Short Notes of Cement Chemistry NARENDRA KUMAR KANCHKAR Quality Controller(Cement) Controller(Cement)
[email protected]
Cement History: Joseph Aspdin took out a patent in 1824 for "Portland Cement," a material he produced by firing finelyground clay and limestone until the limestone !as calcined #e called it Portland Cement because the concrete made from it looked like Portland stone, a !idelyused building stone in $ngland %n 184&, %saac Johnson made the first modern Portland Cement by firing a mi'ture of chalk and clay at much higher temperatures, similar to those th ose used today At these temperatures (14))C1&))C*, clinkering occurs and minerals form !hich are +ery reacti+e and more strongly cementitious e+elopment of rotary kilns Addition of gypsum to control setting -se of ball mills to grind clinker and ra! materials ma terials .otary kilns gradually replaced the original +ertical shaft kilns used for making lime from the 18/)s .otary kilns heat the clinker mainly by radiati+e heat transfer and this is more efficient at higher temperatures, enabling higher burning temperatures to be achie+ed Also, because the clinker is constantly mo+ing !ithin the kiln, a fairly uniform clinkering temperature is achie+ed in the hottest part of the kiln, the burning 0one he t!o other principal technical de+elopments, gypsum addition to control setting and the use of ball mills to grind the clinker, !ere also introduced at around the end of the 1/th century %n india first cement plant installation at Porbandar (u3rat* in 1/14
Cement Definition: Cement is a binder, a substance that sets and hardens independently, and can bind other materials together such as sand, bricks (ci+il material* Cement is defined as a hydraulic binder !hich !hen mi'ed !ith !ater forms a paste !hich sets and hardens by mass of hydration reaction and processes and !hich after hardening, retains its strength and hardening e+en under !ater, Cement used in construction is characteri0ed as hydraulic or non-hydraulic #ydraulic cements (Portland cement* harden because of hydration chemical reactions that occur independently of the mi'tures !ater content5 they can harden e+en under!ater or !hen constantly e'posed to !et !eather he chemical reaction that results !hen the anhydrous cement po!der is mi'ed !ith !ater produces hydrates that are not !atersoluble 6aterial made by heating a mi'ture of limestone and clay in a kiln at about 14&) C, then grinding to a fine po!der !ith a small addition of gypsum Combination of C7A, C7, C2, C4A9 and mi' gypsum in fe! :uantity is called cement
1
Cement Manufacturing Technologies: Wet Process Dry Suspension (SP) Process Dry Pre calciner (PC) Process (Present time use)
• • •
Wet Process: These 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 Process: In SP plant, the ground raw meal is feed to a four f our 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 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 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. 2. 3. 4. 5. 6.
1F& 2F 1E& 2E 1D & 2D 1C & 2C 1B & 2B 1A & 2A
280-332OC 370-420OC 540-600 OC 630-710 OC 770-850 770-850 C 857-890 OC
30-33 % 25-30 % 20-25 % 15-20 % 10-15 10-15 % 2-5 %
10 % 23 % 40 % 55 % 24 % 90-95 %
4 Zone occurs in kiln: -1.Dehydration Zone(1100OC) 2. Calcinations Zone(1250 OC)3. Clinkersition Zone O
O
(1400 C) 4. Cooling Zone.(1000 C) 2
*Examples of raw materials for portland cement manufacture. Calcium Silicon Aluminum Iron Coal Limestone Clay Clay/Bauxite Clay Anthracite Marl Marl Shale Iron ore Bituminous Calcite Sand Fly ash Mill scale Lignite Aragonite Shale Aluminium ore refuse Shale Pith Shale Fly ash Blast furnace dust Pet Cock
Sea Shells
Rice hull ash
Cement kiln dust
Slag
*Summary of the different ways to represent some cement minerals and products.
Chemical Name
Chemical Formula Oxide Formula
3CaO.Al2O3
Cement Notation C3S C2S C3A
Mineral Name Alite Belite Aluminate
Tricalcium Silicate
Ca3SiO5
3CaO.SiO2
Dicalcium Silicate
Ca2SiO4
2CaO.SiO2
Tricalcium Aluminate
Ca3Al2O6
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
Calcium oxide
CaO
C
CaO
H2
Gypsum Lime
Reaction Occurring in Pre heater to kiln:
1. 2. 3. 4. 5. 6. 7.
Evaporation of free water Release of combine water from clay Dissociation of magnesium carbonate Dissociation of Calcium carbonate Dissociation of lime and clay Commencement Commencement of liquid formation Further formation of liquid and completion Of clinker compound
- 100oC - 500 oC - 900 oC o - above900 C o o - 900 C-1200 C o o - 1200 C-1280 C o - above1280 C
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.
:- 800oC :-900oC :-1000oC
= Formation of 2CaO.Fe 2O3 = Formation of 2CaO.Fe 2O3.CaO.Fe2O3 = Formation of 2CaO.SiO2+2CaO.Al 2O3 SiO2+Ferrite Phase = Formation of 2CaO.SiO2, 5CaO.3(Al 2O3) 5CaO.Al2O3, 3CaO.SiO2, Ferrite Phase = Formation of 2CaO.SiO2, 3CaO.SiO2
:-1100oC :-1200oC 3
12CaO.7Al2O3, SiO2+2CaO.Fe 2O3, 3CaO.SiO2, = Formation of 3CaO.Al 2O3, 3CaO.SiO2 2CaO.SiO2 + Ferrite Phase = Formation of 3CaO.Al 2O3, 3CaO.SiO2 2CaO.SiO2+ Ferrite Phase
:-1300oC :-1400oC
Effects of Various Factors on Raw mix Burnability:
Characteristic /Modulus
Limiting range
Preferable range
Silica modulus (SM)
1.9-3.2
2.3-2.7
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
0-4
0.5-2%
Fluorides
0-0.6
0.030.08%
Chlorides
0.06
Up to 0.015%
Effects If SM High Result in hard burning, high hi gh 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, form ation, deteriorates refractory, increases 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. 4
Phase data for a Type I OPC paste made with a w/c of 0.45. 3
Volume % At Mixing Mature Paste 23.40 1.17 7.35 0.78
Phase C3S C2S C3A
Density (g/cm ) 3.15 3.28 3.03
4.42
0.00
C4AF Gypsum (CH2)
3.73
2.87
1.39
2.32
3.47
0.00
C-S-H (solid) C-S-H C-S-H (with (with gel gel pores) pores) Portlandite (CH)
2.65
0
29.03
1.90
0
49.99
2.24
0
13.96
Ettringite (AFt) Monosulfoaluminate (AFm) Water Gel porosity Capillary porosity
1.78
0
6.87
2.02
0
15.12
1.00
58.49
31.69
--
0
20.96
--
58.49
10.73
a
$R%D&CT' Bulk Density:(RAW !"NA# $R%D&CT' 3
3
3
Cilnker = 130 !g"# $%y&s' = 1.3 #t"# $ *ron = 2+00 !g"# $,ie stone = 1400 !g"# 3 3 3 3 ly ash = 550 !g"# $Coal = 50 !g"# $ and = 100 !g"# $Cock = 40-40 !g"# $ 3 3 Ceent = 1500 !g"# $/a eal = 1250 !g"# $
3
$roerties of the ma)or cement minerals: About 90-95% of a Portland cement is comprised of the four main cement minerals, which are C 3S, C2S, C3A, and C 4AF, 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 C 3S and the C 2S contribute virtually all of the beneficial properties by generating the main hydration product, C-S-H gel. However, the C 3S hydrates much more quickly than the C 2S and thus is responsible for the early strength development. The C 3A and C 4AF 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 C 3S gives cement pastes most of its strength, particularly at early times. Pure C3S can form with three different crystal structures. At temperatures below 980˚C the equilibrium structure is triclinic. At temperatures between 980˚C – 1070˚C the structure is monoclinic, and above 1070˚C it is rhombohedral. In addition, the triclinic and monoclinic structures each have three polymorphs, so there are a total of seven possible structures. However, all of these structures are rather similar and there are no significant differences in the reactivity. The most important feature of the structure is an awkward and asymmetric packing of the calcium and oxygen 5
ions that leaves large “holes” in the crystal lattice. Essentially, the ions do not fit together very well, causing the crystal structure to have a high internal energy. As a result, C 3S is highly reactive. The C3S that forms in a cement clinker contains about 3-4% of oxides other than CaO and SiO 2. 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, Al 2O3, and Fe 2O3, 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 C 3S. There exist seven known polymorphs between room temperature and 1070 oC: three triclinic (denoted with T), three monoclinic (M) and one rhombohedral (R) polymorph. Due to incorporations in the alite crystal lattice, M 1 and M3 polymorphs are present mostly in industrial clinker. Cooling clinker from 1450oC, inversion of the R polymorph to M 3 and further more to M1 occurs, forming small crystals (M3) rich in substituents or large crystals, poor in substituted ions (M 1). Especially, high MgO- concentrations promote high nucleation, resulting in formation of small automorphic M 3- 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. structure. An important aspect of C 2S is that γ -C -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 form is never present in portland cement. The crystal structure of β−C2S is irregular, but considerably less so than that of C 3S, and this accounts for the lower reactivity of C 2S. The C 2S in cement contains slightly higher levels of impurities than C 3S. According to Taylor, the overall substitution of oxides is 4-6%, with significant amounts of Al 2O3, 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
Tricalcium Aluminate (C3A) Tricalcium aluminate (C3A) comprises anywhere from zero to 14% of a portland cement. Like C 3S, it is highly reactive, releasing a significant amount of exothermic heat during the early hydration period. Unfortunately, the hydration products of formed from C 3A contribute little to the strength or other engineering properties of cement paste. In certain environmental conditions (i.e., the presence of sulfate ions), C 3A 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 C 3S, 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 C 3A in portland cement clinker, which typically contains about 13% oxide substitution, is primarily cubic, with smaller amounts of orthorhombic C 3A. The C 3A 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 SiO 2, ~5% substitution of Fe2O3, and about 1% each of Na 2O, K2O, and MgO. The orthorhombic form has similar levels, but with a greater (~5%) substitution of K 2O. 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 C 4AF in cement clinker is generally higher in aluminum than in iron, and there is considerable substitution of SiO 2 and MgO. Taylor. reports a typical composition (in normal chemical notation) to be Ca 2AlFe0.6Mg0.2Si0.15Ti0.5O5. 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. 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 t he mineral oxide compositions given in Table 3.5 results in the following set of equations: 0.716C 3 + 0.635C 2 + 0.566C 3 = = 62.52 (C) 3S + 2S 3A + 0.475C 4 4AF 0.252C 3 + 0.315C 2 + 0.037C 3 = = 21.34 (S) 3S 2S + 3A + 0.036C 4 4AF 0.010C 3 + 0.021C 2 + 0.313C 3 = 4.40 (A) 3S + 2S + 3A + 0.219C 4 4AF 0.007C 3 + 0.009C 2 + 0.051C 3 = = 3.07 (F) 3S + 2S + 3A + 0.214C 4 4AF a
Formula =1.7C-S-4H. b Formula =1.7C-S-1.6H.
+
Rate of Clinker Phase on Properties of Cement: C3A Rapid Rapid High-1day 207
C3S Quick Fast High-14 day Less 120
C2S Slow Slow Low High 62
C4AF Rapid 100
Setting time Hydration Early strength Late strength Heat of Hydration(cal/g) Poor Moderate High High Resistance to Chemical attack low Dying Shrinkage 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.
Secification of *arious Tye of Cement:
TYPE OF CEMENT
LOI
MgO
5%Mx
6%Mx
5% Mx
6%Mx
4%Mx
6%Mx
Low heat cement Rapid hardening Sulphate Resisting Masonary Cement Hydrophobic cement Super sulphate White cement
5% Mx
6%Mx
-
6%Mx
5% Mx
6%Mx
-
6%Mx
5% Mx
6%Mx
-
10%M x
-
6%Mx
PSC
5% Mx 5% Mx
33 G 43 G 53 G
PPC
8%Mx 6%Mx
IR
4% Mx 3% Mx 3% Mx 4% Mx 4% Mx 4% Mx 4% Mx 4% Mx 2% Mx 5% Mx O/# ,
SO3
Finenes s 2 (M /Kg)
3%Mx
>225
3%Mx
>225
3%Mx
>225
3%Mx
>320
3%Mx
>325
2.5% Mx
>225
3%Mx
15%Mx in 45M
3%Mx
Soundnes s LechateAuto Clave 10mm0.8% 10mm0.8% 10mm0.8% 10mm0.8% 10mm0.8% 10mm0.8%
Setting Time IST- FST
Compressive Strength 3 7 28 2 Days(N/mm )
30-600
16
22
33
30-600
23
33
43
30-600
27
37
53
60-600
10
16
35
30-600
27
-
-
30-600
10
16
33
10mm -1%
90m-24H
-
3
5
>350
10mm0.8%
30-600
16
22
31
1.5% Mx
>400
5mm - ---
30-600
15
22
30
-
>225
30-600
15
20
30
3%Mx
>225
30-600
16
22
33
3%Mx
>300
30-600
16
22
33
Special Test:PPC –Drying Shrinkage 0.15%max,
10mm0.8% 10mm0.8% 10mm0.8%
"mortant !ormula &se in Cement Analysis+ Hydraulic Modulus: HM =
Silica Ratio:
Alumina Ratio: Or Iron Modulus
SM =
AM =
CaO SiO2 + Al2O3 +Fe2O3
(Typical Range: 1.7 to 2.3)
SiO2 Al2O3 +Fe2O3
(Typical Range: 1.8 to 2.7)
Al2O3 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 Alumina modulus >0.64) LSF = CaO 2.8 SiO2 + 1.65Al 2O3 +0.35Fe2O3
(Typical Range: 92 to 108)
Lime saturation saturation Factor: (if Alumina modulus 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 SiO 2+ 6.718 Al 2O3 +1.43Fe2O3+2.8SO3)Note: CaO = CaO - F/CaO C2S = 2.867 SiO 2 - 0.7544 C 3S C3A = 2.65 Al 2O3 - 1.692 Fe 2O3 C4AF = 3.043 Fe 2O3 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 SiO 2 + 4.479 Al2O3 +2.86Fe2O3) C2S = 2.867 SiO 2 - 0.7544 C 3S C3 A = 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 SiO 2+ 6.718 Al 2O3 +1.43Fe2O3+2.85 SO3) C2S = 2.867 SiO 2 - 0.7544 C 3S C3A = 2.65 Al 2O3 - 1.692 Fe 2O3 C4AF = 3.043 Fe 2O3
Bogus Factor :as per duda book C4AF = C4AF/ Fe2O3 = 486/160=3.043, 486/160=3.043, C3A = C3A / Al2O3 = 270/102= 2.65 , C3A/ Fe2O3 = 270/160= 1.69, C2S = C2S /SiO2= 172/60=2.87 ,C2S /C3S= 172/228=0.75, C3S = C3S/ CaO = 228/56= 4.07,
LSF =
Liquid Value:
LV= 1.13C3A +1.35C4AF + MgO +Alkalies Burnability Index: BI =
C 3S 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: =
Ash absorption:
=
Coal feed X 100 Clinker Production % of ash in fuel X coal consumption 100
Raw meal to clinker factor: =
Specific Heat:
V=
100-ash absorption 100-LOI
NCV X % of coal Consumption 100
Insoluble Residue: IR (max %) = X+4 (100-X) 100 Blain : Blain = √Time X Factor Factor = STD Blain √Time
(Note: X= % of Fly ash)
10
CYCLONE LOSS:
=
100(! loss Cyclone loss) (100 Cyclone loss) ! loss
Clinker to cement factor:
=
100
Clink.6lyash"lag6additi7es(kg) Clinker cons'ed (kg)
Chemical Composition (General): LOI
SiO2
Al2O3
Fe2O3
CaO
MgO
PPC
5.0
31.0
4.5
3.5
43.0
5.0
Clinker
0.5
21-22
5-6
3-5
62-65
3-6
Limestone
34
12
2.4
1.6
43.0
3.8
Iron Ore
10
13
14
71
1
1.5
16
14
1
1
34
5mx
50-60
20-33
2-7
2-10
Na2O
SO3
+K2O
F/ CaO
1.4
-
.5-1.0
.2-1.0
.5-2
1
.5
42
5 Mx
1.5mx
2.75mx
C3S
C2S
C3A
C4AF
48
28
8
12
Letrite Gypsum Mni Gyps Fly ash
!"sical Anal"sis o# C: 898- /esid'e (sie7e)$ :lain$ ;oral consistence$ e tting tie$ Co&ressi7e strength$ o'ndness-(C<,C) Blain (* -4031 &art-2) = 300 #2"kg ini'
NC$SC
Se%%in& %i'e
S%ren&%!
Au%o cla(e
Le)c!a%e
art-4 0 0 2+ C ± 2 C
art-5 0 0 2+ C ± 2 C
art- 0 0 2+ C ± 2 C
art-3 0 0 2+ C ± 2 C
art-3 0 0 2+ C ± 2 C
5> ± 5$ ;ot less than 0> 300"400 g
5> ± 5$ ;ot less than 0>
5> ± 5$ ;ot less than 0>
300"400 g
5> ± 5$ ;ot less than 0> 100 g
Req.waterX100 sample weight Aicat a&&arat's
;C?0.5?.@t 100 Aicat a&&arat's
200g-c$ 00g-1s62s63s (;C63) ?00 4 100 AiBrating < C8
5> ± 5$ ;ot less than 0> 300"400 g =;C
;C?0.+?.t 100 @ater :ath o 100 C
E50en1 /i'e
s &ossiBle 7icat /eading 5-+ c
s &ossiBle 7icat /eading 5+ c
O%!er
se needle 10 0-+0
se needle 2<5 0-+0 *nitial 30 in ini' inal-00 in ai'
*S) 4+,La. /e'0%ure La.$C!a'.er R)Hu'i1i%" Sa'0le 2ei&!% 3a%er Reuire'en% A00ara%us
Cu.e si6e *S Reuire'en%
+2 ±1hour- 16mpa 1 ±2hour-22mpa +2 ±4hour- 33mpa (#a=;"!g?0.2032) %a'ging 1in dry$ 4 in et +0 3 day- 16mpa + day- 22mpa 2 day- 33mpa 11
C achine 0 215 C$ 2 21 kg"c /-C-24ho'r C#-3 o'r
%a'ging 5 in 25$250 0. > a
@:-24ho'r .@:-3 o'r
35 10 a
7LY ASH Anal"sis 8*S)-99; 898- :,*; (#ini' 320)$,ie /eacti7ity(in. 4.5 #a)$ Dry hrinkage (a .15)$ Co&arati7e trength (;ot less than 0>)
Li'e Reac%i(i%" La. /e'0< $RH /es% S0eci'en
Dr" S!rinka&e
O
O
Reuire 3a%er 8/a.le 7lo2; A&e o# /es%in&
2+ C ± 2 " 5> ± 5
2+ C ± 2 " 5> ± 5
50
25"250
50
0.2; E0. E3 oFF E Ce ent E and 0;E240E00g
0.2; E0. E3 oFF E Ceent E and 100;E400E1500g
0. E3 Ceent E and 400E1500g
+0 ± 5> ith 10 dro& in 0 econd
100-115> ith 25 dro& in 15 econd
105 ± 5> ith 25 dro& in 15 econd
10 Day
35 Day
+$2$0 Day
3$+$2$ Day
24 ho'r ho'r / chaBer O (2+±2 C
)
24 ho'r / chaBer O (2+ C)
24 ho'r ho'r / chaBer O (2+±2 C)
2day / chaBer O (2+±2 C)
/es%in& Con1i%ion
O
2+ C ± 2 " 5> ± 5
1E 2#E . ,ieE oFFE and 150E300#E1350g
Reuire Sa'0le
Co'0ara%i(e S%ren&%!
day ater tank-* O (2+±2 C 2day 9n7ironent ChaBer
day 9n7ironent CB. O (50±2 C)
(2+±2 C< 50>)-** O
+$2$0day ater tank O (2+±2 C)
#=&eciHic gra7ity oH oFF .
;=&eciHic gra7ity oH oFF .
2 dya not less than 0> to Blank strength ;=&eciHic gra7ity oH oFF .
&eciHic gra7ity oH . lie
&eciHic gra7ity oH ceent
&eciHic gra7ity oH ceent
Dry shrinkage= **)*
+$2$0day ater tank O (2+±2 C) :lank trength
S/* 8Sc!e'e o# %es%in& ins0ec%ion; or-1EFORMAT 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
or-2ERAW 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
or-3EPRODUCTION DATA (POST GRINDING DETAILS OF PRODUCTION ACCEPTED & REJECTEDFOR ISI MARK) Shift
Quantity
Passed for ISI Marking
Rejected
Remarks
or-4-EPOZZOLANA (One sample per week) Column 6 of Table 1A (A) Calcined clay p ozzolana Date
Fitness
Lime Reactivity
CompressiveStrength at 28 Days
Drying ShrinkageMax
or-4-: EFLY ASH POZZOLANA (See Column 6 of Table 1 A) SO2+A1203
SiO2
MgO
SO3
Na2O
LOI
Fineness
12
Lime
Compressive
Drying
Soundness
+Fe203
sulphur
reactivity
Strength
Shrikage
Auto clave
or-5ECLINKER (DAILY COMPOSITE SAMPLE) (See Column 6 of Table 1A) Laboratory Ball-Mill Testing is required to b e done when there is change in the source of Raw Material or change in design Date of Total Insoluble SiO2 CaO AlO FeO SO MgO LSFLime Alunin Sample Disposa manuacture loss of Residue Saturation a Pass/Fails l/ Ignition Factor Factor Action
--ECLINKER GROUND WITH GYPSUM (Daily composite sample) (Note under Column 6 of Table 1 A) Date of Grinding
Fineness
Soundness
Setting time
Compressive Strength
AC
IST
3day-
-
LC
- FST
7day-
Sample Pass//fail
28day
Disposal/Actio n taken if sample sample fails
or--:ECLINKER GROUND WITH GYPSUM & POZZOLANA (Column 6 of Table I A) Date of Grinding
Fineness
Soundness
Setting time
Compressive Strength
AC
IST
3day-
-
LC
- FST
7day-
28day
Dry shrinkage (Weekly)
Sample Pass/fail
Disposal/Ac tio
or-+E PORTLAND POZZOLANA CEMENT GRINDING/ B LENDING (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
or-EPORTLAND 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
or-EPORTLAND POZZOLANA POZZOLANA CEMENT PACKING STAGE (Daily/Weekly Composite Samples) (Column 6 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)
of Table 1B)
Sample Pass /Fail
Mode of disposal/Ac tion taken if sample fails
or-10E(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 provi ng 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 5,10,15,20
Reading-1
R-2
R-3
Average 1+2+3/ 3
True Load =app. load*avg. load /Std. difference
Error %
Std. Differ.
=true.Load-app.Load)*100 /applied load
Autoclave pressure gauge - Once in a six months either by licensee’s l icensee’s own dead weight Pressure gauge or from Lab or manufacturer of such such Approved independent agency /NABL accredited Lab gauge having NPL certified calibrator.( dead weight Pressure gauge in 4year)
13
Vibration machine - Once in a month by licensee’s own tachometer. The tachometer shall be calibrated once in three Years from approved out Side agency /NABL accredited Lab Lab having NPL certified calibrator. (12000 ± 400 RPM)
Chemical analysis
rd
Type of analysis: 1 Gravimetric- IR, SO3, SiO2, R2O3 (Residual Oxide/3 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:-
Molaritiey:
Molecular weight Removal OH- ion
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 = Density = Mass Volume
N 1V1 =N2V2
"mortant Molecular ,eight+ O-1$
;a-23$
CaCO3 =100$ C3S=228,
#g-24$
iO2=0$ C2S= 172,
l-2+$
i-2$ -32$
l2O3=102$ C3A= 270,
Cl-34$
Fe2O3 =160, C4AF= 486,
14
!-3$ Ca-40$
e-55.$
MgO= 40, Na2O= 62, CaSO4.2H2O =145
Zn-5.3 K2O = 94
Lime Stone- TC&MC Take 50 ml HCL (0.4N) in conical Flask
Add 1.0 gm lime stone sample
Solution use: = NaOH (0.2N) / 1000= 40(Mwt)*0.2(N)*1000(ml) / 1000= 8gm/L = HCL(0.4N) 36.46(Mwt)*100 / 35.4(Purity)=87.28ml/L-1N 35.4(Purity)=87.28ml/L-1N =87.28ml/L-1N* 0.4 (Req.N)=34.91 ml/L
= *ndicator dissol7ed in lcohol
:oil ini' 2in
dd *ndicatorhyno&thleen C2014O4 #t-31.33$&-.2-.
Cool
8itrate ith ;aO (0.2;) slo2 %i%ra%ion 9nd &oint hite to &ink colo'r
8ake ;aO :'rette reading
8C = 100-:'rette reading
dd ecess10"20l ;aO 0.2 ;aO 0.2; :oil aBo't 1in.
dd *ndicator-
Calculation: CC = TC – MC CaO = CC / 1.786 MgO = MC / 2.09
8hyo&thleen
Cool 8itrate ith C, (0.4;)
7as% %i%ra%ion 9nd &oint &'r&le to hite- &ink
8ake C, :'rette
#C = I9.;aO I9.;aO-J2?C,-:/KL -J2?C,-:/KL 0.4
reading
Q.1 why multiply 1.786 for CaO? = CaO/CaCo3 Q.2 why multiply 2.09 for MgO? = MgO/MgCo3 Q.3 why multiply 0.84 for MC? 15
Cement- IR & SO3
or cid reaction
1.0 gm cement sample Dissol7ed 1:1 HCL
Solution use: = 2N- Na2CO3= 10.6 gm sodium carbonate dissolved in 100 ml distilled water (Eq.wt = 53, Mwt 105.99 g/mol) = 1:1 HCL = 50 ml HCL dissolved in 50 ml Distil water.(Mwt 36.46 g/mol) = BaCl2 = 10 gm BaCl2 BaCl2 dissolved in 100 ml ml distilled water.
Heat below boils Tem Tem . 15 15 minu minute te Filter- 40 N. paper
Wash Hot water Filtrate
Residue
:oil 6 add hot :aCl2
React with Na2CO3 -30 ml
or :ase reaction
10 l loly Cool Hor &&t
Heat 10 minute below boil temp.
Hor (4 ho'r)
Filter- 40 N. paper
or lkali
ilter 42 ; &a&er
Wash with 1:99 HCl & Hot water
Wash Hot water
Dryad in Oven
Dryad in Oven
Ignited at 1000oC Minimum 30 min
Ignited at 1000oC
reo7e
Weight Weight IR Weight X 34.3 = SO3
IR= Final weightweight-Initial weight
Q.1 what is IR? Material which is not reacts (dissolved) with Acid and basis. Q.2 why multiply 34.3 for SO3? Because So3 is found in BaSO4 Form = (SO3/BaSO4)*100 = (80/137+32+64)*100 = (80/233)100 =0.3433*100 = 34.33 IR (max %) =
X+4 (100-X) (Note: X= % of Fly ash) 100 =methyl Orange use checking for alkali removes.
1
Clinker, Cement & Raw material (SiO2, R2O3) All Raw materials & Cement
Clinker Sample
0.5 g sa&le 6 'sion i.
0.5 g sa&le in Beaker
*n latin' cr'ciBle
dd ;4Cl 2-3g (i ell)
o
'se 1000 C Hor 1 ho'r
dd Con. C,- 5l$ :ake on ot &late < cool it
dd C, (1E1)$ 20-30 l
dd C, (1E1)$ 10-20 l
@ash Cr'ciBle ith 2O
6Distilled water + Heat
add ;4Cl 6 :ake on ot ilter ith 40; &a&er
&late < cool it dd C, (1E1)$ 20-30 l iltrate
6eat *solate /2O3
eat it 6dd ; 4Cl 2-3g
/esid'e
@ash ith hot Distilled water o
Dry (o7en) 6 *gnite at 1000 C
OidiFing
:oil it 6 dd ;O3 (1E1)$ 0.5l
agent
iO2= ( t * t)?200 dd ;4O (1E1)
&&t
2 dro& 2O4 6 2 dro& 2O
Hor ilter ith 41; &a&er
dd 20 l
iltrate in 500l
't on ot &late < dry
/esid'e
Hlask o
Dry (o7en) 6 *gnite at 1000 C
iO2= ( t * t)?200
CaO < #gO rocess net &age
Use Solu%ion: ;4O(1E1) 250 l ;3 6 250 l 2O ;O3 (1E1)'sion i.= (;a 2CO36!2CO3)
/2O3= ( t * t)?200
Reac%ion: = # iO3 6 2Cl # Cl2 6 2iO3 = 2iO36 97a&oration iO2 6(2O) = iO2 6 *&'. 6 4 i4 622O 2iO3 6 22 i = (eCl3 6 lCl3) 6 3;4O Je(O)3 6 l(O)3K 6 3;4Cl =Je(O)3 6 l(O)3K 6 *gnition e2O3 6 l2O3
1+
Clinker, Cement & Raw material (CaO, MgO)-EDTA method Hter Hiltrat Hiltrate e /2O3 sol'tion sol'tion ake ake ' 500 l
For-CaO
For- MgO
8ake 20 l aliM'ot sol'tion
8ake 20 l aliM'ot sol'tion
dd 8ri ethanol aine (89)
dd 8ri ethanol aine (89)
5 l (or *solation)$ C15;O3$
5 l (or *solation)$ C15;O3$
#t-14.1 g"
#t-14.1 g"
dd %lycerol
dd 9riochroe Black 8 (9:8)
5 l
(or *solation)$ C3O3$
*ndicator$ C202;3;aO+
#t-2.10 g"
#t-41.3 g"
dd atton < /eader (
dd 10-20 l :'HHer ol'tion
*ndicator$ C2114;2O+
(or &-10)
#t-43.42 g"
#t-000 g"
dd 10-20 l odi' (4.0;)
8itrate ith 9D8
ydroide ;aO (or &-12)
(ethylene di aine tetra
#t-40 g"
acetate) #t-3+2.34 g" (end colo'r red- &ink to Bl'e)
8itrate ith 9D8 (ethylene di aine tetra acetate) #t-3+2.34 g" (end colo'r red- &ink to &'r&le) J0.050 > 'ol< ED/A8+<+-;> A1 > A' >100K D..
J0.04032 > 'ol< ED/A8+<+-;> 8 A2) A1)> A' > 100K D..
Aol'e taken a&le eight = A1- 9D8 :'rette reading = A'- Aol'e ake '& = DiHHerence actor actor - as &er 9D8 standard
Aol'e taken a&le eight = A1- 9D8 :'rette reading = A2- Cao titration :/ = A'- Aol'e ake '& = D as &er 9D8 standard
Solu%ion Use: = :'HHer sol'tion- +0 g ;4Cl dissol7ed in 5+0 l ;4O. = 4.0; ;aO- 10 g dissol7ed in 1000 l 2O. =9D8- 3.+224 g dissol7ed in 2O 100 l and ake '& 1000 l sol'tion. = Zn sol'tion (0.01;)-0.53+ g diss. *n 0.1; C,
Reac%ion: 26 6 = Ca 6 9D8.2;a
Di So1iu' Sal%
9.D.8. 8;D/D*8*O; (DiHHerence actor) = 10 l Zn sol (0.1;).6 9:8 6:'HH er sol. 8itrate ith 9D8 (end colo'r &ink to Bl'e) #1A1=#2A2$ #2=0.01 10l ":./. 1
6
2;a 6 9D8.Ca
26
Ferr Ferric ic Oxid Oxidee (Fe2 (Fe2O3 O3)) Te Test stii g by EDTA method in Cement (In OPC)
Make the the solu soluti tion on to 250 250 ml ml in in a stan standa dard rd volu volum m tric flask afte afterr rem remov oval al of of sili silica ca.. Mea Measu sure re 25 ml of of a id solu ion of the sample through pipette in a flask. dd ver dilu dilute te amm ammon oniu ium m hydr hydrox oxid idee (1: (1:6) 6) till till tur turbi bi ity appears.
clear the the tur turbi bidi dity ty with with a min minim imum um amou amount nt of dil dil te hydr chloric acid(1:10) and a few drops in excess to adjust the pH 1 to 1.5. Shake well.
Add 100 mg mg of sulph sulphosa osalicy licylic lic acid acid and and titrate titrate wi wi th 0.01 EDTA solution carefully to a colouress or ale yellow solution.
CALCULATION:-
1 ml of 0.01 Fe2O3(
EDTA EDTA = 0.7985 mg Fe 2O3 ) = 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
1
Alumin Alumina a (Al2O3) (Al2O3) Testing Testing b EDTA method in Cement
After testing of Fe2O3 add 15 ml of standard EDTA t 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 am onium acetate solution by stirring until the the c col olou ou changes from red to yellow add 25 ml of ammo ium acetate in excess to attain a pH of 5.5 -6.0
Heat the solution to boiling for one minute and then c ol.Add 0.5 mg solid solid xylenol orange indicator nd bismuth nitrate solution slowly with constant stirring.
Add 2-3 Titrate
l of bismuth nitrate solution in excess. ith EDTA to a sharp yellow endpoint
CALCULATION:1 ml of 0.01M EDTA = 0.5098 mg Al2O3
Al2O3(%) = 0.05098 X
1 X M X 250 X 100
W X 25 V1= V2-V3-(V4 X factor of Bi(NO3)3 Whe Where,V1= volume of ED A for alumina V2 = total total volu volume me of ED EDT T used in titration V3 = vol volume ume of EDT EDTA A use used for iron V4 = total tal volume of bism th nitrate solution used in the titration. W= weight of sample M = Molarity of EDTA
20
RapidCaoof Clinker/PPCby KMnO4 method (ASTM) PPC Cement 0.2 g sa&le 6 'sion i. *n latin' cr'ciBle o
'se 1000 C Hor 1 ho'r
Clinker Sample /OPC 0.2 g sa&le 6 dd 1E1 cl
N'st :oil6 Contin'e in ot late dd ethyl Orange- He
dd C, (1E1)$ 20-30 l
dro& @ash Cr'ciBle ith 2O
dd ;4O (1E1) 'ntil Colo'r yello
N'st :oil dd l'& s' 0.2 g O,*C cid ('ntil Colo'r lightly &ink) dd 20l hot oni' Oalate (50>) (@hite)
ilter ith 40 ;o. a&er
@ash ith hot ater liM'ot 8ake /esid'e in Beaker
dd 2O4 (1E1)
8itrate ith !#nO4 0.01++ 0.01++2 2; :./. 0.5 actor " a&le
KMnO4 S/ANDARD*SA/*ON ?5. g !#nO4 dissol7ed in 1000l 2O Hor 0.1++2; ol'tion. ?0.+ g O,*C cid 6 2O6 1E1 2o4 titrate ith !#no4. actor = 5":/ 21
sol'tion O8
7as% CaO 8ake 0.5g sa&le dd 1E1 cl (20 l &&ro) N'st :oil ilter @ith 41 ;o a&er in 500 l ro'nd Botto Hlask< ake '& 500 l Cool < shake ell
8ake 20 l aliM'ot sa&le in Conical lask
dd a&&ro 5 l glycerol dd &&ro 1 l 89 dd ;aO ( 2 &ellet) @ine /ed Color ky :l'e
dd 'ol< ED/A8+<+-;> A1 > A' >100K D.. Aol'e taken a&le eight
= A1- 9D8 :'rette reading
= A'- Aol'e ake '& = DiHHerence actor - as &er 9D8 standard O/ :/ 2.04 = CaO> (or 20 l Aol'e taken)
22
ilter O't
Iron (Raw material) -Dichromate method:(ASTM) 0.5 g sa&le 6 'sion i. *n latin' cr'ciBle
o
'se in 1000 C ini' 30 in
Cool and ash t. cr'ciBle ith 1E1 Cl
Clinker sample
@ash cr'ciBle ith Distilled
0.5 g clinker sa&le dissol7ed
ater
in Cl -1E1
:oil < add nCl2 Dro& ise till colo'rless sol'tion
Co&letely cool (/oo 8e&.)
dd :ari' di &henol alHonate
!2Cr2O+caliBration to
(:D) *ndicator = take 20 l 2O 6 0 .5 g 6
dd 5-10 l gCl2 and cid
cid it're 6:D *nd. 6 titrate ith
it're #asking agent
otassi' dichroate 8itrate ith ! 2Cr2O+otassi'
actor= 20":/
dichroate
*ron= :./ > actor (!2Cr2O+)
ol'tion re&arationE =cid i.- 15> 2O46 15>3O4 6+0> 2O =!2Cr2O+(;"1) 3.0+ g dissol7ed in 1000l 2O =:D 1g dissol7ed in 100 l dil. C, (10>) =nCl2 5 g dissol7ed in 100 l dil. C, (10>) ='sion i ;a2CO36!2CO3 = gCl2- 5 g dissol7ed in 1000l 2O
/eactionE 36 26 = 2e 6 n 26 = 2e 6 !2Cr2O+
23
26
2e 6 n 36 2e
46
Free Lime Test:(Clinker)
ol'tion re&arationE
8ake 1 g Clinker sa&le in Beaker
= 1 %lycerol E 5 9thanol
dd 10 l 9thylene %lycol
't Hor 45 in in ater Bath ilter ith 40; &a&er /esid'e o't
iltrate dd :roocrsol %rate %reen
/eactionE Ca(O)2 6 2Cl
*ndicator 8itrate ith 0.1; C,
CaCl2 6 2O
actor= CaO " 2 C,
9nd Colo'r %reen to golden ello "CaO= :./ 0.2 (C, actor)
= Normality of HCL =. Purity *1000*Specific Gravity / 100 * Equivalent t = Normality of HCL =. !"# * 1000 * 1.1$%/100*"#.& 1.1$%/100*"#.& = 11.#' N.!N1% = So 0.1N HCL=N1(1 = N)() =11.#'*() =11.#'*() = 0.1*1000 =()= 0.1*1000/11.#' =
24
8.59ml
Cloride Test (Cl):-0.1% max
ol'tion re&arationE
8ake 1 g sa&le in Beaker
Dissol7ed 1E3 ;O3
ilter 41; &a&er in Conical 8ake aliM'ot sa&le dd 10 l g;O3 l g;O3 (0.1;)
/esid'e o't
dd 2l ;itro :enFene
dd 4 Dro& erric *ndicator ;4.e (O4)2.122O 8itrate ith onia thyo saynte (.01;) ;4C;
9nd Colo'r hite to
0.354 100 (10 (10--:/ :/)) a&le eight
25
/eactionE # Cl Cl2 6 2 ; ;O3 #(;O3)262Cl Cl 6 g;O3 gCl 6 ;O3 g;O3 6 ;4C; gC; 6 ;4;O3
Alkali Test (Na2O+K2O):-( PPC=0.8% max) 8ake 0.25 g sa&le in latin' cr'ciBle 10 l and Backing
dd 2l ;O3
ol'tion re&arationE Blank Solu%ion: 2.5 l ;O3 6 2.5 l l'ina s'l&hate 6 250 l 2O.
S%an1ar1 Solu%ion: NaCl: 1.5 ;aCl Dissol7ed *n 1000l 2O (Hor 1000&&). KCl: 1.53 !Cl Dissol7ed *n 1000l 2O (Hor 1000&&).
dd 10 l ClO4 (er Choleric acid)
't ot &late < '& to yr'&y 9tract dissol7ed to 1E1 ;O3 in Bicker
ilter 41; &a&er in 250 l Aol'etric lack #ake '& 250 l ith 2O
Aol'e ake'& 100 && reading a&le eight 10
?re heater Coating sa&le in (aBo't) ;a2O= 1-2> < !2O=12-1>.
2
/esid'e o't
Reactiv Silica Test: (Fly ash) (IS-3812) 8ake 0.5 g sa&le in Beaker
dd 50 l Cl (1E1)
:oil and Cool dd 1 g !O 4 ho'r 't on ot &late < Aol'e aintain 0 l By 2O
ilter 40; a&er
/esid'e o't
liM'ot ol'tion Bake
Dissol7ed ith 1E1 Cl 6 eat
ilter 40; &a&er /esid'e dry in o7en O
/esid'e *gnite 1000 C
/= *nitial @t. inal @t. ?200
2+
Sulpher Test: (Coal), ESCHKA Method (IS 1350-P3) 8ake 0.1 g sa&le &latin' cr'ciBle dd 1-2 g 9C! it're
ol'tion re&arationE = 0.13+4 = ":aO4 = 9C! it're = (2E1) #go6 ;a2CO3 (,ight Calcined agnesia oide 6nhydro's odi' carBonate)
O
'se at 00 C Dissol7ed to 1E1 Cl ilter 41; &a&er
/esid'e o't
liM'ot ol'tion :oil
dd 20 l :aCl2
Cool
ilter 42; a&er
O
/esid'e *gnite at 00 C
sh 0.13+4 100
Coal ?ra1in&: Coal is the coBination oH Organic (CarBon) and *norganic (i02$ /2O3 etc) aterial. *t is 'se Hor heating &'r&ose.
?ra1e : C D 9 % n-grade 8y&e oH CoalE
A@M UH cal$& P1.5 G200 1.5-24.0 200-500 24.0-2.+ 500-440 2.+-34.1 440-4200 34.1-40.2 4200-330 40.2-4+.1 330-2400 4+.1-55.1 2400-1300 G55.1 P1300 1. nthracite nthracite 2.:'tein's 2.:'tein's 3. ,ignite 4. ith
2
"n-ian Stan-ar- Reference&se in Cement Chemistry
Cement IS 269:1989 – Specification for ordinary Portland cement, 33 grade 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 hydrophobic Portland cement IS 8112:1989 Specification for 43 grade 43 grade ordinary Portland (43-S) IS 8229:1986 Specification for oil-well cement. IS 12269:1987 Specification for 53 grade 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 f or 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 2
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 #ethods oH test Hor 2O5.
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 fl y 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. * 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 30
IS 712:1964 Hydrated Limes. *S No<
*- 4032
*- 4031-1
*- 4031-2
*'0or%an% oin%
?8he diHHerence Beteen check deterinations By 9D8 ethod shall not eceed 0.2 &ercent Hor calci' oide and agnesia$ 0.15 $ 0.2 &ercent Hor silicaand al'ina$ and 0.1 &ercent Hor other constit'ents. ?8he ai' acce&taBle diHHerence in the &ercentage oH each alkali :eteen the loest and highest 7al'e oBtained shall Be 0.04. ? Check the sie7e aHter e7ery 100 sie7ing ? E>RESS*ON O7 RESUL/S /e&ort the 7al'e oH /$ to the nearest 0. * &ercent$ as the resid'e on the 0 & sie7e Hor the ceent tested. 8he standard de7iation oH the re&eataBility is aBo't 0.2 &ercent and oH t he re&rod'ciBility is aBo't 0.3 &ercent. 8he ceent Bed 7ol'e and the a&&arat's constant shall Be recaliBrated ith the reHerence ceentE a) aHter 1 000 tests$ B) *n the case oH 'singE-another ty&e oH anoeter Hl'id$ another ty&e oH Hilter &a&er$ anda ne anoeter t'BeQ and c) at systeatic de7iations oH the secondaryreHerence ceent.
*- 4031-3 *- 4031-4 *- 4031-5
31
Bag Testing: Mass 9
Len& %! 94
3i1% ! 4
S%i%c !es -4
En1s 4+
icks 4+
8?'s ;
8C';
8C';
er D'
er D'
er D'
F<+
94<+
4<
-4
,F<++
,F<+
E##ec%i(e (al(e Si6e 8-+ 5 ;
Seepage of Cement
8C';
MAX-100 (Gms/Ba g)
3ar0 3a" 9
3ar0 Elon&a%ions
3e#% 3a" 9
3e#% Elon&a%ions
/o0$ Bo%%o' 4+
<+
F<-
-<+
<-
-<+
4<+
--<+
<+
S%ren&%! in K?7 7a.ric
Sea'
= CaCO3 Maximum = 8.00% + 1.00%
"mortant 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 w ith 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 t on clinker Production. = 1.8 GJ/t Energy consumed for 1 ton clinker production in 6 stage Pre heater. = Chromic Acid Acid use forwashing glass glass ware. ware. (10gm K 2Cr2O7 + 200 ml H2SO4) !2Cr2O+ 6 4 2O4
!2O46 Cr2(O4)364 2O 6 3O
X-ray: = nʎ= 2d sinθ l ayer, sin θ= angle of wave) (n= n'Ber oH a7e$ ʎ= wave length, d= distance two layer, When bombarding of cathode ray on high melting point metal than reflected ray is called X ray. = C3 6 2O
C 6 Ca (O)2 6 ly ash
C
/eHerencesE-(http://iti.northwestern.edu/cement/monograph/Monograph1_4.html) (http://www.understanding-cement.com/parameters.html) *Cement_Data_Book_Duda_III *Cement_Data_Book_Duda_I II edition. editi on. ? IS book 1727,3812,4031,4032,1350. * jaypee cement testing manual. * Taylor cement chemistry. Note: writer not responsible for any mistake. 32
Thank you.......... yo u............. ...
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