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Short Note of Cement Chemistry

Short Note of Cement Chemistry

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Short Note of Cement Chemistry

Indian Standard Code 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

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
1

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 retentivity 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.

Use sand in cement
IS 650:1991 Specification for standard sand for testing of cement. IS 456:2000 Code of practice plain and reinforced concrete

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 allied materials: Part 3 Determination of iron oxide, alumina, calcium oxide and magnesia

Gypsum
IS 1288:1982 Methods of test mineral gypsum. IS 1289:1960 Methods of sampling mineral gypsum IS 1290:1982 Mmineral gypsum.

Bag
IS 12154:1987 Methods of Light weight jute bags for packing cement IS 2580:1995 Methods of Jute sacking bags for packing cement IS 11652:1986 High density polyethylene (HDPE) woven sacks for packing cement IS 12174:1987 Jute synthetic union bags for packing cement IS 11653:1986 Polypropylene (PP) woven sacks for packing cement

2

Formula use in cement analysis.
Hydraulic Modulus: HM = CaO SiO2 + Al2O3 +Fe2O3 SiO2 Al2O3 +Fe2O3 Al2O3 Fe2O3 (Typical Range: 1.7 to 2.3)

Silica Ratio:

SM =

(Typical Range: 1.8 to 2.7)

Alumina Ratio: Or Iron Modulus

AM =

(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 Lime saturation Factor: LSF = CaO X 100 2.8 SiO2 + 1.2Al2O3 +0.65Fe2O3 Lime saturation Factor: (if Alumina modulus >0.64) LSF = CaO 2.8 SiO2 + 1.65Al2O3 +0.35Fe2O3 Lime saturation Factor: (if Alumina modulus <0.64) LSF = CaO 2.8 SiO2 + 1.1Al2O3 +0.7Fe2O3

(Typical Range: 0.66 to 1.02)

(Typical Range: 95 to 110)

(Typical Range: 92 to 108)

(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 ) Note: CaO = CaO - F/CaO C2S = 2.867 SiO2 - 0.7544 C3S C3A = 2.65 Al2O3 - 1.692 Fe2O3 C4AF = 3.043 Fe2O3 C3S = Tri Calcium Silicate. (Molecular weight = 228 g/g mol) C2S = Di Calcium Silicate. (Molecular weight = 172 g/g mol) C3A = Tri Calcium Aluminate. (Molecular weight =270 g/g mol) C4AF = Tetra Calcium Aluminate Ferate. (Molecular weight = 486 g/g mol) (if Alumina modulus <0.64) C3S = 4.071 CaO – (7.602 SiO2 + 4.479 Al2O3 +2.86Fe2O3) C2S = 2.867 SiO2 - 0.7544 C3S C3A = 0 C4AF+ C2F =2.1 Al2O3 +1.702Fe2O3 Note: CaO = CaO - F/CaO

Bogus’ formula for Cement Constituent
(if Alumina modulus >0.64) Note: CaO = CaO - F/CaO C3S = 4.071 CaO – (7.602 SiO2 + 6.718 Al2O3 +1.43Fe2O3+2.85 SO3) C2S = 2.867 SiO2 - 0.7544 C3S C3A = 2.65 Al2O3 - 1.692 Fe2O3 C4AF = 3.043 Fe2O3

3

Liquid Value: LV= 1.13 C3A +1.35 C4AF + 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 % of ash in fuel X coal consumption/ 100 100-ash absorption 100-LOI

Ash absorption:

=

Raw meal to clinker factor: =

Specific Heat:

V=

NCV X % of coal Consumption 100

Insoluble Residue: IR (max %) = X+4 (100-X) (Note: X= % of Fly ash) 100 (Note: In PPC Cement Fly ash use not less than 15% and not more than 35%) (Note: In PSC Cement Slag use not less than 25% and not more than 70%) Blain : Blain = √Time X Factor Factor = √Time STD Blain CYCLONE LOSS: = 100 (KF loss – Cyclone loss ) (100 – Cyclone loss) X KF loss = X 100

Clinker to cement factor:

Clink. + Fly ash/Slag + additives (kg) Clinker consumed (kg)

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. Bulk Density : 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,
4

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

Grade A B C D E F G Un-grade Type of Coal:

A+M % UHV cal/g <19.5 >6200 19.5-24.0 6200-5600 24.0-28.7 5600-4940 28.7-34.1 4940-4200 34.1-40.2 4200-3360 40.2-47.1 3360-2400 47.1-55.1 2400-1300 >55.1 <1300 1. Anthracite 2.Buteminus 3. Lignite 4. Pith

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 IS- 4031 Lab Tempture Lab/Chamber R-Humidity Sample weight Water Requirement Apparatus NC Part-4 270C ± 20C 65% ± 5, Not less than 90% 300/400 gm Req.waterX100
sample weight

Setting time Part-5 270C ± 20C 65% ± 5, Not less than 90% 300/400 gm NC*0.85*S.Wt 100 Vicat apparatus As possible vicat Reading 5-7 cm

Strength Part-6 270C ± 20C 65% ± 5, Not less than 90% 200gm-cm, 600gm-1s+2s+3s (NC+3) *800 4 100 Vibrating & CSTm

Auto clave Part-3 270C ± 20C 65% ± 5, Not less than 90% 300/400 gm =NC AC machine 2150C, 21 kg/cm2 RH-C-24hour ACM-3 Hour

Le-chate Part-3 270C ± 20C 65% ± 5, Not less than 90% 100 gm NC*0.78*S.wt 100 Water Bath 100oC RH-C-24hour WB-3 Hour

Vicat apparatus As possible vicat Reading 5-7 cm Use needle 5mm

Expend Time

72 ±1hour- 16mpa 168 ±2hour-22mpa 672 ±4hour- 33mpa

Use needle Gaugeing Gaugeing 1min dry, 4 min wet 2mm 5 min 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 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

Other

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 & REJECTED FOR ISI MARK)
Shift Quantity Passed for ISI Marking Rejected Remarks

5

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

Form-4-B : FLY ASH POZZOLANA (See Column 6 of Table 1 A)
SO2+ A1203 +Fe203 SiO2 MgO SO3 sulphur Na2O LOI Fineness Lime reactivity Compressive Strength Drying Shrikage Soundness 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 LSF Lime Alunina Sample Disposal/ manuacture loss of Residue Saturation Factor Pass/Fails Action Ignition Factor taken if sample fails

Form-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
3day7day28day

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
3day7day28day

Dry shrinkage (Weekly)

Sample Pass/fail

Disposal/Actio n taken if sample fails

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 Action taken if sample fails

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

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

6

FLY ASH TESTING (physical- IS-1727) Lime reactivity
Test Specimen: 50mm Age at testing: 10 day’s Temperature: 500C ± 20C Humidity (RH): 90 -100% Material for mortar : = 1-hydrate lime : 2M*- pozzolana : 9- sand(3type) M* = Specific gravity of pozzolana / Specific gravity of Lime Water requirement = Flow-70mm ± 5mm, 10 drop in 6 second. IS require compressive St. = 4.5 N/mm2, min Pozzolana Specific gravity = weight of pozzolana in gm / displaced volume in ml. Pozzolana min Blain = 320 Drying Shrinkage % max (IS) = 0.15 Molecular weight: 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

Chemical Composition: General
PPC Clinker Limestone Iron Ore Gypsum Fly ash IScode 1489 4032 1760 1288 3812 LOI 5.0 0.5 34 SiO2 31.0 21-22 12 Al2O3 4.5 5-6 2.4 Fe2O3 3.5 3-5 1.6 CaO 43.0 62-65 43.0 MgO 5.0 3-6 3.8 Na2O +K2O .5-1.0 SO3 1.4 .2-.5 F/ CaO .5-2 C3S C2S C3A C4AF

2-14

50-60

20-33

2-7

2-10

Min

min

Rate of Clinker Phase on Properties of Cement: Setting time Hydration Early strength Late strength Heat of Hydration(cal/g) Resistance to Chemical attack Dying Shrinkage Alite C3S Belite C2S Aluminate C3A C4AF C3A Rapid Rapid High-1day 207 Poor C3S Quick Fast High-14 day Less 120 Moderate C2S Slow Slow Low High 62 High low C4AF Rapid 100 High -

= Responsible for early Strength. = Give ultimate (late) Strength along with alite. = Contributes to early strength, Help faster setting, Liberates more heat in concrete = Not contribution to Strength, Requited to reduce the burning Temperature for clinkerisation
Mostly occurs as a glassy interstitial phase.

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. Molaritiey: gm mole number / Volume in letter.
7

Lime Stone- TC & MC
Take 50 ml HCL (0.4N) in conical Flask 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

Add 1.0 gm lime stone sample

= Indicator dissolved in Alcohol

Boil minimum 2min

Add IndicatorPhynopthleen C20H14O4 Mwt-318.33,pH-8.2-9.8

Cool Titrate with NaOH (0.2N) slow titration End point white to pink colour Take NaOH Burette reading Add exis 10/20ml NaOH (0.2N) Boil about 1min. TC = 100-Burette reading

Add IndicatorThymopthleen

Cool Titrate with HCL (0.4N) Fast titration End point purple to whitepink colour Take HCL Burette reading MC = [Ex.NaOH-{2*HCL-BR}] X0.84

Q.1 why multiply 1.786 for CaO? Q.2 why multiply 2.09 for MgO? Q.3 why multiply 0.84 for MC?
8

Calculation CC = TC – MC CaO = CC / 1.786 MgO = MC / 2.09

Cement- IR & SO3
1.0 gm cement sample Dissolved 1:1 HCL Only Heat 800C 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
Filter- 40 N. paper Wash Hot water

Filtrate Residue Boil + add BaCl2

Wash with Na2CO3

Wash Hot water

For Basis reaction
Dryad in Oven Ignited at 1000oC Minim 30 min Weight IR

Slowly Cool for ppt form Filter 42 N paper

Wash Hot water Dryad in Oven Ignited at 1000oC Weight 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) 100 (Note: X= % of Fly ash)

9

Clinker, Cement & Raw material (SiO2, R2O3)

All Raw materials & Cement
0.5 gm sample + Fusion mix. In Platinum crucible Fuse 1000oC for 1 hour Add HCL (1:1), 20-30 ml Bake on Hot plate & cool it Wash Crucible with H2O Add HCL (1:1), 20-30 ml +Heat

Clinker Sample
0.5 gm sample in beaker Add NH4Cl 2-3gm(mix well) Add Con. HCL- 5ml, Bake on Hot plate & cool it Add HCL (1:1), 10-20 ml +
Distilled water + Heat

Filter with 40N paper

Filtrate Heat it +Add NH4Cl, 2-3gm

Residue Wash with hot Distilled water Dry (oven) + Ignite at 1000oC
For Isolate R2O3

Heat it +Add NH4Cl 2-3gm
Masking/ Oxidizing agent

Boil it + Add HNO3 (1:1), 0.5ml Add NH4OH (1:1)-ppt form Filter with 41N paper Filtrate in 500ml flask paper CaO & MgO Process next page Residue

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

paper Dry (oven) + Ignite at 1000oC R2O3= (F wt – I wt)*200

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

10

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-00 g/m Titrate with EDTA (ethylene di amine tetra acetate) Mwt-000 g/m (end colour red- pink to purple)
{0.0005608 X V1 X Vmu X 100} D.F. Volume taken X Sample weight = V1- EDTA Burette reading = Vmu- Volume make up = DF -

For- MgO
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 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-000 g/m (end colour red- pink to blue)
{0.0004032 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 -

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.

Reaction: = CaCl2 +(NH4)2C2O4 CaC2O4 +2NH4Cl = CaC2O4 + H2O CaC2O4.H2O CaO +CO2 +CO =

11

Iron (Raw material) -Dichromate method
0.5 gm sample + Fusion mix. In Platinum crucible Fuse in 1000oC minimum 30 min Cool and wash Pt. crucible with 1:1 HCl Wash crucible with Distilled water

Clinker sample
0.5 gm clinker sample dissolved in HCl -1:1

Boil & add SnCl2 Drop wise till colourless solution Completely cool (Room Temp.)

Add Barium di phenol Salfonate (BDS) Indicator Add 5-10 ml HgCl2 and Acid mixture –Masking agent Titrate with K2Cr2O7 Potassium dichromate Iron= B.R X Factor (K2Cr2O7)

Solution Preparation: =Acid mix.- 1 H2SO4+1 HCL +3 H2O = K2Cr2O7 – = BDS – = SnCl2 – = Fusion mix -

Reaction: = 2Fe3+ + Sn2+ = 2Fe2+ + K2Cr2O7

2Fe2+ + Sn4+ 2Fe3+

12

Free Lime in Clinker
Take 0.1 gm Clinker sample in beaker Add 10 ml Ethylene Glycol Put for 45 min in water bath Filter with 40N paper Filtrate Add Bromocrsol Grate Green Indicator Titrate with 0.1N HCL End Colour –Green to golden Yello F/CaO= B.R X 0.28

Solution Preparation:

Residue out

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

hcl

Phase of Clinker formation:
It is know that fuel economy or improved burnability in the formation of clinker can be effected through the following stage of clinker burning.

= Formation of 2CaO.Fe2O3 = Formation of 2CaO.Fe2O3.CaO.Fe2O3 = Formation of 2CaO.SiO2+2CaO.Al2O3 SiO2+Ferrite Phase = Formation of 2CaO.SiO2, 5CaO.3(Al2O3) 5CaO.Al2O3, 3CaO.SiO2, Ferrite Phase = Formation of 2CaO.SiO2, 3CaO.SiO2 12CaO.7Al2O3, SiO2+2CaO.Fe2O3, 3CaO.SiO2,
13

:- 800oC :-900oC :-1000oC :-1100oC :-1200oC

= Formation of 3CaO.Al2 O3, 3CaO.SiO2 2CaO.SiO2 + Ferrite Phase = Formation of 3CaO.Al2 O3, 3CaO.SiO2 2CaO.SiO2+ Ferrite Phase Effects of Various Factors on Raw mix Burnability: Characteristic /Modulus Silica modulus (SM) Limiting range 1.9-3.2 Preferable range 2.3-2.7

:-1300oC :-1400oC

Effects If SM High Result in hard burning, high fuel consumption, difficulty in coating formation, radiation from shell is high, deteriorates the kiln lining If AM High Impacts harder burning, high fuel consumption, Increases C3A decreases C4AF, reduces liquid phase & kiln output, if AM is too low and raw mix is without free silica, clinker sticking and balling is too high. A higher LSF Make it difficult to burn raw mix, increases C3S, reduces C2S, deteriorates refractory lining, increases radiation from shell, increases kiln exit gas temperature. A higher silica Increases fuel and power consumption, causes difficulty in coating formation, deteriorates refractory, increases radiation of heat kiln shell, A higher MgO Favours dissociation of C2S and CaO and lets C3S form quickly, tends the balling easy in the burning zone and affects kiln operation. A high alkali Improves burnability at lower temperature & deteriorates at higher, increase liquid content and coating formation, lowers the solubility of CaO in melt, breaks down alite & belite phases, creates operational problem due to external & internal cycle. A higher Sulphur compound Acts as an effective mineraliser and modifier of alkali cycle by forming less volatiles, A higher fluorides Leads to modify the kinetic of all burning reaction , lowers the temperature of C3S formation by 150-200 A higher chlorides Higher Cl forms more volatiles % causes operational problem due to its complete volatilization in burning zone, increases liquid formation & melting point of the absorbed phase is drastically change. ====0====

Alumina modulus (AM)

1.5-2.5

1.3-1.6

Lime saturation factor (LSF)

0.661.02

0.92-0.96

Free silica

0-3

As low as possible

MgO

0-5

0-3

Alkalies

0-1

0.2-0.3%

Sulphur compound Fluorides

0-4

0.5-2% 0.030.08%

0-0.6

Chlorides

0.06

Up to 0.015%

14

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