GB/T 6150.4-2023Methods for chemical analysis of tungsten concentrates—Part 4: Determination of sulfur content—High frequency-infrared absorption method and combustion-iodometric method (English PDF)

Foreword

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

This document is Part 4 of GB/T 6150 "Chemical Analysis Methods for Tungsten Concentrates". GB/T 6150 has released the following parts.

---Part 1: Determination of tungsten trioxide content by ammonium tungstate ignition 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 phosphomolybdenum yellow spectrophotometry and inductively coupled plasma atomic emission spectrometry;

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

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

---Part 6: Gravimetric method for determination of wet water content;

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

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

---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;

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

---Part 12: 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;

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

---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.

This document replaces GB/T 6150.4-2008 "Chemical analysis method of tungsten concentrate - Determination of sulfur content by high-frequency infrared absorption method" and is consistent with Compared with GB/T 6150.4-2008, in addition to structural adjustments and editorial changes, the main technical changes are as follows.

a) The measurement range of Method 1 has been changed from 0.1%~2% to 0.10%~4.00% (see Chapter 1, 2008 edition of Chapter 1);

b) Added "Terms and Definitions" (see Chapter 3);

c) The weighing amounts of the sample and flux in Method 1 have been changed (see 4.5.1, 4.5.5, 6.1 and 6.5.1 of the 2008 edition);

d) Changed "precision" (see 4.7, Chapter 7 of the 2008 edition);

e) The combustion-iodometric method is added, with a measurement range of 1.00%~10.00% (see Chapter 5);

f) Added "Test Report" (see Chapter 6);

g) Quality Assurance and Control (Chapter 8 of the 2008 edition) has been deleted.

Introduction

Tungsten concentrate is an important strategic resource. Tungsten and tungsten alloys produced from tungsten concentrate as an important industrial raw material have high melting point, high specific Due to its heavy weight and high hardness, it is widely used in mechanical processing, metallurgy, mining, electronic telecommunications, construction industry, weapons industry, aerospace and other fields.

GB/T 6150 aims to establish through experimental research a complete set of chemical compositions that are practical and adaptable to the production and trade needs of tungsten concentrate products.

Methodological standards for analysis. Limited by the length of the document, usage requirements, scope of application, and technical independence between each analysis method, etc. Therefore, GB/T 6150 is planned to consist of 20 parts.

---Part 1: Determination of tungsten trioxide content. Ammonium tungstate ignition gravimetric method. The purpose is to establish the determination of tungsten trioxide content method.

---Part 2: Determination of tin content by potassium iodate titration and inductively coupled plasma atomic emission spectrometry. The purpose is to ensure Determination method of tin content.

---Part 3: Determination of phosphorus content by phosphomolybdenum yellow spectrophotometry and inductively coupled plasma atomic emission spectrometry. The purpose is To establish a method for determining phosphorus content.

---Part 4: Determination of sulfur content by high-frequency induction infrared absorption method and combustion-iodometric method. The purpose is to establish the determination of sulfur content method.

---Part 5: Determination of calcium content by EDTA volumetric method and flame atomic absorption spectrometry. The purpose is to establish the measurement of calcium content Determine the method.

---Part 6: Gravimetric method for determination of wet water content. The purpose is to establish a method for determining wet water content.

---Part 7: Determination of tantalum and niobium content by plasma emission spectrometry and spectrophotometry. The purpose is to establish that tantalum and niobium contain Quantity measurement method.

---Part 8: Determination of molybdenum content by thiocyanate spectrophotometry. The purpose is to establish a method for determining molybdenum content.

---Part 9: Determination of copper content by flame atomic absorption spectrometry. The purpose is to establish a method for measuring copper content.

---Part 10: Determination of lead content by hydride generation atomic fluorescence spectrometry and flame atomic absorption spectrometry. The purpose is to ensure Method for determination of vertical lead content.

---Part 11: Determination of zinc content by flame atomic absorption spectrometry. The purpose is to establish a method for determining zinc content.

---Part 12: Determination of silica content by silicon molybdenum blue spectrophotometry and gravimetric method. The purpose is to establish the silica content method of determination.

---Part 13: Determination of arsenic content by atomic fluorescence spectrometry and DDTC-Ag spectrophotometry. The aim was to establish the arsenic content method of determination.

---Part 14: Determination of manganese content by ferrous ammonium sulfate volumetric method and flame atomic absorption spectrometry. The aim is to establish the manganese content method of determination.

---Part 15: Determination of bismuth content by hydride generation atomic fluorescence spectrometry and flame atomic absorption spectrometry. The purpose is to ensure Method for determination of bismuth content.

---Part 16: Determination of iron content by sulfosalicylic acid spectrophotometry. The purpose is to establish a method for determining iron content.

---Part 17: Determination of antimony content by atomic fluorescence spectrometry. The purpose is to establish a method for determining antimony content.

---Part 18: Determination of barium content by inductively coupled plasma atomic emission spectrometry. The purpose is to establish the determination of barium content method.

---Part 19: Determination of fluorine content by ion selective electrode method. The purpose is to establish a method for measuring fluorine content.

---Part 20: Determination of mercury content by spectrophotometry. The purpose is to establish a method for measuring mercury content.

GB/T 6150.4-2008 has been released and implemented for more than ten years, and it is no longer fully applicable to the current "Tungsten Concentrate" product standard (YS/T 231-2015). In the standard, there are new changes in the sulfur content indicators for different brands of tungsten concentrates. Among them, fifth-grade scheelite and black The sulfur content of tungsten concentrate can reach up to 4.5%, and the current standards can no longer meet the testing requirements of upstream and downstream customers in the tungsten industry for sulfur content in products.

Moreover, as sulfur is an important element affecting the quality of tungsten concentrate products, there are further strict requirements for the accurate determination of sulfur content. Whereas Therefore, it is necessary to revise GB/T 6150.4-2008 to ensure that the standard adapts to industry changes and meets market demand.

This document makes up for the shortcomings of the narrow measurement range of the high-frequency induction infrared absorption method by adding the combustion-iodometric method, and expands the scope of the method.

The scope is more in line with the needs of the tungsten industry for product testing. At the same time, the weighing amounts of iron and tin fluxes in the high-frequency induction infrared absorption method were changed.

This solves the problem of sample splashing during the measurement process. This document further improves the applicability and accuracy of the standard, and plays an important role in improving the quality of tungsten concentrate products.

It is of great significance to promote its production, trade and expand application demand.

1 Scope

This document describes a method for the determination of sulfur content in tungsten concentrates.

This document is applicable to the determination of sulfur content in tungsten concentrate and includes two methods (Method 1.High-frequency induction infrared absorption method; Method 2.Combustion-iodometric method). Method 1 measurement range (mass fraction). 0.10%~4.00%; Method 2 measurement range (mass fraction). 1.00%~ 10.00%. For overlapping measurement ranges, Method 2 will be used as the arbitration method.

2 Normative reference documents

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

GB/T 8170 Numerical rounding rules and representation and determination of limit values

GB/T 17433 Basic terminology for chemical analysis of metallurgical products

3 Terms and definitions

The terms and definitions defined in GB/T 17433 apply to this document.

4 Method 1.High-frequency induction infrared absorption method