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GB/T 6150.3-2023Methods for chemical analysis of tungsten concentrates—Part 3: Determination of phosphorus content—The phosphorus molybdenum yellow spectrophotometry and inductively coupled plasma atomic emission spectrometry (English PDF)

钨精矿化学分析方法 第3部分:磷含量的测定 磷钼黄分光光度法和电感耦合等离子体原子发射光谱法

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Issued by

SAMR; SAC

Level / Type

National · Recommended

Issue date

November 27, 2023

Implementation date

June 1, 2024

Scope

GB/T 6150.3-2023 is the English-translated version of 钨精矿化学分析方法 第3部分:磷含量的测定 磷钼黄分光光度法和电感耦合等离子体原子发射光谱法.

GB/T 6150.3-2023 is part 3 of the Chinese national series for the chemical analysis of tungsten concentrates and covers the determination of phosphorus by two methods: phosphomolybdenum yellow spectrophotometry as method 1, over a mass fraction of 0.0050 % to 1.00 %, and inductively coupled plasma atomic emission spectrometry as method 2, above 1.00 % and up to 10.00 %.

In method 1 the sample is alkali-fused and leached, phosphorus is co-precipitated with beryllium hydroxide using beryllium sulfate as the carrier to separate it from other elements, and the absorbance of the ammonium vanadate-ammonium molybdate colour in nitric acid is read at 420 nm against a working curve; the text states that residual tungsten, arsenic and silicon do not then affect the result.

It replaces GB/T 6150.3-2009, was issued on 27 November 2023 and has applied since 1 June 2024.

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Document preview — GB/T 6150.3-2023

National Standard of the People's Republic of China

ICS
77.120.99
Classification
H 14
Replacing
GB/T 6150.3-2009

Issued by: State Administration for Market Regulation; Standardization Administration of the PRC

Contents

  • Foreword
  • Introduction
  • 1 Scope
  • 2 Normative reference documents
  • 3 Terms and definitions
  • 4 Method 1. Phosphomolybdenum yellow spectrophotometry

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 3 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 6150.3-2009 "Methods for chemical analysis of tungsten concentrate - Determination of phosphorus content by phosphomolybdenum yellow spectrophotometric method" and is consistent with Compared with GB/T 6150.3-2009, in addition to structural adjustments and editorial changes, the main technical changes are as follows:

a) The measurement range of Method 2 has been increased (see Chapter 1);

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

c) Added "water" (see 4.2.1);

d) Added "numeric rounding" (see 4.6);

e) "Precision" has been changed (see 4.7, Chapter 8 of the 2009 edition);

f) Added method 2 inductively coupled plasma atomic emission spectrometry (see Chapter 5);

g) Quality Assurance and Control has been deleted (see Chapter 9 of the 2008 edition).

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 set of complete, practical and chemical chemistry that is suitable for the production and trade of tungsten concentrate products.

Methodological standards for compositional 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. The purpose is to establish a gravimetric method for determining the content of tungsten trioxide in tungsten concentrate.

---Part 2. Determination of tin content. The purpose is to establish titration method and inductively coupled plasma atomic emission spectrometry method for the determination of tungsten Methods for tin content in concentrates.

---Part 3. Determination of phosphorus content. The purpose is to establish spectrophotometry and inductively coupled plasma atomic emission spectrometry to measure Method for determining phosphorus content in tungsten concentrate.

---Part 4. Determination of sulfur content. The purpose is to establish high-frequency induction infrared absorption method and combustion-iodometric method to determine sulfur in tungsten concentrate. content method.

---Part 5. Determination of calcium content. The purpose is to establish a method for determining the calcium content in tungsten concentrate using volumetric method and atomic absorption spectrometry. method.

---Part 6. Determination of wet water content. The purpose is to establish a gravimetric method for determining the wet water content in tungsten concentrate.

---Part 7. Determination of tantalum and niobium content. The purpose is to establish inductively coupled plasma emission spectrometry and spectrophotometry.

Method for determination of tantalum and niobium content in tungsten concentrate.

---Part 8. Determination of molybdenum content. The purpose is to establish a method for spectrophotometric determination of molybdenum content in tungsten concentrate.

---Part 9. Determination of copper content. The purpose is to establish a method for determination of copper content in tungsten concentrate using flame atomic absorption spectrometry.

---Part 10. Determination of lead content. The purpose is to establish atomic fluorescence spectrometry and flame atomic absorption spectrometry for the determination of tungsten concentrate lead content.

---Part 11. Determination of zinc content. The purpose is to establish a method for determination of zinc content in tungsten concentrate by flame atomic absorption spectrometry.

---Part 12. Determination of silica content. The purpose is to establish a spectrophotometric and gravimetric method for the determination of silica in tungsten concentrates. content method.

---Part 13. Determination of arsenic content. The purpose is to establish atomic fluorescence spectrometry and spectrophotometry to determine arsenic content in tungsten concentrate. Methods.

---Part 14. Determination of manganese content. The purpose is to establish volumetric method and flame atomic absorption spectrometry method to determine the manganese content in tungsten concentrate. Methods.

---Part 15. Determination of bismuth content. The purpose is to establish atomic fluorescence spectrometry and flame atomic absorption spectrometry for the determination of tungsten concentrate method of bismuth content.

---Part 16. Determination of iron content. The purpose is to establish a method for spectrophotometric determination of iron content in tungsten concentrate.

---Part 17. Determination of antimony content. The purpose is to establish a method for determining the antimony content in tungsten concentrate using atomic fluorescence spectrometry.

---Part 18. Determination of barium content. The purpose is to establish an inductively coupled plasma atomic emission spectrometry method for the determination of barium in tungsten concentrate. content method.

---Part 19. Determination of fluorine content. The purpose is to establish an ion selective electrode method for determining the fluorine content in tungsten concentrate.

---Part 20. Determination of mercury content. The purpose is to establish a spectrophotometric and gravimetric method for the determination of mercury content in tungsten concentrate.

The presence of phosphorus in tungsten concentrate products under acidic conditions leads to a decrease in the precipitation rate of tungsten trioxide and affects the quality of subsequent products. Therefore, the phosphorus content Testing is critical. The tungsten concentrate product standards were revised in 2015 (YS/T 231-2015), adding high-impurity tungsten concentrate products, among which There have been new changes in various technical indicators, including an increase in phosphorus content from 1% to 10%. At the same time, analysis and detection technology has also developed and improved. Appreciate Therefore, it is indeed necessary to revise GB/T 6150.3-2009 to ensure that the standard adapts to industry changes and market demands.

This document expands the measurement scope of the method and adds inductively coupled plasma atomic emission spectrometry, which is more in line with the product testing requirements of the tungsten industry. needs. This document further improves the applicability of the standard, improves the quality of tungsten concentrate products, promotes its production, trade and expands application needs. It is of great significance in seeking.

1 Scope

This document describes the method for the determination of phosphorus content in tungsten concentrate, including phosphomolybdenum yellow spectrophotometry (Method 1) and inductively coupled plasma Atomic emission spectrometry (method 2).

This document is applicable to the determination of phosphorus content in tungsten concentrate. Method 1 determination range (mass fraction). 0.0050%~1.00%. Method 2 test Fixed range (mass fraction). >1.00%~10.00%.

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 6682 Specifications and test methods for water used in analytical laboratories

GB/T 8170 Numerical rounding rules and expression 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. Phosphomolybdenum yellow spectrophotometry

4.1 Principle

After alkali fusion and leaching of the sample, beryllium sulfate is used as a carrier to co-precipitate phosphorus and beryllium hydroxide to separate them from other elements. Nitrate at a certain acidity In the acid solution, use ammonium vanadate-ammonium molybdate as the chromogen, measure the absorbance at 420nm with a spectrophotometer, and calculate the phosphorus content through the working curve.

After separation, residual tungsten, arsenic, silicon, etc. will not affect the determination.

4.2 Reagents or materials

Unless otherwise stated, only reagents confirmed to be of analytical grade were used in the analysis.

4.2.1 Water, GB/T 6682, Level 2.

4.2.2 Potassium hydroxide (excellent grade pure).

4.2.3 Ammonia water (rho=0.90g/mL).

4.2.4 Absolute ethanol.

4.2.5 Nitric acid (1 1). superior grade pure.

4.2.6 Nitric acid (1 10). superior grade pure.

......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.

Referenced standards

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Editions of GB/T 6150.3

EditionTitleRevisionStatus
GB/T 6150.3-2023Methods for chemical analysis of tungsten concentrates—Part 3: Determination of phosphorus content—The phosphorus molybdenum yellow spectrophotometry and inductively coupled plasma atomic emission spectrometrycurrent editionCurrent
GB/T 6150.3-2009Methods for chemical analysis of tungsten concentrates—Part 3: Determination of phosphorus content—The phosphorus molybdenum yellow spectrophotometry and inductively coupled plasma atomic emission spectrometryprevious editionSuperseded

This page sells the current edition, GB/T 6150.3-2023. Earlier editions are listed for reference only.

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