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GB/T 4324.12-2012: Methods for chemical analysis of tungsten -- Part 12: Determination of silicon content -- Chlorization-molybdenum blue spectrophotometry
Status: Valid GB/T 4324.12: Evolution and historical versions
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivered in | Standard Title (Description) | Status | PDF |
| GB/T 4324.12-2012 | English | 209 |
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Methods for chemical analysis of tungsten -- Part 12: Determination of silicon content -- Chlorization-molybdenum blue spectrophotometry
| Valid |
GB/T 4324.12-2012
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| GB/T 4324.12-1984 | English | 199 |
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Methods for chemical analysis of tungsten--The chloritization-molybdenum blue photometric method for the determination of silicon content
| Obsolete |
GB/T 4324.12-1984
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PDF similar to GB/T 4324.12-2012
Basic data | Standard ID | GB/T 4324.12-2012 (GB/T4324.12-2012) | | Description (Translated English) | Methods for chemical analysis of tungsten -- Part 12: Determination of silicon content -- Chlorization-molybdenum blue spectrophotometry | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | H63 | | Classification of International Standard | 77.120.99 | | Word Count Estimation | 9,933 | | Older Standard (superseded by this standard) | GB/T 4324.12-1984 | | Regulation (derived from) | National Standards Bulletin No. 41 of 2012 | | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China | | Summary | This standard specifies the tungsten powder, tungsten, tungsten trioxide, tungsten blue, purple, tungsten, tungsten carbide, tungsten acid, ammonium paratungstate, metatungstate in the determination of silicon. This section applies to tungsten powder, tun | GB/T 4324.12-2012: Methods for chemical analysis of tungsten -- Part 12: Determination of silicon content -- Chlorization-molybdenum blue spectrophotometry
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Methods for chemical analysis of tungsten Part 12. Determination of silicon content Chlorization-molybdenum blue spectrophotometry
ICS 77.120.99
H63
National Standards of People's Republic of China
Replacing GB/T 4324.12-1984
Chemical analysis of tungsten
Part 12. Determination of the amount of silicon
Chloride - Molybdenum blue spectrophotometric method
Part 12. Determinationofsiliconcontent-
Issued on. 2012-12-31
2013-10-01 implementation
Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
Standardization Administration of China released
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 Part of 124,324.
This section drafted in accordance with GB/T 1.1-2009 given rules.
This Part replaces GB/T 4324.12-1984 "chemical analysis of tungsten chloride - molybdenum blue spectrophotometric determination of silicon content." This portion
GB/T 4324.12-1984 compared to the main technical changes are as follows.
--- Tungsten chloride after separating body, "added sodium carbonate melt in a high temperature furnace" to "plus hydrofluoric acid - nitric acid to dissolve the residue" and without positive
Butanol extraction and separation, the color directly in the aqueous phase is measured;
--- Scope added tungsten blue, purple tungsten, tungsten carbide, ammonium paratungstate; measurement range from "0.0005% to 0.030%" instead
"0.0004% - 0.030%";
--- The "measurement frequency" in the "three" to "twice."
The non-ferrous metal part by the National Standardization Technical Committee (SAC/TC243) centralized.
This section is drafted. Zhuzhou Cemented Carbide Group Co., Ltd., China Nonferrous Metals Industry Institute of Standards Metrology and Quality.
The main drafters of this section. Xiong Jing, Zhang Ying, Yin Hua, Weirui screen, easy Jianbo, Peng Yu, Yang Jianguo, Zhao Sheng Chi.
This part of the standard replaces the previous editions are.
--- GB/T 4324.12-1984.
Chemical analysis of tungsten
Part 12. Determination of the amount of silicon
Chloride - Molybdenum blue spectrophotometric method
1 Scope
This section provides tungsten powder, tungsten trioxide, tungsten, tungsten blue, purple tungsten, tungsten carbide, tungsten acid, ammonium paratungstate, ammonium metatungstate Determination of silicon content
method.
This Part applies to tungsten powder, tungsten trioxide, tungsten, tungsten blue, purple tungsten, tungsten carbide, tungsten acid, ammonium paratungstate, ammonium tungstate partial determination of silicon content.
Determination of the range of 0.0004% to 0.030%.
2 Method summary
The sample was separated from the main body of tungsten chloride, potassium chloride residue in the presence of hydrofluoric acid - nitric acid is dissolved, boric acid inhibiting influence of fluoride ions, plus molybdenum
Ammonium generation silicon molybdenum heteropoly acid. In the oxalic acid - sulfuric acid medium, using 1,2,4-acid and sodium sulfite as the reducing agent, reduction of silicon molybdenum yellow silicon molybdenum blue,
800nm \u200b\u200bwavelength spectrophotometer measured absorbance.
3 Reagents
Unless otherwise indicated, this part of the reagents used are in line with national standards or industry standard analytical reagents, which are twice distilled water
Distilled water.
3.1 hydrofluoric acid by azeotropic distillation purification or superior grade pure purity above.
3.2 nitric acid (ρ = 1.42g/mL), pure class distinctions.
3.3 potassium chloride solution (10g/L).
3.4 boric acid solution (60g/L). Weigh 60g excellent pure boric acid, heated and dissolved in water and diluted to 1000mL, and mix. when necessary
filter.
3.5 potassium permanganate solution (10g/L), with the preparation.
3.6 ammonium molybdate solution (100g/L). Weigh 50g excellent pure ammonium molybdate, heated and dissolved in water and diluted to 500mL, and mix. when necessary
Filtered and stored in a plastic bottle.
3.7 oxalic acid - sulfuric acid mixed solution. Weigh 30g of oxalic acid in 1000mL beaker, 200mL of water, sulfuric acid was slowly added 300mL
(11) were stirred and dissolved, and diluted with water to 1000mL, mixing, stored in a plastic bottle.
3.8 Silicon reductant. Weigh 5g of anhydrous sodium sulfite and 0.050g1- amino-2-naphthol-4-sulfonic acid dissolved in water and diluted to 50mL, mix
Mix to dissolve, formulated with time.
3.9 silicon standard stock solution. Weigh 0.1069g pre-calcined at 900 ℃ silica (wSiO2≥99.99%) in a platinum crucible,
Add 4g of anhydrous sodium carbonate and placed 900 ℃ ~ 950 ℃ high temperature furnace to melt red transparent (about 12min). Remove the cooling water washed crucible
Crucible bottom, extraction with boiling water in a plastic cup frit, wash the platinum crucible and cooled. Transferred to 500mL volumetric flask, dilute to the mark, mix,
Store in plastic bottle. This solution 1mL containing 100μg silicon.
3.10 Silicon standard solution. Pipette 25.00mL silicon standard stock solution (3.9) in 500mL flask, add 1g of anhydrous sodium carbonate, shake
Move to dissolve, dilute with water to volume, and mix, stored in a plastic bottle. This solution 1mL containing 5μg silicon.
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