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YS/T 556.3-2009Methods for chemical analysis of antimony concentrates. Part 3: Determination of lead content. Flame atomic absorption spectrometric method (English PDF)

锑精矿化学分析方法 第3部分:铅量的测定火焰原子吸收光谱法

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Issued by

Ministry of Industry and Information Technology

Level / Type

National · Recommended

Issue date

December 4, 2009

Implementation date

June 1, 2010

Scope

YS/T 556.3-2009 is the English-translated version of 锑精矿化学分析方法 第3部分:铅量的测定火焰原子吸收光谱法.

YS/T 556.3-2009 — This section YS/T 556 specifies the method for determination of the amount of lead antimony concentrate. This section applies to the determination of antimony in the amount of lead in concentrate, measuring range. 0.0040% to 1.00%.

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Document preview — YS/T 556.3-2009

National Standard of the People's Republic of China

ICS
73.060
Classification
D 42
Replacing
YS/T 556.3-2006

Issued by: Ministry of Industry and Information Technology

Contents

  • Foreword
  • 1 Scope
  • 2 Method summary
  • 3 Reagents
  • 3.6 Lead standard stock solution
  • 3.7 Lead standard solution
  • 4 Instrument

Foreword

YS/T 556-2009 "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 15. antimony, tin measured by hydride generation - atomic fluorescence spectrometry;

--- Part 16. Determination of antimony metal content by inductively coupled plasma emission spectrometry.

This section YS/T 556 Part 3.

"Antimony concentrates - Determination of lead content" in this section instead of YS/T 556.3-2006 (formerly GB/T 15080.3-1994).

Compared with YS/T 556.3-2006, this part of the following changes.

--- Text format has been modified;

--- Table 1 and plotted in the curve of the concentration of lead standard was modified;

--- Complements the precision and quality assurance and control provisions.

The non-ferrous metal part by the National Standardization Technical Committee and 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. Hunan Nonferrous Metal Research Institute.

Participated in the drafting of this section. Tin Mine Twinkling Star Antimony Industry Co., Ltd., Hunan Chenzhou Mining Co., Ltd.

1 Scope

This section YS/T 556 specifies the method for determination of the amount of lead antimony concentrate.

This section applies to the determination of antimony in the amount of lead in concentrate, measuring range. 0.0040% to 1.00%.

2 Method summary

After the sample was dissolved in nitric acid with hydrochloric acid and evaporated to dryness, repeat adding hydrobromide volatile except antimony in dilute hydrochloric acid medium, using air - acetylene flame to the original Sub absorption spectrometer wavelength 283.3nm at measuring the absorbance of lead. In the standard curve obtained lead content. Impurities do not interfere with the test compound Determination.

3 Reagents

Unless otherwise indicated, the reagents used in this section refer to water and analytical grade and third grade water.

3.1 hydrochloride (rho1.19g/mL).

3.2 HCl (1 + 1).

Nitrate 3.3 (rho1.42g/mL).

3.4 nitric acid (1 + 1).

3.5 hydrobromide (rho1.48g/mL).

3.6 Lead standard stock solution

Weigh 1.0000g metallic lead (Pb>=99.99%) in 250mL beaker, add 20mL of nitric acid (3.4), heat gently to dissolve completely, Boiling 2min ~ 3min get rid of nitrogen oxides, remove the cooled to room temperature and transferred to 1000mL volumetric flask, dilute to the mark with water, mix uniform. This solution 1mL lead 1mg.

3.7 Lead standard solution

Pipette 10.00mL (3.6) solution in 100mL flask, add 5mL hydrochloric acid (3.2), dilute to the mark and mix. this Solution 1mL lead 100µg.

4 Instrument

Atomic absorption spectroscopy (AAS), attached to the hollow core lead cathode lamp.

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

--- Characteristic concentration. In line with the determination of the sample solution matrix solution features lead concentration should not exceed 0.20µg/mL.

--- Precision. measuring the highest concentration of the standard solution absorbance 10 times the standard deviation should not exceed 1.5% of the average absorbance;

Measure the lowest concentration of the standard solution (not "zero" concentration of the standard) absorbance of 10 times the standard deviation should not exceed the maximum 0.5% 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 of not less than 0.7.

Atomic absorption spectrometer reference operating conditions.

--- Wavelength 283.3nm;

......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 4 pages — is available in the English PDF.

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