This national standard specifies the reference method for chemical analysis of cement and substitution method which is deemed will produce identical result. In case of any disagreement, the reference method should prevail. This national standard is applicable to Portland cement, ordinary Portland cement, slag Portland cement, Portland-pozzolana cement, fly-ash Portland cement, composite Portland cement, clinkers for the above stated cement and other cements which this national standard is suitable for.
Foreword
1. Scope
2. Standard Reference
3. Basic Requirements of Test
3.1 Test frequency and requirements
3.2 Expression of mass, volume, volume ratio, titer value, and the result
3.3 Permitted Deviation
3.4 Ignition
3.5 Constant weight
3.6 Cl-ion test (silver nitrate test)
4 Reagents and Materials
4.1 Hydrochloric acid (1+1); (1+2); (1+9); (1+10); (1+11); (3+97)
4.2 Nitric acid (1+9)
4.3 Sulfuric acid (1+2); (1+4); (1+9); (5+95)
4.4 Phosphoric acid (1+1)
4.5 Hydrogen peroxide (1+1)
4.6 Formate (1+1)
4.7 Ammonia (1+1); (1+2)
4.8 Sodium hydroxide (NaOH)
4.9 Caustic soda dissolving (10g/L):
4.10 Caustic soda dissolving (15g/L):
4.11 Potash solution (200g/L):
4.12 Sal ammoniac (NH4Cl)
4.13 Anhydrous sodium carbonate (Na2CO3):
4.14 Silver nitrate solution (5g/L):
4.15 Ammonium Nitrate solution (20g/L):
4.16 Ammonium Molybdate solution (50g/L):
4.17 Ascorbic acid solution (5g/L):
4.18 Potassium pyrosulfate(K2S2O7):
4.19 Barium chloride solution (100g/L):
4.20 Stannous chloride (SnCl2?2H2O)
4.21 Stannous chloride-phosphoric acid solution:
4.22 Ammonia zinc sulphate of solution(100g/L):
4.23 Gelatin water (5g/L):
4.24 Starch solution (10g/L):
4.25 Lithium borate:
4.26 Strontium chloride solution (strontium 50g/L):
4.27 Cesium chloride solution (saturated 50g/L):
4.28 Diantipyrylmethane solution (30g/L hydrochloric acid solution):
4.29 Potassium Periodate (KIO4).
4.30 Sodium carbonate- borax mixed flux:
4.31 Ammonium carbonate solution (100g/L):
4.32 EDTA- copper solutions:
4.33 PH3 buffer solution:
4.34 PH4.3 buffer solution:
4.35 PH10 buffer solution:
4.36 Triethanolamine [N (CH2CH2OH)3]:(1+2)
4.37 Seignette salt solution (100g/L):
4.38 Hydroxylamine hydrochloride (NH2OH?HCL)
4.39 Potassium chloride (KCl):
4.40 Potassium Fluoride solution (150g/L):
4.41 Potassium fluoride solution (20g/L):
4.42 potassium chloride solution (50g/L):
4.43 Potassium chloride-ethanol solution (50g/L):
4.44 PH6.0 total ionic strength adjnstment buffer (TISAB) solution:
4.45 Absolute ethyl alcohol (C2H5OH):
4.46 Glycol [1, 2-(CH2OH)2]:
4.47 Barium chromate solution (10g/L):
4.48 Type H 732 styrene strong acid cation exchange resin (1X12):
4.49 Sodium hydroxide absolute ethyl alcohol solution (0.4g/L):
4.50 Glycerol absolute ethyl alcohol solution:
4.51 Silicon dioxide (SiO2) standard solution
4.51.1 Formulation of standard solution
4.51.2 Illustration of the working curve
4.52 Titanium dioxide (TiO2) Standard solution
4.52.1 Formulation of standard solution
4.52.2 Illustration of the working curve
4.53 Manganese monoxide (MnO) standard solution
4.53.1 Formulated with manganese sulfate (MnSO4?H2O)
4.53.2Formulation with mangano-manganic oxide (Mn3O4)
4.54 Ferric oxide (Fe2O3) standard solution
4.54.1 Formulation of standard solution
4.54.2 Illustration of the working curve
4.55 Standard solution of magnesium oxide (MgO)
4.55.1 Formulation of standard solution
4.55.2 Illustration of the working curve
4.56 Standard solution of potassium oxide (K2O) and sodium oxide (Na2O)
4.56.1 Formulation of standard solution of potassium oxide
4.56.2 Formulation of sodium oxide standard solution
4.56.3 Illustration of the working curve
4.57 Standard solution of sulfur trioxide (SO3)
4.57.1 Formulation of standard solution
4.57.2 Formulation of ionic strength regulating solution
4.57.3 Illustration of the working curve
4.58 Standard volumetric solution of potassium iodate [ c(1/6KIO3) = 0.03mol/L]:
4.59 Potassium dichromate reference solution [c(1/6K2Cr2O7) = 0.03mol/L]
4.60 Sodium thiosulfate standard volumetric solution [c (Na2S203,) = 0.03mol/L]
4.60.1 Formulation of standard volumetric solution
4.60.2 Standardization
4.61 Calcium carbonate standard solution [c (CaCO3) = 0.024mol/L]
4.62 EDTA standard volumetric solution [ c (EDTA) = 0.015mol/L]
4.62.1 Formulation of standard volumetric solution
4.62.2 EDTA standard volumetric solution's calibration
4.62.3 Calculation of the titer value EDTA standard volumetric solution to all the oxides
4.63 Standard volumetric solution of cupric sulfate [C (EDTA) = 0.015mol/L])
4.63.1 Formulation of standard volumetric solution
4.63.2 The calibration of volume ratio of EDTA standard volumetric solution and cupric sulfate standard volumetric solution
4.64 Sodium hydroxide standard volumetric solution [C (NaOH)=0.15mol/L])
4.64.1 Formulation of standard volumetric solution
4.64.2 Calibration of sodium hydroxide standard volumetric solution's concentration
4.64.3 Titer value of sodium hydroxide standard volumetric solution to silicon dioxide should be calculated according to equation (12).
4.65 Standard volumetric solution of sodium hydroxide. [c(NaOH) =0.06mol/L]
4.65.1 Formulation of standard volumetric solution
4.65.2 Sodium hydroxide standard volumetric solution's PH indicator calibration
4.65.3 Titer value of sodium hydroxide standard volumetric solution to sulfur trioxide should be calculated according to equation (14).
4.66 Fluorine (F-) Standard solution
4.66.1 Formulation of standard solution
4.66.2 Illustration of the working curve
4.67 Hydrochloric acid standard volumetric solution [c (HCl)] = 0.1mol/L)
4.67.1 Formulation of standard volumetric solution
4.67.2 Hydrochloric acid standard volumetric solution's PH indicator calibration
4.67.3 Calibration of hydrochloric acid standard volumetric solution to calcium oxide
4.68 Benzoic acid absolute ethyl alcohol standard volumetric solution [c(C6H5OOH) = 0.1mol/L]
4.68.1 Formulation of standard volumetric solution
4.68.2 Calibration of the titer value of benzoic acid absolute ethyl alcohol standard volumetric solution to calcium oxide
4.69 Methyl red indicator solution:
4.70 Sulfosalicylic acid sodium salt indicator solution:
4.71 Bromphenol blue indicator solution:
4.72 1-(2-azopyridines)-2-naphthol (PAN) indicator solution:
4.73 calcein-methyl thymol blue-phenolphthalein mixed indicator (CMP mixed indicator for short):
4.74 Acid chrome blue K-Naphthol green B mixed indicator:
4.75 Methyl red indicator solution:
4.76 Methyl red-bromocresol green mixed indicator solution:
5 Instrument and Facility
5.1 Balance:
5.2 Platinum, silver or porcelain crucible:
5.3 Platinum vessel:
5.4 Porcelain evaporating dish:
5.5 Muffle furnace:
5.6 Filter paper:
5.7 Glass volumetric apparatus:
5.8 Magnetic stirring apparatus:
5.9 Spectrophotometer:
5.10 Flame photometer:
5.11 Atomic absorption spectrophotometer:
5.12 Ionometer or acidimeter:
5.13 Device for the determination of sulfide and sulfate
6 Preparation of Cement's Test Specimen
7 Determination of the Loss on Ignition (Reference Method)
7.1 Method synopsis
7.2 Analytical procedure
7.3 Expression of the result
7.4 Permitted deviation
8 Determination of the Loss on Ignition (Reference method)
8.1 Method synopsis
8.2 Analytical procedure
8.3 Expression of the result
8.4 Permitted deviation
9. Determination of the Silicon Dioxide (Reference Method)
9.1 Method synopsis
9.2 Analytical procedure
9.2.1 Determination of pure silicon dioxide
9.2.2 Decomposition of the residue that has been processed by hydrofluoric acid.
9.2.3 Determination of soluble silicon dioxide
9.3 Expression of the result
9.4 Permitted deviation
10 Determination of the Ferric Oxide (Reference Method)
10.1 Method synopsis
10.2 Analytical procedure
10.3 Expression of the result
10.4 Permitted deviation
11 Determination of the Alumina (Reference Method)
11.1 Method synopsis
11.2 Analytical procedure
11.3 Expression of the result
11.4 Permitted deviation
12 Determination of the Calcium Oxide (Reference Method)
12.1 Method synopsis
12.2 Analytical procedure
12.3 Expression of the result
12.4 Permitted deviation
13 Determination of Magnesium (Reference Method)
13.1 Method synopsis
13.2 Analytical procedure
13.2.1 Decompound with hydrofluoric acid- perchloric acid
13.2.2 Fusion of lithium boric acid
13.2.3 Determination of magnesium
13.3 Expression of the result
13.4 Permitted deviation
14 Determination of Sulfate-sulfur Trioxide (Reference Method)
14.1 Method synopsis
14.2
14.3 Expression of the result
14.4 Permitted deviation
15 Determination of Titanium Dioxide (Reference Method 2)
15.1 Method synopsis
15.2 Analytical procedure
15.3 Expression of the result
15.4 Permitted deviation
16 Determination of the Manganese Monoxide (Reference Method)
16.1 Method synopsis
16.2 Analytical procedure
16.3 Expression of the result
16.4 Permitted deviation
17 Determination of Potassium Oxide and Sodium Oxide (Reference Method)
17.1 Method synopsis
17.2 Analytical procedure
17.3 Expression of the result
17.4 Permitted deviation
18 Determination of the Sulfide (Reference Method)
18.1 Method synopsis
18.2 Analytical procedure
18.3 Expression of the result
18.4 Permitted deviation
19. Determination of the Silicon Dioxide (Substitution Method)
19.1 Method synopsis
19.2 Analytical procedure
19.3 Expression of the result
19.4 Permitted deviation
20. Determination of the Alumina (Substitution Method)
20.1 Method synopsis
20.2 Analytical procedure
20.3 Expression of the result
20.4 Permitted deviation
21. Determination of the Calcium Oxide (Substitution Method)
21.1 Method synopsis
21.2 Analytical procedure
21.3 Expression of the result
21.4 Permitted deviation
22 Determination of Magesium (Substitution Method)
22.1 Complex formation titration
22.1.1 Method synopsis
22.1.2 Analytical procedure
22.1.3 Permitted deviation
22.2 Atomic absorption spectrometry
22.2.1 Method synopsis
22.2.2 Analytical procedure
22.2.3 Expression of the result
22.2.4 Permitted deviation
23 Determination of Ferric Oxide (Substitution Method)
23.1 Method synopsis
23.2 Analytical procedure
24 Determination of Manganese Monoxide (Substitution Method)
25 Determination of Potassium Oxide and Sodium Oxide (Substitution Method)
25.1 Method synopsis
25.2 Analytical procedure
25.3 Expression of the result
25.4 Permitted deviation
26 Determination of Sulfate-sulfur Trioxide (Substitution Method)
26.1 Iodimetric analysis
26.1.1 Method synopsis
26.1.2 Analytical procedure
26.1.3 Expression of the result
26.2 Barium sulfate - barium chromate spectrophotometric method
26.2.1 Method synopsis
26.2.2 Analytical procedure
26.2.3 Expression of the result
26.3 Ion-exchange method
26.3.1 Method synopsis
26.3.2 Analytical procedure
26.3.3 Expression of the result
26.4 Permitted deviation
27 Determination of Fluorin (Substitution Method)
27.1 Method synopsis
27.2 Analytical procedure
27.3 Expression of the result
27.4 Permitted deviation
28 Determination of Free Calcium Oxide (Substitution Method)
28.1 Glycol method
28.1.1 Method synopsis
28 .1.2 Analytical procedure
28.1.3 Expression of the result
28.2 Glycidol method
28.2.1 Method synopsis
28.2.2 Analytical procedure
28.2.3 Expression of the result
28.3 Permitted deviation
