Foreword 1
1. Scope 10
2. Standard Reference 10
3. Basic Requirements of Test 11
3.1 Test frequency and requirements 11
3.2 Expression of mass, volume, volume ratio, titer value, and the result 11
3.3 Permitted Deviation 11
3.4 Ignition 12
3.5 Constant weight 12
3.6 Cl-ion test (silver nitrate test) 12
4 Reagents and Materials 12
4.1 Hydrochloric acid (1+1); (1+2); (1+9); (1+10); (1+11); (3+97) 13
4.2 Nitric acid (1+9) 13
4.3 Sulfuric acid (1+2); (1+4); (1+9); (5+95) 13
4.4 Phosphoric acid (1+1) 13
4.5 Hydrogen peroxide (1+1) 13
4.6 Formate (1+1) 13
4.7 Ammonia (1+1); (1+2) 13
4.8 Sodium hydroxide (NaOH) 13
4.9 Caustic soda dissolving (10g/L): 13
4.10 Caustic soda dissolving (15g/L): 13
4.11 Potash solution (200g/L): 13
4.12 Sal ammoniac (NH4Cl) 14
4.13 Anhydrous sodium carbonate (Na2CO3): 14
4.14 Silver nitrate solution (5g/L): 14
4.15 Ammonium Nitrate solution (20g/L): 14
4.16 Ammonium Molybdate solution (50g/L): 14
4.17 Ascorbic acid solution (5g/L): 14
4.18 Potassium pyrosulfate(K2S2O7): 14
4.19 Barium chloride solution (100g/L): 14
4.20 Stannous chloride (SnCl2•2H2O) 14
4.21 Stannous chloride-phosphoric acid solution: 14
4.22 Ammonia zinc sulphate of solution(100g/L): 14
4.23 Gelatin water (5g/L): 14
4.24 Starch solution (10g/L): 14
4.25 Lithium borate: 14
4.26 Strontium chloride solution (strontium 50g/L): 14
4.27 Cesium chloride solution (saturated 50g/L): 15
4.28 Diantipyrylmethane solution (30g/L hydrochloric acid solution): 15
4.29 Potassium Periodate (KIO4). 15
4.30 Sodium carbonate- borax mixed flux: 15
4.31 Ammonium carbonate solution (100g/L): 15
4.32 EDTA- copper solutions: 15
4.33 PH3 buffer solution: 15
4.34 PH4.3 buffer solution: 15
4.35 PH10 buffer solution: 15
4.36 Triethanolamine [N (CH2CH2OH)3]:(1+2) 15
4.37 Seignette salt solution (100g/L): 15
4.38 Hydroxylamine hydrochloride (NH2OH•HCL) 15
4.39 Potassium chloride (KCl): 15
4.40 Potassium Fluoride solution (150g/L): 15
4.41 Potassium fluoride solution (20g/L): 15
4.42 potassium chloride solution (50g/L): 16
4.43 Potassium chloride-ethanol solution (50g/L): 16
4.44 PH6.0 total ionic strength adjnstment buffer (TISAB) solution: 16
4.45 Absolute ethyl alcohol (C2H5OH): 16
4.46 Glycol [1, 2-(CH2OH)2]: 16
4.47 Barium chromate solution (10g/L): 16
4.48 Type H 732 styrene strong acid cation exchange resin (1X12): 16
4.49 Sodium hydroxide absolute ethyl alcohol solution (0.4g/L): 16
4.50 Glycerol absolute ethyl alcohol solution: 16
4.51 Silicon dioxide (SiO2) standard solution 17
4.51.1 Formulation of standard solution 17
4.51.2 Illustration of the working curve 17
4.52 Titanium dioxide (TiO2) Standard solution 17
4.52.1 Formulation of standard solution 17
4.52.2 Illustration of the working curve 18
4.53 Manganese monoxide (MnO) standard solution 18
4.53.1 Formulated with manganese sulfate (MnSO4•H2O) 18
4.53.2Formulation with mangano-manganic oxide (Mn3O4) 18
4.54 Ferric oxide (Fe2O3) standard solution 19
4.54.1 Formulation of standard solution 19
4.54.2 Illustration of the working curve 19
4.55 Standard solution of magnesium oxide (MgO) 19
4.55.1 Formulation of standard solution 20
4.55.2 Illustration of the working curve 20
4.56 Standard solution of potassium oxide (K2O) and sodium oxide (Na2O) 20
4.56.1 Formulation of standard solution of potassium oxide 20
4.56.2 Formulation of sodium oxide standard solution 21
4.56.3 Illustration of the working curve 21
4.57 Standard solution of sulfur trioxide (SO3) 22
4.57.1 Formulation of standard solution 22
4.57.2 Formulation of ionic strength regulating solution 22
4.57.3 Illustration of the working curve 22
4.58 Standard volumetric solution of potassium iodate [ c(1/6KIO3) = 0.03mol/L]: 22
4.59 Potassium dichromate reference solution [c(1/6K2Cr2O7) = 0.03mol/L] 23
4.60 Sodium thiosulfate standard volumetric solution [c (Na2S203,) = 0.03mol/L] 23
4.60.1 Formulation of standard volumetric solution 23
4.60.2 Standardization 23
4.61 Calcium carbonate standard solution [c (CaCO3) = 0.024mol/L] 25
4.62 EDTA standard volumetric solution [ c (EDTA) = 0.015mol/L] 25
4.62.1 Formulation of standard volumetric solution 25
4.62.2 EDTA standard volumetric solution's calibration 25
4.62.3 Calculation of the titer value EDTA standard volumetric solution to all the oxides 26
4.63 Standard volumetric solution of cupric sulfate [C (EDTA) = 0.015mol/L]) 27
4.63.1 Formulation of standard volumetric solution 27
4.63.2 The calibration of volume ratio of EDTA standard volumetric solution and cupric sulfate standard volumetric solution 27
4.64 Sodium hydroxide standard volumetric solution [C (NaOH)=0.15mol/L]) 27
4.64.1 Formulation of standard volumetric solution 27
4.64.2 Calibration of sodium hydroxide standard volumetric solution's concentration 28
4.64.3 Titer value of sodium hydroxide standard volumetric solution to silicon dioxide should be calculated according to equation (12). 28
4.65 Standard volumetric solution of sodium hydroxide. [c(NaOH) =0.06mol/L] 29
4.65.1 Formulation of standard volumetric solution 29
4.65.2 Sodium hydroxide standard volumetric solution's PH indicator calibration 29
4.65.3 Titer value of sodium hydroxide standard volumetric solution to sulfur trioxide should be calculated according to equation (14). 29
4.66 Fluorine (F-) Standard solution 30
4.66.1 Formulation of standard solution 30
4.66.2 Illustration of the working curve 30
4.67 Hydrochloric acid standard volumetric solution [c (HCl)] = 0.1mol/L) 31
4.67.1 Formulation of standard volumetric solution 31
4.67.2 Hydrochloric acid standard volumetric solution's PH indicator calibration 31
4.67.3 Calibration of hydrochloric acid standard volumetric solution to calcium oxide 31
4.68 Benzoic acid absolute ethyl alcohol standard volumetric solution [c(C6H5OOH) = 0.1mol/L] 32
4.68.1 Formulation of standard volumetric solution 32
4.68.2 Calibration of the titer value of benzoic acid absolute ethyl alcohol standard volumetric solution to calcium oxide 32
4.69 Methyl red indicator solution: 33
4.70 Sulfosalicylic acid sodium salt indicator solution: 33
4.71 Bromphenol blue indicator solution: 33
4.72 1-(2-azopyridines)-2-naphthol (PAN) indicator solution: 33
4.73 calcein-methyl thymol blue-phenolphthalein mixed indicator (CMP mixed indicator for short): 33
4.74 Acid chrome blue K-Naphthol green B mixed indicator: 33
4.75 Methyl red indicator solution: 33
4.76 Methyl red-bromocresol green mixed indicator solution: 33
5 Instrument and Facility 34
5.1 Balance: 34
5.2 Platinum, silver or porcelain crucible: 34
5.3 Platinum vessel: 34
5.4 Porcelain evaporating dish: 34
5.5 Muffle furnace: 34
5.6 Filter paper: 34
5.7 Glass volumetric apparatus: 34
5.8 Magnetic stirring apparatus: 34
5.9 Spectrophotometer: 34
5.10 Flame photometer: 34
5.11 Atomic absorption spectrophotometer: 34
5.12 Ionometer or acidimeter: 34
5.13 Device for the determination of sulfide and sulfate 34
6 Preparation of Cement's Test Specimen 35
7 Determination of the Loss on Ignition (Reference Method) 35
7.1 Method synopsis 35
7.2 Analytical procedure 35
7.3 Expression of the result 35
7.4 Permitted deviation 36
8 Determination of the Loss on Ignition (Reference method) 36
8.1 Method synopsis 36
8.2 Analytical procedure 36
8.3 Expression of the result 37
8.4 Permitted deviation 37
9. Determination of the Silicon Dioxide (Reference Method) 38
9.1 Method synopsis 38
9.2 Analytical procedure 38
9.2.1 Determination of pure silicon dioxide 38
9.2.2 Decomposition of the residue that has been processed by hydrofluoric acid. 40
9.2.3 Determination of soluble silicon dioxide 40
9.3 Expression of the result 41
9.4 Permitted deviation 41
10 Determination of the Ferric Oxide (Reference Method) 41
10.1 Method synopsis 41
10.2 Analytical procedure 41
10.3 Expression of the result 41
10.4 Permitted deviation 42
11 Determination of the Alumina (Reference Method) 42
11.1 Method synopsis 42
11.2 Analytical procedure 42
11.3 Expression of the result 42
11.4 Permitted deviation 43
12 Determination of the Calcium Oxide (Reference Method) 43
12.1 Method synopsis 43
12.2 Analytical procedure 43
12.3 Expression of the result 43
12.4 Permitted deviation 44
13 Determination of Magnesium (Reference Method) 44
13.1 Method synopsis 44
13.2 Analytical procedure 44
13.2.1 Decompound with hydrofluoric acid- perchloric acid 44
13.2.2 Fusion of lithium boric acid 45
13.2.3 Determination of magnesium 45
13.3 Expression of the result 45
13.4 Permitted deviation 46
14 Determination of Sulfate-sulfur Trioxide (Reference Method) 46
14.1 Method synopsis 46
14.2 46
14.3 Expression of the result 47
14.4 Permitted deviation 47
15 Determination of Titanium Dioxide (Reference Method 2) 47
15.1 Method synopsis 47
15.2 Analytical procedure 47
15.3 Expression of the result 48
15.4 Permitted deviation 48
16 Determination of the Manganese Monoxide (Reference Method) 48
16.1 Method synopsis 48
16.2 Analytical procedure 49
16.3 Expression of the result 49
16.4 Permitted deviation 50
17 Determination of Potassium Oxide and Sodium Oxide (Reference Method) 50
17.1 Method synopsis 50
17.2 Analytical procedure 50
17.3 Expression of the result 50
17.4 Permitted deviation 51
18 Determination of the Sulfide (Reference Method) 51
18.1 Method synopsis 51
18.2 Analytical procedure 51
18.3 Expression of the result 52
18.4 Permitted deviation 52
19. Determination of the Silicon Dioxide (Substitution Method) 53
19.1 Method synopsis 53
19.2 Analytical procedure 53
19.3 Expression of the result 54
19.4 Permitted deviation 54
20. Determination of the Alumina (Substitution Method) 54
20.1 Method synopsis 54
20.2 Analytical procedure 55
20.3 Expression of the result 55
20.4 Permitted deviation 55
21. Determination of the Calcium Oxide (Substitution Method) 56
21.1 Method synopsis 56
21.2 Analytical procedure 56
21.3 Expression of the result 56
21.4 Permitted deviation 56
22 Determination of Magesium (Substitution Method) 57
22.1 Complex formation titration 57
22.1.1 Method synopsis 57
22.1.2 Analytical procedure 57
22.1.3 Permitted deviation 58
22.2 Atomic absorption spectrometry 59
22.2.1 Method synopsis 59
22.2.2 Analytical procedure 59
22.2.3 Expression of the result 59
22.2.4 Permitted deviation 60
23 Determination of Ferric Oxide (Substitution Method) 60
23.1 Method synopsis 60
23.2 Analytical procedure 60
24 Determination of Manganese Monoxide (Substitution Method) 61
25 Determination of Potassium Oxide and Sodium Oxide (Substitution Method) 62
25.1 Method synopsis 62
25.2 Analytical procedure 62
25.3 Expression of the result 62
25.4 Permitted deviation 63
26 Determination of Sulfate-sulfur Trioxide (Substitution Method) 63
26.1 Iodimetric analysis 63
26.1.1 Method synopsis 63
26.1.2 Analytical procedure 64
26.1.3 Expression of the result 64
26.2 Barium sulfate - barium chromate spectrophotometric method 65
26.2.1 Method synopsis 65
26.2.2 Analytical procedure 65
26.2.3 Expression of the result 65
26.3 Ion-exchange method 66
26.3.1 Method synopsis 66
26.3.2 Analytical procedure 66
26.3.3 Expression of the result 66
26.4 Permitted deviation 67
27 Determination of Fluorin (Substitution Method) 67
27.1 Method synopsis 67
27.2 Analytical procedure 67
27.3 Expression of the result 68
27.4 Permitted deviation 68
28 Determination of Free Calcium Oxide (Substitution Method) 68
28.1 Glycol method 68
28.1.1 Method synopsis 68
28 .1.2 Analytical procedure 69
28.1.3 Expression of the result 69
28.2 Glycidol method 69
28.2.1 Method synopsis 69
28.2.2 Analytical procedure 70
28.2.3 Expression of the result 70
28.3 Permitted deviation 70
