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GB/T 12690.20-2024 English PDF

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GB/T 12690.20-2024: Chemical analysis methods for non-rare earth impurities of rare earth metals and their oxides - Part 20: Determination of minor amounts of fluorine and chlorine in rare earth oxides - Ion chromatography method
Status: Valid

GB/T 12690.20: Evolution and historical versions

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GB/T 12690.20-2024English199 Add to Cart 3 days [Need to translate] Chemical analysis methods for non-rare earth impurities of rare earth metals and their oxides - Part 20: Determination of minor amounts of fluorine and chlorine in rare earth oxides - Ion chromatography method Valid GB/T 12690.20-2024
GB/T 12690.20-1990English199 Add to Cart 2 days [Need to translate] Rare-earth metals and their oxides--Determination of iron content--Potassium thiocyanate, 1, 10-phenanthroline spectrophotometric method Obsolete GB/T 12690.20-1990

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Standard similar to GB/T 12690.20-2024

GB/T 11064.9   GB/T 11064.2   GB/T 13747.5   GB/T 12690.21   GB/T 12690.12   GB/T 12690.19   

Basic data

Standard ID GB/T 12690.20-2024 (GB/T12690.20-2024)
Description (Translated English) Chemical analysis methods for non-rare earth impurities of rare earth metals and their oxides - Part 20: Determination of minor amounts of fluorine and chlorine in rare earth oxides - Ion chromatography method
Sector / Industry National Standard (Recommended)
Classification of Chinese Standard H14
Classification of International Standard 77.120.99
Word Count Estimation 10,119
Date of Issue 2024-11-28
Date of Implementation 2025-06-01
Issuing agency(ies) State Administration for Market Regulation, China National Standardization Administration

GB/T 12690.20-2024: Chemical analysis methods for non-rare earth impurities of rare earth metals and their oxides - Part 20: Determination of minor amounts of fluorine and chlorine in rare earth oxides - Ion chromatography method



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Chemical analysis methods for non-rare earth impurities of rare earth metals and their oxides - Part 20.Determination of minor amounts of fluorine and chlorine in rare earth oxides - Ion chromatography method Non-rare earth impurities in rare earth metals and their oxides Chemical analysis methods Part 20.Trace amounts of fluorine in rare earth oxides Determination of Chloride-Ion Chromatography Chemical analysis methods for non-rare earth impurities of rare earth metals and their oxides- Part 20.Determination of minor amounts of fluorine and chlorine in rare earth oxides-Ion chromatography method ICS 77.120.99 CCS H 14 National Standard of the People's Republic of China Published on 2024-11-28 Implemented on 2025-06-01 State Administration for Market Regulation The National Standardization Administration issued

Table of Contents

Preface ... Ⅲ Introduction Ⅳ 1 Scope ... 1 2 Normative references ... 1 3 Terms and Definitions ... 1 4 Principle ... 1 5 Reagents or materials ... 1 6 Instruments and Equipment ... 2 7 samples ... 2 8 Test steps ... 3 8.1 Test Materials 3 8.2 Parallel tests 3 8.3 Blank test ... 3 8.4 Preparation of analytical solution 3 8.5 Preparation of series of standard solutions ... 3 8.6 Drawing of standard curve 3 8.7 Determination 4 9 Experimental data processing ... 4 10 Precision ... 4 10.1 Precision raw data and statistics 4 10.2 Repeatability ... 4 10.3 Reproducibility 5

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 for standardization documents" Drafting is required. This document is part 20 of GB/T 12690 "Chemical analysis methods for non-rare earth impurities in rare earth metals and their oxides". The following parts have been published. Part 1.Determination of carbon and sulfur content - High frequency infrared absorption method; Part 2.Gravimetric method for determination of loss on ignition of rare earth oxides; Part 3.Gravimetric method for determination of water content in rare earth oxides; Part 4.Determination of oxygen and nitrogen content by pulse ﹘ infrared absorption method and pulse ﹘ thermal conductivity method; Part 5.Determination of cobalt, manganese, lead, nickel, copper, zinc, aluminum, chromium, magnesium, cadmium, vanadium and iron; Part 6.Determination of iron content - Potassium thiocyanate, 1,10 x phenanthroline spectrophotometric method; Part 7.Determination of silicon content; - Part 8.Determination of sodium content; - Part 9.Determination of chlorine content - Silver nitrate turbidimetric method; Part 10.Determination of phosphorus content - Molybdenum blue spectrophotometric method; Part 11.Determination of magnesium content - Flame atomic absorption spectrometry; Part 12.Determination of thorium content - Arsenazo III spectrophotometric method and inductively coupled plasma mass spectrometry; Part 13.Determination of molybdenum and tungsten content - Inductively coupled plasma optical emission spectrometry and inductively coupled plasma mass spectrometry; Part 14.Determination of the amount of titanium; - Part 15.Determination of calcium content; - Part 16.Determination of fluoride content - Ion selective electrode method; Part 17.Determination of niobium and tantalum in rare earth metals; Part 18.Determination of zirconium content; - Part 19.Determination of arsenic and mercury content; - Part 20.Determination of trace amounts of fluorine and chlorine in rare earth oxides - Ion chromatography; Part 21.Determination of sulfate content in rare earth oxides - Barium sulfate turbidimetric method. Please note that some of the contents of this document may involve patents. The issuing organization of this document does not assume the responsibility for identifying patents. This document was proposed and coordinated by the National Rare Earth Standardization Technical Committee (SAC/TC 229). This document was drafted by. Hunan Rare Earth Metal Materials Research Institute Co., Ltd., Qiandong Rare Earth Group Co., Ltd., Jiangxi Tungsten The company has cooperated with the Rare Earth Product Quality Supervision and Inspection Center, Baotou Rare Earth Research Institute, Guohe General Testing Evaluation and Certification Co., Ltd., Fujian Changting Jinlong Rare Earth Co., Ltd., Qingdao Shenghan Chromatography Technology Co., Ltd. The main drafters of this document are. Wang Guichao, Zhang Manning, Liu Rongli, Shi Xuefeng, Wen Bin, Xu Na, Liu Pengyu, Liu Chun, Wang Jinfeng, Chen Yanqun, Luo Zhiya, Zou Shihui, Wang Ling, Tian Haifeng, Zhao Yan, Zhang Xiuyan, Deng Yu, Zhang Jinmei.

Introduction

In the field of chemical composition analysis of rare earth products, my country has established detection methods for total rare earth content, non-rare earth impurities, and rare earth impurities. GB/T 12690 Chemical analysis methods for non-rare earth impurities in rare earth metals and their oxides GB/T 12690.12～26-1990 "Chemical analysis methods for rare earth metals and their oxides" is the basis, and GB/T 8762.3- 1988 "Emission spectrometry for determination of acid-soluble silicon dioxide in fluorescent grade yttrium oxide" GB/T 8762.4-1988 "Emission spectrometry for determination of acid-soluble silicon dioxide in fluorescent grade yttrium oxide" Determination of the amount of iron oxide, lead oxide, nickel oxide and copper oxide by emission spectrometry" GB/T 8762.6-1988 "Determination of the amount of iron oxide, lead oxide, nickel oxide and copper oxide by emission spectrometry" GB/T 11074.3-7-1989 Chemical Analysis Method for Samarium Oxide The integrated series of method standards It uses advanced detection methods and basically covers all rare earth metals and their rare earth oxide matrices, providing The method provides a quick and accurate method for the determination of rare earth impurity content with good operability. According to the differences in the test objects, test methods, and the differences between the rare earth metals and rare earth oxide matrices, GB/T 12690 is proposed to be 21 parts. Part 1.Determination of carbon and sulfur content - High frequency infrared absorption method; Part 2.Gravimetric method for determination of loss on ignition of rare earth oxides; Part 3.Gravimetric method for determination of water content in rare earth oxides; Part 4.Determination of oxygen and nitrogen content by pulse ﹘ infrared absorption method and pulse ﹘ thermal conductivity method; Part 5.Determination of cobalt, manganese, lead, nickel, copper, zinc, aluminum, chromium, magnesium, cadmium, vanadium and iron; Part 6.Determination of iron content - Potassium thiocyanate, 1,10 x phenanthroline spectrophotometric method; Part 7.Determination of silicon content; - Part 8.Determination of sodium content; - Part 9.Determination of chlorine content - Silver nitrate turbidimetric method; Part 10.Determination of phosphorus content - Molybdenum blue spectrophotometric method; Part 11.Determination of magnesium content - Flame atomic absorption spectrometry; Part 12.Determination of thorium content - Arsenazo III spectrophotometric method and inductively coupled plasma mass spectrometry; Part 13.Determination of molybdenum and tungsten content - Inductively coupled plasma optical emission spectrometry and inductively coupled plasma mass spectrometry; Part 14.Determination of the amount of titanium; - Part 15.Determination of calcium content; - Part 16.Determination of fluoride content - Ion selective electrode method; Part 17.Determination of niobium and tantalum in rare earth metals; Part 18.Determination of zirconium content; - Part 19.Determination of arsenic and mercury content; - Part 20.Determination of trace amounts of fluorine and chlorine in rare earth oxides - Ion chromatography; Part 21.Determination of sulfate content in rare earth oxides - Barium sulfate turbidimetric method. The above standards are established in accordance with the conventional detection elements in the production and trade of rare earth metals and their oxides. Each part includes a or multiple detection methods, clearly define the scope of application, selection of reagent materials and test equipment, standardize the test steps, and pass multiple laboratories Multiple tests and verifications provide precision data, establishing a rigorous and standardized work foundation for the quality inspection of rare earth metals and their oxides. The process of preparing high-purity rare earth oxides contains trace amounts of fluorine and chlorine impurities. Ion chromatography is characterized by its fast detection speed, good selectivity, The advantages of low interference, low detection limit, high sensitivity and ability to simultaneously determine multiple anions have made it increasingly used in the analysis of trace fluorine and chlorine. This document uses ion chromatography to establish a standardized and easy-to-operate High-precision testing standards. Non-rare earth impurities in rare earth metals and their oxides Chemical analysis methods Part 20.Trace amounts of fluorine in rare earth oxides Determination of Chloride-Ion Chromatography

1 Scope

This document describes a method for the determination of trace amounts of fluorine and chlorine in rare earth oxides. This document is applicable to the determination of fluorine and chlorine content in rare earth oxides. Determination range (mass fraction). fluorine 0.001 0% to 0.010%; Chlorine 0.001 0%～0.010%.

2 Normative references

The contents of the following documents constitute the essential clauses of this document through normative references in this document. For referenced documents without a date, only the version corresponding to that date applies to this document; for referenced documents without a date, the latest version (including all amendments) applies. in this document. GB/T 6379.2 Accuracy (trueness and precision) of measurement methods and results Part 2.Determination of repeatability of standard measurement methods Basic methods of sex and reproducibility GB/T 6682 Specifications and test methods for water used in analytical laboratories GB/T 8170 Rules for rounding off values and expression and determination of limit values JJG 823 Ion Chromatograph

3 Terms and definitions

There are no terms or definitions that require definition in this document.

4 Principle

The sample is decomposed by sulfuric acid, and the fluorine and chlorine in it escape with water vapor and are separated from the sample, absorbed by water, and determined by ion chromatography. Fluorine and chlorine were identified qualitatively by peak time and quantified by standard curve method.

5 Reagents or materials

Unless otherwise specified, only reagents of confirmed high purity or above and first-grade water that complies with GB/T 6682 were used in the analysis. Use certified standard solutions. 5.1 Sodium fluoride, reference substance. 5.2 Sodium chloride, reference substance. 5.3 Hydrogen peroxide [w(H2O2)≥30%]. 5.4 Sulfuric acid (2 1). 5.5 Eluent. Select a suitable eluent according to the instructions for use of the separation column.

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