Cement testing

Cement Testing as Per BIS, and Manufacturing process

1. 1

Short Notes of Cement Chemistry
NARENDRA KUMAR KANCHKAR
Quality Controller(Cement)
[email protected]

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 lik e Portland stone, a widely-used building
stone in England.
In 1845, Isaac Johnson made the first modern Portla nd 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 ind ependently, 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 hydrati on 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 rea ction 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.

2. 2

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 800
O
C. 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. 1F& 2F 280-332
O
C 30-33 % 10 %
2. 1E& 2E 370-420
O
C 25-30 % 23 %
3. 1D & 2D 540-600
O
C 20-25 % 40 %
4. 1C & 2C 630-710
O
C 15-20 % 55 %
5. 1B & 2B 770-850
O
C 10-15 % 24 %
6. 1A & 2A 857-890
O
C 2-5 % 90-95 %

4 Zone occurs in kiln: -1.Dehydration Zone(1100
O
C) 2. Calcinations Zone(1250
O
C)3. Clinkersition Zone
(1400
O
C) 4. Cooling Zone.(1000
O
C)

3. 3

*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 FormulaOxide Formula Cement
Notation
Mineral
Name Tricalcium Silicate Ca 3SiO5 3CaO.SiO 2 C 3S Alite
Dicalcium Silicate Ca 2SiO4 2CaO.SiO 2 C 2S Belite
Tricalcium Aluminate Ca 3Al2O6 3CaO.Al 2O3 C 3A Aluminate
Tetracalcium
Aluminoferrite
Ca
2AlFeO5 4CaO.Al 2O3.Fe2O3 C 4AF Ferrite
Calcium hydroxide Ca(OH) 2 CaO.H 2O CH Portlandite
Calcium sulfate dihydrate CaSO4.2H2O CaO.SO 3.2H2O C H
2 Gypsum
Calcium oxide CaO CaO C Lime

Reaction Occurring in Pre heater to kiln:
1. Evaporation of free water - 100
o
C
2. Release of combine water from clay - 500
o
C
3. Dissociation of magnesium carbonate - 900
o
C
4. Dissociation of Calcium carbonate - above900
o
C
5. Dissociation of lime and clay - 900
o
C-1200
o
C
6. Commencement of liquid formation - 1200
o
C-1280
o
C
7. Further formation of liquid and completion - above1280
o
C
Of clinker compound
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.

= Formation of 2CaO.Fe
2O3 :- 800
o
C
= Formation of 2CaO.Fe
2O3.CaO.Fe2O3 :-900
o
C
= Formation of 2CaO.SiO
2+2CaO.Al2O3 :-1000
o
C
SiO2+Ferrite Phase
= Formation of 2CaO.SiO
2, 5CaO.3(Al2O3) :-1100
o
C
5CaO.Al2O
3, 3CaO.SiO2, Ferrite Phase
= Formation of 2CaO.SiO
2, 3CaO.SiO2 :-1200
o
C

4. 4

12CaO.7Al 2O3, SiO2+2CaO.Fe2O3, 3CaO.SiO2,
= Formation of 3CaO.Al
2O3, 3CaO.SiO2 :-1300
o
C
2CaO.SiO
2 + Ferrite Phase
= Formation of 3CaO.Al
2O3, 3CaO.SiO2 :-1400
o
C
2CaO.SiO
2+ Ferrite Phase
Effects of Various Factors on Raw mix Burnability:
Characteristic
/Modulus
Limiting
range
Preferable
range
Effects

Silica modulus
(SM)
1.9-3.2 2.3-2.7
If SM High
Result in hard burning, high fuel consumption,
difficulty in coating formation, radiation from shell
is high, deteriorates the kiln lining
Alumina
modulus (AM)
1.5-2.5 1.3-1.6
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.
Lime
saturation
factor (LSF)
0.66-
1.02
0.92-0.96
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.
Free silica 0-3
As low as
possible
A higher silica
Increases fuel and power consumption, causes
difficulty in coating formation, deteriorates
refractory, increases radiation of heat kiln shell,
MgO 0-5 0-3
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.
Alkalies 0-1 0.2-0.3%
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.
Sulphur
compound
0-4 0.5-2%
A higher Sulphur compound
Acts as an effective mineraliser and modifier of
alkali cycle by forming less volatiles,
Fluorides 0-0.6
0.03-
0.08%
A higher fluorides
Leads to modify the kinetic of all burning reaction ,
lowers the temperature of C3S formation by 150-200
Chlorides 0.06
Up to
0.015%
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.

5. 5

Phase data for a Type I OPC paste made with a w/c of 0.45.


Volume %
Phase Density (g/cm
3
) At Mixing Mature Paste
C3S 3.15 23.40 1.17
C2S 3.28 7.35 0.78
C3A 3.03 4.42 0.00
C4AF 3.73 2.87 1.39
Gypsum (CH2) 2.32 3.47 0.00
C-S-H (solid)
a
2.65 0 29.03
C-S-H (with gel pores)
b
1.90 0 49.99
Portlandite (CH) 2.24 0 13.96
Ettringite (AFt) 1.78 0 6.87
Monosulfoaluminate (AFm) 2.02 0 15.12
Water 1.00 58.49 31.69
Gel porosity -- 0 20.96
Capillary porosity -- 58.49 10.73
Bulk Density:(RAW & FINAL PRODUCT)

Cilnker = 1360 Kg/M
3
,Gypsum = 1.38 Mt/M
3
, Iron = 2700 Kg/M
3
,Lime stone = 1400 Kg/M
3

Fly ash = 550 Kg/M
3
,Coal = 850 Kg/M
3
, Sand = 1600 Kg/M
3
,Cock = 480-640 Kg/M
3
,
Cement = 1500 Kg/M
3
,Raw meal = 1250 Kg/M
3
,
Properties of the major cement minerals:
About 90-95% of a Portland cement is comprised of the four main cement minerals, which are C 3S,
C
2S, 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 C
3S and the C2S contribute virtually all of the beneficial properties
by generating the main hydration product, C-S-H gel. However, the C
3S hydrates much more quickly
than the C
2S and thus is responsible for the early strength development. The C 3A 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 (C
3S)
C
3S is the most abundant mineral in Portland cement, occupying 40–70 wt% of the cement, and it is
also the most important. The hydration of C
3S gives cement pastes most of its strength, particularly at
early times.
Pure C
3S can form with three different crystal structures.6 Vt6 temperatures6 below6 ETwtH6 the6
equilibrium structure is triclinic. At temperatures6 between6 ETwtH6 ?6 UwvwtH6 the6 structure6 is6
monoclinicL6and6above6UwvwtH6it6is6rhombohedralS6[n 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

6. 6

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, C
3S is highly reactive.
The C
3S that forms in a cement clinker contains about 3-4% of oxides other than CaO and SiO 2.
Strictly speaking, this mineral should therefore be called alite rather than C
3S. However, as discussed
in Section 3.2, we will avoid using mineral names in this monograph. In a typical clinker the C
3S
would contain about 1 wt% each of MgO, Al
2O3, and Fe2O3, along with much smaller amounts of
Na
2O, 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 C
3S.

There exist seven known polymorphs between room temperature and 1070
o
C: three triclinic (denoted
with T), three monoclinic (M) and one rhombohedral (R) polymorph. Due to incorporations in the alite
crystal lattice, M
1 and M3 polymorphs are present mostly in industrial clinker. Cooling clinker from
1450
oC, 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 (M
1). Especially, high MgO- concentrations
promote high nucleation, resulting in formation of small automorphic M
3- crystals.The different
polymorphs do not show significant differences in the hydraulic properties.



Dicalcium Silicate (C
2S)
As with C
3S, C2S can form with a variety of different structures. There is a high temperature a
structure with three polymorphs, a b structure in that is in equilibrium at intermediate temperatures,
and a low temperature g structure. An important aspect of C
2S is that g-C 2S has a very stable crystal
structure that is completely uncreative in water. Fortunately, the b structure is easily stabilized by the
other oxide components of the clinker and thus the g form is never present in portland cement. The
crystal structure of b-C
2S is irregular, but considerably less so than that of C 3S, and this accounts for
the lower reactivity of C
2S. The C2S in cement contains slightly higher levels of impurities than C 3S.
According to Taylor, the overall substitution of oxides is 4-6%, with significant amounts of Al
2O3,
Fe
2O3, 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:
α-belite, α’H-belite, α’L-belite, β-belite (H = “high” and L = “low” symmetry) and
γ-belite (Fig. 2-7), which differ in structural and hydraulic properties. The α’- polymorphs are the
most hydraulic forms of belite, whereas
γ-belite is a non-hydraulic polymorph and does not account
for the setting and hardening of cement.
β-belite is also a hydraulic polymorph, but less hydraulic
than the
α’- 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
β-C2S is not stabilized during cooling and/or by inclusions affording a part
β-γ-C2S inversion. γ-C2S crystals are less dense (more voluminous) than β-C2S crystals, which
causes cracking of other
β-C2S crystals, forming a voluminous powder and dust

7. 7

Tricalcium Aluminate (C
3A)
Tricalcium aluminate (C
3A) comprises anywhere from zero to 14% of a portland cement. Like C 3S, it
is highly reactive, releasing a significant amount of exothermic heat during the early hydration
period. Unfortunately, the hydration products of formed from C
3A contribute little to the strength or
other engineering properties of cement paste. In certain environmental conditions (i.e., the presence
of sulfate ions), C
3A and its products can actually harm the concrete by participating in expansive
reactions that lead to stress and cracking.
Pure C
3A forms only with a cubic crystal structure. The structure is characterized by Ca
+2
atoms and
rings of six AlO
4 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
Al
2O3 in the C3A structure can be replaced by other oxides, and at high levels of substitution this can
lead to other crystal structures. The C
3A in portland cement clinker, which typically contains about
13% oxide substitution, is primarily cubic, with smaller amounts of orthorhombic C
3A. The C3A and
C
4AF 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 SiO
2, ~5%
substitution of Fe
2O3, and about 1% each of Na2O, K2O, and MgO. The orthorhombic form has
similar levels, but with a greater (~5%) substitution of K
2O.

Tetracalcium Aluminoferrite (C
4AF)
A stable compound with any composition between C
2A and C2F can be formed, and the cement
mineral termed C
4AF 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 C
4AF in cement clinker is generally higher in
aluminum than in iron, and there is considerable substitution of SiO
2 and MgO. Taylor. reports a
typical composition (in normal chemical notation) to be Ca
2AlFe0.6Mg0.2Si0.15Ti0.5O5. 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:

0.716C
3S + 0.635C 2S + 0.566C 3A + 0.475C 4AF = 62.52 (C)
0.252C
3S + 0.315C 2S + 0.037C 3A + 0.036C 4AF = 21.34 (S)
0.010C
3S + 0.021C 2S + 0.313C 3A + 0.219C 4AF = 4.40 (A)
0.007C
3S + 0.009C 2S + 0.051C 3A + 0.214C 4AF = 3.07 (F)

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

8. 8

Rate of Clinker Phase on Properties of Cement:

C3A C3S C2S C4AF
Setting time Rapid Quick Slow -
Hydration Rapid Fast Slow Rapid
Early strength High-1day High-14 day Low -
Late strength - Less High -
Heat of
Hydration(cal/g)
207 120 62 100
Resistance to
Chemical attack
Poor Moderate High High
Dying Shrinkage - - low -
Alite C3S = Responsible for early Strength.
Belite C
2S = Give ultimate (late) Strength along with alite.
Aluminate C
3A = Contributes to early strength, Help faster setting, Liberates more heat in
concrete
C
4AF = Not contribution to Strength, Requited to reduce the burning Temperature
for clinkerisationMostly occurs as a glassy interstitial phase.

Specification of Various Type of Cement:
TYPE OF
CEMENT
LOI MgO IR SO3
Finenes
s
(M
2
/Kg)
Soundnes
s
Lechate-
Auto
Clave
Setting
Time
IST- FST
Compressive
Strength
3 7 28
Days(N/mm 2
)
33 G

5%Mx 6%Mx
4%
Mx
3%Mx >225
10 mm-
0.8
%
30-600
16 22 33
43 G

5%
Mx
6%Mx

3%
Mx

3%Mx >225
10
mm-
0.8
%
30-600
23 33 43
53 G

4%Mx 6%Mx

3%
Mx

3%Mx >225
10mm-
0.8
%
30-600
27 37 53
Low heat
cement
5%
Mx
6%Mx
4%
Mx
3%Mx >320
10mm-
0.8
%
60-600
10 16 35
Rapid
hardening
-
6%Mx
4%
Mx

3%Mx >325
10mm-
0.8
%
30-600
27 - -
Sulphate
Resisting
5%
Mx
6%Mx
4%
Mx
2.5%
Mx
>225
10mm-
0.8
%
30-600
10 16 33
Masonary
Cement
-
6%Mx
-
3%Mx
15%Mx
in 45M
10mm -1% 90m-24H - 3 5
Hydrophobic
cement
5%
Mx
6%Mx
4%
Mx
3%Mx >350
10mm-
0.8
%
30-600
16 22 31
Super
sulphate
-

10%M
x
4%
Mx
1.5%
Mx
>400 5mm - --- 30-600 15 22 30
White cement

-
6%Mx
2%
Mx
- >225
10mm-
0.8
%
30-600
15 20 30
PSC

5%
Mx
8%Mx
5%
Mx
3%Mx >225
10mm-
0.8
%
30-600
16 22 33
PPC

5%
Mx
6%Mx
FORM
ULA

3%Mx >300
10mm-
0.8
%
30-600
16 22 33 Special Test:PPC –Drying Shrinkage 0.15%max,

9. 9

Important Formula Use in Cement Analysis.
Hydraulic Modulus: HM = CaO
SiO
2 + Al2O3 +Fe2O3 (Typical Range: 1.7 to 2.3)

Silica Ratio: SM = SiO
2
Al
2O3 +Fe2O3 (Typical Range: 1.8 to 2.7)


Alumina Ratio: AM = Al
2O3
Or Iron Modulus Fe
2O3 (Typical Range: 1.0 to 1.7)

Lime saturation Factor: (For OPC Cement)
LSF = CaO- 0.7 SO
3
2.8 SiO2 + 1.2Al2O3 +0.65Fe2O3 (Typical Range: 0.66 to 1.02)

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 (Typical Range: 92 to 108)

Lime saturation Factor: (if Alumina modulus <0.64)
LSF = CaO
2.8 SiO2 + 1.1Al2O3 +0.7Fe2O3 (Typical Range: 92 to 108)
Bogus’ formula for Clinker Constituent
(if Alumina modulus >0.64)

C
3S = 4.071 CaO – (7.602 SiO2+ 6.718 Al2O3 +1.43Fe2O3+2.8SO3)
Note: CaO = CaO - F/CaO
C
2S = 2.867 SiO2 - 0.7544 C3S
C
3A = 2.65 Al2O3 - 1.692 Fe2O3
C4AF = 3.043 Fe2O3
C3S = Tri Calcium Silicate. (Molecular weight = 228 g/g mol)
C
2S = Di Calcium Silicate. (Molecular weight = 172 g/g mol)
C
3A = Tri Calcium Aluminate. (Molecular weight =270 g/g mol)
C
4AF = Tetra Calcium Aluminate Ferate. (Molecular weight = 486 g/g mol)

(if Alumina modulus <0.64)
C
3S = 4.071 CaO – (7.602 SiO2 + 4.479 Al2O3 +2.86Fe2O3) Note: CaO = CaO - F/CaO
C
2S = 2.867 SiO2 - 0.7544 C3S
C
3A = 0
C4AF+ C2F =2.1 Al2O3 +1.702Fe2O3
Bogus’ formula for Cement Constituent
(if Alumina modulus >0.64)
Note: CaO = CaO - F/CaO
C
3S = 4.071 CaO – (7.602 SiO2+ 6.718 Al2O3 +1.43Fe2O3+2.85 SO3)
C
2S = 2.867 SiO2 - 0.7544 C3S
C
3A = 2.65 Al2O3 - 1.692 Fe2O3
C4AF = 3.043 Fe2O3

10. 10
















Liquid Value:
LV= 1.13C
3A +1.35C4AF + MgO +Alkalies

Burnability Index:
BI = C
3S
C
4AF + 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: = 100-ash absorption
100-LOI

Specific Heat: V = NCV X % of coal Consumption
100

Insoluble Residue:
IR (max %) = X+4 (100-X) (Note: X= % of Fly ash)
100
Blain :
Blain = √Time X Factor
Factor = STD Blain

√Time
Bogus Factor :as per duda book
C4AF = C4AF/ Fe2O3 = 486/160=3.043,
C
3A = C3A / Al2O3 = 270/102= 2.65, C 3A/ Fe2O3 = 270/160= 1.69,
C
2S = C2S /SiO2= 172/60=2.87,C2S /C 3S= 172/228=0.75,
C
3S = C3S/ CaO = 228/56= 4.07,


LSF =

11. 11


CYCLONE LOSS: = 100(KF loss – Cyclone loss)
(100 – Cyclone loss) X KF loss

Clinker to cement factor: = Clink.+Flyash/Slag+additives(kg)
Clinker consumed (kg)

Chemical Composition (General):

LOI SiO2 Al2O3 Fe2O3 CaO MgO
Na2O
+K2O
SO3
F /
CaO
C3S C2S C3A C4AF
PPC 5.0 31.0 4.5 3.5 43.0 5.0 1.4 -
Clinker 0.5 21-22 5-6 3-5 62-65 3-6 .5-1.0 .2-1.0 .5 -2 48 28 8 12
Limestone 34 12 2.4 1.6 43.0 3.8
Iron Ore 10 13 14 71 1 1.5
Letrite
Gypsum 16 14 1 1 34 1 .5 42
Mni Gyps
Fly ash 5mx 50-60 20-33 2-7 2-10 5 Mx 1.5mx 2.75mx
Physical Analysis of PPC:
TEST- Residue (sieve), Blain, Normal consistence, Setting time, Compressive strength,
Soundness-(AC&LC)
Blain (IS -4031 part-2) = 300 M
2
/kg minimum

NC/SC Setting time Strength Auto clave Le-chate
IS- 4031 Part-4 Part-5 Part-6 Part-3 Part-3
Lab
Tempture
27
0
C ± 2
0
C 27
0
C ± 2
0
C 27
0
C ± 2
0
C 27
0
C ± 2
0
C 27
0
C ± 2
0
C
Lab/Chamber
R-Humidity
65% ± 5,
Not less than
90%
65% ± 5, Not
less than 90%
65% ± 5,
Not less than 90%
65% ± 5,
Not less than
90%
65% ± 5,
Not less than
90%
Sample
weight
300/400 gm 300/400 gm 200gm-cm,
600gm-1s+2s+3s
300/400 gm 100 gm

Water
Requirement
Req.waterX100
sample weight
NC*0.85*S.Wt
100
(NC+3) *800
4 100
=NC NC*0.78*S.wt
100
Apparatus Vicat
apparatus
Vicat apparatus Vibrating & CSTm AC machine
215
0
C,
21 kg/cm
2

Water Bath
100
o
C
Expend Time As possible
vicat Reading
5-7 cm
As possible
vicat Reading 5-
7 cm
72 ±1hour- 16mpa
168 ±2hour-22mpa
672 ±4hour- 33mpa
(MPa=N/Kg*0.2032)
RH-C-24hour
ACM-3 Hour
WB-24hour
H.WB-3 Hour
Other

Use needle
10mm
Use needle
2&5mm
Gauging
1min dry, 4 min wet
Gauging
5 min

Cube size 60-70mm 60-70mm 70mm 25,250mm 35mm
IS
Requirement
Initial – 30 min
minimum
Final-600 min
maximum
3 day- 16mpa
7 day- 22mpa
28 day- 33mpa
0.8 % max 10 mm max
X 100

12. 12

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%)

Lime Reactivity Dry Shrinkage Comparative Strength
Lab Temp.
/RH
27
O
C ± 2 / 65% ± 5 27
O
C ± 2 / 65% ± 5 27
O
C ± 2 / 65% ± 5
Test
Specimen
50mm 25/250mm 50mm
Require
Sample
1: 2M: 9
H. Lime: Pozz: Sand
150:300M:1350gm
0.2N :0.8 :3
Pozz : Ce

ment : Sand
60N:240:900gm
0.2N :0.8 :3
Pozz : Cement : Sand
100N:400:1500gm
0.8 :3
Cement : Sand
400:1500gm
Require
Water (Table
Flow)
70 ± 5% with 10
drop in 06 Second
100-115% with 25
drop in 15 Second
105 ± 5% with 25
drop in 15 Second

Age of
Testing
10 Day 35 Day 7,28,90 Day 3,7,28, Day
Testing
Condition
2day RH chamber
(27±2
O
C&>90%)

8day Environment
Cmb.
(50±2
O
C&>90%)
24 hour RH chamber
(27±2
O
C&>90%)
6day water tank-
I
(27±2
O
C
28day Environment
Chamber
(27±2
O
C& 50%)-II
24 hour RH chamber

(27±2
O
C&>90%)

7,28,90day water
tank
(27±2
O
C)
24 hour RH
chamber
(27
O
C&>90%)

7,28,90day
water tank
(27±2
O
C)
Dry shrinkage = II-I
28 dya not less than
80% to blank
strength
Blank Strength

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

N=Specific gravity of Pozz.
Specific gravity of cement

N=Specific gravity of Pozz.
Specific gravity of cement



STI (Scheme of testing & inspection)
Form-1:
FORMAT FOR MAINTENANCE OF TEST RECORDS WEIGHMENT CO NTROL 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 PRODUCTIO N ACCEPTED & REJECTEDFOR ISI MARK)
Shift Quantity Passed for ISI Marking Rejected Remark s


Form-4-A:
POZZOLANA (One sample per week) Column 6 of Table 1A (A) Calcined clay pozzolana
Date Fitness Lime Reactivity CompressiveStrength at 2 8 Days Drying ShrinkageMax


Form-4-B :
FLY ASH POZZOLANA (See Column 6 of Table 1 A)
SO2+A1203 SiO2 MgO SO3 Na2O LOI Fineness Lime Compre ssive Drying Soundness

13. 13

+Fe203 sulphur reactivity Strength Shrikage Auto cl ave

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
manuacture
Total
loss of
Ignition
Insoluble
Residue
SiO2 CaO AlO FeO SO MgO LSFLime
Saturation
Factor
Alunin
a
Factor
Sample
Pass/Fails
Disposa
l/
Action


-6-A:
CLINKER GROUND WITH GYPSUM (Daily composite sample) (Note under Column 6 of Table 1 A)
Date of
Grinding

Fineness Soundness
AC - LC
Setting time
IST - FST
Compressive Strength
3day- 7day- 28day
Sample
Pass//fail

Disposal/Actio
n taken if sample
fails



Form-6-B:
CLINKER GROUND WITH GYPSUM & POZZOLANA (Column 6 of Ta ble I A)
Date of
Grinding

Fineness Soundness
AC - LC
Setting time
IST - FST
Compressive Strength
3day- 7day- 28day
Dry
shrinkage
(Weekly)

Sample
Pass/fail

Disposal/Ac
tio


Form-7
: PORTLAND POZZOLANA CEMENT GRINDING/ BLENDING (Dail y/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
IST-
FST
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 :
Blaine’s 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 licensee’s 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 Reading-1 R-2 R-3 Average True Load Erro r % Std.
Differ.
5,10,15,20 1+2+3/ 3 =app. load*avg. load
/Std. difference =true.Load-app.Load)*100
/applied load


Autoclave pressure gauge - Once in a six months either by licensee’s 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)

14. 14

Vibration machine - Once in a month by licensee’s 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/3
rd
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:- Molecular weight
Removal H
+
ion

In Basic from:- Molecular weight
Removal OH
-
ion


Molaritiey: 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 = N
1V1 =N2V2
Density = Mass
Volume

Important Molecular weight.
O-16, Na-23, Mg-24, Al-27, Si-28, S-32, Cl-34, K-39, Ca-40, Fe-55.8, Zn-65.39

CaCO3 =100, SiO2=60, Al2O3=102,
Fe2O3 =160, MgO= 40, Na2O= 62, K2O = 94
C3S=228, C2S= 172, C3A= 270, C4AF= 486, CaSO
4.2H2O =145

15. 15

Titrate with NaOH
(0.2N) slow titration
Lime Stone- TC&MC
















































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?
Take 50 ml HCL (0.4N)
in conical Flask
Add 1.0 gm lime stone
sample
Boil minimum 2min
Add Indicator-
Phynopthleen C20H14O4
Mwt-318.33,pH-8.2-9.8
Cool
Take NaOH Burette
reading
TC = 100-Burette reading
Add excess10/20ml
NaOH (0.2N)
Boil about 1min.
Add Indicator-
Thymopthleen
Cool
Titrate with HCL (0.4N)
Fast titration
Take HCL Burette
reading
MC = [Ex.NaOH-{2*HCL-BR}] X0.84
End point white to
pink colour
End point purple
to white- pink
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
Calculation:
CC = TC – MC
CaO = CC / 1.786
MgO = MC / 2.09

16. 16

Cement- IR & SO3






























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.





1.0 gm cement sample
Dissolved 1:1 HCL
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
Wash with 1:99 HCl &
Hot water
Wash Hot water
Dryad in Oven

Ignited at 1000
o
C
Minimum 30 min

Weight IR

Slowly Cool for ppt
form (4 hour)
Filter 42 N paper
Dryad in Oven

Ignited at 1000
o
C

Weight

Weight X 34.3 = SO3

Solution use:
= 2N- Na
2CO3= 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.
For Acid
reaction
For Base
reaction
IR=
Final weight-Initial weight

Heat 10 minute below
boil temp.
Filter- 40 N. paper
For Alkali
remove

17. 17

Clinker, Cement & Raw material (SiO2, R2O3)
All Raw materials & Cement Clinker Sample



























Wash Crucible with H2O
add NH4Cl + Bake on Hot
plate & cool it
Filter with 40N paper
Add HCL (1:1), 20-30 ml
+Heat
0.5 gm sample in beaker
Add NH4Cl 2-3gm (mix well)
0.5 gm sample + Fusion mix.
In Platinum crucible
Fuse 1000
o
C for 1 hour
Add HCL (1:1), 20-30 ml
Add Con. HCL- 5ml,
Bake on Hot plate & cool it
Add HCL (1:1), 10-20 ml
+Distilled water + Heat
Filtrate
Residue
Heat it +Add NH4Cl 2-3gm
Wash with hot Distilled water
Boil it + Add HNO3 (1:1), 0.5ml

Add NH4OH (1:1)
Dry (oven) + Ignite at 1000
o
C
Filter with 41N paper
SiO2= (F wt – I wt)*200
2 drop H2SO4 + 2 drop H2O
Add 20 ml HF
Put on Hot plate & dry
SiO2= (F wt – I wt)*200
Filtrate in 500ml
flask
Residue
R2O3= (F wt – I wt)*200
Dry (oven) + Ignite at 1000
o
C
CaO & MgO Process
next page
Use Solution:
NH4OH(1:1) –
250 ml NH
3 + 250 ml H2O
HNO
3 (1:1)-
Fusion mix.= (Na
2CO3+K2CO3)

Reaction:
= M SiO3 + 2HCl M Cl2 + H2SiO3
= H2SiO3+ Evaporation SiO2 +(H2O)
= SiO2 + Impu. + 4HF SiF4 +2H2O H 2SiO3 + 2H2 SiF6
= (FeCl3 + AlCl3) + 3NH4OH {Fe(OH) 3 + Al(OH)3} + 3NH4Cl
={Fe(OH)3 + Al(OH)3} + Ignition Fe2O3 + Al2O3





Oxidizing
agent
Isolate
R2O3
ppt
form

18. 18

Clinker, Cement & Raw material (CaO, MgO)-EDTA method

For-CaO For- MgO












(end colour red- pink to blue)

(end colour red- pink to purple)











Take 20 ml aliquot solution
After filtrate R2O3 solution make up 500 ml
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 Patton & Reader (P&R)
Indicator, C21H14N2O7S
Mwt-438.42 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
{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

Take 20 ml aliquot solution
Add Tri ethanol amine (TEA)
5 ml (For Isolation), C6H15NO3,
Mwt-149.19 g/m
Add Eriochrome black T (EBT)
Indicator, C20H2N3NaO7S
Mwt-461.38 g/m
Add 10-20 ml Buffer Solution
(For pH-10)
Mwt-000 g/m
Titrate with EDTA
(ethylene di amine tetra
acetate) Mwt-372.34 g/m
{0.04032 X mol. EDTA(0.01)X (V2- V1)X Vmu X 100} D.F.
Volume taken X Sample weight
= V1- EDTA Burette reading
= V2- Cao titration BR
= Vmu- Volume make up
= 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:
= Ca
2+
+ EDTA.2Na
+
2Na
+
+ EDTA.Ca
2+


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.

19. 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
clear the turbidity with a
hydrochloric acid(1:10) and a few drops in excess to
Add 100 mg of sulphosalicylic acid and titrate with
0.01M EDTA solution carefully to a colouress or pale

CALCULATION:
1 ml of 0.01M EDTA = 0.7985 mg Fe

Fe2O3(%) = 0.07985 X V X M X 250 X 100

Where,V= volume of EDTA used and
W= weight of sample
M = Molarity of EDTA










19
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) 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:-

1 ml of 0.01M EDTA = 0.7985 mg 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

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
1:6) till turbidity
minimum amount of dilute
hydrochloric acid(1:10) and a few drops in excess to
Add 100 mg of sulphosalicylic acid and titrate with
0.01M EDTA solution carefully to a colouress or pale

20. Alumina (Al2O3) Testing by EDTA method in Cement
After testing of Fe
EDTA to the same flask add 1ml H3PO4(1:3)
and 5 ml of H2SO4(1:3) and one drop of thymol


add ammonium acetate solution by stirring until
the colour changes from red to yellow add 25 ml
of ammonium acetate in


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


Add 2-3 ml of bismuth nitrate solution in
Titrate with EDTA to a sharp yellow endpoint

CALCULATION:-
1 ml of 0.01M EDTA = 0.5098 mg Al

Al2O3(%) = 0.05098 X V1 X M X 250 X 100
W X 25

V1= V2-V3-(V4 X factor of Bi(NO
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
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.

3 ml of bismuth nitrate solution in excess.
Titrate with EDTA to a sharp yellow endpoint
1 ml of 0.01M EDTA = 0.5098 mg Al2O3
(%) = 0.05098 X V1 X M X 250 X 100
W X 25
(V4 X factor of Bi(NO3)3
Where,V1= volume of EDTA for alumina
of EDTA used in titration
V3 = volume of EDTA used for iron
V4 = total volume of bismuth nitrate solution

21. 21

RapidCaoof Clinker/PPCby KMnO4 method (ASTM)
PPC Cement Clinker Sample /OPC



























Wash Crucible with H2O
Add NH4OH (1:1)
until Colour yellow
0.2 gm sample + Add 1:1 Hcl
0.2 gm sample + Fusion mix.
In Platinum crucible
Fuse 1000
o
C for 1 hour
Add HCL (1:1), 20-30 ml
Just Boil+ Continue in Hot Plate
Add methyl Orange- few
drop
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
Aliquot
solution
OUT
Titrate with KMnO4
(0.01772 N)
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
B.R. X 0.5 X Factor / Sample
wt.
Add H2SO4 (1:1)

22. 22

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
Filter
Out




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

Add P&R Indicator 0.05gm (Approx)



Sky Blue

Titrate With 0.01N EDTA


(until No Color Change)





Calculate


{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





OR


BR X 2.804 = CaO%


(For 20 ml Volume taken)

23. 23

Iron (Raw material) -Dichromate method:(ASTM)






Clinker sample





















0.5 gm sample + Fusion mix. In
Platinum crucible
Fuse in 1000
o
C minimum 30 min
Cool and wash Pt. crucible with
1:1 HCl
Wash crucible with Distilled
water
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
Add 5-10 ml HgCl2 and Acid
mixture –Masking agent
Titrate with K2Cr2O7Potassium
dichromate
Iron= B.R X Factor (K2Cr2O7)
Solution Preparation:
=Acid mix.- 15% H2SO4+ 15%H3PO4 +70% H2O
=K
2Cr2O7(N/16)– 3.07 gm dissolved in 1000ml
H2O
=BDS – 1gm dissolved in 100 ml dil. HCL (10%)
=SnCl
2– 5 gm dissolved in 100 ml dil. HCL (10%)
=Fusion mix – Na2CO3+K2CO3
= HgCl2- 56 gm dissolved in 1000ml H2O



Reaction:
= 2Fe
3+
+ Sn
2+
2Fe
2+
+ Sn
4+

= 2Fe
2+
+ K2Cr2O7 2Fe
3+




K2Cr2O7calibration to FAS

= take 20 ml H2O + 0.5 gm FAS +
Acid mixture +BDS Ind. + titrate with
Potassium dichromate
Factor= 20/BR

24. 24

Free Lime Test:(Clinker)















= 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









Take 1 gm Clinker sample in
beaker
Add 10 ml Ethylene Glycol
Put for 45 min in water bath
Filter with 40N paper
Filtrate
Residue out
Add Bromocrsol Grate Green
Indicator
Titrate with 0.1N HCL

End Colour –Green to golden
Yellow

F/CaO= B.R X 0.28 (HCL Factor)

Solution Preparation:
= 1 Glycerol : 5 Ethanol
Reaction:
Ca(OH)2 + 2HCl CaCl2 + H2O
Factor= CaO / 2 HCL

25. 25

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

Solution Preparation:
Reaction:
M Cl2 + 2 HNO3 M(NO3)2+2HCl
HCl + AgNO3 AgCl + HNO3
AgNO3 + NH4SCN AgSCN + NH4NO3





0.3546 X 100 X (10-BR)
Sample weight

26. 26

Alkali Test (Na2O+K2O):-( PPC=0.8% max)

















*Pre heater Coating sample in (about) Na2O= 1-2% & K2O=12-16%.






Take 0.25 gm sample in
Platinum crucible
10 ml HF and backing
Add 2ml HNO3
Add 10 ml HClO4
(Per Choleric acid)
Put Hot plate & up to Syrupy
Residue out
Extract dissolved to 1:1 HNO3
in bicker
Filter 41N paper in 250 ml
Volumetric Flack

Make up 250 ml with H2O

Solution Preparation:
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).


Volume makeup X 100 X ppm reading
Sample weight X 10
6

27. 27

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 1000
O
C
RS= Initial Wt. – Final Wt.
*200

28. 28

Sulpher Test: (Coal), ESCHKA Method (IS 1350-P3)















Coal Grading: Coal is the combination of Organic (Carbon) and Inorganic (Si02, R2O3 etc) material. It is use for
heating purpose.

Grade
A+M % UHV cal/g
A <19.5 >6200
B 19.5-24.0 6200-5600
C 24.0-28.7 5600-4940
D 28.7-34.1 4940-4200
E 34.1-40.2 4200-3360
F 40.2-47.1 3360-2400
G 47.1-55.1 2400-1300
Un-grade >55.1 <1300
Type of Coal: 1. Anthracite 2.Buteminus 3. Lignite 4. Pith



Take 0.1 gm sample platinum
crucible
Add 1-2 gm ESCHKA mixture
Fuse at 800
O
C
Dissolved to 1:1 HCl
Filter 41N paper
Aliquot Solution Boil
Solution Preparation:
= 0.1374 = S /BaSO4
= ESCHKA mixture = (2:1) Mgo+ Na2CO3
(Light Calcined magnesia oxide
+Anhydrous Sodium carbonate)
Residue out
Add 20 ml BaCl2
Cool
Filter 42N Paper
Residue Ignite at 900
O
C
Ash X 0.1374 X100

29. 29

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
IS 4031(Part 2):1999 Methods of physical tests for hydraulic cement: Part 2 Determination of
fineness by specific surface by Blaine air permeability method
IS 4031(Part 3):1988 Methods of physical tests for hydraulic cement: Part 3 Determination of
soundness
IS 4031(Part 4):1988 Methods of physical tests for hydraulic cement: Part 4 Determination of
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
IS 4031(Part 6):1988 Methods of physical tests for hydraulic cement: Part 6 Determination of
compressive strength of hydraulic cement (other than masonry cement)
IS 4031(Part 7):1988 Methods of physical tests for hydraulic cement: Part 7 Determination of
compressive strength of masonry cement
IS 4031(Part 8):1988 Methods of physical tests for hydraulic cement: Part 8 Determination of
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
IS 4031(Part 10):1988 Methods of physical tests for hydraulic cement: Part 10 Determination of
drying shrinkage

30. 30

IS 4031(Part 11):1988 Methods of physical tests for hydraulic cement: Part 11 Determination of
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
IS 4031(Part 14):1989 Methods of physical tests for hydraulic cement: Part 14 Determination of
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

31. 31

IS 712:1964 Hydrated Limes.
IS No. Important Point
IS- 4032
*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.
IS- 4031-P1
* 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.
IS- 4031-P2
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

32. 32


Bag Testing:

Mass
75
Leng
th
74
Widt
h
48
Stitc
hes
14
Ends
40
Picks
40
Effective
valve Size
(10 x 22)
Seepage
of
Cement
Strength in KGF
Fabric Seam
(Gms
)
(Cm) (Cm)
Per
Dm
Per
Dm
Per
Dm
(Cm)
MAX-100
(Gms/Ba
g)
Warp
Way
87
Warp
Elongations
%
Weft
Way
87
Weft
Elongations
%
Top/
Bottom
40
69.0 74.0 48.5 14 39.00 39.0 11.0 22.50 55.0 89.1 2 1.0 86.1 21.0 42.0

= 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 27±2 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 K
2Cr2O7 + 200 ml H2SO4)
K2Cr2O7 + 4 H2SO4 K2SO4+ Cr2(SO4)3+4 H2O + 3O
X-ray: = nʎ= 2d sinθ
(n= number of wave, ʎ= wave length, d= distance two layer, sinθ= 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.

33. 33


Thank you.............