Influence of process on quality
And quality control on process
Why we maintain quality ?
It is need of the customer
Customer is the king .He sees us in quality price ratio
To day mason decides the quality but tomorrow engineer
will decide the quality in our country ( house construction
, etc)
What will happen to us ?
Customer is the king. He is a better business man than you.
Tomorrow’s market is competitive with quality/ price ratio.
Customer creates the customers.
Bon’t brand the quality alone , brand your service too.
Mining
crushing
preblending
Raw meal
preparation
Raw meal
blending
Pyro
process
Clinkercooling
Cement
grinding
Packing &
despatch
Process steps
Concern
for Environm
ent
Q
uality
control
Process flow diagram and integration of quality
Quality control
Variation makes the process and quality to struggle and custome
unhappy
customer
Mining
Well developed mines
Geology and location of boreholes
Bore
Hole
sample
Function of PGNA
Analyser
Cf 252
Variation is a devil
In any process
Lime saturation factor on clinker basis
If MgO is below 2 %
LSF = 100( CaO – free CaO+0.75 MgO)
(2.85 SiO2) + ( 1.18 Al2O3) +(0.65 Fe2O3)
If MgO is above 2 %
LSF = 100( CaO – free CaO+1.5 MgO)
(2.85 SiO2) + ( 1.18 Al2O3) +(0.65 Fe2O3)
95 – harder to burn, tendency to high free lime & C3S clinker
, high early strength high fuel consumption
< 95 , easy to burn , excess coating , excess liquid phase ,
possible brick infiltration reduced cement strength , low free lime
acceptable standard deviation = 1.2
Raw meal residue
Depends upon the
Mineralogy , ie
Calcite or quartz
90 mic = 8 – 15 %
212 mic = 0.5 – 3 %
time
Variation from
mines
Variation
After
pre blending
Variation after
Raw milling
Variation in quality control
Set point
Auto sampler position
- 20 mm
Liter weight
. Rapid burning ( short burning zone ) and rapid cooling of clinker
improves the clinker quality. smaller C3S crystals with
micro cracks)
Slow burning
Fast burning
C3S
Clinker when it is quenched in cooler it creates micro cracks which
needs less energy for comminution during grinding.
C3S
Clinker cooling
C2S
Reactions during clinker cooling
Resorption of alite
Liquid phase + C3S C2S + C3A + C2(A,F)
Decomposition of alite
very slow cooling
reducing conditions
C3S C2S + CaO
Crystallization of liquid phase
Slow cooling: large crystals – improved reactivity
MgO crystals grow on
cooling (periclase)
Properties of cement
• Portland cement
• Portland pozzolana cement
• Portland slag cement
• Sulfate resistant cement
• Oil well cement
• Rapid hardening cement
• White cement
Cement quality tests
• Setting time
• Compressive strength (mortar)
• Modulus of rupture ( bending strength)
• Fineness( blaine or Particle size distribution)
• Expansion ( Le Chatelier & Auto clave)
( soundness)
• Chemical analysis
X-4.0(100-
X) /100 <
35%
3.03.03.0Insoluble residue % (max)
0.8 -
1.02
0.8 -
1.02
0.66 -
1.02
LSF CaO- 0.7 SO3/(2.8S+1.2A+0.65F)
PPC53S53 Gr43 Gr
specifications
5.04.04.05.0LOI
3.03.03.03.0SO3 % max
6.05.06.06.0Magnesia ,MgO %,max
0.050.100.10Cl max
> 45C3S
10.0----C3A max
BIS specifications for various grades of cement
1051010.0Soundness ,LeChat expansion , (mm) max
30/60060/60030/60030/600Setting time, initial ( min) / final (max) ,
minutes
300.0370.0225.0225.0Fineness sqm /kg , min
162727233 days+/_ 1 hr
Compressive strength, Mpa , min
0.80.80.80.8Soundness, Autoclave %
0.15Drying shrinkage
3353534328 days +/ - 4 hrs
2237.533337 Days +/_ 2 hrs
Blaine apparatus air
permeability test
(Part - 5) Determination of Initial and Final Setting
Times4031 (Part-5)
Early stiffening – false set or flash set
If less gypsum no gypsum flash set occurs
If cement temperature > 130 deg c gypsum dehydrates and flash set occurs
Setting time ASTM specification
In concrete chemistry ettringite is a hexacalcium aluminate trisulfate hydrate, of
general formula: (CaO)6(Al2O3)(SO3)3·32H2O or; CaO)3(Al2O3)(CaSO4)3·32H2O
Influencing parameters on
Cement strength
1 3 7 28 90 days
Strength MPa
C3S
C2S
C3A
C4AF
60
0
20
30
40
50
= f (C3S)
28
7
3
1
MPa 70
60
50
40
30
20
10
40 45 50 55 60 65 % C3S
= f (Wk)
28
7
3
1
0
MPa 70
60
50
40
30
20
10
0 0.5 1.0 % Wk
A 1% increase in LOI
result in decrease in
strength
1 day by 25 %
2 8days by 3 % and
90 days by 2 %
Cement strength is measured in 1 day, 3 days ,7days and 28 days
Measurement compressive strength BIS 4031 (Part-8)1988(Part - 8)
Determination of Compressive strength of hydraulic Cement
Compression testing
50*50mm
Compressive strength – influencing parameters
Compressive strength
1 d 3 d 7 d 28 d
Influencing Normal range 5 – 15 20 – 35 30 - 45 45 - 60
Parameters OPC
C3S 45 – 65 % + + + +
C3A 6 – 12 % + + + +
Ks 0.2 – 1.5 % + + +/0/- -
SO3 2 – 4 % +/0/- +/0/- +/0/- +/0/-
Blaine 280 – 300 + + + +
m2/kg
Wk 0 - 0.3% - - - -
Quantitative rules of thumb
C3S : 1 – 28 d : + 0.5 Mpa / %
Ks ; 1 d : + 4 Mpa / %
: 3 d : + 4 Mpa / %
: 7 d : - 2 Mpa / %
: 28 d : - 10 Mpa / %
(SO3) tot : 1 - 28 d : - 5 Mpa / % from
optimum
Blaine : 1 d : + 0.04 Mpa / (m2/ kg)
3- 28 d : + 0.08 Mpa / (m2/ kg)
One day strength is contributed mainly by
C3A , Soluble alkalies, and C3S
3 day is contributed mainly by C3S
7 days strength is contributed by mainly
C3S
28 days strength is mainly contributed by
C2S
Apart from the above cement strength is enhanced by
higher fineness of cement
Less C3S crystal size achieved by rapid burning
and quenching the clinker in cooler
Higher fineness of rawmeal also reduces the
crystal size of clinker minerals , ie ., C3S & C2S which
enhances the hydraulic reactivity
Cement strength – influencing parameters
Wk , prehydration of clinker
Prehydration of clinker minerals can occur
1. As a result of incorrect internal water cooling in cement mill
2. when storing too hot cement in a silo
3. When clinker and especially cement is exposed to humidity
Please note:
If clinker has more soluble alkalis and sulfates it is highly
hygroscopic especially when pet coke is fired.
In cement silos they form Syngenite , K2SO4.2 CaSO4. H2O which
forms lumps and block the cement silos. Hence venting is must
to evacuate moisture and silo cleaning.
cements having soluble alkalis and sulfates preferably packed in
paper bags to avoid depletion of strength.
Thumb rule formulae for prediction of strength
FLS predicted the formula for cement ground to 300 kgs/ m2
With 4 % gypsum
strength,
d28 = 52 - 10.( Ks) + 0.15.(C3S)
The content of soluble alkalis Ks is dependent on the total alkali
content and SO3 content in clinker.
As per Knofel it is
F 28 = (3*C3S)+ (2*C2S) + C3A – C4AF N / mm2
Strength prediction
for 3 d = 97 + 35.8 Ma + 38.1K2SO4 + 28.7 Ms – 1.3 C3S Kg/ cm2
7 d = 300 + 13.4 Ms + 2.8 C2S + 56.1 Ma – 15.4 K2SO4 + 15.5 Na2O
28 d = 490 – 55.3 K2SO4 + 1.3 C3S (or)
= 490 – 86 K2O + 2 C3S – 26 Na2O
Influence of fineness on cement strength
For cements with the same specific surface the increase of the uniformity
factor results in increase of strength of all ages.
1. The specific surface , the percentage of fractions 3- 32 mm and the
uniformity factor n really influences the development of cement strength.
The influence of 3 - 32 mm fraction and the uniformity factor is higher in
cement with higher in specific surface ( > 3400 cm2/ g)
2. The fractions with particle size less than 3 mm contributes only to early
strength while the fraction with particle size more than 24 mm influences
strength development significantly.
3. While the fractions 3 – 16 mm and 16 – 32 mm seems to be more
significant factor for specific surface 3500 – 4000 cm2/ g) . This is
relevant only if the granulometric distribution is continuous and steep.
4. The optimistic granulometric distribution of a cement is a continuous
and steep ( with high uniformity factor) distribution with a high (65 %)
content in 3 – 32 mm fraction and specifically in 16 - 24 mm fraction and
low content of fine particles ( < 3 mm , 10 % ) and specific surface of
2500 – 3000 cm2/ g according to Blaine.( high efficiency separator and
grinding media distribution plays significantly here)
Properties of cement minerals
Characteristics C3S C2S C3A C4AF
Setting quick slow rapid nil
Hydration rapid slow rapid nil
3 days heat 1.1 cal / g 0.4 cal / g 2 cal / g nil
liberation
Early strength high upto low upto not much nil
Contribution 14 days 14 days beyond one day
Late strength less later high later nil nil
contribution
Resistance to moderate high poor high
Chemical attack
Drying shrinkage nil low nil nil
Measurement of expansion for free lime ( IS 4031 Part3 -1988
Expansion due to free CaO=< 10 mm
Auto clave test for
expansion of cement
(Part - 3)
Determination of
Soundness
198
8
4031
(Part-3)
25*25*282mm
Expansion limit < 0.8mm
Autoclave
Calorie
meter
Tube samplers for bulk cement
MgO Crystals
Or Periclase
Free lime clusters
Problems and solutions
1. Grinding problems
a) False set lower cement mill temperature
add less gypsum
add part anhydrite
b) reduced strength high mill temperature
less water cooling
correct water cooling
2. Silo storage
a) False set short storage time
cooling of cement < 70 deg c
b) reduced strength increase gypsum dehydration in
mill
c) lump formation and add less gypsum, use partly
silo blockage (syngenite anhydrate , decrease K2O content
formation, K2SO4.2CaSO4.H2O to avoid the formation of Syngenite
Problems solutions
3 ) Bag storage
a. reduced strength short storage time
b. lump formation add TEA during grinding
(tri ethanal amine)
add hydrophobic agents
c. crust formation plastic coated bags
d. abnormal setting plastic covering pallets
quality
Process
Quality is a set point and process is variable
Right
Process
quality
Process is a set point and quality is variable
wrong
Thanks you for your kind attention
And spending your valuable business hours
K.P.PRADEEP KUMAR
Sr.GM Operation
Karikkali works
Chettinad Cements Ltd

Influence of process on quality

  • 1.
    Influence of processon quality And quality control on process
  • 2.
    Why we maintainquality ? It is need of the customer Customer is the king .He sees us in quality price ratio To day mason decides the quality but tomorrow engineer will decide the quality in our country ( house construction , etc) What will happen to us ?
  • 3.
    Customer is theking. He is a better business man than you. Tomorrow’s market is competitive with quality/ price ratio. Customer creates the customers. Bon’t brand the quality alone , brand your service too.
  • 4.
  • 5.
    Process flow diagramand integration of quality Quality control
  • 6.
    Variation makes theprocess and quality to struggle and custome unhappy customer
  • 7.
  • 8.
    Geology and locationof boreholes Bore Hole sample
  • 11.
  • 13.
    Variation is adevil In any process
  • 16.
    Lime saturation factoron clinker basis If MgO is below 2 % LSF = 100( CaO – free CaO+0.75 MgO) (2.85 SiO2) + ( 1.18 Al2O3) +(0.65 Fe2O3) If MgO is above 2 % LSF = 100( CaO – free CaO+1.5 MgO) (2.85 SiO2) + ( 1.18 Al2O3) +(0.65 Fe2O3) 95 – harder to burn, tendency to high free lime & C3S clinker , high early strength high fuel consumption < 95 , easy to burn , excess coating , excess liquid phase , possible brick infiltration reduced cement strength , low free lime acceptable standard deviation = 1.2
  • 19.
    Raw meal residue Dependsupon the Mineralogy , ie Calcite or quartz 90 mic = 8 – 15 % 212 mic = 0.5 – 3 %
  • 21.
    time Variation from mines Variation After pre blending Variationafter Raw milling Variation in quality control Set point
  • 26.
  • 30.
  • 36.
    . Rapid burning( short burning zone ) and rapid cooling of clinker improves the clinker quality. smaller C3S crystals with micro cracks)
  • 37.
  • 39.
    C3S Clinker when itis quenched in cooler it creates micro cracks which needs less energy for comminution during grinding. C3S Clinker cooling C2S
  • 40.
    Reactions during clinkercooling Resorption of alite Liquid phase + C3S C2S + C3A + C2(A,F) Decomposition of alite very slow cooling reducing conditions C3S C2S + CaO Crystallization of liquid phase Slow cooling: large crystals – improved reactivity MgO crystals grow on cooling (periclase)
  • 56.
  • 58.
    • Portland cement •Portland pozzolana cement • Portland slag cement • Sulfate resistant cement • Oil well cement • Rapid hardening cement • White cement
  • 59.
    Cement quality tests •Setting time • Compressive strength (mortar) • Modulus of rupture ( bending strength) • Fineness( blaine or Particle size distribution) • Expansion ( Le Chatelier & Auto clave) ( soundness) • Chemical analysis
  • 60.
    X-4.0(100- X) /100 < 35% 3.03.03.0Insolubleresidue % (max) 0.8 - 1.02 0.8 - 1.02 0.66 - 1.02 LSF CaO- 0.7 SO3/(2.8S+1.2A+0.65F) PPC53S53 Gr43 Gr specifications 5.04.04.05.0LOI 3.03.03.03.0SO3 % max 6.05.06.06.0Magnesia ,MgO %,max 0.050.100.10Cl max > 45C3S 10.0----C3A max BIS specifications for various grades of cement
  • 61.
    1051010.0Soundness ,LeChat expansion, (mm) max 30/60060/60030/60030/600Setting time, initial ( min) / final (max) , minutes 300.0370.0225.0225.0Fineness sqm /kg , min 162727233 days+/_ 1 hr Compressive strength, Mpa , min 0.80.80.80.8Soundness, Autoclave % 0.15Drying shrinkage 3353534328 days +/ - 4 hrs 2237.533337 Days +/_ 2 hrs
  • 62.
  • 66.
    (Part - 5)Determination of Initial and Final Setting Times4031 (Part-5) Early stiffening – false set or flash set If less gypsum no gypsum flash set occurs If cement temperature > 130 deg c gypsum dehydrates and flash set occurs
  • 67.
    Setting time ASTMspecification
  • 68.
    In concrete chemistryettringite is a hexacalcium aluminate trisulfate hydrate, of general formula: (CaO)6(Al2O3)(SO3)3·32H2O or; CaO)3(Al2O3)(CaSO4)3·32H2O
  • 69.
  • 70.
    1 3 728 90 days Strength MPa C3S C2S C3A C4AF 60 0 20 30 40 50
  • 71.
    = f (C3S) 28 7 3 1 MPa70 60 50 40 30 20 10 40 45 50 55 60 65 % C3S
  • 72.
    = f (Wk) 28 7 3 1 0 MPa70 60 50 40 30 20 10 0 0.5 1.0 % Wk A 1% increase in LOI result in decrease in strength 1 day by 25 % 2 8days by 3 % and 90 days by 2 %
  • 73.
    Cement strength ismeasured in 1 day, 3 days ,7days and 28 days Measurement compressive strength BIS 4031 (Part-8)1988(Part - 8) Determination of Compressive strength of hydraulic Cement
  • 75.
  • 76.
    Compressive strength –influencing parameters Compressive strength 1 d 3 d 7 d 28 d Influencing Normal range 5 – 15 20 – 35 30 - 45 45 - 60 Parameters OPC C3S 45 – 65 % + + + + C3A 6 – 12 % + + + + Ks 0.2 – 1.5 % + + +/0/- - SO3 2 – 4 % +/0/- +/0/- +/0/- +/0/- Blaine 280 – 300 + + + + m2/kg Wk 0 - 0.3% - - - -
  • 77.
    Quantitative rules ofthumb C3S : 1 – 28 d : + 0.5 Mpa / % Ks ; 1 d : + 4 Mpa / % : 3 d : + 4 Mpa / % : 7 d : - 2 Mpa / % : 28 d : - 10 Mpa / % (SO3) tot : 1 - 28 d : - 5 Mpa / % from optimum Blaine : 1 d : + 0.04 Mpa / (m2/ kg) 3- 28 d : + 0.08 Mpa / (m2/ kg)
  • 78.
    One day strengthis contributed mainly by C3A , Soluble alkalies, and C3S 3 day is contributed mainly by C3S 7 days strength is contributed by mainly C3S 28 days strength is mainly contributed by C2S Apart from the above cement strength is enhanced by higher fineness of cement Less C3S crystal size achieved by rapid burning and quenching the clinker in cooler Higher fineness of rawmeal also reduces the crystal size of clinker minerals , ie ., C3S & C2S which enhances the hydraulic reactivity Cement strength – influencing parameters
  • 79.
    Wk , prehydrationof clinker Prehydration of clinker minerals can occur 1. As a result of incorrect internal water cooling in cement mill 2. when storing too hot cement in a silo 3. When clinker and especially cement is exposed to humidity Please note: If clinker has more soluble alkalis and sulfates it is highly hygroscopic especially when pet coke is fired. In cement silos they form Syngenite , K2SO4.2 CaSO4. H2O which forms lumps and block the cement silos. Hence venting is must to evacuate moisture and silo cleaning. cements having soluble alkalis and sulfates preferably packed in paper bags to avoid depletion of strength.
  • 80.
    Thumb rule formulaefor prediction of strength FLS predicted the formula for cement ground to 300 kgs/ m2 With 4 % gypsum strength, d28 = 52 - 10.( Ks) + 0.15.(C3S) The content of soluble alkalis Ks is dependent on the total alkali content and SO3 content in clinker. As per Knofel it is F 28 = (3*C3S)+ (2*C2S) + C3A – C4AF N / mm2 Strength prediction for 3 d = 97 + 35.8 Ma + 38.1K2SO4 + 28.7 Ms – 1.3 C3S Kg/ cm2 7 d = 300 + 13.4 Ms + 2.8 C2S + 56.1 Ma – 15.4 K2SO4 + 15.5 Na2O 28 d = 490 – 55.3 K2SO4 + 1.3 C3S (or) = 490 – 86 K2O + 2 C3S – 26 Na2O
  • 81.
    Influence of finenesson cement strength For cements with the same specific surface the increase of the uniformity factor results in increase of strength of all ages. 1. The specific surface , the percentage of fractions 3- 32 mm and the uniformity factor n really influences the development of cement strength. The influence of 3 - 32 mm fraction and the uniformity factor is higher in cement with higher in specific surface ( > 3400 cm2/ g) 2. The fractions with particle size less than 3 mm contributes only to early strength while the fraction with particle size more than 24 mm influences strength development significantly. 3. While the fractions 3 – 16 mm and 16 – 32 mm seems to be more significant factor for specific surface 3500 – 4000 cm2/ g) . This is relevant only if the granulometric distribution is continuous and steep. 4. The optimistic granulometric distribution of a cement is a continuous and steep ( with high uniformity factor) distribution with a high (65 %) content in 3 – 32 mm fraction and specifically in 16 - 24 mm fraction and low content of fine particles ( < 3 mm , 10 % ) and specific surface of 2500 – 3000 cm2/ g according to Blaine.( high efficiency separator and grinding media distribution plays significantly here)
  • 82.
    Properties of cementminerals Characteristics C3S C2S C3A C4AF Setting quick slow rapid nil Hydration rapid slow rapid nil 3 days heat 1.1 cal / g 0.4 cal / g 2 cal / g nil liberation Early strength high upto low upto not much nil Contribution 14 days 14 days beyond one day Late strength less later high later nil nil contribution Resistance to moderate high poor high Chemical attack Drying shrinkage nil low nil nil
  • 83.
    Measurement of expansionfor free lime ( IS 4031 Part3 -1988 Expansion due to free CaO=< 10 mm
  • 84.
    Auto clave testfor expansion of cement (Part - 3) Determination of Soundness 198 8 4031 (Part-3) 25*25*282mm Expansion limit < 0.8mm
  • 85.
  • 87.
    Tube samplers forbulk cement
  • 88.
  • 90.
  • 92.
    Problems and solutions 1.Grinding problems a) False set lower cement mill temperature add less gypsum add part anhydrite b) reduced strength high mill temperature less water cooling correct water cooling 2. Silo storage a) False set short storage time cooling of cement < 70 deg c b) reduced strength increase gypsum dehydration in mill c) lump formation and add less gypsum, use partly silo blockage (syngenite anhydrate , decrease K2O content formation, K2SO4.2CaSO4.H2O to avoid the formation of Syngenite Problems solutions
  • 93.
    3 ) Bagstorage a. reduced strength short storage time b. lump formation add TEA during grinding (tri ethanal amine) add hydrophobic agents c. crust formation plastic coated bags d. abnormal setting plastic covering pallets
  • 94.
    quality Process Quality is aset point and process is variable Right
  • 95.
    Process quality Process is aset point and quality is variable wrong
  • 96.
    Thanks you foryour kind attention And spending your valuable business hours K.P.PRADEEP KUMAR Sr.GM Operation Karikkali works Chettinad Cements Ltd