GB/T 6150.13-2022Methods for chemical analysis of tungsten concentrates—Part 13: Determination of arsenic content—Atomic fluorescence spectrometry and the silver diethyldithiocarbamate (DDTC-Ag) spectrophotometry (English PDF)
钨精矿化学分析方法 第13部分:砷含量的测定 原子荧光光谱法和DDTC-Ag分光光度法
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Issued by
SAMR; SAC
Level / Type
National · Recommended
Issue date
October 14, 2022
Implementation date
February 1, 2023
Scope
GB/T 6150.13-2022 is the English-translated version of 钨精矿化学分析方法 第13部分:砷含量的测定 原子荧光光谱法和DDTC-Ag分光光度法.
GB/T 6150.13-2022 is part 13 of the Chinese national series for the chemical analysis of tungsten concentrates and covers the determination of arsenic by two methods: atomic fluorescence spectrometry as method 1, over a mass fraction of 0.0010 % to 0.20 %, and silver diethyldithiocarbamate (DDTC-Ag) spectrophotometry as method 2, over 0.010 % to 0.50 %.
Clause 1 states that where the two ranges overlap, method 1 is the arbitration method.
In method 1 the sample is decomposed with sulfuric acid and ammonium sulfate, tungsten, iron and manganese are complexed with citric acid in an ammonia medium, pentavalent arsenic is pre-reduced to the trivalent form with thiourea and ascorbic acid, and the hydride generated with potassium borohydride is measured for its fluorescence intensity.
It replaces GB/T 6150.13-2008, was issued on 14 October 2022 and has applied since 1 February 2023.
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Document preview — GB/T 6150.13-2022
National Standard of the People's Republic of China
- ICS
- 77.120.99
- Classification
- H 14
- Replacing
- GB/T 6150.13-2008
Issued by: State Administration for Market Regulation; Standardization Administration of the PRC
Contents
- Foreword
- Introduction
- 1 Scope
- 2 Normative references
- 3 Terms and Definitions
- 4 Method 1.Atomic Fluorescence Spectrometry
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 13 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 6150.13-2008 "Chemical Analysis of Tungsten Concentrates Determination of Arsenic Content by Hydride Atomic Absorption Spectrometry and DDTC-Ag Spectrophotometry", compared with GB/T 6150.13-2008, except for structural adjustment and editorial changes, the main technical changes as follows.
a) The detection method was changed from hydride atomic absorption spectrometry to atomic fluorescence spectrometry, and the measurement range was changed from 0.005%~ 0.50% is changed to 0.0010%~0.20% (see Chapter 1 and Chapter 4, Chapter 1 of the 2008 edition);
b) Change the tolerance to reproducibility (see 4.7.3, 5.7.2, 8.2, 16.2 of the 2008 edition);
c) Added the chapter "Test Report" (see Chapter 6).
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 compositions for the production and trade of tungsten concentrate products through experimental research. methodological standards for sub-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 the amount of tantalum and niobium 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 6150.13-2008 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 6150.13-2008 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 a method for the determination of arsenic content in tungsten concentrates. Including atomic fluorescence spectrometry (method 1) and DDTC-Ag spectrophotometry method (method two).
This document applies to the determination of arsenic content in tungsten concentrates. Method one measuring range (mass fraction). 0.0010%~0.20%; method two measuring Fixed range (mass fraction). 0.010%~0.50%. For the overlapping part of the measurement range, method 1 is used as the arbitration method.
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 Method 1.Atomic Fluorescence Spectrometry
4.1 Principle
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 arsenic is pre-reduced with thiourea-ascorbic acid. to trivalent arsenic. In the hydride generator, arsenic was reduced to hydride by potassium borohydride, and its fluorescence intensity was measured by atomic fluorescence spectrometer.
4.2 Reagents or materials
Unless otherwise stated, only reagents confirmed to be analytically pure were used in the analysis.
4.2.1 Water, GB/T 6682, Class II.
4.2.2 Ammonium sulfate.
4.2.3 Sulfuric acid (rho=1.84g/mL).
4.2.4 Hydrochloric acid (rho=1.19g/mL), excellent grade pure.
4.2.5 Ammonia (rho=0.88g/mL).
4.2.6 Citric acid solution (500g/L).
4.2.7 Sulfuric 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
Similar standards
Editions of GB/T 6150.13
| Edition | Title | Revision | Status |
|---|---|---|---|
| GB/T 6150.13-2022 | Methods for chemical analysis of tungsten concentrates—Part 13: Determination of arsenic content—Atomic fluorescence spectrometry and the silver diethyldithiocarbamate (DDTC-Ag) spectrophotometry | current edition | Current |
| GB/T 6150.13-2008 | Methods for chemical analysis of tungsten concentrates—Part 13: Determination of arsenic content—Atomic fluorescence spectrometry and the silver diethyldithiocarbamate (DDTC-Ag) spectrophotometry | previous edition | Superseded |
This page sells the current edition, GB/T 6150.13-2022. Earlier editions are listed for reference only.
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Related Standards
GB/T 6682-2008 — Water for analytical laboratory use - Specification and test methods
GB/T 8170-2008 — Rules of rounding off for numerical values & expression and judgement of limiting values
GB/T 6150.1-2023 — Methods for chemical analysis of tungsten concentrates—Part 1: Determination of tungsten trioxide content—Ammonium tungstate igniting gravimetric method
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