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.

1
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 Getting sample loss Degree ofcalcinations

(Approx)
1. 1F& 2F 280-332OC 30-33 % 10 %
2. 1E& 2E 370-420OC 25-30 % 23 %
3. 1D & 2D 540-600OC 20-25 % 40 %
4. 1C & 2C 630-710OC 15-20 % 55 %
5. 1B & 2B 770-850OC 10-15 % 24 %
6. 1A & 2A 857-890OC 2-5 % 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 Mineral
Notation Name
Tricalcium Silicate Ca3SiO5 3CaO.SiO2 C3S Alite
Dicalcium Silicate Ca2SiO4 2CaO.SiO2 C2S Belite
Tricalcium Aluminate Ca3Al2O6 3CaO.Al2O3 C3A Aluminate
Tetracalcium Ca2AlFeO5 4CaO.Al2O3.Fe2O3 C4AF Ferrite
Aluminoferrite
Calcium hydroxide Ca(OH)2 CaO.H2O CH Portlandite
Calcium sulfate dihydrate CaSO4.2H2O CaO.SO3.2H2O C H2 Gypsum
Calcium oxide CaO CaO C Lime

Reaction Occurring in Pre heater to kiln:

1. Evaporation of free water - 100oC

2. Release of combine water from clay - 500oC
3. Dissociation of magnesium carbonate - 900oC
4. Dissociation of Calcium carbonate - above900oC
5. Dissociation of lime and clay - 900oC-1200oC
6. Commencement of liquid formation - 1200oC-1280oC
7. Further formation of liquid and completion - above1280oC
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.Fe2O3 :- 800oC

= Formation of 2CaO.Fe2O3.CaO.Fe2O3 :-900oC
= Formation of 2CaO.SiO2+2CaO.Al2O3 :-1000oC
SiO2+Ferrite Phase
= Formation of 2CaO.SiO2, 5CaO.3(Al2O3) :-1100oC
5CaO.Al2O3, 3CaO.SiO2, Ferrite Phase
= Formation of 2CaO.SiO2, 3CaO.SiO2 :-1200oC

3
 12CaO.7Al2O3, SiO2+2CaO.Fe2O3, 3CaO.SiO2,
= Formation of 3CaO.Al2O3, 3CaO.SiO2 :-1300oC
2CaO.SiO2 + Ferrite Phase
= Formation of 3CaO.Al2O3, 3CaO.SiO2 :-1400oC
2CaO.SiO2+ Ferrite Phase

Effects of Various Factors on Raw mix Burnability:

Characteristic Limiting Preferable Effects

/Modulus range range
If SM High
Silica modulus Result in hard burning, high fuel consumption,
1.9-3.2 2.3-2.7
(SM) difficulty in coating formation, radiation from shell
is high, deteriorates the kiln lining
If AM High
Impacts harder burning, high fuel consumption,
Alumina Increases C3A decreases C4AF, reduces liquid phase
1.5-2.5 1.3-1.6
modulus (AM) & kiln output, if AM is too low and raw mix is
without free silica, clinker sticking and balling is too
high.
A higher LSF
Lime Make it difficult to burn raw mix, increases C3S,
0.66-
saturation 0.92-0.96 reduces C2S, deteriorates refractory lining, increases
1.02
factor (LSF) radiation from shell, increases kiln exit gas
temperature.
A higher silica
As low as Increases fuel and power consumption, causes
Free silica 0-3
possible difficulty in coating formation, deteriorates
refractory, increases radiation of heat kiln shell,
A higher MgO
Favours dissociation of C2S and CaO and lets C3S
MgO 0-5 0-3
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
Alkalies 0-1 0.2-0.3%
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
Sulphur
0-4 0.5-2% Acts as an effective mineraliser and modifier of
compound
alkali cycle by forming less volatiles,
A higher fluorides
0.03-
Fluorides 0-0.6 Leads to modify the kinetic of all burning reaction ,
0.08%
lowers the temperature of C3S formation by 150-200
A higher chlorides
Higher Cl forms more volatiles % causes operational
Up to
Chlorides 0.06 problem due to its complete volatilization in burning
0.015%
zone, increases liquid formation & melting point of
the absorbed phase is drastically change.

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Phase data for a Type I OPC paste made with a w/c of 0.45.
Volume %
3
Phase Density (g/cm ) 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/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 40–70 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 980˚C the
equilibrium structure is triclinic. At temperatures between 980˚C – 1070˚C the structure is
monoclinic, and above 1070˚C 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 α
structure with three polymorphs, a β structure in that is in equilibrium at intermediate temperatures,
and a low temperature γ structure. An important aspect of C2S is that γ-C2S has a very stable crystal
structure that is completely uncreative in water. Fortunately, the β structure is easily stabilized by the
other oxide components of the clinker and thus the γ form is never present in portland cement. The
crystal structure of β−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: 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

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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.

7
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 207 120 62 100
Hydration(cal/g)
Resistance to Poor Moderate High High
Chemical attack
Dying Shrinkage - - low -
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
C4AF = Not contribution to Strength, Requited to reduce the burning Temperature
for clinkerisationMostly occurs as a glassy interstitial phase.

Specification of Various Type of Cement:

Soundnes
Compressive
Finenes s Setting
TYPE OF Strength
LOI MgO IR SO3 s Lechate- Time
CEMENT 2 3 7 28
(M /Kg) Auto IST- FST 2
Days(N/mm )
Clave
33 G 4% 10mm-
5%Mx 6%Mx 3%Mx >225 30-600 16 22 33
Mx 0.8%
43 G 5% 3% 10mm-
6%Mx 3%Mx >225 30-600 23 33 43
Mx Mx 0.8%
53 G 3% 10mm-
4%Mx 6%Mx 3%Mx >225 30-600 27 37 53
Mx 0.8%
Low heat 5% 4% 10mm-
6%Mx 3%Mx >320 60-600 10 16 35
cement Mx Mx 0.8%
Rapid 4% 10mm-
- 6%Mx 3%Mx >325 30-600 27 - -
hardening Mx 0.8%
Sulphate 5% 4% 2.5% 10mm-
6%Mx >225 30-600 10 16 33
Resisting Mx Mx Mx 0.8%
Masonary - 15%Mx
- 6%Mx 3%Mx 10mm -1% 90m-24H - 3 5
Cement in 45M
Hydrophobic 5% 4% 10mm-
6%Mx 3%Mx >350 30-600 16 22 31
cement Mx Mx 0.8%
Super 10%M 4% 1.5%
- >400 5mm - --- 30-600 15 22 30
sulphate x Mx Mx
White cement 2% 10mm-
- 6%Mx - >225 30-600 15 20 30
Mx 0.8%
PSC 5% 5% 10mm-
8%Mx 3%Mx >225 30-600 16 22 33
Mx Mx 0.8%
PPC 5% FORM 10mm-
6%Mx ULA 3%Mx >300 30-600 16 22 33
Mx 0.8%
Special Test:PPC –Drying Shrinkage 0.15%max,

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Important Formula Use in Cement Analysis.
Hydraulic Modulus: HM = CaO
SiO2 + Al2O3 +Fe2O3 (Typical Range: 1.7 to 2.3)

Silica Ratio: SM = SiO2

Al2O3 +Fe2O3 (Typical Range: 1.8 to 2.7)

Alumina Ratio: AM = Al2O3

Or Iron Modulus Fe2O3 (Typical Range: 1.0 to 1.7)

Lime saturation Factor: (For OPC Cement)

LSF = CaO- 0.7 SO3
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)

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) Note: CaO = CaO - F/CaO
C2S = 2.867 SiO2 - 0.7544 C3S
C3 A = 0
C4AF+ C2F =2.1 Al2O3 +1.702Fe2O3
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: = 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
10
CYCLONE LOSS: = 100(KF loss – Cyclone loss)
(100 – Cyclone loss) X KF loss X 100

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

Clinker consumed (kg)

Chemical Composition (General):

Na2O F/
LOI SiO2 Al2O3 Fe2O3 CaO MgO SO3 C3S C2S C3A C4AF
+K2O CaO
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 M2/kg minimum

NC/SC Setting time Strength Auto clave Le-chate

IS- 4031 Part-4 Part-5 Part-6 Part-3 Part-3
Lab 270C ± 20C 270C ± 20C 270C ± 20C 270C ± 20C 270C ± 20C
Tempture
Lab/Chamber 65% ± 5, 65% ± 5, Not 65% ± 5, 65% ± 5, 65% ± 5,
R-Humidity Not less than less than 90% Not less than 90% Not less than Not less than
90% 90% 90%
Sample 300/400 gm 300/400 gm 200gm-cm, 300/400 gm 100 gm
weight 600gm-1s+2s+3s
Water Req.waterX100 NC*0.85*S.Wt (NC+3) *800 =NC NC*0.78*S.wt
Requirement sample weight 100 4 100 100
Apparatus Vicat Vicat apparatus Vibrating & CSTm AC machine Water Bath
apparatus 2150C, 100oC
21 kg/cm2
Expend Time As possible As possible 72 ±1hour- 16mpa RH-C-24hour WB-24hour
vicat Reading vicat Reading 5- 168 ±2hour-22mpa ACM-3 Hour H.WB-3 Hour
5-7 cm 7 cm 672 ±4hour- 33mpa
(MPa=N/Kg*0.2032)
Other Use needle Use needle Gauging Gauging
10mm 2&5mm 1min dry, 4 min wet 5 min
Cube size 60-70mm 60-70mm 70mm 25,250mm 35mm
IS Initial – 30 min 3 day- 16mpa 0.8 % max 10 mm max
Requirement minimum 7 day- 22mpa
Final-600 min 28 day- 33mpa
maximum
11
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.
27OC ± 2 / 65% ± 5 27OC ± 2 / 65% ± 5 27OC ± 2 / 65% ± 5
/RH
Test
50mm 25/250mm 50mm
Specimen
0.2N :0.8 :3 0.8 :3
1: 2M: 9 Pozz : Ce 0.2N :0.8 :3 Cement : Sand
Require
H. Lime: Pozz: Sand Pozz : Cement : Sand 400:1500gm
Sample
150:300M:1350gm ment : Sand 100N:400:1500gm
60N:240:900gm
Require
70 ± 5% with 10 100-115% with 25 105 ± 5% with 25
Water (Table
drop in 06 Second drop in 15 Second drop in 15 Second
Flow)
Age of
10 Day 35 Day 7,28,90 Day 3,7,28, Day
Testing
24 hour RH chamber 24 hour RH
2day RH chamber (27±2OC&>90%) 24 hour RH chamber
chamber
(27±2OC&>90%) (27±2OC&>90%)
6day water tank-I (27OC&>90%)
Testing
(27±2OC
Condition 8day Environment 7,28,90day water
28day Environment 7,28,90day
Cmb. tank
Chamber water tank
(50±2OC&>90%) (27±2OC)
(27±2OC& 50%)-II (27±2OC)
28 dya not less than Blank Strength
Dry shrinkage= II-I 80% to blank
strength
M=Specific gravity of Pozz. N=Specific gravity of Pozz. N=Specific gravity of Pozz.
Specific gravity of H. lime Specific gravity of cement 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 Name of the Source of supply and Details of analysis for
Date of testing
material Material consignment No. 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 Lime Compressive Drying Soundness
12
 +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 Fineness Soundness Setting time Compressive Strength Sample Disposal/Actio
Grinding AC - LC IST - FST 3day- 7day- 28day Pass//fail n taken if sample
fails

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

Date of Fineness Soundness Setting time Compressive Strength Dry Sample Disposal/Ac
Grinding AC - LC IST - FST 3day- 7day- 28day shrinkage Pass/fail tio
(Weekly)

Form-7: PORTLAND POZZOLANA CEMENT GRINDING/ BLENDING (Daily/Weekly Composite sample) (Column 5 of Table 1B)
Date of Loss on MgO Insoluble SO3 Fineness Soundness Setting Compressive Drying Sample Acti
Grinding Ignition Material Le-ch Time Strength Shrinkage Pass/Fail on
Auto IST 3 7 28 (Weekly) take
Clave /FST days

Form-8:PORTLAND POZZOLANA CEMENT CRINDING (For Alternate hourly Samples) (Column 5 of Table 1B)
Date of Time at Fineness Setting Time Sample Mode of disposal/Action
Grinding (IST)-(FST) fail/pass taken if sample fails

Form-9:PORTLAND POZZOLANA CEMENT PACKING STAGE (Daily/Weekly Composite Samples) (Column 6 of Table 1B)
Date Loss MgO Insoluble SO3 Chloride Fine Soundness Setting Compressive Drying Sample Mode of
of On Materia Content ness Le Auto time Strength Shrinkage Pass disposal/Ac
Pcking Igniti (Weekly Ch Clav IST- 3 7 28 (Weekly) /Fail tion taken if
on FST days sample fails

Form-10:(See Clause 3 of STI)

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

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 Error % Std.
Differ.
5,10,15,20 1+2+3/ 3 =app. load*avg. load =true.Load-app.Load)*100
/Std. difference /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)

13
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/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:- 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 = N1V1 =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, CaSO4.2H2O =145

14
Lime Stone- TC&MC

Take 50 ml HCL (0.4N) Solution use:

in conical Flask = 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
Add 1.0 gm lime stone =87.28ml/L-1N* 0.4 (Req.N)=34.91 ml/L
sample = Indicator dissolved in Alcohol

Boil minimum 2min

Add Indicator-
Phynopthleen C20H14O4
Mwt-318.33,pH-8.2-9.8

Cool

Titrate with NaOH

(0.2N) slow titration

End point white to Take NaOH Burette

TC = 100-Burette reading
pink colour reading

Add excess10/20ml
NaOH (0.2N)

Boil about 1min.

Add Indicator-
Thymopthleen Calculation:
CC = TC – MC
CaO = CC / 1.786
MgO = MC / 2.09
Cool

Titrate with HCL (0.4N)

Fast titration

End point purple Take HCL Burette

MC = [Ex.NaOH-{2*HCL-BR}] X0.84
to white- pink reading

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 Solution use:
Dissolved 1:1 HCL = 2N- Na2CO3= 10.6 gm sodium carbonate
dissolved in 100 ml distilled water
(Eq.wt = 53, Mwt 105.99 g/mol)
For Acid = 1:1 HCL = 50 ml HCL dissolved in 50 ml
Heat below boils
reaction Temp. 15 minute Distil water.(Mwt 36.46 g/mol)
= BaCl2 = 10 gm BaCl2 dissolved in 100 ml
Filter- 40 N. paper distilled water.

Wash Hot water

Filtrate
Residue

Boil + add hot BaCl2

React with Na2CO3 -30
10 ml
ml

Heat 10 minute below Slowly Cool for ppt

For Base
boil temp. form (4 hour)
reaction
Filter- 40 N. paper
Filter 42 N paper

Wash with 1:99 HCl &

Hot water Wash Hot water

For Alkali Dryad in Oven Dryad in Oven

remove
Ignited at 1000oC Ignited at 1000oC
Minimum 30 min
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. 0.5 gm sample in beaker
In Platinum crucible 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

Wash Crucible with H2O
+Distilled water + Heat

add NH4Cl + Bake on Hot

plate & cool it Filter with 40N paper

Add HCL (1:1), 20-30 ml Residue

+Heat Filtrate

Isolate Wash with hot Distilled water

R2O3 Heat it +Add NH4Cl 2-3gm

Oxidizing Dry (oven) + Ignite at 1000oC

agent Boil it + Add HNO3 (1:1), 0.5ml

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

Filter with 41N paper

Add 20 ml HF

Filtrate in 500ml Residue Put on Hot plate & dry

flask
Dry (oven) + Ignite at 1000oC SiO2= (F wt – I wt)*200

CaO & MgO Process

next page R2O3= (F wt – I wt)*200

Use Solution: Reaction:

NH4OH(1:1) – = M SiO3 + 2HCl M Cl2 + H2SiO3
250 ml NH3 + 250 ml H2O = H2SiO3+ Evaporation SiO2 +(H2O)
HNO3 (1:1)- = SiO2 + Impu. + 4HF SiF4 +2H2O H2SiO3 + 2H2 SiF6
Fusion mix.= (Na2CO3+K2CO3) = (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
Take 20 ml aliquot solution
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
(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
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
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
For- MgO
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
(end colour red- pink to blue)
{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
Reaction:
= Ca2++ EDTA.2Na+ 2Na++ EDTA.Ca2+
Di Sodium Salt
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 2-33 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 Clinker Sample /OPC

0.2 gm sample + Fusion mix.
0.2 gm sample + Add 1:1 Hcl
In Platinum crucible

Fuse 1000oC for 1 hour Just Boil+ Continue in Hot Plate

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

drop

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

Aliquot
solution
Take Residue in beaker
OUT

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
 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 Filter

flask& make up 500 ml 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)

22
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
Clinker sample

Wash crucible with Distilled 0.5 gm clinker sample dissolved

water in HCl -1:1

Boil & add SnCl2 Drop wise till

colourless solution

Completely cool (Room Temp.)

K2Cr2O7calibration to FAS
Add Barium di phenol Salfonate
(BDS) Indicator

Add 5-10 ml HgCl2 and Acid = take 20 ml H2O + 0.5 gm FAS +

mixture –Masking agent Acid mixture +BDS Ind. + titrate with
Potassium dichromate

Titrate with K2Cr2O7Potassium Factor= 20/BR

dichromate

Iron= B.R X Factor (K2Cr2O7)

Solution Preparation: Reaction:

=Acid mix.- 15% H2SO4+ 15%H3PO4 +70% H2O = 2Fe3+ + Sn2+ 2Fe2+ + Sn4+
=K2Cr2O7(N/16)– 3.07 gm dissolved in 1000ml = 2Fe2+ + K2Cr2O7 2Fe3+
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

23
Free Lime Test:(Clinker)
Solution Preparation:
Take 1 gm Clinker sample in
= 1 Glycerol : 5 Ethanol
beaker

Add 10 ml Ethylene Glycol

Put for 45 min in water bath

Filter with 40N paper

Residue out
Filtrate

Add Bromocrsol Grate Green

Indicator Reaction:
Ca(OH)2 + 2HCl CaCl2 + H2O

Titrate with 0.1N HCL 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
Solution Preparation:
Take 1 gm sample in beaker

Dissolved 1:3 HNO3

Filter 41N paper in Conical

Take aliquot sample

Residue out
Add 10 ml AgNO3 (0.1N)

Add 2ml Nitro Benzene

Reaction:
M Cl2 + 2 HNO3 M(NO3)2+2HCl
Add 4 Drop Ferric Indicator HCl + AgNO3 AgCl + HNO3
NH4.Fe (SO4)2.12H2O AgNO3 + NH4SCN AgSCN + NH4NO3

Titrate with Ammonia thyo

saynte (.01N) NH4SCN

End Colour – white to

0.3546 X 100 X (10-BR)

Sample weight

25
Alkali Test (Na2O+K2O):-( PPC=0.8% max)

Take 0.25 gm sample in Solution Preparation:

Platinum crucible Blank Solution: 2.5 ml HNO3 + 2.5 ml
Alumina sulphate + 250 ml H2O.
10 ml HF and backing Standard Solution:
NaCl: 1.885 NaCl Dissolved In 1000ml
Add 2ml HNO3 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

Residue out
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
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 Solution Preparation:

crucible = 0.1374 = S /BaSO4
= ESCHKA mixture = (2:1) Mgo+ Na2CO3
(Light Calcined magnesia oxide
Add 1-2 gm ESCHKA mixture +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+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

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
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

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

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Bag Testing:

Mass Leng Widt Stitc Ends Picks Effective Seepage Strength in KGF
75 th h hes 40 40 valve Size of
74 48 14 (10 x 22) Cement Fabric Seam

MAX-100 Warp Warp Weft Weft Top/

(Gms Per Per Per
(Cm) (Cm) (Cm) (Gms/Ba Way Elongations Way Elongations Bottom
) Dm Dm Dm
g) 87 % 87 % 40

69.0 74.0 48.5 14 39.00 39.0 11.0 22.50 55.0 89.1 21.0 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 K2Cr2O7 + 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.
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 Thank you.............

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