YS/T 556.2-2009Methods for chemical analysis of antimony concentrates. Part 2: Determination of arsenic content. Potassium bromate titration method (English PDF)

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 2.

"Antimony concentrates - Determination of arsenic content" in this section instead of YS/T 556.2-2006 (formerly GB/T 15080.2-1994).

Compared with YS/T 556.2-2006, this part of the following changes.

--- Text format has been modified;

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

This section arbitration.

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.

1 Scope

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

This section applies to the determination of the amount of arsenic in antimony concentrate. Measuring range. 0.10% to 2.00%.

2 Method summary

Sample with sulfuric acid - potassium sulfate dissolved, filter paper made after carbonation reducing agent and co-solvent, not less than hydrochloric acid solution 9mol/L, the use of benzene Extract arsenic trichloride, arsenic back-extracted with water. In hydrochloric acid medium, methyl orange as indicator, titration of trivalent arsenic with potassium bromate standard.

3 Reagents

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

3.1 potassium sulfate.

3.2 sulfate (rho1.84g/mL).

3.3 hydrochloride (rho1.19g/mL).

3.4 benzene.

3.5 sulfate (1 + 1).

3.6 HCl (3 + 1).

3.7 HCl (1 + 1).

3.8 methyl orange indicator (1g/L).

3.9 Sodium hydroxide solution (200g/L).

3.10 arsenic standard solution (1mg/mL).

Weigh 1.3203g trioxide reference reagent (previously at 100 °C ~ 105 °C drying 1h, placed in a desiccator, cooled to room Temperature), placed in a beaker of 250mL, 20mL was added sodium hydroxide solution (3.9) was dissolved to a clear, 100mL water was added, 10 mL of sulfuric acid (3.5), cooled to room temperature and transferred to 1000mL volumetric flask, dilute with water to volume, and mix.

3.11 potassium bromate standard titration solution (Ba KBrO3 about 0.2mol/L).

3.11.1 preparation. Weigh 0.28g of potassium bromate placed in 250mL beaker, add 100mL water dissolved and transferred to 1000mL volumetric flask the diluted with water to volume, and mix.

3.11.2 Calibration. Pipette three 10.00mL arsenic standard solution (3.10), were added to 45mL containing hydrochloric acid (3.3) of 125mL liquid separation Funnel, and mix. 5.4.3 - 5.4.6 by the following conduct.

Along with the calibration blank test.

According to equation (1) calculate the standard volumetric potassium bromate solution (3.11) of the actual concentration.

Where.

Ba --- potassium bromate standard volumetric solution (3.11) of the actual concentration in units of moles per liter (mol/L);

Vp 1 --- titration of arsenic consumption of potassium bromate standard solution (3.11) of the volume, in milliliters (mL);

V0 --- calibration blank solution volume of consumption of potassium bromate standard titration solution (3.11), expressed in milliliters (mL);