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GB/T 1574-2007 English PDF (GBT1574-2007)

GB/T 1574-2007 English PDF (GBT1574-2007)

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GB/T 1574-2007: Test method for analysis of coal ash

This standard specifies the reagents and materials, instruments and equipment, analysis procedure, result calculation and method precision for the determination of ferrum, calcium, magnesium, potassium, sodium, manganese, phosphorus, silicon, aluminum, titanium and sulphur in coal ash.
GB/T 1574-2007
GB
National Standard
of the PEOPLE Republic of China
ICS 73.040
D 21
Replacing GB/T 1574-1995, GB/T 4634-1996, GB/T 18856.13-2002
Test Method for Analysis of Coal Ash
ISSUED ON. NOVEMBER 1, 2007
IMPLEMENTED ON. JUNE 1, 2008
Jointly issued by. General Administration of Quality Supervision,
Inspection and Quarantine (AQSIQ);
Standardization Administration (SAC) of the People's
Republic of China.
Table of Content
1 Scope??...??4
2 Normative References??...??4
3 Reagents??...??4
4 Instruments and Equipment??...??4
5 Preparation of Ash Sample??...??5
6 Semi-microanalysis Method of Silica, Ferric Oxide, Titanium Dioxide, Aluminum Oxide, Calcium Oxide and Magnesium Oxide??...??5
6.1 Preparation of Test Solution??...??5
6.2 Determination of Silicon Dioxide (Silicon Molybdenum Blue Spectrophotometric Method)??...??6
6.3 Continuous Determination of Ferric Oxide and Titanium Dioxide
(Spectrophotometric Method with Ferrotitanium Reagent)??...??9
6.4 Separate Determination of Titanium Dioxide (Diantipyryl Methane
Spectrophotometric Method)??...??12
6.5 Determination of Aluminum Oxide (Complexometric Titration with Villiaumite Replacing EDTA)??...??14
6.6 Determination of Calcium Oxide (EGTA Complexometric Titration)??...??16 6.7 Determination of Magnesium Oxide (EDTA Complexometric Titration)??...??18 7 Macro-analysis Method of Silicon Dioxide, Ferric Oxide, Aluminum Oxide, Calcium Oxide, Magnesium Oxide and Titanium Dioxide??...??20
7.1 Determination of Silicon Dioxide (Animal Glue Condensing Mass Method)??...??20 7.2 Continuous Determination of Ferric Oxide and Aluminum Oxide
(Complexometric Titration with EDTA)??...??22
7.3 Determination of Calcium Oxide (EDTA Complexometric Titration)??...??26 7.4 Determination of Magnesium Oxide (Complexometric Titration with EDTA, Subtraction Method)??...??28
7.5 Determination of Titanium Dioxide (Spectrophotometric Method with
Hydrogen Peroxide)??...??30
8 Determination of Sulfur Trioxide??...??32
8.1 Barium Sulfate Mass Method??...??32
8.2 Combustion Neutralization Method??...??34
8.3 Coulomb Titration??...??38
9 Determination of Phosphorus Pentoxide (Phosphorus Molybdenum Blue
Spectrophotometric Method)??...??41
9.1 Method 1??...??41
9.2 Method 2??...??43
10 Determination of Potassium Oxide and Sodium Oxide (Flame Photometry)??...??46 11 Method for Determination of Potassium, Sodium, Ferrum, Calcium, Magnesium and Manganese (Atomic Absorption Method)??...??48
12 Test Report??...??53
Foreword
This standard replaces GB/T 1574-1995 Analysis of Coal Ash, GB/T 4634-1996 Determination of Potassium, Sodium, Iron, Calcium, Magnesium and Manganese in Coal Ash by Atomic Absorption Spectrometric Method, and GB/T 18856.13-2002 Test Methods for Quality of Coal Water Mixture - Part 13. Determination for the Ash of Coal Water Mixture. This standard integrates the 3 standards - GB/T 1574-1995, GB/T 4634-1996 and GB/T 18856.13-2002.
Compared with GB/T 1574-1995, GB/T 4634-1996 and GB/T 18856.13-2002, the main changes of this standard are as follows.
?€? The volume of standard working solution of titanium dioxide was modified (6.3.3.1 in GB/T 1574-1995; 6.3.3.1.1 in this edition);
?€? A method to separately determine titanium dioxide was added (see 6.4); ?€? Wrong units were modified (9.1.2.10 and 9.1.2.11 in GB/T 1574-1995; 9.2.2.10 and 9.2.2.11 in this edition);
?€? Errors in formula were modified (9.2.7 in GB/T 1574-1995; Formula 26 in 9.2.4 of this edition);
?€? Content of "note" was added (see 11.2);
?€? Appendix A in the former standard (GB/T 4634-1996) was deleted.
This standard was proposed by the China National Coal Association.
This standard shall be under the jurisdiction of National Technical Committee on Coal of Standardization Administration of China.
Drafting organization of this standard. the Coal Analysis Laboratory of Coal Research Institute.
Chief drafting staffs of this standard. Zhang Kerui, Xia Huili, Chen Suize, Deng Xiumin, Zhou Guoyue, Wang Zhiqian, and Sui Yan.
The previous editions replaced by this standard are as follows.
- GB 1574-1979, GB/T 1574-1995;
- GB/T 4634-1984, GB/T 4634-1996;
- GB/T 18856.13-2002.
Test Method for Analysis of Coal Ash
1 Scope
This standard specifies the reagents and materials, instruments and equipment, analysis procedure, result calculation and method precision for the determination of ferrum, calcium, magnesium, potassium, sodium, manganese, phosphorus, silicon, aluminum, titanium and sulphur in coal ash.
This standard is applicable to coal, coke, coal water slurry and coal gangue. 2 Normative References
The following documents contain provisions which, through reference in this text, constitute provisions of this standard. For dated references, subsequent amendments (excluding correction) or revisions of these publications do not apply. However, the parties who enter into agreement according to these specifications are encouraged to research whether the latest editions of these labels are applicable. For any undated references, the latest edition of the document referred to applies.
GB/T 483 General Rules for Analytical and Testing Methods of Coal
3 Reagents
Water mentioned in this standard is deionized water or distilled water with equivalent purity.
4 Instruments and Equipment
4.1 Muffle furnace. with temperature regulating device, thermocouple, and pyrometer; it can maintain at (815 ?? 10) ??C and shall have corresponding constant-temperature area; upper part of its back wall is chimney with diameter of 25mm~30mm, lower part has a hole (for insertion of thermocouple) whose position shall be such that the heat contact-point of the thermocouple can be 20mm~30mm away from the furnace bottom; a ventilation hole (diameter. about 20mm) shall be on the furnace door.
4.2 High-temperature muffle furnace. with temperature control device; it can maintain at (1000??10)??C.
6.3 Continuous Determination of Ferric Oxide and Titanium Dioxide
(Spectrophotometric Method with Ferrotitanium Reagent)
6.3.1 Method summary
Under the condition of pH= 4.7~4.9, ferric ion reacts with ferrotitanium reagent to generate purple complex; use spectrophotometric method to determine ferric oxide. Add adequate amount of ascorbic acid, so that purple of the solution disappears; titanic ion reacts with ferrotitanium reagent to generate yellow complex, use spectrophotometric method to determine titanium dioxide.
6.3.2 Reagents and materials
6.3.2.1 Ascorbic acid.
6.3.2.2 Ferrotitanium reagent solution. 20 g/L. Weigh 2 g of ferrotitanium reagent (C6H4O8S2Na2); dissolve it into water; dilute to 100 mL with water.
6.3.2.3 Ammonia water (GB/T 631). volume ratio is (1+6).
6.3.2.4 Hydrochloric acid (GB/T 622) solution. volume ratio is (1 + 19). 6.3.2.5 Sulfuric acid solution. volume fraction is 50mL/L. Measure 5 mL of sulfuric acid (GB/T 625); add water slowly; dilute to 100 mL with water.
6.3.2.6 Buffer solution. pH = 4.7. Weigh 68 g of sodium acetate trihydrate (CH3COONa???3H2O) (GB/T 693) or 41 g of anhydrous sodium acetate (CH3COONa) (GB/T 694); place into a 400 mL beaker; add water to dissolve; add 29 mL of glacial acetic acid (GB/T 676); dilute to 1 L with water.
6.3.2.7 Standard stock solution of ferric oxide. 1 mg/mL.
Accurately weigh 1.0000g (accurate to 0.0002g) of ferric oxide GR which has been dried at 105??C~110??C for 1 h; place it in a 400 mL beaker; add 50mL of concentrated hydrochloric acid (GB/T 622, GR); put on watch-glass; heat it until they are diss...

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