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GB/T 12690.1-2022 English PDF

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GB/T 12690.1-2022: Chemical analysis methods for non-rare earth impurities of rare earth metals and their oxides - Part 1: Determination of carbon and sulfur contents - High frequency-infrared absorption method
Status: Valid

GB/T 12690.1: Historical versions

Standard IDUSDBUY PDFLead-DaysStandard Title (Description)Status
GB/T 12690.1-2022199 Add to Cart 3 days Chemical analysis methods for non-rare earth impurities of rare earth metals and their oxides - Part 1: Determination of carbon and sulfur contents - High frequency-infrared absorption method Valid
GB/T 12690.1-2015199 Add to Cart 3 days Chemical analysis methods for non-rare earth impurity of rare earth metals and their oxides -- Part 1: Determination of carbon and sulfur contents -- High frequency-infrared absorption method Obsolete
GB/T 12690.1-2002239 Add to Cart 3 days Chemical analysis methods for non-RE impurity of rare earth metals and their oxides -- Determination of carbon and sulfur contents -- High frequency-infrared absorption method Obsolete
GB/T 12690.1-1990199 Add to Cart 2 days Lanthanum oxide--Determination of cerium oxide, praseodymium oxide, nedeodynium oxide, samarium oxide and yttrium oxide--Induetively coupled plasma atomic emission spectrographic method Obsolete

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Basic data

Standard ID: GB/T 12690.1-2022 (GB/T12690.1-2022)
Description (Translated English): Chemical analysis methods for non-rare earth impurities of rare earth metals and their oxides - Part 1: Determination of carbon and sulfur contents - High frequency-infrared absorption method
Sector / Industry: National Standard (Recommended)
Classification of Chinese Standard: H14
Classification of International Standard: 77.120.99
Word Count Estimation: 10,136
Date of Issue: 2022-12-30
Date of Implementation: 2023-07-01
Older Standard (superseded by this standard): GB/T 12690.1-2015
Issuing agency(ies): State Administration for Market Regulation, China National Standardization Administration

GB/T 12690.1-2022: Chemical analysis methods for non-rare earth impurities of rare earth metals and their oxides - Part 1: Determination of carbon and sulfur contents - High frequency-infrared absorption method



---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
ICS 77.120.99 CCSH14 National Standards of People's Republic of China Replace GB/T 12690.1-2015 Non-rare earth impurities in rare earth metals and their oxides chemical analysis method Part 1.Determination of carbon and sulfur content High Frequency-Infrared Absorption Method Released on 2022-12-30 and implemented on 2023-07-01 State Administration for Market Regulation Released by the National Standardization Management Committee

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. This document is the first part of GB/T 12690 "Methods for Chemical Analysis of Non-Rare Earth Impurities in Rare Earth Metals and Their Oxides". GB/T 12690 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 ignition loss in rare earth oxides; --- Part 3.Gravimetric method for the determination of water content in rare earth oxides; --- Part 4.Determination of oxygen and nitrogen content - pulse-infrared absorption method and pulse-thermal conductivity method; --- Part 5.Determination of cobalt, manganese, lead, nickel, copper, zinc, aluminum, chromium, magnesium, cadmium, vanadium, iron; --- Part 6.Determination of iron content Potassium thiocyanate, 1,10-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 spectrophotometry; --- Part 11.Determination of the amount of magnesium flame atomic absorption spectrometry; --- Part 12.Determination of thorium content Arsenazo III spectrophotometry and inductively coupled plasma mass spectrometry; --- Part 13.Determination of molybdenum and tungsten content Inductively coupled plasma emission spectrometry and inductively coupled plasma mass spectrometry; --- Part 14.Determination of titanium content; --- Part 15.Determination of calcium content; --- Part 16.Determination of the amount of fluorine ion selective electrode method; --- Part 17.Determination of the amount of niobium and tantalum in rare earth metals; --- Part 18.Determination of the amount of zirconium; --- Part 19.Determination of the amount of arsenic and mercury. This document replaces GB/T 12690.1-2015 "Methods for Chemical Analysis of Non-Rare Earth Impurities in Rare Earth Metals and Their Oxides - Part 1. Determination of carbon and sulfur content by high-frequency-infrared absorption method", compared with GB/T 12690.1-2015, except for structural adjustment and editorial changes, the main The technical changes are as follows. a) Changed the measurement range from "0.0050%~1.00%" to "carbon 0.0020%~1.00%; sulfur 0.0020%~ 0.20%" (see Chapter 1, Chapter 1 of the.2015 edition); b) The method summary has been changed (see Chapter 4, Chapter 2 of the.2015 edition); c) Changed the carbon and sulfur content range and quantity of the standard sample (see 5.5, 3.5 of the.2015 edition); d) Added reagents and specifications (see 5.6, 5.7); e) Added cleaning agent (see 5.8); f) Added instrument maintenance measures (see 6.1); g) Added equipment and precision (see 6.2); h) Changed the sample handling method (see Chapter 7, Chapter 5 of the.2015 edition); i) The sample weight has been changed (see 8.1, 6.1 of the.2015 edition); j) Changed the calibration of the working curve (see 8.4, 6.4 of the.2015 edition); k) Changed the addition amount and order of flux and samples (see 8.5, 6.5 of the.2015 edition); l) Changed "precision" and changed "allowable difference" to "reproducibility" (see Chapter 10, Chapter 8 of the.2015 edition). Please note that some contents of this document may refer to patents. The issuing agency of this document assumes no responsibility for identifying patents. This document is proposed and managed by the National Rare Earth Standardization Technical Committee (SAC/TC229). This document was drafted by. Guohe General Testing and Evaluation Certification Co., Ltd., Baotou Rare Earth Research Institute, National Standard (Beijing) Inspection and Certification Co., Ltd. Co., Ltd., Ganzhou Nonferrous Metallurgy Research Institute Co., Ltd., Sichuan Leshan Ruifeng Metallurgy Co., Ltd., Jiangxi South Rare Earth High-Tech Co., Ltd. Company, Youyan Rare Earth New Materials Co., Ltd., Yiyang Hongyuan Rare Earth Co., Ltd. The main drafters of this document. Chen Caixia, Wu Wenqi, Zhang Xiuyan, Li Tian, Hu Mengqiao, Luo Yansheng, Hu Xuan, Cao Zhenhua, Zhang Wenxing, Feng Xinrui, Xu Jing, Guo Cainv, Liu Wei, Sun Haifeng, Zhang Lijiu, Chen Xiongfei, Bai Xiaoyan, Liu Pengyu, Cheng Zihui, Qu Xiang, Zhao Yan, Xie Yanyan. The release status of previous versions of this document and the documents it replaces are as follows. ---First published as GB/T 12690.13-1990 in.1990; ---The first revision in.2002 was GB/T 12690.1-2002, and the second revision in.2015; --- This is the third revision.

Introduction

In the field of chemical composition analysis of rare earth products, my country has established comparative testing methods for the total amount of rare earth, non-rare earth impurities, and rare earth impurities. For a comprehensive standard system. This series of standards GB/T 12690 "Chemical Analysis Methods for Non-Rare Earth Impurities in Rare Earth Metals and Their Oxides" is based on the original Based on the standard GB/T 12690.12~26-1990 "Chemical Analysis Methods of Rare Earth Metals and Their Oxides", GB/T 8762.3- 1988 "Molybdenum Blue Spectrophotometric Method for Determination of Acid-soluble Silica in Fluorescent Grade Yttrium Oxide", GB/T 8762.4-1988 "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 "Medium Oxidation of Fluorescent Europium Oxide Determination of Lead, Nickel Oxide, Iron Oxide and Copper Oxide by Emission Spectrometry", GB/T 11074.3~7-1989 "Chemical Analysis Methods of Samarium Oxide", etc. Finally, a comprehensive analysis method standard for non-rare earth impurities in all rare earth metals and their oxides will be formed. Integrated series of methods The standard cites advanced detection methods and basically covers all rare earth metals and their rare earth oxide substrates. The determination of non-rare earth impurity content provides a fast and accurate method standard, and has good operability. According to the different detection objects, detection methods, and the differences between the rare earth metals and rare earth oxide substrates, etc., GB/T 12690 consists of 19 parts constitute. --- Part 1.Determination of carbon and sulfur content High-frequency-infrared absorption method; --- Part 2.Gravimetric method for determination of ignition loss in rare earth oxides; --- Part 3.Gravimetric method for the determination of water content in rare earth oxides; --- Part 4.Determination of oxygen and nitrogen content - pulse-infrared absorption method and pulse-thermal conductivity method; --- Part 5.Determination of cobalt, manganese, lead, nickel, copper, zinc, aluminum, chromium, magnesium, cadmium, vanadium, iron; --- Part 6.Determination of iron content Potassium thiocyanate, 1,10-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 spectrophotometry; --- Part 11.Determination of the amount of magnesium flame atomic absorption spectrometry; --- Part 12.Determination of thorium content Arsenazo III spectrophotometry and inductively coupled plasma mass spectrometry; --- Part 13.Determination of molybdenum and tungsten content Inductively coupled plasma emission spectrometry and inductively coupled plasma mass spectrometry; --- Part 14.Determination of titanium content; --- Part 15.Determination of calcium content; --- Part 16.Determination of the amount of fluorine ion selective electrode method; --- Part 17.Determination of the amount of niobium and tantalum in rare earth metals; --- Part 18.Determination of the amount of zirconium; --- Part 19.Determination of the amount of arsenic and mercury. The above-mentioned standards for each part are set up in order according to the routine detection elements in the production and trade of rare earth metals and their oxides. Each part includes a One or more detection methods, respectively clarify the scope of application, the selection of reagent materials and test equipment, standardize the test steps, and pass through a number of laboratories Multiple tests and verifications have provided precision data, establishing a rigorous and standardized basis for standardization work for the quality verification of rare earth metals and their oxides. The high-frequency-infrared absorption method used in this document has the advantages of wide measurement range, accurate and reliable analysis results, easy operation, and simultaneous determination of carbon, It has been widely used in metallurgy, geology and other related analysis fields. The carbon precision data in this document are obtained by 8 companies in 2020 The laboratory conducted a joint test on 6 samples with different carbon content levels, and each laboratory determined the carbon content of each level in the repeatability condition. 11 times were determined independently under the conditions; the sulfur precision data was determined by the joint experiment of 7 laboratories on 4 samples with different sulfur content levels. Every Each laboratory independently determined the sulfur content of each level 11 times under repeatable conditions. Common test data according to GB/T 6379.2 "measurement method Accuracy (Trueness and Precision) of Methods and Results - Part 2.Basic Methods for Determining the Repeatability and Reproducibility of Standard Measurement Methods meter analysis. Non-rare earth impurities in rare earth metals and their oxides chemical analysis method Part 1.Determination of carbon and sulfur content High Frequency-Infrared Absorption Method

1 Scope

This document describes methods for the determination of carbon and sulfur content in rare earth metals and their oxides. This document is applicable to the determination of carbon and sulfur content in rare earth metals and their oxides. Measuring range (mass fraction). Carbon 0.0020%~ 1.00%; sulfur 0.0020%~0.20%.

2 Normative references

The contents of the following documents constitute the essential provisions of this document through normative references in the text. Among them, dated references For documents, only the version corresponding to the date is applicable to this document; for undated reference documents, the latest version (including all amendments) is applicable to this document. GB/T 8170 Numerical rounding off rules and expression and determination of limit values

3 Terms and Definitions

This document does not have terms and definitions that need to be defined.

4 Method Summary

In the presence of flux, an oxygen flow is introduced into the high-frequency induction furnace to burn the sample at high temperature, and the carbon generates carbon monoxide or/and carbon dioxide. carbon gas, and sulfur produces sulfur dioxide gas. The mixed gas first enters the sulfur dioxide infrared cell to measure the sulfur content, and then undergoes catalytic oxidation, and the The sulfur dioxide is converted to sulfur trioxide and absorbed. The remaining gas enters the carbon infrared cell to determine the carbon content.

5 Reagents or Materials

5.1 Tungsten flux. wC< 0.0008%, wS< 0.0008%. 5.2 Tin flux. wC< 0.0008%, wS< 0.0008%. 5.3 Pure iron flux. wC< 0.0008%, wS< 0.0008%. 5.4 Special crucible for carbon and sulfur. burn at 1200°C for 2 hours, cool naturally and place in a desiccator for later use. 5.5 Standard sample. within the range of carbon content (mass fraction) 0.0020%~1.00%, sulfur content (mass fraction) 0.0020%~0.20% Select an appropriate certified reference sample. 5.6 Caustic soda asbestos. the particle size is 0.7mm~1.2mm (10 mesh~20 mesh). 5.7 Anhydrous magnesium perchlorate. the particle size is 0.7mm~1.2mm (10 mesh~20 mesh). 5.8 Acetone (analytical grade).
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