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GB/T 42240-2022: Nanotechnology - Measurement of metallic impurities in graphene powder - Inductively coupled plasma mass spectrometry
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Nanotechnology - Measurement of metallic impurities in graphene powder - Inductively coupled plasma mass spectrometry
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GB/T 42240-2022
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Basic data | Standard ID | GB/T 42240-2022 (GB/T42240-2022) | | Description (Translated English) | Nanotechnology - Measurement of metallic impurities in graphene powder - Inductively coupled plasma mass spectrometry | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | G30 | | Classification of International Standard | 71.040.50 | | Word Count Estimation | 26,284 | | Date of Issue | 2022-12-30 | | Date of Implementation | 2023-07-01 | | Issuing agency(ies) | State Administration for Market Regulation, China National Standardization Administration | GB/T 42240-2022: Nanotechnology - Measurement of metallic impurities in graphene powder - Inductively coupled plasma mass spectrometry
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ICS 71.040.50
CCSG30
National Standards of People's Republic of China
Determination of Metallic Impurities in Nanotechnology Graphene Powders
Inductively Coupled Plasma Mass Spectrometry
Posted on 2022-12-30
2023-07-01 implementation
State Administration for Market Regulation
Released by the National Standardization Management Committee
table of contents
Preface III
Introduction IV
1 Scope 1
2 Normative references 1
3 Terms and Definitions 1
4 Principle 2
5 Reagent or material 2
6 Instruments and equipment 3
7 sample 4
8 Test Step 5
9 Experiment data processing 6
10 Measurement uncertainty7
11 Test report 8
Appendix A (Informative) ICP-MS Test Reference Conditions 9
Appendix B (informative) Comparison of different sample processing methods 10
Appendix C (Informative) Standard Calibration Curves of Several Metal Impurities 13
Appendix D (Informative) Determination and Test Example of Metal Impurities in Graphene Powder Samples 15
Appendix E (Informative) Test Report Template 18
Reference 20
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.
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 was proposed by the Chinese Academy of Sciences.
This document is under the jurisdiction of the National Nanotechnology Standardization Technical Committee (SAC/TC279).
This document is drafted by. National Nanoscience Center, China Institute of Metrology, Guangzhou Special Pressure Equipment Testing and Research Institute, Shanghai Yi
Yao Instrument Technology Development Co., Ltd., Beijing Institute of Science and Technology Analysis and Testing Institute (Beijing Physical and Chemical Analysis and Testing Center), Capital Division
Fan University, South China University of Technology, Beijing Graphene Research Institute, Beijing Jitian Instrument Co., Ltd., Taizhou Graphene Research and Testing Platform Co., Ltd.
company.
The main drafters of this document. Liu Renxiao, Tian Guolan, Yin Zongjie, Li Maodong, Ren Lingling, Ge Guanglu, Guo Yuting, Ni Chenjie, Yu Xuelei,
Liu Weili, Zhang Lan, Zhang Ronghua, Liu Xu, Chi Yawen, Ding Rong.
Introduction
Graphene powder is currently the main form of graphene products in my country, and has been used in new energy batteries, thermal management, heavy-duty coatings and other industrial fields.
Preliminary realization of large-scale application. Graphene powder can be produced through different production processes such as mechanical exfoliation, reduction oxidation, intercalation dissociation, small molecule synthesis, etc.
preparation. Due to differences in production processes, production equipment, raw materials, etc., the ratio of metal impurity elements contained in graphene powders produced by different manufacturers
There are also significant differences in species and content. Metal impurities will directly affect the application performance of graphene powder, graphene application technology development and production
The development of the industry urgently needs to establish a standardized analytical test method for accurate and reliable detection of metal impurities in graphene powder.
Inductively Coupled Plasma Mass Spectrometry (ICP-MS) technology can realize the simultaneous rapid trace quantitative detection of various inorganic elements and isotopes
It has wide dynamic linear range and high sensitivity. The development of a quantitative test method for metal impurities in graphene powder based on ICP-MS technology is under test
The test is technically feasible, but three problems need to be solved. (1) Sample processing. the crystal structure of graphene is composed of carbon atoms covalently bonded by π-π
The hexagonal close-packed honeycomb formed by the combination of graphene and chemical bonds is difficult to be opened, and the sample to be tested by ICP-MS technology should be a solution, so it is necessary to mix graphene
The powder is completely digested. The "high temperature ashing" sample processing method is commonly used in the testing of carbon materials such as graphite, but due to the low apparent density of graphene,
In the process of heating and ashing, it is easy to drift and inevitably introduce large errors; concentrated sulfur that has a strong digestion effect on graphene powder
Acid, perchloric acid, hydrogen peroxide, etc. may produce obvious polyatomic ion interference during the test and affect the accuracy of the test results, or under high temperature and high pressure
There is a high risk of explosion and explosion under airtight conditions, so it is first necessary to develop an applicable and scalable sample processing method. (2) Multi-element standard calibration
Curve establishment and quantitative testing. the quantitative testing of inorganic impurities using ICP-MS technology requires the establishment of standard calibration curves for the measured elements, and
There are more than 20 types of metal impurity elements contained in industrialized graphene powder, and the content of each element has a very wide distribution range, ranging from a few micrograms to
Every kilogram (μg/kg) to thousands of milligrams per kilogram (mg/kg), so it is necessary to consider how to establish a standard calibration curve for each element to be measured;
In addition, for elements that are susceptible to environmental influences, spectral line interference, and matrix interference, it is possible to establish appropriate methods or select appropriate test modes to
Get the most accurate and reliable test results possible. (3) Recovery rate of standard addition. due to the complex composition of the graphene powder measurement sample and the influence factors of the test
If there are many, the recovery rate of standard addition can be used to verify the reliability of the test analysis method. This document provides solutions to the above three problems and establishes
Standardized quantitative test and analysis method for metal impurities in graphene powder.
Determination of Metallic Impurities in Nanotechnology Graphene Powders
Inductively Coupled Plasma Mass Spectrometry
Warning. The reagents (nitric acid, hydrofluoric acid) used for sample digestion in this document are highly oxidizing and corrosive, and the operation process must be strictly
Comply with the experimental conditions and instrument operating instructions, pay attention to safety protection.
1 Scope
This document describes a method for the determination of metallic impurities in graphene powders by inductively coupled plasma mass spectrometry.
This document is applicable to the determination of metal impurities in graphene powder. Other carbon-based nanomaterials, such as carbon nanotubes, carbon fibers, porous carbon, etc.
The determination of contained metal impurities shall be carried out according to the reference.
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 5009.268 National food safety standard Determination of multi-elements in food
3 Terms and Definitions
The following terms and definitions apply to this document.
3.1
graphene graphene
graphene layer graphenelayer
single-layer graphene single-layergraphene; monolayergraphene
A monolayer of carbon atoms that combines one carbon atom with three surrounding carbon atoms to form a honeycomb structure.
NOTE 1.It is an important building block of many carbon nanoobjects.
Note 2.Since graphene has only one layer, it is often called monolayer graphene. Graphene is abbreviated as 1LG to distinguish it from bilayer graphite abbreviated as 2LG
ene and few-layer graphene abbreviated as FLG.
NOTE 3.Graphene has boundaries and has defects and grain boundaries where carbon-carbon bonds have been disrupted.
[Source. GB/T 30544.13-2018, 3.1.2.1]
3.2
Graphene powder graphene powder
It is a black or brownish-yellow powder mainly composed of graphene and related two-dimensional materials.
Note. Graphene powder includes single-layer graphene (1LG), double-layer graphene (2LG), few-layer graphene (FLG), graphene nanosheet (GNP), mechanical exfoliation stone
Graphene, chemically dissociated graphene, small molecule synthesis (CVD, PVD) graphene, reduced graphene oxide (rGO), graphene oxide (GO), etc.
3.3
Few-layer graphene few-layer graphene; FLG
Two-dimensional materials that consist of stacks of three to ten complete graphene layers.
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