GB/T 8151.13-2012Methods for chemical analysis of zinc concentrates - Part 13: Determination of germanium content - Hydride generation-atomic fluorescence spectrometry and the phenyl fluorone spectrophotometric method (English PDF)
锌精矿化学分析方法 第13部分：锗量的测定 氢化物发生-原子荧光光谱法和苯芴酮分光光度法
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Issued by
SAMR; SAC
Level / Type
National · Recommended
Issue date
December 31, 2012
Implementation date
October 1, 2013
Scope
GB/T 8151.13-2012 is the English-translated version of 锌精矿化学分析方法 第13部分：锗量的测定 氢化物发生-原子荧光光谱法和苯芴酮分光光度法.
This part of GB/T 8151 specifies the determination of the amount of germanium in zinc concentrates by hydride generation atomic fluorescence spectrometry and by phenylfluorone spectrophotometry.
Clause 1 says it applies to the determination of the amount of germanium in zinc concentrate and gives a measuring range of 0.00050 % to 0.10 % for the first method and, as the draft prints it, the same 0.00050 % to 0.10 % for the second.
The foreword says that GB/T 8151, Methods for chemical analysis of zinc concentrates, is divided into twenty parts, that this is Part 13 and that the part was drafted in accordance with the rules given in GB/T 1.1-2009.
The draft prints clause 1 Scope and then the first method, hydride generation atomic fluorescence spectrometry, with 2.1 Method summary, 2.2 Reagents and 2.3 Instrument, and breaks off at 2.3.
Subclause 2.1 describes the procedure: the sample is dissolved with hydrofluoric acid and phosphoric acid in a nitric acid and sulfuric acid medium, germanium is reduced by potassium borohydride in the hydride generator to form its hydride, argon carries the hydride into the quartz furnace atomizer and the fluorescence intensity is measured on the atomic fluorescence spectrometer; 2.3 calls for an atomic fluorescence spectrometer with a high intensity germanium hollow cathode lamp.
Subclause 2.2 requires reagents recognised as analytical reagents and distilled or deionized water or water of equivalent purity, and among the reagents it lists hydrogen peroxide, a potassium hydroxide solution of 5 g/L, a potassium borohydride solution of 40 g/L prepared on the day of use, a germanium standard stock solution made from 0.1000 g of metal germanium of not less than 99.9 % and containing 100 µg of germanium per millilitre, and a germanium standard solution of 1 µg per millilitre diluted from it; several acid names in that list are mangled in the draft and are left out here.
The foreword records that, against the 2000 edition, the text format was modified and precision and test reports were added, that the National Standardization Technical Committee (SAC/TC243) has the part in charge and that MCC Huludao Nonferrous Metals Group Co., Ltd. is the responsible drafting unit.
It replaces GB/T 8151.13-2000, was issued on 31 December 2012 and has applied since 1 October 2013, the frontispiece giving the two dates on a single line in reverse order.
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Document preview — GB/T 8151.13-2012
National Standard of the People's Republic of China
- ICS
- 77.120.60
- Classification
- H 13
- Replacing
- GB/T 8151.13-2000
Issued by: State Administration for Market Regulation; Standardization Administration of the PRC
Contents
- Foreword
- 1 Scope
Foreword
GB/T 8151 "Methods for chemical analysis of zinc concentrates" is divided into 20 parts.
--- Part 1. Determination of the amount of zinc Na2EDTA precipitation titration and extraction separation Na2EDTA titration;
--- Part 2. Determination of sulfur content - Combustion neutralization titration method;
--- Part 3. Determination of iron content Na2EDTA titration;
--- Part 4. Determination of silicon dioxide content - Molybdenum blue spectrophotometric method;
--- Part 5. Determination of lead content by flame atomic absorption spectrometry;
--- Part 6. Determination of copper content - Flame atomic absorption spectrometry;
--- Part 7. Determination of arsenic content by hydride generation - atomic fluorescence spectrometry and potassium bromate titration;
--- Part 8. Determination of cadmium content by flame atomic absorption spectrometry;
--- Part 9. Determination of the amount of fluorine ion selective electrode method;
--- Part 10. Determination of tin content by hydride generation - atomic fluorescence spectrometry;
--- Part 11. Determination of antimony content hydride generation - atomic fluorescence spectrometry;
--- Part 12. Determination of the amount of silver by flame atomic absorption spectrometry;
--- Part 13. Determination of the amount of germanium hydride generation - atomic fluorescence spectroscopy and spectrophotometry Phenylfuoron;
--- Part 14. Determination of nickel content by flame atomic absorption spectrometry;
--- Part 15. Determination of the amount of mercury atomic fluorescence spectrometry;
--- Part 16. Determination of cobalt content by flame atomic absorption spectrometry;
--- Part 17. Determination of the amount of zinc hydroxide precipitation -Na2EDTA titration;
--- Part 18. Determination of the amount of zinc ion exchange -Na2EDTA titration;
--- Part 19. Determination of the amount of gold and silver gray Chuihuo lead analysis or assay and flame atomic absorption spectrometry;
--- Part 20. Copper, lead, iron, arsenic, cadmium, antimony, calcium, magnesium content - Inductively coupled plasma atomic emission spectrometry.
This is Part 13 GB/T 8151's.
Rules in this section in accordance with GB/T 1.1-2009 given draft.
This Part replaces GB/T 8151.13-2000 "Methods for chemical analysis of zinc concentrates - Determination of germanium content." Compared with GB/T 8151.13-2000, the main changes are as follows.
--- Text format has been modified;
--- Added precision and test reports.
Part 1 of hydride generation - atomic fluorescence spectrometry; Method 2 with Phenyl spectrophotometric method to make.
The arbitration method.
The non-ferrous metal part by the National Standardization Technical Committee (SAC/TC243) centralized.
1 Scope
This section GB/T 8151 provisions of the determination of the amount of germanium in zinc concentrate.
This section applies to the determination of the amount of germanium in zinc concentrate measurement range of 1. 0.00050% to 0.10%; Tier 2 measuring range. 0.00050% to 0.10%.
2 1 Hydride Generation - Atomic Fluorescence Spectrometry
2.1 Method summary
Sample with hydrofluoric acid, phosphoric acid is dissolved in nitric acid - sulfuric acid medium at the hydride generator, germanium is potassium borohydride reduction hydride generation It was with argon gas into the quartz furnace atomizer, the fluorescence intensity measured on the atomic fluorescence spectrometer.
2.2 Reagents
Unless otherwise indicated in the analysis using only recognized as analytical reagent and distilled or deionized water or equivalent purity.
2.2.1 Nitrate (rho1.42g/mL).
2.2.2 Sulfate (rho1.84g/mL).
2.2.3 Phosphate (rho1.69g/mL).
2.2.4 Hydrofluoric acid (rho1.13g/mL).
2.2.5 Hydrogen peroxide.
2.2.6 Ammonia (rho0.90g/mL).
2.2.7 Sulfuric acid (11).
2.2.8 Phosphoric acid (11).
2.2.9 mixed acid solution. Add water to 500mL 100mL beaker, then add 50mL sulfuric acid (2.2.2), then add 200mL Phosphate (2.2.8). After cooling, dilute with water to 500mL.
2.2.10 Potassium hydroxide solution (5g/L).
2.2.11 Potassium borohydride solution (40g/L). Weigh 20.0g of potassium borohydride were dissolved in 500mL of potassium hydroxide solution (2.2.10), when Day preparation.
2.2.12 germanium standard stock solution. Weigh accurately 0.1000g metal germanium (wGe>=99.9%) in 150mL beaker, 15mL over Hydrogen peroxide (2.2.5), 2mL aqueous ammonia (2.2.6) and a small amount of water, dissolved by heating in boiling water bath, cooled to room temperature after removing, by washing with water into 1000mL container Volumetric flask, dilute to volume, and mix. This solution 1mL containing 100µg germanium.
2.2.13 Germanium standard solution. Pipette 5.00mL Germanium standard stock solution (2.2.12) in 500mL flask, add 25mL phosphate (2.2.8), dilute with water to volume, and mix. This solution 1mL containing 1µg germanium.
2.3 Instrument
Atomic fluorescence spectrometer, with high-intensity hollow cathode lamp germanium.
......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.
Similar standards
Editions of GB/T 8151.13
| Edition | Title | Revision | Status |
|---|---|---|---|
| GB/T 8151.13-2012 | Methods for chemical analysis of zinc concentrates - Part 13: Determination of germanium content - Hydride generation-atomic fluorescence spectrometry and the phenyl fluorone spectrophptometric method | current edition | Current |
| GB/T 8151.13-2000 | Methods for chemical analysis of zinc concentrates - Part 13: Determination of germanium content - Hydride generation-atomic fluorescence spectrometry and the phenyl fluorone spectrophptometric method | previous edition | Superseded |
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Related Standards
GB/T 8151.14-2012 — Methods for chemical analysis of zinc concentrates - Part 14: Determination of nickel content - The flame atomic absorption spectrometric method
GB/T 8151.12-2000 — Methods for chemical analysis of zinc concentrates -Determination of silver content
GB/T 8151.14-2000 — Methods for chemical analysis of zinc concentrates -Determination of nickel content
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GB/T 8151.13-2012
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