANA (See Column 6 of Table 1 A)

Form-5:CLINKER (DAILY COMPOSITE SAMPLE) (See Column 6 of Table 1A)

Form-6-B:CLINKER GROUND WITH GYPSUM & POZZOLANA (Column 6 of Table I A)

Form-10:(See Clause 3 of STI)

Result of Calibration (Test records indicating