GB/T 4324.4-2012Methods for chemical analysis of tungsten - Part 4: Determination of antimony content - Hydrogenate atomic absorption spectrometry (English PDF)

Foreword

GB/T 4324 "chemical analysis of tungsten" is divided into 28 parts.

--- Part 1. Determination of lead content - flame atomic absorption spectrometry;

--- Part 2. Determination of bismuth content hydride generation atomic absorption spectrometry;

--- Part 3. Determination of tin content hydride generation atomic absorption spectrometry;

--- Part 4. Determination of antimony content hydride generation atomic absorption spectrometry;

--- Part 5. Determination of arsenic content by hydride generation atomic absorption spectrometry;

--- Part 6. Determination of iron content of phenanthroline spectrophotometry;

--- Part 7. Determination of cobalt content by inductively coupled plasma atomic emission spectrometry;

--- Part 8. Determination of the amount of nickel by inductively coupled plasma atomic emission spectrometry and flame atomic absorption spectrometry Diacetyldioxime Gravimetric method;

--- Part 9. Determination of cadmium content by inductively coupled plasma atomic emission spectrometry and flame atomic absorption spectrometry;

--- Part 10. Determination of copper content - Flame atomic absorption spectrometry;

--- Part 11. Determination of aluminum content by inductively coupled plasma atomic emission spectrometry;

--- Part 12. Determination of the amount of silicon tetrachloride - molybdenum blue spectrophotometric method;

--- Part 13. Inductively coupled plasma calcium atomic emission spectrometry;

--- Part 14. Chlorinated Volatile residue amount after Gravimetric method;

--- Part 15. Determination of magnesium content - Flame atomic absorption spectrometry and inductively coupled plasma atomic emission spectrometry;

--- Part 16. Determination of loss on ignition - Gravimetric method;

--- Part 17. Determination of sodium content by flame atomic absorption spectrometry;

--- Part 18. Determination of potassium content by flame atomic absorption spectrometry;

--- Part 19. Determination of titanium content of two methane antipyrine spectrophotometry;

--- Part 20. vanadium content - Inductively coupled plasma atomic emission spectrometry;

--- Part 21. Determination of chromium content by inductively coupled plasma atomic emission spectrometry;

--- Part 22. manganese content - Inductively coupled plasma atomic emission spectrometry;

--- Part 23. Determination of sulfur content of combustion conductance method and frequency combustion infrared absorption method;

--- Part 24. Determination of phosphorus content - Molybdenum blue spectrophotometric method;

--- Part 25. Determination of oxygen pulse heating inert gas fusion - infrared absorption method;

--- Part 26. Determination of nitrogen pulse heating inert gas fusion - thermal conductivity method and Nessler reagent spectrophotometric method;

--- Part 27. Determination of carbon content in the high-frequency combustion infrared absorption method;

--- Part 28. Determination of molybdenum content - Thiocyanate spectrophotometric method.

This section GB/T 44324 Part of.

This section drafted in accordance with GB/T 1.1-2009 given rules.

This Part replaces GB/T 4324.4-1984 "spectrophotometric determination of malachite green chemical analysis of tungsten antimony content", and GB/T 4324.4- Compared to 1984, the main technical changes are as follows.

--- Malachite green spectrophotometric measurement methods changed from the original hydride generation atomic absorption spectrometry;

--- Scope added to tungsten blue, purple tungsten, tungsten carbide, ammonium paratungstate. Detection range from "0.00005% to 0.0050%" is replaced by "0.00005% to 0.020%";

--- In order to ensure the application of different sample dissolution methods in the "sample" in the fine, the average particle size of the tungsten carbide coarse particles were defined;

--- The "measurement frequency" in the "three" to "two";

--- Tungsten powder, tungsten, tungsten oxide, tungstic acid, ammonium paratungstate were modified sample dissolution method, an increase of tungsten blue, purple tungsten, tungsten carbide, metatungstate Ammonium dissolving method;

--- Increasing the foreword, precision and test reports, and a standard format editing.

The non-ferrous metal part by the National Standardization Technical Committee (SAC/TC243) centralized.

This section is drafted. Chenzhou Diamond Tungsten Products Co., Ltd., Ganzhou Nonferrous Metallurgy Research Institute, Hunan Nonferrous Metals Co. Shizhuyuan Liability company.

1 Scope

GB/T 4324 provisions of this part of the tungsten powder, tungsten trioxide, tungsten, tungsten blue, purple tungsten, tungsten carbide, tungsten acid, ammonium metatungstate, ammonium paratungstate Determination of antimony content.

This Part applies to tungsten powder, tungsten measure, tungsten trioxide, tungsten blue, purple tungsten, tungsten carbide, tungsten acid, ammonium metatungstate, ammonium paratungstate antimony content set. Determination range of 0.00005% to 0.020%.

2 Method summary

Tungsten powder, tungsten, tungsten blue, fine particles of tungsten carbide and sodium hydroxide, hydrogen peroxide decomposition; tungsten trioxide, tungstic acid, ammonium paratungstate, metatungstate acid With ammonium hydroxide decomposition; blue tungsten, tungsten carbide coarse particles after burning into tungsten trioxide decomposition with sodium hydroxide. Citric acid complex body of tungsten with Ascorbic acid reducing pentavalent antimony to trivalent, at 6% hydrochloric acid medium conditions, with potassium iodide, thiourea impurity ions eliminate interference by flow injection Shot - hydride generator and atomic absorption spectrometer used for the determination of antimony content.

3 Reagents

Unless otherwise indicated in the analysis using only recognized as analytical grade reagents and distilled or deionized water or equivalent purity.

3.1 Hydrogen peroxide (rho = 1.10g/mL), pure class distinctions.