YS/T 244.1-2008Chemical analysis methods of high purity aluminium. Part 1: Determination of iron content by 1, 10-phenanthroline-thiocyanate 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 1.

The partial replacement of YS/T 244.1-1994 "Chemical analysis methods of high purity aluminum phenanthroline - thiocyanate photometric method for determination of iron content." this part is YS/T 244.1-1994 revision. Compared with YS/T 244.1-1994, 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 provides high purity determination of iron content.

This section applies to the determination of high purity iron content. Measurement range. ~ 0.00010% 0.00050%.

2 Method summary

Sample decomposition with hydrochloric acid, in 2mol/L ~ 3mol/L hydrochloric acid, and methyl isobutyl ketone extraction of iron (III), was added phenanthroline - thiocyanate A mixed solution of potassium, so as to form a ternary complex of iron, measured at 520nm wavelength spectrophotometer absorbance.

5mg high purity nickel and impurities present not interfere with the determination.

3 Reagents

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

3.1 ethanol, pure class distinctions.

3.2 methyl isobutyl ketone.

3.3 hydrochloric acid (1 + 1), the quartz distiller purified by distillation.

Hydrochloride 3.4 (1 + 3), of high purity.

3.5 hydrochloric acid (1 + 20), the quartz distiller purified by distillation.

3.6 solution of potassium thiocyanate (500g/L), pure class distinctions.

3.7 Hydrogen peroxide (30%).

3.8 phenanthroline solution (1g/L).

3.9 Mixed solution. 10mL solution of potassium thiocyanate (3.6), 10mL phenanthroline solution (3.8) and 80mL water and mix. The time is now equipped with.

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

3.11 iron standard stock solution. Weigh 0.1000g metallic iron (purity 99.9%), placed in 100mL beaker, add 20mL hydrochloric acid (3.3), was slowly heated to dissolve completely, cooled to room temperature, transferred to 1L volumetric flask, dilute to the mark with water and mix. The standard storage solution Liquid 1mL containing 0.1mg iron.

3.12 Iron standard solution. Pipette 10.00mL iron standard stock solution (3.11), placed in 100mL flask, diluted with hydrochloric acid (3.5) to the mark, and mix. Then from this solution Pipette 20.00mL in 100mL flask, diluted with hydrochloric acid (3.5) to the mark and mix. this Standard solution 1mL containing 2µg iron.

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.

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