YS/T 226.2-2009Methods for chemical analysis of selenium. Part 2: Determination of antimony content. Hydride generation-atomic fluorescence spectrometry (English PDF)

Foreword

YS/T 226 "selenium chemical analysis method" is divided into 13 parts.

--- Part 1. Determination of bismuth content - Hydride Generation - Atomic Fluorescence Spectrometry

--- Part 2. Determination of antimony content Hydride Generation - Atomic Fluorescence Spectrometry

--- Part 3. Determination of aluminum content Chromazurol S- cetylpyridinium bromide spectrophotometric method

--- Part 4. Determination of mercury content of dithizone - CTC colorimetric titration

--- Part 5. Determination of the amount of silicon molybdenum blue spectrophotometry

--- Part 6. Determination of sulfur content symmetrical diphenyl semicarbazide spectrophotometry

--- Part 7. Determination of magnesium content - Flame atomic absorption spectrometry

--- Part 8. Determination of copper content - Flame atomic absorption spectrometry

--- Part 9. Determination of iron content by flame atomic absorption spectrometry

--- Part 10. Determination of nickel content by flame atomic absorption spectrometry

--- Part 11. Determination of lead content by flame atomic absorption spectrometry

--- Part 12. Determination of the amount of selenium sodium thiosulfate volumetric method

--- Part 13. silver, aluminum, arsenic, boron, mercury, bismuth, copper, cadmium, iron, gallium, indium, magnesium, nickel, lead, silicon, antimony, tin, tellurium, titanium, zinc contents Inductively Coupled Plasma Mass Spectrometry this section YS/T Part 2 226.

The partial replacement of YS/T 226.2-1994 "Determination of antimony content of selenium in Malachite green photometric method." And YS/T 226.2-1994 Compared to the main section has the following changes.

Atomic Fluorescence Spectrometry - --- hydride generation by the malachite green spectrophotometry changed.

--- Measurement range expanded from 0.0002% ~ 0.0020 to 0.0002% to 0.010%.

--- Supplementary terms of quality assurance and control, increasing the repeatability limit.

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

This section is responsible for drafting unit. Jinchuan Group Limited.

This section is drafted. Guangzhou Nonferrous Metal Research Institute.

Participated in the drafting of this section. Jinchuan Group Ltd., Tongling Nonferrous Metals Group Holdings Limited.

1 Scope

This section YS/T 226 specifies the method for determination of selenium antimony content.

This section applies to the determination of selenium antimony content. Measurement range. 0.0002% to 0.010%.

2 Method summary

Sample with nitric acid, hydrochloric acid dissolved in 5mol/L ~ 6mol/L HCl medium, with hydroxylamine chloride restore selenium to elemental selenium, and it Impurity elements separated. In hydrochloric acid medium with potassium borohydride as a reducing agent, with argon as the carrier gas, and the resulting hydride introduced into a quartz furnace atomic Gasifier, the fluorescence intensity was measured antimony at the atomic fluorescence spectrometer.

3 Reagents and materials

Unless otherwise indicated, the reagents used in the analysis of analytical grade reagent, analysis of water in distilled water or equivalent purity.

3.1 hydroxylamine chloride.

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

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

3.4 sulfate (rho1.84g/mL), pure class distinctions.

3.5 HCl (1 + 1).

Hydrochloride 3.6 (1 + 4).

Hydrochloride 3.7 (1 + 9).

3.8 sulfate (1 + 3).

3.9 solution of potassium borohydride (20g/L). Weigh 10.0g of potassium borohydride were dissolved in 500mL of potassium hydroxide solution (5g/L), and now with Active.

3.10 thiourea - ascorbic acid solution (50g/L + 50g/L). Weigh respectively thiourea, ascorbic acid each 25g, dissolved in water and diluted to 500mL, now with the current.

3.11 Antimony standard stock solution. Weigh 0.5000g metal antimony (Sb mass fraction >=99.95%) placed in 250mL beaker, add 20mL sulfuric acid (3.4), completely dissolved by heating and then cooled, diluted with sulfuric acid (3.8) and transferred to 1000mL volumetric flask, and then sulfuric acid (3.8) Dilute to volume, and mix. This solution 1mL containing 500µg antimony.

3.12 Antimony standard solution A. Pipette 10.00mL antimony standard stock solution (3.11) into 250mL volumetric flask (3.6) with dilute hydrochloric acid to the mark, and mix. This solution 1mL containing 20µg antimony.

3.13 Antimony standard solution B. Pipette 10.00mL antimony standard solution A (3.12) into 200mL volumetric flask, diluted with hydrochloric acid (3.7) to Volume, and mix. This solution 1mL containing 1µg antimony.

3.14 argon (Ar mass fraction >=99.99%).

4 Instrument

Atomic fluorescence spectrometer, with antimony special hollow cathode lamps and intermittent flow sampling device.

Under optimum working conditions for those who can reach the following indicators can be used.