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GB/T 6150.10-2023Methods for chemical analysis of tungsten concentrates—Part 10: Determination of lead content—Hydride generation atomic fluorescence spectrometry and flame atomic absorption spectrometry (English PDF)

钨精矿化学分析方法 第10部分:铅含量的测定 氢化物发生原子荧光光谱法和火焰原子吸收光谱法

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Issued by

SAMR; SAC

Level / Type

National · Recommended

Issue date

August 6, 2023

Implementation date

March 1, 2024

Scope

GB/T 6150.10-2023 is the English-translated version of 钨精矿化学分析方法 第10部分:铅含量的测定 氢化物发生原子荧光光谱法和火焰原子吸收光谱法.

GB/T 6150.10-2023 is part 10 of the Chinese methods for chemical analysis of tungsten concentrates and determines lead by two methods.

Method 1, hydride generation atomic fluorescence spectrometry, covers a lead mass fraction of 0.0010 % to 0.30 % and method 2, flame atomic absorption spectrometry, covers 0.10 % to 0.50 %, with method 2 acting as the arbitration method where the ranges overlap.

In method 1 the sample is decomposed with hydrochloric acid in a boiling water bath, nitric and perchloric acid are heated to thick white smoke to strip the tungsten matrix, oxalic acid masks calcium, manganese and bismuth, potassium ferricyanide serves as oxidant and potassium borohydride reduces lead to its hydride for reading against a working curve.

It replaces GB/T 6150.10-2008, was issued on 6 August 2023 and applies from 1 March 2024.

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Document preview — GB/T 6150.10-2023

National Standard of the People's Republic of China

ICS
77.120.99
Classification
H 14
Replacing
GB/T 6150.10-2008

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.Hydride generation atomic fluorescence spectrometry

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 10 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 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 6150.10-2008 "Method for chemical analysis of tungsten concentrate - Determination of lead content by flame atomic absorption spectrometry" and is consistent with Compared with GB/T 6150.10-2008, in addition to structural adjustments and editorial changes, the main technical changes are as follows.

a) The measurement range of the method has been changed (see Chapter 1, Chapter 1 of the 2008 edition);

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

c) Added the detection method hydride generation atomic fluorescence spectrometry (see Chapter 4);

d) Changed the sample weight for flame atomic absorption method (see 5.5.1, 6.1 of the 2008 edition);

e) "Precision" was changed, and "permissible difference" was changed to "reproducibility" (see 4.7, 5.7, Chapter 8 of the 2008 edition);

f) "Quality Assurance and Control" is deleted (see Chapter 9 of the 2008 edition);

g) Added "Test Report" (see Chapter 6).

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.

Since 1985, 2 versions of GB/T 6150 have been released. It has been more than ten years since GB/T 6150.10-2008 was released and implemented.

The applicable product standards have been revised in 2015 (YS/T 231-2015), and various technical indicators have undergone new changes.

Chemicalization, upstream and downstream customers in the tungsten industry also have new requirements for product testing, and analytical testing technology has also developed and progressed. The country has strict requirements on various industries.

Environmental protection also has further strict requirements. In view of this, it is indeed necessary to revise GB/T 6150.10-2008 to ensure that the standard adapts to Industry changes and market demands.

By improving and changing the analytical methods in existing standards, replacing them with new detection instruments or expanding the detection range, it is important to maintain The main ways to analyze the adaptability of method standards. This revision adds the hydride atomic fluorescence spectrometry method, which makes the detection limit of the method lower and can Increase the applicability of this document, thereby increasing the standard adoption rate and better serving and promoting production, trade and application needs.

1 Scope

This document specifies the method for determination of lead content in tungsten concentrate.

This document is applicable to the determination of lead content in tungsten concentrate and includes two methods (Method 1.Hydride generation atomic fluorescence spectrometry; Method 2.Flame atomic absorption spectrometry). Method 1 determination range (mass fraction). 0.0010%~0.30%; method 2 determination range (mass fraction)

Number).0.10%~0.50%. 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 6682 Specifications and test methods for water used in analytical laboratories

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.Hydride generation atomic fluorescence spectrometry

4.1 Principle

The sample is decomposed with hydrochloric acid in a boiling water bath, nitric acid is added, and perchloric acid is heated and dissolved until thick white smoke is emitted, and a large amount of the acidity of the tungsten matrix is removed.

In the solution, oxalic acid is used as a masking agent for interfering elements such as calcium, manganese, and bismuth, and potassium ferricyanide is used as an oxidant. In the hydride generator, lead is hydroborated.

Potassium is reduced to hydride, its fluorescence intensity is measured on an atomic fluorescence spectrometer, and the mass concentration of lead is found on the working curve.

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

4.2.3 Nitric acid (rho=1.42g/mL, excellent grade pure).

4.2.4 Perchloric acid (rho=1.67g/mL, excellent grade pure).

4.2.5 Nitric acid (1 1).

......
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 6150.10

EditionTitleRevisionStatus
GB/T 6150.10-2023Methods for chemical analysis of tungsten concentrates—Part 10: Determination of lead content—Hydride generation atomic fluorescence spectrometry and flame atomic absorption spectrometrycurrent editionCurrent
GB/T 6150.10-2008Methods for chemical analysis of tungsten concentrates—Part 10: Determination of lead content—Hydride generation atomic fluorescence spectrometry and flame atomic absorption spectrometryprevious editionSuperseded

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