YS/T 244.4-2008Chemical analysis methods of high purity aluminium. Part 4: Determination of gallium content by butylrhodamine B photometric 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.

This is Part 4.

The partial replacement of YS/T 244.4-1994 "spectrophotometric determination of the amount of high-purity aluminum gallium chemical analysis Butylrhodamine B".

This part is YS/T 244.4-1994 revision. Compared with YS/T 244.4-1994, the main changes are as follows.

--- 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 gallium content.

This section applies to the determination of high-purity aluminum gallium content. Measurement range. ~ 0.00002% 0.00020%.

2 Method summary

In the presence of nickel salt, hydrochloric acid sample was dissolved in 4.5mol/L HCl medium, gallium and Dingjidanming B forms a complex with benzene extraction. 562nm wavelength spectrophotometer measured absorbance. High purity aluminum impurities present not interfere with the determination.

3 Reagents

Reagent preparation and analysis of water are deionized water or water of equivalent purity.

3.1 ethanol, pure class distinctions.

3.2 benzene.

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

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

3.5 titanium trichloride solution (15%).

3.6 Butyl Rhodamine B solution (2g/L). Weigh 0.2g Butyl Rhodamine B in 100mL beaker, 80mL hydrochloric acid (3.3) solution Solution, transferred to 100mL volumetric flask, diluted with hydrochloric acid (3.3) to the mark and mix.

3.7 nickel chloride (NiCl2 · 6H2O) solution (4g/L). 0.5mL per 100mL solution containing hydrochloric acid (3.3).

3.8 gallium standard stock solution. Weigh 0.1344g gallium oxide (99.99%) in the 200mL beaker, 100mL of hydrochloric acid (3.3), completely dissolved by heating at a low temperature (not allow to boil), cooled to room temperature, transferred to 500mL volumetric flask, diluted with hydrochloric acid (3.3) to engrave Degree, and mix. This solution 1mL containing 0.2mg gallium.

3.9 Gallium standard solution. Pipette 10.0mL gallium standard stock solution (3.8) in 100mL volumetric flask, dilute to the mark with hydrochloric acid (3.3), Mix well. Then from this solution weighed 10.0mL in 200mL flask, diluted with hydrochloric acid (3.3) to the mark and mix. This solution 1mL Gallium-containing 1µg.

4 Instruments and equipment

4.1 Spectrophotometer.

4.2 electric centrifuge.

5 Sample

Sample 5.1 with hydrochloric acid (3.4) 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.