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GB/T 12690.12-2024: Chemical analysis methods for non-rare earth impurities of rare earth metals and their oxides - Part 12: Determination of thorium and uranium contents - Inductively coupled plasma mass spectrum method
Status: Valid GB/T 12690.12: Evolution and historical versions
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivered in | Standard Title (Description) | Status | PDF |
| GB/T 12690.12-2024 | English | 279 |
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Chemical analysis methods for non-rare earth impurities of rare earth metals and their oxides - Part 12: Determination of thorium and uranium contents - Inductively coupled plasma mass spectrum method
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GB/T 12690.12-2024
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| GB/T 12690.12-2003 | English | 359 |
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Chemical analysis methods for non-rare earth impurities of rare earth metals and their oxides -- Determination of thorium content -- Arsenazo Ⅲ spectrophotometric method and inductively coupled plasma mass spectrum method
| Obsolete |
GB/T 12690.12-2003
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| GB/T 12690.12-1990 | English | 199 |
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Neodymium and samarium--Determination of oxygen content--Impulse-infrared absorption method
| Obsolete |
GB/T 12690.12-1990
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PDF similar to GB/T 12690.12-2024
Basic data | Standard ID | GB/T 12690.12-2024 (GB/T12690.12-2024) | | Description (Translated English) | Chemical analysis methods for non-rare earth impurities of rare earth metals and their oxides - Part 12: Determination of thorium and uranium contents - Inductively coupled plasma mass spectrum method | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | H14 | | Classification of International Standard | 77.120.99 | | Word Count Estimation | 14,117 | | Date of Issue | 2024-04-25 | | Date of Implementation | 2024-11-01 | | Older Standard (superseded by this standard) | GB/T 12690.12-2003 | | Issuing agency(ies) | State Administration for Market Regulation, China National Standardization Administration | GB/T 12690.12-2024: Chemical analysis methods for non-rare earth impurities of rare earth metals and their oxides - Part 12: Determination of thorium and uranium contents - Inductively coupled plasma mass spectrum method
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ICS 77:120:99
CCSH14
National Standards of People's Republic of China
Replaces GB/T 12690:12-2003
Non-rare earth impurities in rare earth metals and their oxides
Chemical analysis methods: Part 12: Determination of thorium and uranium content
Inductively Coupled Plasma Mass Spectrometry
Released on 2024-04-25
2024-11-01 Implementation
State Administration for Market Regulation
The National Standardization Administration issued
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 Part 12 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: Determination of loss on ignition of rare earth oxides - Gravimetric method;
--- Part 3: Determination of water content in rare earth oxides - Gravimetric method;
--- 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 and iron
--- Part 6: Determination of iron content Potassium thiocyanate and 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 spectrophotometric method;
--- Part 11: Determination of magnesium content - Flame atomic absorption spectrometry;
--- Part 12: Determination of thorium content by arsenazo III spectrophotometry 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 titanium content;
--- 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:
This part replaces GB/T 12690:12-2003 "Chemical analysis methods for non-rare earth impurities in rare earth metals and their oxides - Part 12
Determination of thorium content - Arsenazo III spectrophotometric method and inductively coupled plasma mass spectrometry" is consistent with GB/T 12690:12-2003
In addition to structural adjustments and editorial changes, the main technical changes are as follows:
a) Deleted Method 1 “Arsenazo III spectrophotometric method”;
b) The measurement range of method 2 was changed from "0:0001%~0:010%" to "0:00005%~
0:020%”; the determination range of uranium content was increased to “0:00005%~0:020%” (see Chapter 1, Chapter 10 of the:2003 edition);
c) Added “Normative References” and “Terms and Definitions” (see Chapter 2 and Chapter 3);
d) Added instructions for reagents and water used in analysis (see Chapter 5);
e) The specific requirements for instruments and equipment have been changed (see Chapter 6, Chapter 13 of the:2003 edition);
f) The sample pretreatment conditions have been changed (see 7:1, 14:1 of the:2003 edition);
g) The weighing amount of the sample pretreatment has been changed (see 8:1, 15:2 of the:2003 edition);
h) The preparation of the series of standard solutions has been changed (see 8:4, 15:3 of the:2003 edition);
i) The preparation of analytical solution has been changed (see 8:5, 15:2 of the:2003 edition);
j) Added the drawing of standard curve (see 8:6:1);
k) The calculation formula for test data processing has been changed (see Chapter 9, Chapter 16 of the:2003 edition);
l) Quality assurance and control (see Chapter 18 of the:2003 edition) has been deleted:
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/TC229):
This document was drafted by: Jiangxi Tungsten and Rare Earth Product Quality Supervision and Inspection Center, Hunan Rare Earth Metal Materials Research Institute Co:, Ltd:
Ltd:, Fujian Changting Jinlong Rare Earth Co:, Ltd:, Baotou Rare Earth Research Institute, Dingnan Dahua New Materials Resources Co:, Ltd:, Qiandong Rare Earth Group Co:, Ltd:
Co:, Ltd:, Quannan County New Resources Rare Earth Co:, Ltd:
The main drafters of this document are: Xu Na, Sun Na, Zeng Qingping, Chen Rong, Wang Guichao, Wang Jinfeng, Wang Baohua, Zhang Manning, Wen Bin, Zhang Kun, Chen Tianlian,
Chang, C:, Chen, Y:, Cao, Y:, and Wang, S: H:
The previous versions of this document and the documents it replaces are as follows:
---First published in:1990 as GB/T 12690:12-1990, first revised in:2003;
---This is the second revision:
Introduction
In the field of chemical composition analysis of rare earth products, my country has established a relatively large number of detection systems for the total amount of rare earths, non-rare earth impurities, and rare earth impurities:
GB/T 12690 "Chemical analysis of non-rare earth impurities in rare earth metals and their oxides" is based on the original standard
GB/T 12690:12~26-1990 "Chemical analysis methods for rare earth metals and their oxides" was used as the basis, and GB/T 8762:3-1988 was incorporated:
"Determination of Acid-soluble Silica in Fluorescent Yttrium Oxide Using Molybdenum Blue Spectrophotometry", GB/T 8762:4-1988 "Determination of Acid-soluble Silica in Fluorescent Yttrium Oxide Using Molybdenum Blue Spectrophotometry"
GB/T 8762:6-1988 "Emission spectrometry for the determination of lead oxide, nickel oxide and copper oxide in fluorescent grade europium oxide"
GB/T 11074:3~7-1989 Chemical Analysis Method for Samarium Oxide, etc:
Finally, a comprehensive analysis standard for non-rare earth impurities in all rare earth metals and their oxides is formed:
Advanced detection methods are used, and basically cover all rare earth metals and their rare earth oxide matrices, for non-rare earth metals and their oxides:
The determination of soil impurity content provides a quick and accurate method specification 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 consists of
20 parts:
--- Part 1: Determination of carbon and sulfur content - High frequency-infrared absorption method;
--- Part 2: Determination of loss on ignition of rare earth oxides - Gravimetric method;
--- Part 3: Determination of water content in rare earth oxides - Gravimetric method;
--- 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, aluminium, chromium, magnesium, cadmium, vanadium and iron;
--- Part 6: Determination of iron content Potassium thiocyanate and 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 spectrophotometric method;
--- Part 11: Determination of magnesium content - Flame atomic absorption spectrometry;
--- Part 12: Determination of thorium and uranium content - 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 titanium content;
--- 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:
The above standards are established in accordance with the conventional detection elements in the production and trade of rare earth metals and their oxides:
One or more detection methods, respectively clarify the scope of application, the selection of reagent materials and test equipment, standardize the test steps, and have been tested by 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:
Rare earth ores are mostly associated radioactive minerals: In the process of their development and utilization and preparation into various rare earth products, the natural radioactivity in the associated minerals
The volatile substances will also be migrated and redistributed: ICP-MS requires less sample, has a low detection limit, is fast in measurement, and can measure multiple elements simultaneously:
The advantages of ICP-MS analysis have been increasingly applied to trace nuclide analysis:
For every detail in the testing process, standardized, easy-to-operate and highly accurate testing standards have been established:
Non-rare earth impurities in rare earth metals and their oxides
Chemical analysis methods: Part 12: Determination of thorium and uranium content
Inductively Coupled Plasma Mass Spectrometry
Warning - Laboratories using this document should be equipped with lead barrels for sample storage: This document does not address all possible safety issues:
The user is responsible for taking appropriate safety and health measures and ensuring that the conditions stipulated by relevant national laws and regulations are met:
1 Scope
This document describes a method for the determination of thorium and uranium in rare earth metals and their oxides:
This document is applicable to the determination of thorium and uranium in rare earth metals and their oxides: Determination range (mass fraction): thorium content 0:00005%~
0:020%; uranium content 0:00005%~0:020%:
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 to
This document:
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
JJF1159 Calibration Specification for Quadrupole Inductively Coupled Plasma Mass Spectrometer
3 Terms and definitions
There are no terms or definitions that require definition in this document:
4 Method Summary
The sample was decomposed by nitric acid and directly measured by mass spectrometry in a dilute nitric acid medium with argon plasma as the ion source: The instrument was calibrated by the internal standard method:
Factors that affect the measurement, such as drift and matrix effect:
5 Reagents and Materials
Unless otherwise specified, only reagents of analytical grade or above and those in compliance with the laboratory grade specified in GB/T 6682 were used in the analysis:
Water: Liquid reagents are stored in plastic bottles, and certified standard solutions are preferred:
5:1 Hydrogen peroxide [w(H2O2)≥30%]:
5:2 Hydrofluoric acid (19):
5:3 Nitric acid (1 1):
5:4 Nitric acid (2 98):
5:5 Thorium standard solution (ρ=1000μg/mL): certified standard solution:
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