YS/T 981.3-2014Methods for chemical analysis of high pure indium. Determination of silicon content. Molybdenum blue spectrophotometric method (English PDF)

Foreword

YS/T 981 "Methods for chemical analysis of high purity indium" is divided into five sections.

--- Part 1. magnesium, aluminum, silicon, sulfur, iron, nickel, copper, zinc, arsenic, silver, cadmium, tin, thallium, lead quality measurement resolution glow discharge mass Spectroscopy;

--- Part 2. Inductively magnesium, aluminum, iron, nickel, copper, zinc, silver, cadmium, tin, lead coupled plasma mass spectrometry;

--- Part 3. Determination of the amount of silicon molybdenum blue spectrophotometric method;

--- Part 4. Determination of tin content Phenylfluorone - bromo cetyl trimethylamine absorptiometry;

--- Part 5. Determination of thallium content Rhodamine B photometric method.

This section YS/T 981 Part 3.

This section drafted in accordance with GB/T 1.1-2009 given rules.

The non-ferrous metal part by the National Standardization Technical Committee (SAC/TC243) centralized.

This section is responsible for drafting units. non-ferrous metals and electronic materials analysis and testing center.

This section participated in the drafting unit. China Nonferrous Metals Industry Institute of Standards Metrology and Quality, Jinchuan Group Co., Ltd., a semiconductor Emei Institute materials, widely Xi Debang Technology Co., Ltd.

1 Scope

This section YS/T 981 specifies the method for determination of silicon content in high-purity indium.

This section applies to the determination of 99.9999% purity Indium content of silicon. Determination range 5 × 10-5% ~ 2 × 10-4%.

2 Method summary

After the sample is dissolved by nitric acid, hydrofluoric acid is added conversion insoluble silica, boric acid complex with an excess of fluoride ions in a pH range from 1 to 1.5 Silicon and ammonium molybdate generate beta-type silicon molybdenum complex, then in 1.5mol/L sulfuric acid solution to isoamyl alcohol extraction, tin dichloride reduction, have Phase was measured at 630nm wavelength absorbance. Less than 2mg indium, 5µg arsenic, 5µg phosphorus, 0.5µg germanium does not interfere with the determination.

3 Reagents and Instruments

3.1 water is deionized water, the resistivity of > 18Mohm · cm.

3.2 nitric acid (rho = 1.19g/mL), pure class distinctions stored in plastic dropper bottle.

3.3 nitric acid (11), formulated by the nitric acid (3.2), stored in plastic dropper bottle.

3.4 sulfuric acid (rho = 1.84g/mL), pure class distinctions.

3.5 sulfate (4.5mol/L), the preparation of sulfuric acid (3.4).

3.6 sulfate (1.5mol/L), the preparation of sulfuric acid (3.4).

3.7 ethanol.

3.8 hydrofluoric acid (12), pure class distinctions, the platinum distiller purified by distillation or polytetrafluoroethylene sub-boiling distillation purified by distillation, stored in polyethylene drop Bottle.

3.9 isoamyl alcohol, distilled after use.

3.10 boric acid solution. 60g/L, weighed 6g boric acid solution in 100mL of water. Store in a polyethylene bottle.

3.11 ammonium molybdate solution. 100g/L extra virgin. Weigh 10g ammonium molybdate solution 100mL hot water. Store in a polyethylene bottle.

3.12 tartaric acid solution. 100g/L, weighed 10g tartaric acid in 100mL of water. Store in a polyethylene bottle.

3.13 tin dichloride solution. 2g/L, weighed 0.2g tin dichloride dissolved 100mL1.5mol/L sulfuric acid solution. The time is now equipped with.

3.14 Silicon standard solution (A). Weigh 2.5300g sodium silicate (Na2SiO3 · 9H2O), a 50mL beaker with a small amount of water moist, Add boiling water, stirring constantly to dissolve, let cool after moved into 500mL volumetric flask, dilute with water to the mark. Store in a polyethylene bottle. this Solution of silicon-containing 0.5g/L.

3.15 Silicon standard solution (B). Take 1.00mL solution (3.14) and transferred to 250mL volumetric flask, dilute to the mark, shake. Storage Polyethylene bottle. Solution of silicon-containing 2µg/mL.

4 Apparatus and materials

4.1 Spectrophotometer.

4.2 platinum crucible. 30mL.