GB/T 1819.13-2017Methods for chemical analysis of tin concentrates—Part 13: Determination of magnesium oxide content,calcium oxide content—Flame atomic absorption 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 13.

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

This Part Replaces GB/T 1819.13-2004 "Methods for chemical analysis of tin concentrates - Determination of magnesium oxide and calcium oxide content - Flame atomic absorption Income spectroscopy. " This section compared with GB/T 1819.13-2004, the main changes are as follows.

--- The upper limit of determination of magnesia from "2.00%" to "3.50%"; Determination of calcium oxide from the original "7.00%" Change to "15.00%";

--- Calcium oxide standard solution preparation concentration from the original "6.00µg/mL" to "10.00µg/mL";

--- Modify the precision part;

--- Increase the test report terms.

1 Scope

GB/T 1819 provisions of this part of the tin concentrate magnesium oxide, calcium oxide determination.

This section applies to the determination of tin concentrate magnesium oxide, calcium oxide. Measurement range Magnesium oxide 0.010% ~ 3.50%; Calcium oxide 0.050% ~ 15.00%.

2 Method summary

Sample with hydrochloric acid, nitric acid, hydrofluoric acid, perchloric acid decomposition, in dilute hydrochloric acid medium, strontium chloride, lanthanum chloride suppression of interference elements, the use of air Gas - acetylene flame, atomic absorption spectrometer at a wavelength of 285.2nm Department, measuring the absorbance of magnesium oxide; at a wavelength of 422.6nm, measuring oxygen Calcium absorbance.

3 Reagent

Unless otherwise stated, only reagents and primary water that were identified as superior grade were used in the analysis.

3.1 Hydrochloric acid (p = 1.19 g/mL).

3.2 Nitric acid (p = 1.42 g/mL).

Hydrofluoric acid (rho = 1.13 g/mL).

3.4 Perchloric acid (rho = 1.67 g/mL).

3.5 Hydrochloric acid (1 1).

3.6 Strontium chloride solution (50g/L). Weigh 50g of strontium chloride (SrCl2 · 6H2O) in 250mL beaker, dissolved completely dissolved in water Into 1000mL volumetric flask, add 200mL hydrochloric acid (3.1), cooled to room temperature, diluted with water to the mark, and mix.

3.7 Lanthanum chloride solution (50g/L) Weigh 50g of lanthanum oxide (wLa2O3 >= 99.99%) in a 250mL beaker, moistened with a small amount of water, Slowly add 90mL hydrochloric acid (3.1), low temperature heating and dissolving completely, remove and cool to room temperature. Move into 1000mL volumetric flask and dilute with water To the mark, mix well.

3.8 Magnesium oxide standard storage solution Weigh 0.2500g magnesia (wMgO >= 99.99%, pre-fired at 800 °C 2h, placed in a desiccator Cooled to room temperature), placed in 250mL beaker, moistened with a small amount of water, add 5mL hydrochloric acid (3.5), cover the surface dish, Full, remove the cooling, water and wash the surface of the glass and the cup, into a 1000mL volumetric flask, diluted with water to the mark, mix well. This solution 1mL Containing 250µg magnesium oxide.

3.9 Magnesium oxide standard solution Pipette 10.00mL magnesia standard stock solution (3.8) placed in 500mL volumetric flask, add 10mL Hydrochloric acid (3.1), diluted with water to the mark, mix well. 1 mL of this solution contains 5 µg of magnesium oxide.

3.10 Calcium oxide standard storage solution Weigh 0.8924g of calcium carbonate (wCaCO3 >= 99.99%, pre-dried at 120 °C, placed in a desiccator Cooled to room temperature), placed in 250mL beaker, moistened with a small amount of water, add 15mL hydrochloric acid (3.5), cover the surface dish, All, remove the cooling, water and wash the surface of the glass and the cup, into a 500mL volumetric flask, diluted with water to the mark, mix well. This solution contains 1mL […]