GB/T 37211.2-2018Methods for chemical analysis of germanium metal—Part 2: Determination of aluminium,iron,copper,nickle,lead,cadmium, magnesium,cobalt,indium,zinc content—Inductively coupled plasma mass spectrometry method (English PDF)

Foreword

GB/T 37211 "Metal germanium chemical analysis method" is divided into two parts.

--- Part 1. Determination of arsenic content - Arsenic speckle method;

--- Part 2. Determination of aluminum, iron, copper, nickel, lead, calcium, magnesium, cobalt, indium and zinc content by inductively coupled plasma mass spectrometry.

This part is the second part of GB/T 37211.

This part is drafted in accordance with the rules given in GB/T 1.1-2009.

1 Scope

This part of GB/T 37211 stipulates the base metals such as reduced antimony ingot, reduced niobium powder, district melting ingot and its waste, tantalum single crystal and its waste. Determination of the content of aluminum, iron, copper, nickel, lead, calcium, magnesium, cobalt, indium and zinc.

This section applies to the determination of the content of impurity elements such as aluminum, iron, copper, nickel, lead, calcium, magnesium, cobalt, indium and zinc in metal ruthenium. Measuring range. 0.005 x 10^-4%~1.00 x 10^-4%.

2 Principle of the method

After the sample is oxidized and dissolved by aqua regia, it generates volatile ruthenium tetrachloride, which is evaporated to a metal impurity ion after low temperature (70 ° C ~ 100 ° C) evaporation.

After separation, the residue was evaporated and dissolved in nitric acid to make a volume, which was measured on an inductively coupled plasma mass spectrometer (ICP-MS).

3 Reagents

3.1 Preparation solution and analysis water are deionized water or water of considerable purity, the resistivity is not less than 18Mohm·cm, and the vessels used in the experiment are all After soaking in dilute nitric acid (14) for overnight, rinse thoroughly with pure water for use.

3.2 Hydrochloric acid (rho=1.19g/mL). MOS grade or equivalent purity.

3.3 Nitric acid (rho=1.42g/mL). MOS grade or equivalent purity.

3.4 Wangshui. Mix hydrochloric acid (3.2) and nitric acid (3.3) in a ratio of 3.1.

3.5 Multi-element mixed standard solution A. It is prepared by domestic and foreign certified standard materials that can be traced back to the source. Aluminum, iron, copper, nickel, The mass concentrations of lead, calcium, magnesium, cobalt, indium and zinc are each 100 µg/mL.

3.6 Mixing standard solution B. Pipette 10.00mL of mixed standard solution A (3.5) into a 100mL volumetric flask, add 5mL of nitric acid (3.3), dilute to the mark with water and mix. 1 mL of this solution contained 10 µg each of aluminum, iron, copper, nickel, lead, calcium, magnesium, cobalt, indium, and zinc.

3.7 Mixing standard solution C. Pipette 10.00mL of mixed standard solution B (3.6) into a 100mL volumetric flask and add 5mL of nitric acid (3.3). Dilute to the mark with water and mix. 1 mL of this solution contained 1 µg of each of aluminum, iron, copper, nickel, lead, calcium, magnesium, cobalt, indium, and zinc.

3.8 Mixing standard solution D. Pipette 10.00mL of mixed standard solution C (3.7) into a 100mL volumetric flask, add 5mL of nitric acid (3.2), dilute to the mark with water and mix. 1 mL of this solution contained 100 ng each of aluminum, iron, copper, nickel, lead, calcium, magnesium, cobalt, indium, and zinc.

3.9 Mixed internal standard solution A. It is prepared by using certified standard materials that can be traced back to the source at home and abroad. The quality of lanthanum, cerium and lanthanum in this solution The concentration was 100 µg/mL.

3.10 Mixing internal standard solution B. Pipette 10.00mL of mixed internal standard solution A (3.9) into a 100mL volumetric flask, add 2mL Nitric acid (3.3), dilute to the mark with water and mix. 1 mL of this solution contained 10.00 µg each of hydrazine, hydrazine, and hydrazine.