Cement Testig Notes
Cement Testig Notes
Cement Testig Notes
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.
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.
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,
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.
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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:
*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
It is know that fuel economy or improved burnability in the formation of clinker can be effected
through the following stage of clinker burning.
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12CaO.7Al2O3, SiO2+2CaO.Fe2O3, 3CaO.SiO2,
= Formation of 3CaO.Al2 O3, 3CaO.SiO2 :-1300oC
2CaO.SiO2 + Ferrite Phase
= Formation of 3CaO.Al2 O3, 3CaO.SiO2 :-1400oC
2CaO.SiO2+ Ferrite Phase
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Phase data for a Type I OPC paste made with a w/c of 0.45.
Volume %
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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 C 3S,
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 C4 AF 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.
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ions that leaves large “holes” in the crystal lattice. Essentially, the ions do not fit together very well,
causing the crystal structure to have a high internal energy. As a result, C 3S is highly reactive.
The 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 C 3S. However, as discussed
in Section 3.2, we will avoid using mineral names in this monograph. In a typical clinker the C 3S
would contain about 1 wt% each of MgO, 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.
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typical composition (in normal chemical notation) to be Ca 2 AlFe0.6Mg0.2Si0.15Ti0.5O5. 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:
a
Formula =1.7C-S-4H. b Formula =1.7C-S-1.6H.
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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 5% 6% 4% 3% 10mm -
>225 30-600 16 22 33
Mx Mx Mx Mx 0.8%
43 G 5% 6% 3% 3% 10mm -
>225 30-600 23 33 43
Mx Mx Mx Mx 0.8%
53 G 4% 6% 3% 3% 10mm -
>225 30-600 27 37 53
Mx Mx Mx Mx 0.8%
Low heat 5% 6% 4% 3% 10mm -
>320 60-600 10 16 35
cement Mx Mx Mx Mx 0.8%
Rapid 6% 4% 3% 10mm -
- >325 30-600 27 - -
hardening Mx Mx Mx 0.8%
Sulphate 5% 6% 4% 2.5% 10mm -
>225 30-600 10 16 33
Resisting Mx Mx Mx Mx 0.8%
Masonary 6% - 3% 15%Mx
- 10mm -1 % 90m-24H - 3 5
Cement Mx Mx in 45M
Hydrophobic 5% 6% 4% 3% 10mm -
>350 30-600 16 22 31
cement Mx Mx Mx Mx 0.8%
Super 10% 4% 1.5%
- >400 5mm - --- 30-600 15 22 30
sulphate Mx Mx Mx
White cement 2% 10mm -
- 6%Mx - >225 30-600 15 20 30
Mx 0.8%
PSC 5% 8% 5% 3% 10mm -
>225 30-600 16 22 33
Mx Mx Mx Mx 0.8%
PPC 5% 6% FORM 3% 10mm -
ULA
>300 30-600 16 22 33
Mx Mx Mx 0.8%
Special Test: PPC –Drying Shrinkage 0.15%max,
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Lime saturation Factor: (if Alumina modulus <0.64)
LSF = CaO
2.8 SiO2 + 1.1Al2O3 +0.7Fe2O3 (Typical Range: 92 to 108)
C3S = 4.071 CaO – (7.602 SiO2 + 6.718 Al2O3 +1.43Fe2O3 ) 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)
LSF =
Liquid Value:
LV= 1.13 C3A +1.35 C4AF + MgO +Alkalies
Burnability Index:
BI = C3S
C4AF + C3A
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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
Insoluble Residue:
IR (max %) = X+4 (100-X) (Note: X= % of Fly ash)
100
Blain :
Blain = √Time X Factor
Factor = STD Blain
√Time
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
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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
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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%)
Form-3: PRODUCTION DATA (POST GRINDING DETAILS OF PRODUCTION ACCEPTED & REJECTED FOR 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 Compressive Strength at 28 Days Drying Shrinkage Max
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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 LSF Lime 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-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
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)
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)
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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.
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
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Lime Stone- TC & MC
Add Indicator-
Phynopthleen C20H14O4
Mwt-318.33,pH-8.2-9.8
Cool
Add Indicator-
Thymopthleen Calculation:
CC = TC – MC
CaO = CC / 1.786
MgO = MC / 2.09
Cool
Filtrate
Residue
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Clinker, Cement & Raw material (SiO2, R2O3)
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Clinker, Cement & Raw material (CaO, MgO)-EDTA method
After filtrate R2O3 solution make up 500 ml
Add Tri ethanol amine (TEA) Add Tri ethanol amine (TEA)
5 ml (For Isolation), C6H15NO3, 5 ml (For Isolation), C6H15NO3,
Mwt-149.19 g/m Mwt-149.19 g/m
Add Glycerol 5 ml
(For Isolation), C3H8O3,
Mwt-92.10 g/m
{0.05608 X mol. EDTA(0.01)X V1 X Vmu X100} D.F. {0.04032 X mol. EDTA(0.01)X (V2- V1)X Vmu X 100} D.F.
Volume taken X Sample weight Volume taken X Sample weight
= V1- EDTA Burette reading = V1- EDTA Burette reading
= Vmu- Volume make up = V2- Cao titration BR
= Difference Factor - as per EDTA standard = Vmu- Volume make up
= DF – as per EDTA standard
Solution Use:
= Buffer solution- 70 gm NH4Cl dissolved in 570
ml NH4OH. Reaction:
= 4.0N NaOH- 160 gm dissolved in 1000 ml H2O. = Ca2+ + EDTA.2Na+ 2Na++ EDTA. Ca2+
=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
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Iron (Raw material) -Dichromate method:
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Free Lime Test: (Clinker)
Solution Preparation:
Take 1 gm Clinker sample in
= 1 Glycerol : 5 Ethanol
beaker
hcl
hcl
hcl
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Cloride Test (Cl):-0.1% max
Solution Preparation:
Take 1 gm sample in beaker
hcl
hcl
hcl
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Alkali Test (Na2O+K2O):-( PPC=0.8% max)
hcl
hcl
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Reactiv Silica Test: (Fly ash)
Add 50 ml HCl
Add 16 gm KOH
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Sulpher Test: (Coal)
Fuse at 800OC
Dissolved1:1 HCl
Filtrate + Boil
20 ml BaCl2
cool
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
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Indian Standard Reference Use 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
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
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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
Mass Leng Widt Stitc Ends Picks Effective Seepage Strength in KGF
69.5 th h hes 40 40 valve Size of
74 48 14 (10 x 22) Cement Fabric Seam
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
= 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).
X-ray: = nʎ = 2d sin θ
(n= number of wave, ʎ = wave length, d= distance two layer, sin θ= angle of wave)
When bombarding of cathode ray on high melting point metal than reflected ray is called X ray.
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.
Thank you.............
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