GB/T 1819.17-2017Methods for chemical analysis of tin concentrates—Part 17: Determination of mercury content—Atomic fluorescence spectrometric method (English PDF)

Foreword

GB/T 1819 "tin concentrate chemical analysis method" is divided into 21 parts.

--- Part 1. Determination of moisture thermal drying method;

--- Part 2. Determination of tin content potassium iodate titration;

--- Part 3. Determination of iron content cerium sulfate titration method;

--- Part 4. Determination of lead content by flame atomic absorption spectrometry and Na2 EDTA titration;

--- Part 5. Determination of arsenic Arsenic antimony molybdenum blue spectrophotometry and iodometric titration;

--- Part 6. Determination of the amount of antimony; malachite green spectrophotometry and flame atomic absorption spectrometry;

--- Part 7. Determination of bismuth content by flame atomic absorption spectrometry;

--- Part 8. Determination of zinc content by flame atomic absorption spectrometry;

--- Part 9. Determination of tungsten oxide content; thiocyanate spectrophotometry;

--- Part 10. Determination of sulfur content High-frequency induction furnace combustion infrared absorption method and potassium iodate titration;

--- Part 11. Determination of the amount of aluminum oxide chromium azure S spectrophotometry;

--- Part 12. Determination of the amount of silica silicon molybdenum blue spectrophotometry and sodium hydroxide titration;

--- Part 13. Determination of magnesia, calcium oxide content; Flame atomic absorption spectrometry;

--- Part 14. Determination of copper content by flame atomic absorption spectrometry;

--- Part 15. Determination of fluorine content ion selective electrode method;

--- Part 16. Determination of silver content; Flame atomic absorption spectrometry;

--- Part 17. Determination of mercury content; atomic fluorescence spectrometry;

--- Part 18. Determination of nickel content by flame atomic absorption spectrometry;

--- Part 19. Determination of cobalt content; Flame atomic absorption spectrometry;

--- Part 20. Determination of cadmium content by flame atomic absorption spectrometry;

--- Part 21. Determination of calcium, magnesium, copper, lead, zinc, arsenic, antimony, bismuth, silver content Inductively coupled plasma atomic emission spectrometry.

This section GB/T 1819 Part 17.

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

This Part replaces GB/T 1819.17-2006 "Determination of mercury content of tin concentrates - Determination of mercury content" and GB/T 1819.17-2006 Compared with the main changes are as follows.

--- Change the determination of the method from cold atomic absorption spectrometry to atomic fluorescence spectrometry.

1 Scope

GB/T 1819 provisions of this part of the determination of mercury content in tin concentrate.

This section applies to the determination of mercury content tin concentrate. Measuring range. 0.00010% ~ 0.10%.

2 Method summary

The sample is dissolved in hydrochloric acid and nitric acid. In a dilute hydrochloric acid medium, the ionic mercury is reduced to stannic mercury by stannous chloride and introduced into quartz by argon gas In a furnace atomizer, the fluorescence intensity of mercury was measured on an atomic fluorescence spectrometer.

3 Reagent

Unless otherwise specified, only reagents that are identified as analytically pure and secondary water are used in the analysis.

3.1 Hydrochloric acid (rho = 1.19g/mL), excellent grade pure.

3.2 Nitric acid (rho = 1.42g/mL), excellent grade pure.

3.3 Mixed acid (hydrochloric acid nitric acid water = 3 1 4).

3.4 Nitric acid (1 9).

3.5 Hydrochloric acid (1 19).

3.6 Stannous chloride solution (200g/L). Weigh 20g of stannous chloride (SnCl2 · 2H2O) in 200mL beaker, add 20mL hydrochloric acid (3.1), slightly heated to dissolve completely, add 80mL water, mix well.

3.7 Potassium permanganate solution (50g/L).

3.8 Mercury standard stock solution Weigh 0.1354g of mercury dichloride (wHgCl2 >= 99.99%) in 100mL beaker, add 5mL nitric acid (3.2), slightly heated to dissolve completely, removed, cooled, transferred to a 1000mL volumetric flask, 10mL potassium permanganate solution (3.7), with nitric acid (3.4) diluted to the mark, mix well. This solution 1 mL contains 100 µg mercury.

3.9 Mercury standard solution A. Pipette 10.00mL mercury standard stock solution (3.8) in 100mL volumetric flask, dilute to the mark with nitric acid (3.4) Mix well. 1 mL of this solution contains 10 µg mercury.

3.10 Mercury standard solution B. Pipette 10.00mL mercury standard solution A (3.9) in 100mL volumetric flask, add 2mL nitric acid (3.2), 1mL potassium permanganate solution (3.7), diluted with water to the mark, mix well. 1 mL of this solution contains 1 µg mercury.

3.11 Mercury standard solution C. Pipette 10.00mL mercury standard solution B (3.10) in 100mL volumetric flask, add 2mL nitric acid (3.2), 1mL potassium permanganate solution (3.7), diluted with water to the mark, mix well. 1 mL of this solution contains 100 ng of mercury. Preparation with time.

4 Instruments

Atomic fluorescence spectrometer with mercury special hollow cathode lamp.

In the best working conditions of the instrument, anyone who can meet the following indicators can be used.