YS/T 990.15-2014Methods for chemical analysis of copper matte. Part 15: Determination of antimony content. Atomic absorption spectrometry (English PDF)

Foreword

YS/T 990 "Methods for chemical analysis of copper matte" is divided into 18 parts.

--- Part 1. Determination of copper content iodometry;

--- Part 2. Determination of gold and silver atomic absorption spectroscopy and fire assay;

--- Part 3. Determination of sulfur content - Gravimetric method and combustion titration method;

--- Part 4. Determination of the amount of bismuth atomic absorption spectrometry;

--- Part 5. Determination of the amount of fluorine ion selective electrode method;

--- Part 6. Determination of lead content - Atomic absorption spectrometry and Na2EDTA titration;

--- Part 7. Determination of cadmium content - Atomic absorption spectrometry;

--- Part 8. Determination of arsenic content by hydride generation - atomic fluorescence spectrometry, diethyl dithiocarbamate spectrophotometry silver and potassium bromate titration;

--- Part 9. Determination of iron content dichromate method;

--- Part 10. Determination of silicon dioxide content molybdenum blue spectrophotometric method and silicon potassium fluoride titration;

--- Part 11. Determination of the amount of nickel atom absorption spectrometry;

--- Part 12. Determination of the amount of chromium oxide of aluminum Azure S Spectrophotometry;

--- Part 13. Determination of magnesium oxide content - Atomic absorption spectrometry;

--- Part 14. Determination of the amount of zinc atomic absorption spectrometry and Na2EDTA titration;

--- Part 15. Determination of antimony content - Atomic absorption spectrometry;

--- Part 16. Determination of mercury content - Cold atomic absorption spectrometry;

--- Part 17. Determination of the amount of cobalt atomic absorption spectrometry;

--- Part 18. lead, zinc, nickel, arsenic, bismuth, antimony, calcium, magnesium, cadmium, cobalt content - Inductively coupled plasma atomic emission spectrometry.

This is Part 15 YS/T 990's.

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 unit. Zhongtiaoshan Nonferrous Metals Group Co., Ltd. Daye Nonferrous Metals Group Holdings Limited.

This section is drafted. Tongling Nonferrous Metals Group Holdings Limited.

Participated in the drafting of this section. Guangzhou Nonferrous Metal Research Institute, Beijing Nonferrous Metal Research Institute, Hangzhou Fuchunjiang Smelting Co., Ltd., Shenzhen Shenzhen City Lingnan Nonferrous Metals Corporation Limited.

1 Scope

This section YS/T 990 specifies the method for determination of copper matte antimony content.

This section applies to the determination of copper in ice antimony content. Determination of the range of 0.10% to 1.20%.

2 Method summary

Samples with hydrochloric acid, nitric acid decomposition, get rid of nitric acid with hydrochloric acid, dilute hydrochloric acid medium, atomic absorption spectrometer at a wavelength of 217.6nm, with Air - acetylene flame measured absorbance.

3 Reagents

Unless otherwise indicated in the analysis using only recognized as analytical grade reagents and distilled or deionized water or equivalent purity.

3.1 potassium chlorate.

3.2 hydrochloric acid (rho = 1.19g/mL).

3.3 nitric acid (rho = 1.42g/mL).

3.4 tartaric acid solution (100g/L).

3.5 Antimony standard stock solution. Weigh 1.197g antimony trioxide (wSb>=99.99%), placed in 200mL beaker, add 50mL nitrate Acid (3.3), low heat until completely dissolved, boil to remove nitrogen oxides, cooling, additional 50mL of nitric acid (3.3), 20mL tartaric acid solution (3.4) and transferred to 1000mL volumetric flask, dilute with water to volume, and mix. This solution 1mL 1mg containing antimony.

3.6 Antimony standard solution. Pipette 10.00mL antimony standard stock solution (3.5) in 100mL flask, a solution of tartaric acid was added 10mL (3.4), 10mL of hydrochloric acid (3.2), dilute to the mark and mix. This solution 1mL containing 100µg antimony.

4 Instrument

Atomic absorption spectrometer, with antimony hollow cathode lamp, the instrument should be deducted with background apparatus.

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

--- Characteristic concentration. the test solution consistent with the measurement matrix solution, the concentration of antimony features should not exceed 0.29µg/mL;

--- Precision. standard solution with the highest concentration of 11 times the absorbance measurements, the standard deviation should not exceed the average absorbance of 1.0%;

With the lowest concentration of standard solution (not "zero" concentration of the standard) measuring the absorbance of 11 times, the standard deviation should not exceed the maximum 0.5% high concentration of the standard average absorbance;

--- Linear curve. The curve is divided into five sections according to concentration, absorbance difference between the absorbance difference between the highest and the lowest segment of the segment Ratio should not be less than 0.85.

5 Sample

5.1 Sample size should not exceed 100µm.