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GB/T 12690.4-2021 English PDF

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GB/T 12690.4-2021: Chemical analysis methods for non-rare earth impurities of rare earth metals and their oxides - Part 4: Determination of oxygen and nitrogen contents - Impulse-infrared absorption and impulse-thermal conductivity method
Status: Valid

GB/T 12690.4: Historical versions

Standard IDUSDBUY PDFLead-DaysStandard Title (Description)Status
GB/T 12690.4-2021139 Add to Cart 3 days Chemical analysis methods for non-rare earth impurities of rare earth metals and their oxides - Part 4: Determination of oxygen and nitrogen contents - Impulse-infrared absorption and impulse-thermal conductivity method Valid
GB/T 12690.4-2003279 Add to Cart 3 days Chemical analysis methods for non-rare earth impurities of rare earth metals and their oxides -- Determination of oxygen and nitrogen content -- Impulse-infrared and impulse-thermal conductance absorption method Obsolete
GB/T 12690.4-1990199 Add to Cart 2 days Cerium oxide--Determination of lanthanum oxide, praseodymium oxide, neodymium oxide, samarium oxide and yttrium oxide contents--Spectrochemical method Obsolete

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Basic data

Standard ID: GB/T 12690.4-2021 (GB/T12690.4-2021)
Description (Translated English): Chemical analysis methods for non-rare earth impurities of rare earth metals and their oxides - Part 4: Determination of oxygen and nitrogen contents - Impulse-infrared absorption and impulse-thermal conductivity method
Sector / Industry: National Standard (Recommended)
Classification of Chinese Standard: H14
Word Count Estimation: 7,734
Issuing agency(ies): State Administration for Market Regulation, China National Standardization Administration

GB/T 12690.4-2021: Chemical analysis methods for non-rare earth impurities of rare earth metals and their oxides - Part 4: Determination of oxygen and nitrogen contents - Impulse-infrared absorption and impulse-thermal conductivity 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.
Chemical analysis methods for non-rare earth impurities of rare earth metals and their oxides - Part 4.Determination of oxygen and nitrogen contents - Impulse-infrared absorption and impulse-thermal conductivity method ICS 77.120.99 CCSH14 National Standards of People's Republic of China Replace GB/T 12690.4-2003 Non-rare earth impurities in rare earth metals and their oxides Chemical analysis method Part 4.Determination of Oxygen and Nitrogen Pulse-infrared absorption method and pulse-thermal conductivity method Released on 2021-10-11 and implemented on 2022-05-01 State Administration of Market Supervision and Administration Issued 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 of Standardization Documents" Drafting. This document is the fourth part of GB/T 12690 "Chemical Analysis Methods of Non-rare Earth Impurities in Rare Earth Metals and Their Oxides". GB/T 12690 The following parts have been released. ---Part 1.Determination of carbon and sulfur content by high-frequency-infrared absorption method; ---Part 2.Determination of Ignition Loss in Rare Earth Oxides by Gravimetric Method; ---Part 3.Gravimetric method for the 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 content; ---Part 6.Determination of iron content potassium thiocyanate, 1,10-phenanthroline spectrophotometry; ---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 Molybdenum Blue Spectrophotometry; ---Part 11.Determination of Magnesium Content 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 the amount of titanium; ---Part 15.Determination of calcium content; ---Part 16.Determination of fluorine content by 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 arsenic and mercury content. This document replaces GB/T 12690.4-2003 "Chemical Analysis Methods for Non-rare Earth Impurities in Rare Earth Metals and Their Oxide Determination of pulse-infrared absorption method and pulse-thermal conductivity method, compared with GB/T 12690.4-2003, except for structural adjustments and editorial changes, The main technical changes are as follows. a) The scope of application has been changed, and the explanation that does not apply to metal ytterbium has been added; the measurement range of oxygen content has been changed from "0.010%~ 0.30%" was revised to "0.0050%~0.30%" (see Chapter 1, Chapter 1 of the.2003 edition); b) Two chapters of "Normative Reference Documents" and "Terms and Definitions" have been added (see Chapter 2 and Chapter 3); c) The mass of the sample is changed, from "Oxygen 0.050g~0.150g, Nitrogen 0.060g~0.070g" to "Oxygen, nitrogen 0.10g~ 0.16g" (see 8.1, 6.1 of the.2003 edition); d) The flux is changed, from "tin particles, nickel flakes" to "nickel capsule or nickel basket fluxing" (see 8.4,.2003 edition 6.6); e) "Precision" is changed, and "allowable difference" is changed to "reproducibility" (see 10.2,.2003 version 8.2); f) Deleted quality assurance and control (see Chapter 9 of the.2003 edition). Please note that some of the contents of this document may involve patents. The issuing agency of this document is not responsible for identifying patents. This document was proposed and managed by the National Rare Earth Standardization Technical Committee (SAC/TC229). Drafting organizations of this document. Baotou Rare Earth Research Institute, National Standard (Beijing) Inspection and Certification Co., Ltd., Steel Research Nac Testing Technology Co., Ltd. Company, Tianjin Baotou Iron and Steel Rare Earth Research Institute Co., Ltd., Hunan Rare Earth Metal Materials Research Institute, Fujian Changting Jinlong Rare Earth Co., Ltd., National Rare Earth Product Quality Supervision and Inspection Center. The main drafters of this document. Yu Yonghai, Wu Wenqi, Jiang Tianyi, Wang Changhua, Hou Hongxia, Bai Weihua, Li Hongwei, Wang Anli, Wu Xitao, Wang Jinfeng, Lin Encheng. The previous versions of this document and the documents replaced are as follows. ---First published in.1990 as GB/T 12690.12-1990, first revised in.1995 as GB/T 15917.4-1995,.2003 The second revision in.2012 was GB/T 12690.4-2003; ---This is the third revision.

Introduction

In the field of analysis of the chemical composition of rare earth products, China has established a test for the total amount of rare earths, non-rare earth impurities, and rare earth impurities. It is a comprehensive standard system. This standard series 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 "Methods for Chemical Analysis of Rare Earth Metals and Their Oxides", GB/T 8762.3- 1988 "Molybdenum Blue Spectrophotometric Method for the Determination of Acid-soluble Silica in Fluorescence Grade Yttrium Oxide", GB/T 8762.4-1988 "Fluorescence 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 "fluorescence grade europium oxide in oxidation Determination of lead, nickel oxide, iron oxide and copper oxide content by emission spectrometry", GB/T 11074.3~.7-1989 "chemical analysis method of samarium oxide", etc. Standards, and finally form a comprehensive analysis method standard for non-rare earth impurities in all rare earth metals and their oxides. The revised method standard cited Advanced detection methods are used, and basically cover all rare earth metals and their rare earth oxide substrates. The establishment of this series of method standards is rare The determination of the content of non-rare earth impurities in earth metals and their oxides provides a quick and accurate method and specification, and has good operability. This revision of this document has been tested and verified by many laboratories, and the "allowable difference" clause has been revised as the "reproducibility" clause, which is given in the standard At least covering the repeatability and re-linearity limits of high, medium high, medium low, and low 4 points, so that the precision requirements of the method tend to be more perfect. Non-rare earth impurities in rare earth metals and their oxides Chemical analysis method Part 4.Determination of Oxygen and Nitrogen Pulse-infrared absorption method and pulse-thermal conductivity method

1 Scope

This document specifies the determination method of oxygen and nitrogen content in rare earth metals (except metal ytterbium). This document is applicable to the determination of oxygen and nitrogen content in rare earth metals (except metal ytterbium). Measuring range (mass fraction). oxygen 0.0050%~ 0.30%; Nitrogen 0.0020%~0.20%.

2 Normative references

The contents of the following documents constitute the indispensable clauses of this document through normative references in the text. Among them, dated quotations Only the version corresponding to that 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 rules and the expression and determination of limit values

3 Terms and definitions

There are no terms and definitions that need to be defined in this document.

4 Principle

In an inert atmosphere, the sample in the graphite crucible is heated and melted, and the oxygen in the sample is precipitated as carbon monoxide or (and) carbon dioxide. After the furnace, enter the infrared detector for measurement. Nitrogen precipitates out as nitrogen and enters the thermal conductivity detector for measurement.

5 Reagents and materials

Unless otherwise specified, only reagents and distilled water or deionized water or equivalent purity water are used in the analysis. 5.1 Nickel bag or nickel basket with cover, the blank value (mass fraction) of oxygen and nitrogen is not more than 0.00050%, and the nickel content (mass fraction) is not less than 99%, and It has been corroded by mixed acid (HNO3 HPO4 HAc) in advance. 5.2 Carbon tetrachloride or acetone, oxygen, nitrogen blank value (mass fraction) is not more than 0.00050%. 5.3 Graphite crucible. 5.4 Oxygen standard samples. Choose three suitable certified standard samples within the range of oxygen content (mass fraction) 0.0050%~0.30%. 5.5 Nitrogen standard samples. Choose three suitable certified standard samples within the range of nitrogen content (mass fraction) 0.0020%~0.20%. 5.6 Helium [φ(He)≥99.99%].
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