YS/T 556.13-2011Methods for chemical analysis of antimony concentrates. Part 13: Determination of nickel content. Flame atomic absorption spectrometric method (English PDF)

Foreword

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

YS/T 556 "Methods for chemical analysis of antimony concentrate," a total of 16 parts.

--- Part 1. Determination of antimony content cerium sulfate titration;

--- Part 2. Determination of arsenic content potassium bromate titration;

--- Part 3. Determination of lead content by flame atomic absorption spectrometry;

--- Part 4. Wet water storage Gravimetric method;

--- Part 5. Determination of zinc content - Flame atomic absorption spectrometry;

--- Part 6. Determination of the amount of selenium by hydride generation - atomic fluorescence spectrometry;

--- Part 7. Determination of the amount of mercury atomic fluorescence spectrometry;

--- Part 8. Determination of sulfur content - Combustion neutralization method;

--- Part 9. Determination of the amount of gold fire assay;

--- Part 10. Determination of copper content - Flame atomic absorption spectrometry;

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

--- Part 12. Determination of bismuth content by flame atomic absorption spectrometry;

--- Part 13. Determination of nickel content by flame atomic absorption spectrometry;

--- Part 14. Determination of the amount of silver by flame atomic absorption spectrometry;

--- Part 16. lead, zinc, copper, cadmium, nickel content - Inductively coupled plasma atomic emission spectrometry.

This section YS/T Part 13 556.

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

This section is responsible for drafting unit. tin mine Twinkling Star Antimony Industry Co., Ltd., Beijing General Research Institute of Mining and Metallurgy.

This section is drafted. Guangzhou Nonferrous Metal Research Institute.

Participated in the drafting of this section. Beijing General Research Institute of Mining and Metallurgy, tin mining flash-antimony industry limited liability company.

1 Scope

This section YS/T 556 specifies the method for determination of nickel content in antimony concentrate.

This section applies to the determination of nickel content in antimony concentrate. Determination of the range of 0.0020 to 0.10%.

2 Method summary

Samples with hydrochloric acid, nitric acid dissolved, except hydrobromic volatile antimony in nitric acid medium by air - acetylene flame atomic absorption spectrometer wave Long 232.0nm measured at an absorbance of nickel. The standard curve method to calculate the amount of nickel.

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 hydrochloric acid (rho = 1.19g/mL).

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

3.3 hydrobromide (rho = 1.48g/mL).

3.4 mixed acid. 3 volumes of hydrochloric acid was mixed with 1 volume of nitric acid.

3.5 Nickel standard solution.

3.5.1 Nickel standard stock solution. Weigh 0.5000g of nickel (wNi>=99.95%) placed in 150mL beaker, add 10mL of nitric acid (3.2), cover sheet pan, over low heat until completely dissolved, remove the cooling. Transferred to 500mL volumetric flask, dilute with water to volume, and mix. this 1mL solution containing nickel 1mg.

3.5.2 Nickel standard solution. Pipette 10.00mL Nickel standard stock solution (3.5.1) in 100mL flask, add 2mL nitric acid (3.2), dilute to the mark and mix. This solution 1mL nickel-containing 100µg.

4 Instrument

Atomic absorption spectrometer, with a nickel hollow cathode lamp.

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

--- Sensitivity. characteristic concentration was 0.055µg/mL.

--- Precision. standard solution with the highest concentration of 10 times the absorbance measurements, the standard deviation should not exceed the average absorbance of 1.0%;

The lowest concentration of standard solution used (instead of "zero" concentration of the solution) absorbance measured 10 times, and the standard deviation should not exceed the maximum concentration 0.5% of the mean absorbance of standard solution.

--- 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 of not less than 0.7.

Atomic absorption spectrometer reference operating conditions.