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GB/T 14352.24-2022: Methods for chemical analysis of tungsten ores and molybdenum ores - Part 24: Determination of germanium content - Inductively coupled plasma mass spectrometry
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Methods for chemical analysis of tungsten ores and molybdenum ores - Part 24: Determination of germanium content - Inductively coupled plasma mass spectrometry
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GB/T 14352.24-2022
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Basic data | Standard ID | GB/T 14352.24-2022 (GB/T14352.24-2022) | | Description (Translated English) | Methods for chemical analysis of tungsten ores and molybdenum ores - Part 24: Determination of germanium content - Inductively coupled plasma mass spectrometry | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | D46 | | Classification of International Standard | 73.060 | | Word Count Estimation | 14,150 | | Date of Issue | 2022-12-30 | | Date of Implementation | 2023-04-01 | | Issuing agency(ies) | State Administration for Market Regulation, China National Standardization Administration | GB/T 14352.24-2022: Methods for chemical analysis of tungsten ores and molybdenum ores - Part 24: Determination of germanium content - Inductively coupled plasma mass spectrometry
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ICS 73.060
CCSD46
National Standards of People's Republic of China
Chemical analysis methods of tungsten ore and molybdenum ore
Part 24.Determination of germanium content
Inductively Coupled Plasma Mass Spectrometry
Posted on 2022-12-30
2023-04-01 Implementation
State Administration for Market Regulation
Released by the National Standardization Management Committee
table of contents
Preface I
Introduction III
1 Scope 1
2 Normative references 1
3 Terms and Definitions 1
4 Principle 1
5 Test conditions 1
6 Reagent or material 1
7 Instruments and Equipment 2
8 sample 3
9 Test Step 3
9.1 Blank test 3
9.2 Verification test 3
9.3 Decomposition of samples 3
9.4 Preparation of Calibration Solution Series 3
9.5 Determination 3
9.6 Drawing of Calibration Curve 4
10 Experimental data processing 4
11 Precision 4
12 Accuracy 4
13 Quality Assurance and Control 5
Appendix A (Informative) Preparation of Elemental Standard Stock Solutions 6
Appendix B (Informative) Ion Exchange Resin Pretreatment and Regeneration Treatment 7
Appendix C (Informative) Homemade Ion Exchange Resin Filter Column 8
Appendix D (Informative) Instrument Reference Working Conditions 9
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 24 of GB/T 14352 "Methods for Chemical Analysis of Tungsten and Molybdenum Ores". GB/T 14352 has been issued with
Lower part.
--- Part 1.Determination of tungsten content;
--- Part 2.Determination of molybdenum content;
--- Part 3.Determination of copper content;
--- Part 4.Determination of lead content;
--- Part 5.Determination of zinc content;
--- Part 6.Determination of cadmium content;
--- Part 7.Determination of cobalt content;
--- Part 8.Determination of nickel content;
--- Part 9.Determination of sulfur content;
--- Part 10.Determination of arsenic content;
--- Part 11.Determination of bismuth content;
--- Part 12.Determination of silver content;
--- Part 13.Determination of tin content;
--- Part 14.Determination of gallium content;
--- Part 15.Determination of germanium content;
--- Part 16.Determination of selenium content;
--- Part 17.Determination of tellurium content;
--- Part 18.Determination of the amount of rhenium;
--- Part 19.Determination of the amount of bismuth, cadmium, cobalt, copper, iron, lithium, nickel, phosphorus, lead, strontium, vanadium and zinc Inductively coupled plasma atomic emission
spectroscopy;
--- Part 20.Determination of the amount of niobium, tantalum, zirconium, hafnium and 15 rare earth elements by inductively coupled plasma mass spectrometry;
--- Part 21.Determination of the amount of arsenic Hydride generation - atomic fluorescence spectrometry;
--- Part 22.Determination of antimony content Hydride generation-atomic fluorescence spectrometry;
--- Part 24.Determination of germanium content Inductively coupled plasma mass spectrometry.
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 by the Ministry of Natural Resources of the People's Republic of China.
This document is under the jurisdiction of the National Natural Resources and Land Spatial Planning Standardization Technical Committee (SAC/TC93).
This document is drafted by. Jiangsu Provincial Institute of Geological Survey.
The main drafters of this document. Cai Yuman, Zhang Peixin, Li Ming, Huang Guangming, Gao Xiaoli, Cao Lei, Xiao Yufang, Jiang Ye, Zhang Qi.
Introduction
Tungsten ore and molybdenum ore are our country's superior resources, and their basic reserves, output and export volume have long been among the top in the world. Molybdenum is a difficult
Molten metal is an indispensable raw material in manufacturing industries such as metallurgy, electrical, chemical, aviation and aerospace. Tungsten is a heat-resistant metal widely used in
Electrical appliances, electronics, petroleum, chemical and military industries, etc. Most of the tungsten ore and molybdenum ore are associated paragenetic components, and there are as many as 30 kinds of parabiotic beneficial components.
Mainly tin, bismuth, beryllium, copper, lead, zinc, arsenic, rhenium, germanium, cadmium, sulfur, selenium, tellurium, gallium, gold, silver, lithium, niobium, tantalum, zirconium, hafnium, rare earth, thorium, scandium, Thallium, Fluorite
etc., the comprehensive utilization value is great. Tungsten and molybdenum resources are not only important strategic mineral resources in the world, but also play an important role in my country's national economy.
The role is also rising and becoming more and more important.
"Chemical Analysis Methods of Tungsten Ore and Molybdenum Ore" is planned to be composed of 24 parts.
--- Part 1.Determination of the amount of tungsten. The purpose is to establish a method for the determination of tungsten by melting sodium peroxide, extracting with hot water, and using thiocyanate spectrophotometry.
Analysis method of tungsten content in ore and molybdenum ore.
--- Part 2.Determination of molybdenum content. The purpose is to establish a method for the determination of tungsten by melting sodium peroxide, extracting with hot water, and using thiocyanate spectrophotometry.
Analysis method of molybdenum content in ore and molybdenum ore.
--- Part 3.Determination of copper content. The purpose is to establish the decomposition of four acids, flame atomic absorption spectrophotometry in hydrochloric acid medium
An analytical method for the determination of copper content in tungsten ore and molybdenum ore.
--- Part 4.Determination of lead content. The purpose is to establish the use of tetra-acid decomposition, flame atomic absorption spectrometry in nitric acid-boric acid medium
An analytical method for the photometric determination of lead content in tungsten ore and molybdenum ore.
--- Part 5.Determination of zinc content. The purpose is to establish the use of tetra-acid decomposition, flame atomic absorption spectrometry in hydrochloric acid-boric acid medium
It is an analytical method for the photometric determination of zinc content in tungsten ore and molybdenum ore.
--- Part 6.Determination of cadmium content. The purpose is to establish the use of tetra-acid decomposition, flame atomic absorption spectrometry in hydrochloric acid-boric acid medium
An analytical method for the photometric determination of cadmium content in tungsten ore and molybdenum ore.
--- Part 7.Determination of the amount of cobalt. The purpose is to establish the use of sodium peroxide melting, hot water extraction, precipitation acidification, and the use of succinyldioxime-sulfo
Salicylic acid-ammonia water-ammonium chloride bottom liquid polarographic method to determine cobalt content in tungsten ore and molybdenum ore and decomposition with four acids, in
Analytical method for determination of cobalt content in tungsten ore and molybdenum ore by flame atomic absorption spectrophotometry in hydrochloric acid-boric acid medium.
--- Part 8.Determination of nickel content. The purpose is to establish the use of sodium peroxide melting, hot water extraction, precipitation acidification, and the use of succinyldioxime-sulfo
Salicylic acid-ammonia water-ammonium chloride bottom solution polarographic method to determine nickel content in tungsten ore and molybdenum ore and decomposition with four acids, in
Analytical method for determination of nickel content in tungsten ore and molybdenum ore by flame atomic absorption spectrophotometry in hydrochloric acid-boric acid medium.
--- Part 9.Determination of sulfur content. The purpose is to establish the determination of sulfur content in tungsten ore and molybdenum ore by high temperature combustion-potassium iodate volumetric method
analysis method.
--- Part 10.Determination of the amount of arsenic. The purpose is to establish the decomposition with nitric acid-sulfuric acid and the silver diethyldithiocarbamate photometric method
Analytical method for determining arsenic content in tungsten ore and molybdenum ore.
--- Part 11.Determination of the amount of bismuth. The purpose is to establish the decomposition of aqua regia and the determination of tungsten ore,
Analytical method for bismuth content in molybdenum ores.
--- Part 12.Determination of silver content. The purpose is to establish the four-acid decomposition, using methyl isobutyl ketone to extract the flame atomic absorption fraction
It is an analytical method for determining silver content in tungsten ore and molybdenum ore by spectrophotometry.
--- Part 13.Determination of the amount of tin. The purpose is to establish the use of sodium peroxide melting, hot water extraction, hydrochloric acid-ammonium chloride bottom liquid polarographic
The analytical method for the determination of tin content in tungsten ore and molybdenum ore and the use of sodium peroxide melting, hot water extraction, hydride atomic fluorescence
An analysis method for the determination of tin content in tungsten ore and molybdenum ore by spectrometry.
--- Part 14.Determination of the amount of gallium. The purpose is to establish the use of sodium peroxide fusion, hot water extraction, extraction and separation with butyl acetate-Luo
Danmin B spectrophotometry is an analytical method for the determination of gallium content in tungsten ore and molybdenum ore.
--- Part 15.Determination of the amount of germanium. The purpose is to establish the use of nitric acid-hydrofluoric acid-sulfuric acid decomposition-sodium peroxide alkali fusion, distillation separation-
An analytical method for the determination of germanium content in tungsten ore and molybdenum ore by benzofluorenone-hexadecyltrimethylammonium bromide spectrophotometry.
--- Part 16.Determination of selenium content. The purpose is to establish the method of decomposition with nitric acid-hydrofluoric acid-sulfuric acid and the photometric method of 3,3'-diaminobenzidine
An analytical method for determining the selenium content in tungsten ore and molybdenum ore.
--- Part 17.Determination of the amount of tellurium. The purpose is to establish the decomposition of nitric acid-hydrofluoric acid-sulfuric acid and the photometric method of butyl rhodamine B
An analysis method for determining the tellurium content in tungsten ore and molybdenum ore.
--- Part 18.Determination of the amount of rhenium. The purpose is to establish the determination of tungsten by using magnesium oxide sintering decomposition, water leaching, and thiocyanate photometry.
Analysis method of rhenium content in ore and molybdenum ore.
--- Part 19.Determination of the amount of bismuth, cadmium, cobalt, copper, iron, lithium, nickel, phosphorus, lead, strontium, vanadium and zinc Inductively coupled plasma atomic emission
spectroscopy. The purpose is to establish the determination of tungsten ore and molybdenum ore by inductively coupled plasma atomic emission spectrometry using tetra-acid decomposition
Methods for the analysis of bismuth, cadmium, cobalt, copper, iron, lithium, nickel, phosphorus, lead, strontium, vanadium and zinc in stone.
--- Part 20.Determination of the amount of niobium, tantalum, zirconium, hafnium and 15 rare earth elements Inductively coupled plasma mass spectrometry. purpose is to
Sodium peroxide melting, hot water extraction, and inductively coupled plasma mass spectrometry for the determination of niobium, tantalum, zirconium,
Analytical methods for the content of hafnium and 15 rare earth elements.
--- Part 21.Determination of the amount of arsenic Hydride generation - atomic fluorescence spectrometry. The purpose is to establish hydrochloric acid-nitric acid decomposition, mining
An analytical method for the determination of arsenic content in tungsten ore and molybdenum ore by hydride generation-atomic fluorescence spectrometry.
--- Part 22.Determination of the amount of antimony Hydride generation - atomic fluorescence spectrometry. The purpose is to establish the use of nitric acid-hydrofluoric acid-sulfuric acid
Solution, using hydride generation-atomic fluorescence spectrometry to determine the content of antimony in tungsten ore and molybdenum ore.
--- Part 23.Determination of rhenium content Inductively coupled plasma mass spectrometry. The purpose is to establish the use of magnesium oxide sintering decomposition, water immersion
The analysis method for the determination of rhenium content in tungsten ore and molybdenum ore by inductively coupled plasma mass spectrometry.
--- Part 24.Determination of germanium content Inductively coupled plasma mass spectrometry. The purpose is to establish the use of sodium hydroxide alkali fusion decomposition,
An analytical method for the determination of germanium content in tungsten ore and molybdenum ore by inductively coupled plasma mass spectrometry.
GB/T 14352.24 is a supplement and improvement to GB/T 14352.15.By changing the way of decomposition, using a single sodium hydroxide base
Melting decomposition, ion exchange method to remove interfering salts and other methods, combined with inductive coupling with high sensitivity, good precision, and strong anti-interference ability
Plasma mass spectrometer detection technology reduces detection costs and improves work efficiency.
This document clarifies the decomposition and determination conditions of tungsten ore and molybdenum ore samples, and determines the methods including method detection limit, measurement range, precision,
Accuracy and other technical indicators and inspection parameters. It enables analysts to determine tungsten ore and molybdenum ore with evidence to base on, so as to provide
Accurate determination of paragenetic components provides reliable quality assurance, which provides a basis for the investigation of tungsten ore and molybdenum ore resources, the development and utilization of related mineral products, and the development and utilization of tungsten ore.
It provides strong technical support for the grade and reserve evaluation of paragenetic components in ores and molybdenum ores.
Chemical analysis methods of tungsten ore and molybdenum ore
Part 24.Determination of germanium content
Inductively Coupled Plasma Mass Spectrometry
Caution --- Personnel using this document should have practical experience in formal laboratory work. This document does not address all possible security issues
question. It is the user's responsibility to take appropriate safety and health measures and ensure compliance with the conditions stipulated in the relevant national laws and regulations.
1 Scope
This document specifies the method for the determination of germanium content in tungsten ore and molybdenum ore by inductively coupled plasma mass spectrometry.
This document is applicable to the determination of germanium content in tungsten ore and molybdenum ore by inductively coupled plasma mass spectrometry.
The detection limit of the germanium content detection method in this document is 0.063 μg/g, and the determination range is 0.2 μg/g~300 μg/g.
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 6682-2008 Analytical laboratory water specifications and test methods
GB/T 14505 General principles and general provisions for chemical analysis methods of rocks and ores
Calibration specification for JJF1159 quadrupole inductively coupled plasma mass spectrometer
3 Terms and Definitions
This document does not have terms and definitions that need to be defined.
4 principles
The sample is melted by sodium hydroxide at high temperature and extracted by water. Germanium exists in the solution in the form of soluble germanate and is diluted to prepare a solution. Take
Part of the solution is separated by cation and anion exchange resins to remove a large amount of sodium salt and a small amount of residual molybdenum. The separated solution was atomized, evaporated
Processes such as emission, dissociation, atomization, and ionization enter the mass spectrometer, and the mass spectrometer performs separation according to the mass-to-charge ratio. For a specific mass-to-charge ratio, at a certain
Within the concentration range, the concentration of the analyte element in the sample is directly proportional to the signal intensity of the mass spectrometer. The content of germanium in the sample was calculated by the calibration curve.
5 Test conditions
The test conditions such as temperature, humidity, voltage and frequency during the detection of the inductively coupled plasma mass spectrometer shall comply with the environmental conditions specified in JJF1159.
Environmental conditions and related requirements.
6 Reagents or materials
Unless otherwise stated, only reagents confirmed to be of analytical grade were used in the analysis.
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