YS/T 820.13-2012Methods for chemical analysis of laterite nickel ores. Part 13: Determination of lead content. Flame atomic absorption spectrometry (English PDF)

Foreword

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

YS/T 820-2012 "Methods for chemical analysis of nickel laterite ore" is divided into 26 parts.

--- Part 1. Determination of nickel content by flame atomic absorption spectrometry;

--- Part 2. Determination of the amount of nickel dimethylglyoxime spectrophotometry;

--- Part 3. Determination of total iron content of dichromate method;

--- Part 4. Determination of phosphorus content - Molybdenum blue spectrophotometric method;

--- Part 5. Determination of cobalt content by flame atomic absorption spectrometry;

--- Part 6. Determination of copper content - Flame atomic absorption spectrometry;

--- Part 7. Determination of calcium and magnesium content by flame atomic absorption spectrometry;

--- Part 8. Determination of the amount of silica silicon potassium fluoride titration;

--- Part 9. scandium, cadmium content - Inductively Coupled Plasma - Mass Spectrometry;

--- Part 10. calcium, cobalt, copper, magnesium, manganese, nickel, zinc and phosphorus content - Inductively Coupled Plasma - Atomic Emission Spectrometry;

--- Part 11. Determination of the amount of fluorine and chlorine ion chromatography;

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

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

--- Part 14. Determination of zinc content - Flame atomic absorption spectrometry;

--- Part 15. Determination of cadmium content by flame atomic absorption spectrometry;

--- Part 16. carbon, sulfur content was measured by high frequency combustion infrared absorption spectroscopy;

--- Part 17. arsenic, antimony, bismuth contents hydride generation - atomic fluorescence spectrometry;

--- Part 18. Determination of mercury content - Cold atomic absorption spectrometry;

--- Part 19. Determination of energy aluminum, chromium, iron, magnesium, manganese, nickel and silicon content dispersive X-ray fluorescence spectrometry;

--- Part 20. Determination of aluminum content by EDTA titration;

--- Part 21. Determination of chromium content ammonium ferrous sulfate titration;

--- Part 22. Determination of magnesium content EDTA titration;

--- Part 23. cobalt, iron, nickel, phosphorus, aluminum oxide, calcium oxide, chromium oxide, magnesium oxide, manganese oxide, silicon dioxide and titanium dioxide volume Wavelength dispersive X-ray fluorescence spectrometry;

--- Part 24. Determination of hygroscopic water weight method;

--- Part 25. Determination of combined water content - Gravimetric method;

--- Part 26. Determination of loss on ignition - Gravimetric method.

This section YS/T 13820-2012 part of.

This standard by the national non-ferrous metals Standardization Technical Committee (SAC/TC243) centralized.

This standard by the Beijing General Research Institute of Mining and Metallurgy, People's Republic of China Bayuquan Exit Inspection and Quarantine, Jinchuan Group Ltd, Drafted.

1 Scope

This section YS/T 820 provides for the determination of lead content of nickel laterite ore.

This section applies to the determination of lead content of nickel laterite ore. Measurement range. 0.010% to 0.50%.

2 Method summary

Sample of nitric acid, hydrochloric acid, hydrofluoric acid, perchloric acid were dissolved. Salts dissolved in nitric acid in acid medium, with air - acetylene flame, the original Sub absorption spectrometer wavelength at 283.3nm measured absorbance of lead, calculate the amount of lead.

3 Reagents

Unless otherwise indicated in the analysis using only recognized as analytical grade reagents and distilled or deionized water or equivalent purity.

Nitrate 3.1 (rho1.42g/mL).

3.2 hydrochloride (rho1.19g/mL).

3.3 Hydrofluoric acid (rho1.15g/mL).

3.4 perchloric acid (rho1.67g/mL).

3.5 nitric acid (11).

3.6 lead standard stock solution. Weigh 1.0000g metallic lead (wPb>=99.99%) in 500mL beaker, add 40mL of nitric acid (3.5), cover with a watch glass, low-temperature dissolution, cooling. Transferred 1000mL volumetric flask, was added 10mL of nitric acid (3.5), diluted with water to the mark with Degree, and mix. 1mL solution containing 1mg lead.

3.7 Lead standard solution. Pipette 10.00mL lead standard stock solution (3.6) in 100mL flask, add 10mL of nitric acid (3.5), Dilute with water to volume, and mix. This solution 1mL containing 100µg lead.

4 Instrument

Atomic absorption spectrometer, with a lead hollow cathode lamp.

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

--- Characteristic concentration. the test solution is consistent with the measurement of the solution, characterized in lead concentration should not exceed 0.45µg/mL ± 0.09µg/mL.

--- Precision. measure 10 times the absorbance of the highest concentration of the standard solution, the standard deviation should not exceed 1% of the average absorbance; most Low concentrations of the standard solution (not a "zero" standard solution) absorbance measured 10 times, and the standard deviation should not exceed the maximum standard concentration 0.5% average absorbance of the 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 0.80.