YS/T 244.6-2008Chemical analysis methods of high purity aluminium. Part 6: Determination of silver content by calalyze reaction system of manganese-persulfric acid method (English PDF)

Foreword

YS/T 244 "Chemical analysis methods of high purity aluminum" is divided into nine sections.

--- Part 1. phenanthroline - thiocyanate spectrophotometric determination of iron content;

--- Part 2. molybdenum blue extraction and spectrophotometric determination of silicon content;

--- Part 3. Two-antipyrine DAM - spectrophotometric determination of titanium content thiocyanate;

--- Part 4. Butyl Rhodamine B spectrophotometric determination of gallium content;

--- Part 5. Determination of copper, zinc and lead content anodic stripping voltammetry;

--- Part 6. Catalytic manganese - sulfuric acid system through the determination of silver content;

--- Part 7. dithizone extraction and spectrophotometric determination of cadmium content;

--- Part 8. crystal violet extraction and spectrophotometric determination of indium content;

--- Part 9. Determination of impurities by inductively coupled plasma mass spectrometry.

Part is divided into 6 sections.

This part is YS/T 275-2000 "high purity" in Appendix A of the amendments, the main changes are as follows.

--- Due to high purity aluminum silver content is very low, it will modify its measurement range is. "~ 0.00050% 0.00008% ';

--- Added "repeatability" clause;

--- Increase the "quality assurance and control" clause.

The non-ferrous metal part by the National Standardization Technical Committee and centralized.

This part of the Fushun Aluminum Co., Ltd., China Nonferrous Metals Industry Institute of Standards Metrology and Quality is responsible for drafting.

This part of the Fushun Aluminum Co. drafted.

1 Scope

This section specifies the determination method of high purity silver content.

This section applies to the determination of high-purity aluminum in silver content. Measurement range. ~ 0.00002% 0.00010%.

2 Method summary

Sample was dissolved with hydrochloric acid, nitric acid. In pH1 ~ pH3 solution with dithizone - CTC silver Enrichment. In an acidic medium Borrowed silver manganese - Determination of silver sulfate through catalytic reaction system.

3 Reagents

Reagent preparation and analysis of water are deionized water and then purified by distillation quartz distiller.

3.1 ethanol, pure class distinctions.

3.2 hydrochloric acid (rho1.19g/mL), pure class distinctions.

3.3 hydrochloric acid (1 + 3), pure class distinctions.

3.4 nitrate (rho1.42g/mL), pure class distinctions.

3.5 Ascorbic acid (50g/L), pure class distinctions.

3.6 dithizone - carbon tetrachloride solution (0.05g/L).

3.7 sulfuric acid (1 + 1), pure class distinctions.

3.8 perchloric acid (700g/L), pure class distinctions.

3.9 phosphoric acid (1 + 1).

3.10 manganese sulfate (0.006mol/L).

3.11 potassium persulfate.

3.12 Silver Standard stock solution. Weigh 0.1575g of silver nitrate (99.99%), dissolved in water and transferred to 1000mL volumetric flask (brown), Dilute with water to volume, and mix. This solution 1mL containing 0.1mg silver.

3.13 Silver standard solution. Pipette 10.0mL silver standard stock solution (3.12) in 100mL volumetric flask, dilute with water to volume, and mix.

Then from this solution Pipette 10.0mL solution in 100mL volumetric flask, dilute to the mark, and this solution 1mL containing 0.1µg silver.

4 Instruments and equipment

Spectrophotometer.

5 Sample

Sample 5.1 with hydrochloric acid (3.3) soaked for more than 3h, washed with deionized water, and dried over anhydrous ethanol (3.1) a dip.

The sample was 5.2 (5.1) drying 2h ~ 3h at 70 °C ~ 80 °C, placed in a desiccator to cool to room temperature.