YS/T 229.3-2013Methods for chemical analysis of high pure lead. Part 3: Determination of antimony content. Atomic fluorescence spectrometry (English PDF)

Foreword

YS/T 229-2013 "high purity chemical analysis of lead" is divided into four parts.

--- Part 1. silver, copper, bismuth, aluminum, nickel, tin, magnesium, and iron - Determination of chemical spectroscopy;

--- Part 2. Determination of arsenic content by atomic fluorescence spectrometry;

--- Part 3. Determination of antimony content - Atomic Fluorescence Spectrometry;

--- Part 4. Determination of trace element contents of glow discharge mass spectrometry.

This is Part 3 YS/T 229's.

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

The partial replacement of YS/T 229.3-1994 determination of antimony content of lead in high purity (malachite green photometric method). And YS/T 229.3-1994 Compared to the main changes are as follows.

--- Changed the measurement method using atomic fluorescence spectrometry;

--- Added "precision" clause;

--- Added "the test report" requirement.

The non-ferrous metal part by the National Standardization Technical Committee (SAC/TC243) centralized.

This section is responsible for drafting unit. Zhuzhou Smelter Group Co., Ltd.

This section participated in the drafting unit. China Nonferrous Guilin Research Institute of Geology and Minerals Co. Ltd., Beijing General Research Institute of Mining and Metallurgy, Baiyin Nonferrous Group CO., LTD.

1 Scope

This section YS/T 229 specifies the method for determination of purity lead antimony content.

This section applies to the determination of antimony content of lead in high purity. Determination of antimony content range. 0.05 × 10-4% ~ 1.0 × 10-4% (mass fraction number).

2 Principle of the method

The sample is dissolved in nitric acid, precipitation of lead chloride, lead body, thiourea - ascorbic acid in the presence of antimony in hydrochloric acid medium is potassium borohydride Hydride reduction of antimony, with argon gas was introduced into the quartz furnace atomizer, the fluorescence intensity was measured antimony on the atomic fluorescence spectrometer.

3 Reagents

Unless otherwise indicated in the analysis using only recognized as a high-purity reagents and water or equivalent purity.

3.1 nitric acid (rho = 1.42g/mL).

3.2 hydrochloric acid (rho = 1.19g/mL).

3.3 nitric acid (12).

3.4 hydrochloride (11).

3.5 hydrochloride (14).

3.6 thiourea - ascorbic acid solution (50g/L). Weigh 5g thiourea (excellent pure), 5g ascorbic acid (excellent pure), dissolved in water, dilute Diluted to 100mL, and mix. The time is now equipped with.

3.7 solution of potassium borohydride (25g/L). Weigh 5g potassium borohydride (excellent pure), was added a solution of 1g of potassium hydroxide in advance (excellent pure) of 200mL of water. The time is now equipped with.

3.8 Antimony standard stock solution. Weigh 0.2740g antimony potassium tartrate (excellent pure), placed in 150mL beaker, add water 100mL low Heated dissolved and transferred to 1000mL volumetric flask, add 10mL of nitric acid (3.1), dilute to the mark and mix. This solution containing 1mL Antimony 100µg.

3.9 Antimony standard solution. Pipette 2.50mL antimony standard stock solution (3.8) in 500mL volumetric flask, was added 50mL of hydrochloric acid (3.2), with Dilute with water to volume, and mix. This solution 1mL antimony-containing 0.50µg.

3.10 argon (purity >=99.99%).

4 Instrument

Atomic fluorescence spectrometer, with high-intensity hollow cathode lamp antimony.