GB/T 6150.17-2022Methods for chemical analysis of tungsten concentrates—Part 17: Determination of antimony content—Atomic fluorescence spectrometry (English PDF)

Foreword

This document is in accordance with the provisions of GB/T 1.1-2020 "Guidelines for Standardization Work Part 1: Structure and Drafting Rules of Standardization Documents" drafted.

This document is Part 17 of GB/T 6150 "Methods for Chemical Analysis of Tungsten Concentrates". GB/T 6150 has released the following parts.

--- Determination of the amount of tungsten trioxide ammonium tungstate burning gravimetric method;

--- Part 2: Determination of tin content by potassium iodate titration and inductively coupled plasma atomic emission spectrometry;

--- Determination of phosphorus content by phosphorous molybdenum yellow spectrophotometry;

--- Determination of sulfur content by high-frequency infrared absorption method;

--- Determination of calcium content by EDTA volumetric method and flame atomic absorption spectrometry;

--- Determination of wet water storage gravimetric method;

--- Determination of the amount of tantalum and niobium plasma emission spectrometry and spectrophotometry;

--- Determination of molybdenum content by thiocyanate spectrophotometry;

--- Determination of copper content by flame atomic absorption spectrometry;

--- Determination of lead content by flame atomic absorption spectrometry;

--- Determination of zinc content by flame atomic absorption spectrometry;

--- Determination of silica content by silicon molybdenum blue spectrophotometry and gravimetric method;

--- Part 13: Determination of arsenic content by atomic fluorescence spectrometry and DDTC-Ag spectrophotometry;

--- Determination of manganese content by ferrous ammonium sulfate volumetric method and flame atomic absorption spectrometry;

--- Determination of the amount of bismuth by flame atomic absorption spectrometry;

--- Determination of iron content by sulfosalicylic acid spectrophotometry;

--- Part 17: Determination of antimony content by atomic fluorescence spectrometry.

This document replaces GB/T 6150.17-2008 "Chemical Analysis of Tungsten Concentrates for Determination of Antimony Content by Hydride Atomic Absorption Spectrometry", Compared with GB/T 6150.17-2008, in addition to structural adjustment and editorial changes, the main technical changes are as follows.

a) Changed the measurement range of the method from 0.002%~0.30% to 0.0010%~0.20% (see Chapter 1, 2008 edition of Chapter 1);

b) Changed the detection method from hydride atomic absorption spectrometry to atomic fluorescence spectrometry (see Chapter 4, 2008 edition of chapter 2);

c) change tolerance to reproducibility (see 10.2, 8.2 of the 2008 edition);

d) Deleted quality assurance and control (see Chapter 9 of the 2008 edition);

e) Added the chapter "Test Report" (see Chapter 11).

Introduction

Tungsten concentrate is an important strategic resource, and tungsten and tungsten alloys are produced as important industrial raw materials.

It has the characteristics of heavy and high hardness, and is widely used in machining, metallurgy, mining, electronic communication, construction industry, weapon industry, aerospace and other fields.

GB/T 6150 aims to establish a set of complete, practical and suitable chemical production and trade requirements for tungsten concentrate products through experimental research.

Methodological standards for compositional analysis. Due to the limitations of document length, usage requirements, scope of application, and technical independence between analytical methods, etc. Therefore, GB/T 6150 is intended to consist of 20 parts.

--- Part 1: Determination of tungsten trioxide content by ammonium tungstate burning gravimetric method;

--- Part 2: Determination of tin content by potassium iodate titration and inductively coupled plasma atomic emission spectrometry;

--- Part 3: Determination of phosphorus content by phosphoro-molybdenum yellow spectrophotometry and inductively coupled plasma atomic emission spectrometry;

--- Part 4: Determination of sulfur content high frequency-infrared absorption method and combustion-iodometric method;

--- Part 5: Determination of calcium content by EDTA volumetric method and flame atomic absorption spectrometry;

--- Part 6: Determination of wet moisture content gravimetric method;

--- Part 7: Determination of tantalum and niobium content by plasma emission spectrometry and spectrophotometry;

--- Part 8: Determination of molybdenum content by thiocyanate spectrophotometry;

--- Part 9: Determination of copper content by flame atomic absorption spectrometry;

--- Part 10: Determination of lead content by hydride generation atomic fluorescence spectrometry and flame atomic absorption spectrometry;

--- Part 11: Determination of zinc content by flame atomic absorption spectrometry;

--- Part 12: Determination of silicon dioxide content by silicon molybdenum blue spectrophotometry and gravimetric method;

--- Part 13: Determination of arsenic content by atomic fluorescence spectrometry and DDTC-Ag spectrophotometry;

--- Part 14: Determination of manganese content by volumetric ammonium ferrous sulfate and flame atomic absorption spectrometry;

--- Part 15: Determination of bismuth content by hydride generation atomic fluorescence spectrometry and flame atomic absorption spectrometry;

--- Part 16: Determination of iron content by sulfosalicylic acid spectrophotometry;

--- Part 17: Determination of antimony content by atomic fluorescence spectrometry;

--- Part 18: Determination of barium content by inductively coupled plasma atomic emission spectrometry;

--- Part 19: Determination of fluorine content by ion-selective electrode method;

--- Part 20: Determination of mercury content by spectrophotometry.

The series of standardization documents for chemical analysis methods of tungsten concentrates are mainly drafted according to the technical indicators in the product standards of tungsten concentrates. Since 1985 Come, has released two versions of GB/T 6150.GB/T 6150.17-2008 has been released and implemented for more than ten years. During this period, its applicable The YS/T 231 product standard has been revised once in 2015, and various technical indicators have undergone new changes. The upstream and downstream customers of the tungsten industry There are also new requirements for product testing, analysis and testing technology has also developed and progressed, and the country has further stringent environmental protection in various industries. grid requirements. In view of this, it is indeed necessary to revise GB/T 6150.17-2008 to ensure that the standard adapts to industry changes and market demands.

This document further enhances the applicability of the standard, in improving the quality of tungsten concentrate products, promoting its production, trade and expanding application demand The face is important.

1 Scope

This document specifies the method for the determination of antimony content in tungsten concentrates.

This document is applicable to the determination of antimony content in tungsten concentrates, the determination range (mass fraction). 0.0010%~0.20%.

2 Normative references

The contents of the following documents constitute essential provisions of this document through normative references in the text. Among them, dated citations documents, only the version corresponding to that date applies to this document; for undated references, the latest edition (including all amendments) applies to this document.

GB/T 6682 Analysis Laboratory Water Specifications and Test Methods

GB/T 8170 Numerical Rounding Rules and Representation and Judgment of Limit Values

3 Terms and Definitions

There are no terms and definitions that need to be defined in this document.

4 Principles

The sample is decomposed by sulfuric acid-ammonium sulfate, tungsten, iron, manganese, etc. are complexed with citric acid in an aqueous ammonia medium, and pentavalent antimony is pre-reduced with thiourea-ascorbic acid. to trivalent antimony. In a hydride generator, antimony was reduced to hydride by potassium borohydride, and the fluorescence intensity was measured on an atomic fluorescence spectrometer.

5 Reagents or materials

Unless otherwise stated, only reagents confirmed to be analytically pure were used in the analysis.

5.1 Water, GB/T 6682, Class II.

5.2 Ammonium sulfate.

5.3 Sulfuric acid (rho=1.84g/mL).

5.4 Hydrochloric acid (rho=1.19g/mL), excellent grade pure.

5.5 Ammonia (rho=0.88g/mL).

5.6 Citric acid solution (500g/L).

5.7 Sulfuric acid (1 1).

5.8 Citric acid-potassium iodide solution. Weigh 20g of citric acid and 5g of potassium iodide, dissolve in water, dilute to 100mL with water, and mix well. time cost Now with.

5.9 Thiourea-ascorbic acid solution. Weigh 10 g of thiourea and 10 g of ascorbic acid respectively, dissolve in water, dilute to 100 mL with water, and mix.