GB/T 8647.11-2019Methods for chemical analysis of nickel－Part 11: Determination of magnesium，aluminum，manganese，cobalt，copper，zinc，cadmium，tin，antimony，lead，bismuth contents－Inductively coupled plasma mass spectrometry (English PDF)

Foreword

GB/T 8647 "Methods for chemical analysis of nickel" is divided into 11 parts.

- Part 1: Determination of iron content - Sulfosalicylic acid spectrophotometric method;

- Part 2: Determination of aluminium content - Electrothermal atomic absorption spectrometric method;

- Part 3: Determination of silicon content - Molybdenum blue spectrophotometric method;

- Part 4: Determination of phosphorous content - Molybdenum blue spectrophotometric method;

- Part 5: Determination of magnesium content - Flame atomic absorption spectrometric method;

- Part 6: Determination of cadmium, cobalt, copper, manganese, lead and zinc contents - Flame atomic absorption spectrometric method;

- Part 7: Determination of arsenic, antimony, bismuth, tin and lead contents - Electrothermal atomic absorption spectrometric method;

- Part 8: Determination of sulphur content - Infra-red absorption method after high frequency induction furnace combustion;

- Part 9: Determination of carbon content - Infra-red absorption method after high frequency induction furnace combustion;

- Part 10: Determination of arsenic, cadmium, lead, zinc, antimony, bismuth, tin, cobalt, copper, manganese, magnesium, silicon, aluminium, iron contents - Atomic emission spectrometric method;

- Part 11: Determination of magnesium, aluminum, manganese, cobalt, copper, zinc, cadmium, tin, antimony, lead, bismuth contents - Inductively coupled plasma mass spectrometry.

This Part is Part 11 of GB/T 8647.

This Part was drafted in accordance with the rules given in GB/T 1.1-2009.

1 Scope

This Part of GB/T 8647 specifies the methods for the determination of magnesium, aluminum, manganese, cobalt, copper, zinc, cadmium, tin, antimony, lead, and bismuth contents in nickel.

This Part applies to the determination of magnesium, aluminum, manganese, cobalt, copper, zinc, cadmium, tin, antimony, lead, and bismuth contents in nickel. The determination range is 0.00010 % ~ 0.0050 %.

2 Method summary

Dissolve the sample in nitric acid, on an inductively coupled plasma mass spectrometer, using the working curve method and the method of online addition of an internal standard mixed solution of scandium, rhodium, and rhenium, determine the contents of magnesium, aluminum, manganese, cobalt, copper, zinc, cadmium, tin, antimony, lead, and bismuth in the test solution.

3 Reagents or materials

Unless otherwise specified, the water used in the analysis is grade 1 water or water of equivalent purity. All test instruments are thoroughly rinsed with hot nitric acid and then rinsed with water.

3.1 Nitric acid (rho = 1.42 g/mL), MOS grade.

3.2 Nitric acid (1 + 1).

3.3 Standard stock solution. Use valid, certified single-element standard stock solutions of magnesium, aluminum, manganese, cobalt, copper, zinc, cadmium, tin, antimony, lead, bismuth, scandium, rhodium, and rhenium, with a mass concentration of 1000 µg/mL.

3.4 Mixed standard solution A. Respectively transfer 1.00 mL of each standard stock solution (3.3) of magnesium, aluminum, manganese, cobalt, copper, zinc, cadmium, tin, antimony, lead, and bismuth into a 100 mL volumetric flask containing 10 mL of nitric acid (3.2), dilute to the mark with water, and mix thoroughly. 1 mL of this solution contains 10 µg of magnesium, aluminum, manganese, cobalt, copper, zinc, cadmium, tin, antimony, lead, and bismuth respectively.

3.5 Mixed standard solution B. Respectively transfer 1.00 mL of each mixed standard solution A (3.4) into a 100 mL volumetric flask containing 10 mL of nitric acid (3.2), dilute to the mark with water, and mix thoroughly. 1 mL of this solution contains 100 ng of magnesium, aluminum, manganese, cobalt, copper, zinc, cadmium, tin, antimony, lead, and bismuth respectively.

3.6 Internal standard mixed standard solution. Use the standard stock solution of scandium, rhodium, and rhenium (3.3) with a mass concentration of 1000 µg/mL, dilute sequentially before use, so that 1 mL of the diluted solution contains 10 ng of scandium, rhodium, and rhenium respectively. The medium is nitric acid (2 + 98).

3.7 Argon (wAr >= 99.99 %).

4 Instrumentation

4.1 Inductively coupled plasma mass spectrometer, with an instrument mass resolution of not less than 0.8 amu ± 0.1 amu.

4.2 The recommended mass numbers for isotope determination of magnesium, aluminum, manganese, cobalt, copper, zinc, cadmium, tin, antimony, lead, bismuth, scandium, rhenium, and rhodium are shown in Table 1.

5 Sample

The sample shall be in the form of crumbs or powder.

6 Test procedure