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GB/T 13747.12-2019: Methods for chemical analysis of zirconium and zirconium alloys -- Part 12: Determination of silicon content -- Molybdenum blue spectrophotometry
Status: Valid GB/T 13747.12: Evolution and historical versions
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivered in | Standard Title (Description) | Status | PDF |
| GB/T 13747.12-2019 | English | 119 |
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Methods for chemical analysis of zirconium and zirconium alloys -- Part 12: Determination of silicon content -- Molybdenum blue spectrophotometry
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GB/T 13747.12-2019
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| GB/T 13747.12-1992 | English | 159 |
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Zirconium and zirconiumalloys. Determination of silicon content. Molybdenum blue spectrophotometric method
| Obsolete |
GB/T 13747.12-1992
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PDF similar to GB/T 13747.12-2019
Basic data | Standard ID | GB/T 13747.12-2019 (GB/T13747.12-2019) | | Description (Translated English) | Methods for chemical analysis of zirconium and zirconium alloys -- Part 12: Determination of silicon content -- Molybdenum blue spectrophotometry | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | H14 | | Classification of International Standard | 77.120.99 | | Word Count Estimation | 6,627 | | Date of Issue | 2019-12-31 | | Date of Implementation | 2020-11-01 | | Older Standard (superseded by this standard) | GB/T 13747.12-1992 | | Issuing agency(ies) | State Administration for Market Regulation, China National Standardization Administration | | Summary | This standard specifies the method for the determination of silicon content in zirconium and zirconium alloys. This standard applies to the determination of silicon content in sponge zirconium, zirconium and zirconium alloys. Measurement range: 0.0010% to 0.040%. | GB/T 13747.12-2019: Methods for chemical analysis of zirconium and zirconium alloys -- Part 12: Determination of silicon content -- Molybdenum blue spectrophotometry
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Methods for chemical analysis of zirconium and zirconium alloys-Part 12. Determination of silicon content-Molybdenum blue spectrophotometry
ICS 77.120.99
H14
National Standards of People's Republic of China
Replaces GB/T 13747.12-1992
Methods for chemical analysis of zirconium and zirconium alloys
Part 12. Determination of silicon content Molybdenum blue spectrophotometric method
2019-12-31 release
2020-11-01 implementation
State Administration of Market Supervision
Published by the National Standardization Administration
Foreword
GB/T 13747 "Chemical analysis methods for zirconium and zirconium alloys" is planned to be divided into 27 parts.
--- Part 1. Determination of tin content potassium iodate titration method and phenylfluorone-polyethylene glycol octylphenyl ether spectrophotometry;
--- Part 2. Determination of iron content 1,10-diazaphenanthrene spectrophotometry and inductively coupled plasma atomic emission spectrometry;
--- Part 3. Determination of nickel content Butadione oxime spectrophotometry and inductively coupled plasma atomic emission spectrometry;
--- Part 4. Determination of chromium content Diphenylcarbazide spectrophotometry and inductively coupled plasma atomic emission spectrometry;
--- Part 5. Determination of aluminum content Chromazurol S-tetradecylpyridine chloride spectrophotometry;
--- Part 6. Determination of copper content 2,9-dimethyl-1,10-diazaphenanthrene spectrophotometry;
--- Part 7. Determination of manganese content potassium periodate spectrophotometry and inductively coupled plasma atomic emission spectrometry;
--- Part 8. Determination of the amount of drilled nitroso R salt spectrophotometric method;
--- Part 9. Determination of magnesium content by flame atomic absorption spectrometry;
--- Part 10. Determination of tungsten content thiocyanate spectrophotometric method;
--- Part 11. Determination of molybdenum content thiocyanate spectrophotometry;
--- Part 12. Determination of silicon content Molybdenum blue spectrophotometry;
--- Part 13. Polarographic determination of lead content;
--- Part 14. Determination of uranium by polarography;
--- Part 15. Determination of boron content by curcumin spectrophotometry;
--- Part 16; determination of chlorine content; silver chloride turbidity method and ion selective electrode method;
--- Part 17. Polarographic method for the determination of cadmium content;
--- Part 18. Determination of vanadium content Benzoylphenylhydroxylamine spectrophotometric method;
--- Part 19. Determination of titanium content diantipyrine methane spectrophotometry and inductively coupled plasma atomic emission spectrometry;
--- Part 20. Determination of tritium content by inductively coupled plasma atomic emission spectrometry;
--- Part 21. Determination of hydrogen content Inert gas melting infrared absorption method/thermal conductivity method;
--- Part 22. Determination of oxygen and nitrogen content Inert gas melting infrared absorption method/thermal conductivity method;
--- Part 23. Determination of nitrogen content-Distillation separation-Nesler reagent spectrophotometry;
--- Part 24. Determination of carbon content, high frequency combustion infrared absorption method;
--- Part 25. Determination of niobium content 5-Br-PADAP spectrophotometry and inductively coupled plasma atomic emission spectrometry;
--- Part 26. Determination of alloys and impurity elements by inductively coupled plasma atomic emission spectrometry;
--- Part 27. Determination of trace impurity elements by inductively coupled plasma mass spectrometry.
This part is Part 12 of GB/T 13747.
This section is drafted in accordance with the rules given in GB/T 1.1-2009.
This section replaces GB/T 13747.12-1992 "Methods for chemical analysis of zirconium and zirconium alloys. Molybdenum blue spectrophotometric determination of silicon content" Headquarters
Compared with GB/T 13747.12-1992, in addition to editorial changes, the main technical changes are as follows.
--- Extended measurement range. The measurement range was expanded from the original 0.0020% ~ 0.040% to 0.0010% ~ 0.040% (see Chapter 1,.1992
Annual Chapter 1);
--- Added sample clauses (see Chapter 5);
--- Added precision clause (see Chapter 8);
--- Added test report clauses (see Chapter 9).
This section is proposed by China Nonferrous Metals Industry Association.
This section is under the jurisdiction of the National Nonferrous Metals Standardization Technical Committee (SAC/TC243).
This section was drafted. Xi'an Han and Tang Analysis Co., Ltd., Western Metal Materials Co., Ltd., Western New Zirconium Nuclear Material Technology
Co., Ltd., Guangdong Industrial Analysis and Testing Center, Baotai Group Co., Ltd., Guizhou Provincial Analysis and Testing Institute.
The main drafters of this section. Luo Lin, Baolin Sun, Jinlei Wang, Leilei Liu, Yang Xin, Wang Kaikai, Liu Houyong, Huang Zengxin, Li Weimin, Hui Poining,
Zhou Zhiping, Xie Hui, Xiong Xiaoyan, Bai Huanhuan, Zhao Wuli, Huang Ying, Zhou Yuanjing.
The previous versions of the standards replaced by this section are.
--- GB/T 13747.12-1992.
Methods for chemical analysis of zirconium and zirconium alloys
Part 12. Determination of silicon content Molybdenum blue spectrophotometric method
1 Scope
This part of GB/T 13747 specifies the determination method of silicon content in zirconium and zirconium alloys.
This section applies to the determination of silicon content in sponge zirconium, zirconium and zirconium alloys. Measurement range. 0.0010% ~ 0.040%.
2 Principle
The sample was dissolved with hydrofluoric acid and nitric acid. Fluoride was masked with boric acid. At about pH 1.5, silicon and ammonium molybdate generate yellow silicon molybdenum heteropoly acid,
After reducing it to silicon molybdenum blue with a reducing agent, the absorbance was measured at a wavelength of 800 nm by a spectrophotometer.
3 reagents
Unless otherwise stated, only reagents and laboratory secondary water identified as analytically pure were used in the analysis.
3.1 Hydrofluoric acid (1 4), excellent grade pure.
3.2 Nitric acid (1 1), excellent grade pure.
3.3 Saturated boric acid solution.
3.4 Potassium permanganate solution (1g/L).
3.5 Ammonium molybdate solution (100g/L). Weigh 50g of ammonium molybdate [(NH4) 6Mo7O24 · 4H2O] and dissolve it in 500mL of water.
3.6 Tartaric acid solution (200g/L).
3.7 Reducing agent solution. Weigh 20g of sodium sulfite and dissolve it in 160mL of water, and then add 0.4g of 1-amino-2-naphthol-4-sulfonic acid.
After adding 40mL of water, it is now ready to use.
3.8 Silicon standard storage solution. Weigh 1.0697 g of dioxide that was previously burned at 1000 ° C for 30 min and cooled to room temperature in a desiccator.
Put silicon (excellent grade) in a platinum crucible, add 5g sodium carbonate and 5g potassium carbonate, and mix well. Melt in 1000 ℃ high temperature furnace for 20min, take out cold
However, in a polytetrafluoroethylene beaker, immerse the frit with hot water, cool it, and transfer it to a 500mL volumetric flask. Dilute to the mark with water, mix, and store.
In a polyethylene bottle. 1 mL of this solution contained 1 mg of silicon.
3.9 Silicon standard solution. Transfer 10.00mL silicon standard storage solution (3.8) to a 1000mL volumetric flask, dilute to the mark with water, mix well, store
Store in a polyethylene bottle. 1 mL of this solution contained 10 μg of silicon.
4 instruments
Spectrophotometer.
5 samples
The sample was processed into chips with a length of not more than 5 mm.
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