GB/T 8207-2007Determination of germanium in coal (English PDF)
煤中锗的测定方法
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Issued by
SAMR; SAC
Level / Type
National · Recommended
Issue date
November 1, 2007
Implementation date
June 1, 2008
Scope
GB/T 8207-2007 is the English-translated version of 煤中锗的测定方法.
GB/T 8207-2007 specifies two spectrophotometric procedures for determining germanium in coal, one using distillation separation with phenylfluorone and one using extraction separation with phenylfluorone, and for each it lays down the reagents and materials, the apparatus, the test procedure, the expression of results and the precision of the method.
Clause 1 requires the distillation separation method to be used for arbitration analysis, applies the standard to lignite, bituminous coal and anthracite, and sets the measuring range at 1 ug/g to 200 ug/g.
Clause 3 describes the distillation method: the general analysis coal sample is ashed and decomposed with a mixture of nitric, phosphoric and hydrofluoric acids, taken up in hydrochloric acid at about 6 mol/L and distilled so that the germanium escapes as germanium tetrachloride and is absorbed in water, separating it from interfering elements, after which colour is developed with phenylfluorone in hydrochloric acid solution of 1.2 mol/L and the absorbance is measured on a spectrophotometer.
The reagent list that follows prescribes deionized or equivalent distilled water, the acids with their relative densities, hydrochloric acid solutions of about 6, 7 and 0.1 mol/L, sodium hydroxide solution, boric acid, ethanol, sodium sulfite solution, gelatin solution at 10 mg/mL and a germanium stock standard solution at 100 ug/mL prepared either from 0.1441 g of spectroscopically pure germanium dioxide or from 0.1000 g of high purity germanium metal; clause 4 then sets out the extraction separation method, including the preparation of its sample and blank solutions.
Clause 2 cites GB/T 483, the general provisions for methods of coal analysis.
The foreword records that the revision altered the terminology, symbols and units of measurement, added a foreword, a scope, normative references and a test report, modified the calculation formula for the results and the precision of the method, and reworked the preparation of the sample and blank solutions for the extraction separation method.
The standard was proposed by the China Coal Industry Association, is administered by the national technical committee on coal standardization and was drafted by the CCRI coal analysis laboratory together with the coalfield geology institute.
It replaces GB/T 8207-1987, was issued on November 1, 2007 and has applied since June 1, 2008.
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Document preview — GB/T 8207-2007
National Standard of the People's Republic of China
- ICS
- 73.040
- Classification
- D 21
- Replacing
- GB/T 8207-1987
Issued by: State Administration for Market Regulation; Standardization Administration of the PRC
Contents
- Foreword
- 1 Scope
- 2 Normative references
- 3 Distillation - benzene Spectrophotometer
Foreword
This standard replaces GB/T 8207-1987 "Determination of germanium in coal." This standard compared with GB/T 8207-1987, the main changes are as follows.
--- Altered the standard terminology, symbols and units of measurement;
--- Increasing the foreword, scope, normative references and test reports of four parts;
--- Modify the results of the calculation formula (1987 version 1.4, this version 3.5);
--- Modify the precision of the method (the 1987 version 1.5, this version 3.6);
--- Modify the extraction and separation - Preparation Phenylfluorone spectrophotometry the sample solution and the blank sample (1987 edition 2.3.2 and 2.3.3, 4.4.2 and 4.4.3 of this edition). The standard proposed by China Coal Industry Association.
1 Scope
This standard specifies the distillation of coal Germanium - Phenylfluorone spectrophotometry and extraction separation - Phenyl spectrophotometric method mention To the reagent materials, equipment, test procedures, results are expressed and precision of the method and the like. When arbitration analysis shall be separated by distillation - Phenyl Colorimetry.
This standard applies to lignite, bituminous coal and anthracite. Measurement range (1 ~ 200) µg/g.
2 Normative references
The following documents contain provisions which, through reference in this standard and become the standard terms. For dated references, subsequent Amendments (not including errata content) or revisions do not apply to this standard, however, encourage the parties to the agreement are based on research Whether the latest versions of these documents. For undated reference documents, the latest versions apply to this standard.
GB/T 483 coal analysis test methods - General provisions
3 Distillation - benzene Spectrophotometer
3.1 Method summary
The general analysis of coal samples ashed with nitric acid, phosphoric acid and hydrofluoric acid mixture exploded, then made into hydrochloric acid (6mol/L) and the solution was evaporated Distilled, in the form of germanium tetrachloride, germanium escape, water absorption and separated from interfering elements. In 1.2mol L solution of hydrochloric acid/color with Phenylfuoron And using a spectrophotometer spectrophotometry.
3.2 Reagents and materials
3.2.1 Water. deionized water or equivalent purity distilled water.
3.2.2 Nitrate (GB/T 626). the relative density of 1.42.
3.2.3 Phosphate (GB/T 1282). the relative density of 1.88.
3.2.4 Hydrofluoric acid (GB/T 620). the relative density of 1.15.
3.2.5 Hydrochloric acid (GB/T 622). the relative density of 1.19.
3.2.6 Sulfuric acid (GB/T 625). the relative density of 1.84.
3.2.7 hydrochloric acid solution. about 6mol/L, 1 volume of hydrochloric acid (3.2.5) plus one volume of water, and mix.
3.2.8 hydrochloric acid solution. about 7mol/L, 580mL of hydrochloric acid (3.2.5) added 420mL of water, and mix.
3.2.9 hydrochloric acid solution. about 0.1mol/L, 8mL hydrochloric acid (3.2.5) added 992mL of water, and mix.
3.2.10 sodium hydroxide solution. 0.1mol/L, 4g of sodium hydroxide (GB/T 622) was dissolved in 1000mL of water.
3.2.11 Boric acid (GB/T 628).
3.2.12 Ethanol (GB/T 679). 95%.
3.2.13 sodium sulfite solution. 12g/100mL, 12g of anhydrous sodium sulfite (HG3-1078) was dissolved in 100mL water.
3.2.14 Gelatin solution. 10mg/mL
Weigh 1g of gelatin was dissolved in 100mL, water (80 ~ 90) °C and filtered. Preparation before use.
3.2.15 Germanium stock standard solution. 100µg/mL
Weigh 0.1441g spectroscopically pure germanium dioxide in the 400mL beaker, add sodium hydroxide solution (3.2.10) 1mL and water 50mL, Heated and dissolved; adding 0.1mol/L hydrochloric acid solution 1mL neutralized and excess 1mL. Solution was transferred to 1L flask, washed with water beaker, Lotion incorporated into the flask; dilute to the mark with water, shake spare.
High purity germanium metal or weighed in the beaker 0.1000g micro ammonia aqueous solution, the solution of 6% hydrogen peroxide (HG3-1082), water Heating the bath to slowly dissolve, then with water into a platinum crucible and evaporated to dryness; 5g of anhydrous sodium carbonate (GB/T 1255) at an elevated temperature
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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.
Referenced standards
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Editions of GB/T 8207
| Edition | Title | Revision | Status |
|---|---|---|---|
| GB/T 8207-2007 | Determination of germanium in coal | current edition | Current |
| GB/T 8207-1987 | Determination of germanium in coal | previous edition | Superseded |
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