GB/T 22661.10-2008Chemical analysis methods of potassium fluoborate - Part 10: Determination of phosphorus pentoxide content - Molybdenum blue photometric method (English PDF)
氟硼酸钾化学分析方法 第10部分：五氧化二磷含量的测定 钼蓝分光光度法
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Issued by
SAMR; SAC
Level / Type
National · Recommended
Issue date
December 29, 2008
Implementation date
November 1, 2009
Scope
GB/T 22661.10-2008 is the English-translated version of 氟硼酸钾化学分析方法 第10部分：五氧化二磷含量的测定 钼蓝分光光度法.
GB/T 22661.10-2008 gives the molybdenum blue photometric method for the phosphorus pentoxide content of potassium fluoroborate. Clause 1 states that this part of GB/T 22661 specifies that determination, that the part applies to the phosphorus pentoxide content of potassium fluoroborate and that the measuring range is not more than 0.050 %.
Clause 2 cites GB/T 22661.1-2008 on the preparation and storage of test samples.
Clause 3, principle of the method, has the sample melted with a mixed sodium carbonate and boric acid solvent, acidified with hydrochloric acid and treated with ammonium molybdate at a pH of not more than 0.3, so that the phosphorus forms a phosphomolybdic heteropoly acid which is reduced to phosphomolybdic blue and whose absorbance is measured on a spectrophotometer at a wavelength of 800 nm.
Clause 4 lists the reagents, among them anhydrous sodium carbonate, boric acid, hydrochloric acid at 3 mol/L and at 6 mol/L, ascorbic acid solution at 25 g/L and ammonium molybdate at 100 g/L, and gives the preparations for the phosphorus pentoxide standard stock solution, at 0.100 mg of P2O5 per millilitre, and for the standard solution, at 0.010 mg of P2O5 per millilitre, which is to be made up immediately before use.
Clause 5 calls for a flat platinum dish 70 mm in diameter and 35 mm high with a platinum cover, a furnace whose temperature can be controlled at 850 degrees Celsius plus or minus 25 degrees, and a spectrophotometer; the draft breaks off there, so the analysis steps and the calculation cannot be reported.
The foreword divides GB/T 22661 into ten parts and names this one as Part 10. The page records no earlier edition. It was issued on 2008-12-29 and has applied since 2009-11-01.
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Document preview — GB/T 22661.10-2008
National Standard of the People's Republic of China
- ICS
- 77.120.10
- Classification
- H 61
Issued by: State Administration for Market Regulation; Standardization Administration of the PRC
Contents
- Foreword
- 1 Scope
- 2 Normative references
- 3 PRINCIPLE OF THE METHOD
- 4 Reagents
- 5 Instruments and equipment
Foreword
GB/T 22661 "potassium fluoroborate chemical analysis method" is divided into 10 parts.
--- Part 1. Preparation and storage of test samples;
--- Part 2. Determination of the weight of water in the wet method;
--- Part 3. Determination of potassium fluoride boric acid sodium hydroxide volumetric method;
--- Part 4. Determination of magnesium by flame atomic absorption spectrometry;
--- Part 5. Determination of calcium content by flame atomic absorption spectrometry;
--- Part 6. Determination of silicon content - Molybdenum blue spectrophotometric method;
--- Part 7. Determination of sodium content by flame atomic absorption spectrometry;
--- Part 8. Determination of the free boronic acid sodium volumetric method;
--- Part 9. Determination of the chlorine content of mercuric nitrate volumetric method;
--- Part 10. Determination of phosphorus pentoxide content - Molybdenum blue spectrophotometric method.
This section GB/T 22661 Part 10. […]
1 Scope
This section GB/T 22661 specifies the method for determination of potassium fluoroborate pentoxide content.
This section applies to the determination of potassium fluoroborate pentoxide content. Measuring range. <=0.050%.
2 Normative references
The following documents contain provisions which, through reference GB/T 22661 in this section constitute provisions of this section. For dated reference documents Member, all subsequent amendments (not including errata content) or revisions do not apply to this section, however, encouraged to reach under this section Parties to research agreement to use the latest versions of these documents. For undated reference documents, the latest versions apply to this section.
GB/T 22661.1-2008 Chemical analysis methods of potassium fluoroborate Part 1: Preparation and storage of test samples
3 PRINCIPLE OF THE METHOD
Sample with sodium carbonate and boric acid mixed solvent melt, acidified with hydrochloric acid, ammonium molybdate added when pH<=0.3, phosphorus formed phosphomolybdic heteropoly Acid, by reduction to phosphomolybdic blue, the 800nm wavelength spectrophotometer measured absorbance.
4 Reagents
4.1 Anhydrous sodium carbonate.
4.2 Boric acid.
4.3 HCl. 3mol/L.
4.4 HCl. 6mol/L.
4.5 Ascorbic acid solution. 25g/L.
Ammonium molybdate 4.6. 100g/L.
4.7 Pentoxide standard stock solution
Weigh 0.1917g potassium dihydrogen phosphate (reference reagents, at 110 °C ± 5 °C drying 2h, cool in a desiccator), was dissolved with water and transferred to 1000mL volumetric flask, dilute with water to volume, and mix. This solution 1mL containing 0.100mgP2O5.
4.8 Pentoxide standard solution
Pipette 10.00mL phosphorus standard stock solution (4.7) into 100mL volumetric flask, dilute with water to volume, and mix. This solution 1mL containing 0.010mgP2O5. The solution was formulated before use now.
5 Instruments and equipment
5.1 platinum dish. flat, diameter 70mm, height 35mm, with platinum cover.
5.2 Furnace.
5.3 Furnace temperature. the temperature can be controlled at 850 °C ± 25 °C.
5.4 Spectrophotometer.
......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.
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Related Standards
GB/T 22661.1-2008 — Chemical analysis methods of potassium fluoborade - Part 1: preparation and storage of test samples
GB/T 22661.9-2008 — Chemical analysis methods of potassium fluoborade - Part 9: Determination of chloride content - Distillation mercury nitration volumetric method
GB/T 22661.8-2008 — Chemical analysis methods of potassium fluoborade - Part 8: Determination of free borade content - Distillation-sodium hydrogen oxidizes titration volumetric method
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