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Cement testing
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Narendra Kanchkar
, Executive Quality Control-cement
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Published on Aug 1, 2015

Cement Testing as Per BIS, and Manufacturing process

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Ian Levy

I never knew that cement was so complex. This suggests that like the discovery of
many steel alloys or vulcanised rubber, there will be better cements developed from
time to time, so that better structures can be created. I only wanted to see if bauxite
can be used to make cement.

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Sandeep Rewaria , Lab Technician / CCR Operator at Lafarge at Lafarge

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Cement testing

1. 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 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.
2. 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 800O 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 280-332O C 30-33 % 10 % 2. 1E& 2E 370-420O C 25-30
% 23 % 3. 1D & 2D 540-600O C 20-25 % 40 % 4. 1C & 2C 630-710O C 15-20 % 55
% 5. 1B & 2B 770-850O C 10-15 % 24 % 6. 1A & 2A 857-890O C 2-5 % 90-95 % 4
Zone occurs in kiln: -1.Dehydration Zone(1100O C) 2. Calcinations Zone(1250O C)3.
Clinkersition Zone (1400O C) 4. Cooling Zone.(1000O C)
3. 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 Ca3SiO5 3CaO.SiO2
C3S Alite Dicalcium Silicate Ca2SiO4 2CaO.SiO2 C2S Belite Tricalcium Aluminate
Ca3Al2O6 3CaO.Al2O3 C3A Aluminate Tetracalcium Aluminoferrite Ca2AlFeO5
4CaO.Al2O3.Fe2O3 C4AF Ferrite 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 - 100o C 2. Release of combine water from clay - 500o C 3.
Dissociation of magnesium carbonate - 900o C 4. Dissociation of Calcium carbonate -
above900o C 5. Dissociation of lime and clay - 900o C-1200o C 6. Commencement
of liquid formation - 1200o C-1280o C 7. Further formation of liquid and completion
- above1280o 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.Fe2O3 :- 800o C =
Formation of 2CaO.Fe2O3.CaO.Fe2O3 :-900o C = Formation of
2CaO.SiO2+2CaO.Al2O3 :-1000o C SiO2+Ferrite Phase = Formation of 2CaO.SiO2,
5CaO.3(Al2O3) :-1100o C 5CaO.Al2O3, 3CaO.SiO2, Ferrite Phase = Formation of
2CaO.SiO2, 3CaO.SiO2 :-1200o C
4. 4. 4 12CaO.7Al2O3, SiO2+2CaO.Fe2O3, 3CaO.SiO2, = Formation of 3CaO.Al2O3,
3CaO.SiO2 :-1300o C 2CaO.SiO2 + Ferrite Phase = Formation of 3CaO.Al2O3,
3CaO.SiO2 :-1400o C 2CaO.SiO2+ 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. 5 Phase data for a Type I OPC paste made with a w/c of 0.45. Volume % Phase
Density (g/cm3 ) 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
6. 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, 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 o C: 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
7. 7. 7 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.
8. 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 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: 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 10mm- 0.8% 30-600 16 22 33 43 G 5% Mx 6%Mx 3%
Mx 3%Mx >225 10mm- 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. 9 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 C3A = 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
10. 10. 10 Liquid Value: LV= 1.13C3A +1.35C4AF + MgO +Alkalies Burnability Index:
BI = C3S 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 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 =
11. 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 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 Tempture 270 C ± 20 C 270 C ± 20 C 270 C ± 20 C 270 C ± 20 C 270 C ±
20 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 2150 C, 21 kg/cm2 Water Bath 100o 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. 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 27O
C ± 2 / 65% ± 5 27O C ± 2 / 65% ± 5 27O 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±2O C&>90%) 8day Environment Cmb. (50±2O
C&>90%) 24 hour RH chamber (27±2O C&>90%) 6day water tank-I (27±2O C
28day Environment Chamber (27±2O C& 50%)-II 24 hour RH chamber (27±2O
C&>90%) 7,28,90day water tank (27±2O C) 24 hour RH chamber (27O C&>90%)
7,28,90day water tank (27±2O 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 CONTROL AT
PACKING STAGE (Clause 6.2) Date Shift No. Of Bag Net mass of bags from
nozzles No.1, No. 2, Remark Form-2:RAW MATERIAL TESTING (CL.7 of STI)
Date of receipt of material Date of testing Name of the Material Source of supply and
consignment No. Details of analysis for Specified requirements Form-
3:PRODUCTION DATA (POST GRINDING DETAILS OF PRODUCTION
ACCEPTED & REJECTEDFOR ISI MARK) Shift Quantity Passed for ISI Marking
Rejected Remarks Form-4-A:POZZOLANA (One sample per week) Column 6 of
Table 1A (A) Calcined clay pozzolana Date Fitness Lime Reactivity
CompressiveStrength at 28 Days Drying ShrinkageMax Form-4-B :FLY ASH
POZZOLANA (See Column 6 of Table 1 A) SO2+A1203 SiO2 MgO SO3 Na2O LOI
Fineness Lime Compressive Drying Soundness
13. 13. 13 +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 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 Table 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 (Daily/Weekly
Composite sample) (Column 5 of Table 1B) Date of Grinding Loss on Ignition MgO
Insoluble Material SO3 Fineness Soundness Le-ch Auto Clave Setting Time IST /FST
Compressive Strength 3 7 28 days Drying Shrinkage (Weekly) Sample Pass/Fail Acti
on take Form-8:PORTLAND POZZOLANA CEMENT CRINDING (For Alternate
hourly Samples) (Column 5 of Table 1B) Date of Grinding Time at Fineness Setting
Time (IST)-(FST) Sample fail/pass Mode of disposal/Action taken if sample fails
Form-9:PORTLAND POZZOLANA CEMENT PACKING STAGE (Daily/Weekly
Composite Samples) (Column 6 of Table 1B) Date of Pcking Loss On Igniti on MgO
Insoluble Materia SO3 Chloride Content (Weekly Fine ness Soundness Le Auto Ch
Clav Setting time 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 Error % 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. 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/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
15. 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. 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 1000o C Minimum 30 min Weight IR Slowly
Cool for ppt form (4 hour) Filter 42 N paper Dryad in Oven Ignited at 1000o C
Weight Weight X 34.3 = SO3 Solution use: = 2N- Na2CO3= 10.6 gm sodium
carbonate dissolved in 100 ml distilled water (Eq.wt = 53, Mwt 105.99 g/mol) = 1:1
HCL = 50 ml HCL dissolved in 50 ml Distil water.(Mwt 36.46 g/mol) = BaCl2 = 10
gm BaCl2 dissolved in 100 ml distilled water. 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. 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
1000o 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 1000o 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 1000o C CaO & MgO Process next page Use Solution:
NH4OH(1:1) – 250 ml NH3 + 250 ml H2O HNO3 (1:1)- Fusion mix.=
(Na2CO3+K2CO3) Reaction: = M SiO3 + 2HCl M Cl2 + H2SiO3 = H2SiO3+
Evaporation SiO2 +(H2O) = SiO2 + Impu. + 4HF SiF4 +2H2O H2SiO3 + 2H2 SiF6
= (FeCl3 + AlCl3) + 3NH4OH {Fe(OH)3 + Al(OH)3} + 3NH4Cl ={Fe(OH)3 +
Al(OH)3} + Ignition Fe2O3 + Al2O3 Oxidizing agent Isolate R2O3 ppt form
18. 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: = Ca2+ + EDTA.2Na+
2Na+ + EDTA.Ca2+ 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. 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. 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. 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
1000o 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. 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. 23 Iron (Raw material) -Dichromate method:(ASTM) Clinker sample 0.5 gm
sample + Fusion mix. In Platinum crucible Fuse in 1000o 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 =K2Cr2O7(N/16)– 3.07 gm
dissolved in 1000ml H2O =BDS – 1gm dissolved in 100 ml dil. HCL (10%) =SnCl2–
5 gm dissolved in 100 ml dil. HCL (10%) =Fusion mix – Na2CO3+K2CO3 = HgCl2-
56 gm dissolved in 1000ml H2O Reaction: = 2Fe3+ + Sn2+ 2Fe2+ + Sn4+ = 2Fe2+ +
K2Cr2O7 2Fe3+ K2Cr2O7calibration to FAS = take 20 ml H2O + 0.5 gm FAS +
Acid mixture +BDS Ind. + titrate with Potassium dichromate Factor= 20/BR
24. 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. 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. 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 106
27. 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
1000O C RS= Initial Wt. – Final Wt. *200
28. 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 800O 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
900O C Ash X 0.1374 X100
29. 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. 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. 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. 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 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.
33. 33. 33 Thank you.............

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