GB/T 37211.1-2018Methods for chemical analysis of germanium metal—Part 1: Determination of arsenic content—Arsenic stain method (English PDF)

Foreword

GB/T 37211 "Germanium metal 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 first 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. Method for determining the content of arsenic in impurity elements.

This section applies to the determination of the arsenic content of impurity elements in base metals. Measuring range. 0.1 x 10^-4%~1.0 x 10^-4%.

2 Principle of the method

After the sample is dissolved in aqua regia, the ruthenium is oxidized from the elemental state to the ionic state Ge4. At 84 ° C, in a hydrochloric acid solution, the ruthenium matrix is tetrachlorinated.

The volatilization form of volatilization, in which the low temperature volatile As3 is oxidized by aqua regia to a non-volatile As5 remains in the residue and then The reduction of As5 to arsine is carried out by using potassium iodide and zinc particles in a hydrochloric acid solution, and the generated arsine hydrogen and the mercury bromide paper act to form a yellow brown The color of the arsenic arsenic spot, the color of the spot color is proportional to the arsenic content. By comparing with the standard color gradation, the arsenic content is obtained.

3 Reagents

3.1 Preparation reagent solution and analysis water are deionized water or water of considerable purity, resistivity is not less than 18Mohm·cm, the experimental device The dishes were boiled and diluted with dilute nitric acid (14) overnight, rinsed thoroughly with pure water, and allowed to air dry.

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

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

3.4 Arsenic-free zinc particles, arsenic content is less than 1 x 10^-5%.

3.5 Wang Shui (currently used), 300mL hydrochloric acid (3.3) 100mL nitric acid (3.2).

3.6 Potassium iodide solution (150g/L). Weigh 15g of pure pure potassium iodide, dissolve in 100mL of water, mix and store in brown bottle.

3.7 Tin dichloride solution (100g/L). Weigh 1g of excellent grade pure tin dichloride, dissolved in 5mL of hot hydrochloric acid, add 5mL of water, mix, now Use the match now.

3.8 lead acetate cotton. immerse the cotton wool in a 40g/L lead pure lead acetate solution (containing 2mL of acetic acid per 100mL lead acetate solution). After 10 minutes, take out the excess solution and dry it at low temperature.

3.9 Mercury bromide test paper. immerse the quantitative filter paper in a 50g/L high-grade purely prepared mercury bromide alcohol solution, take it out after 40 minutes, and empty it. The air is naturally dried.

3.10 Arsenic standard storage solution, commercially available certified standard solution 100µg/mL.

3.11 Arsenic standard solution A. Pipette arsenic standard storage solution (3.10) 10.00mL in a 100mL volumetric flask, dilute with water, make up to the moment Degree, mix. 1 mL of this solution contained 10 µg of arsenic.

3.12 Arsenic Standard Solution B. Pipette 10.00 mL of arsenic standard solution A (3.11), place in a 100 mL volumetric flask, dilute with water, and dilute to volume. Degree, mix. 1 mL of this solution contained 1 µg of arsenic.