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GB/T 17359-2023: Microbeam analysis - Quantitative analysis using energy-dispersive spectrometry (EDS) for elements with an atomic number of 11 (Na) or above
Status: Valid GB/T 17359: Evolution and historical versions
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivered in | Standard Title (Description) | Status | PDF |
| GB/T 17359-2023 | English | 449 |
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Microbeam analysis - Quantitative analysis using energy-dispersive spectrometry (EDS) for elements with an atomic number of 11 (Na) or above
| Valid |
GB/T 17359-2023
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| GB/T 17359-2012 | English | 839 |
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Microbeam analysis -- Quantitative analysis using energy dispersive spectrometry
| Obsolete |
GB/T 17359-2012
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| GB/T 17359-1998 | English | 399 |
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General specification of X-ray EDS quantitative analysis for EPMA and SEM
| Obsolete |
GB/T 17359-1998
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PDF similar to GB/T 17359-2023
Basic data | Standard ID | GB/T 17359-2023 (GB/T17359-2023) | | Description (Translated English) | Microbeam analysis - Quantitative analysis using energy-dispersive spectrometry (EDS) for elements with an atomic number of 11 (Na) or above | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | N53 | | Classification of International Standard | 71.040.99 | | Word Count Estimation | 22,293 | | Date of Issue | 2023-12-28 | | Date of Implementation | 2024-07-01 | | Older Standard (superseded by this standard) | GB/T 17359-2012 | | Issuing agency(ies) | State Administration for Market Regulation, China National Standardization Administration | GB/T 17359-2023: Microbeam analysis - Quantitative analysis using energy-dispersive spectrometry (EDS) for elements with an atomic number of 11 (Na) or above
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ICS 71:040:99
CCSN53
National Standards of People's Republic of China
Replace GB/T 17359-2012
Microbeam analysis of elements with atomic number no less than 11
Quantitative analysis by energy spectroscopy
(ISO 22309:2011,MOD)
Published on 2023-12-28
2024-07-01 Implementation
State Administration for Market Regulation
Released by the National Standardization Administration Committee
Table of contents
PrefaceⅠ
Introduction III
1 Scope 1
2 Normative references 1
3 Terms and Definitions 2
4 Sample preparation 4
5 Instrument preparation 5
6 Analysis Step 5
7 Data Processing 6
7:1 General 6
7:2 Peak identification 6
7:3 Estimation of peak intensity 7
7:4 Calculation of k value 7
7:5 Matrix effect 7
7:6 Application of reference materials 7
7:7 Analysis without standards 7
7:8 Uncertainty of results 8
7:9 Results Report 9
Appendix A (informative) Analysis of elements with atomic numbers less than 1110
Appendix B (informative) Identification of spectral peaks and interference peaks 11
Appendix C (informative) Calibration of spectral peaks 12
Appendix D (informative) Factors affecting the uncertainty of measurement results 13
Appendix E (informative) Data examples of reproducibility studies in a single laboratory and between different laboratories15
Reference 16
Foreword
This document complies with the provisions of GB/T 1:1-2020 "Standardization Work Guidelines Part 1: Structure and Drafting Rules of Standardization Documents"
Drafting:
This document replaces GB/T 17359-2012 "Quantitative Analysis by Microbeam Analysis Energy Spectroscopy": Compared with GB/T 17359-2012, except for the
In addition to structural adjustments and editorial changes, the main technical changes are as follows:
a) Absorption correction, atomic number correction, Bremsstrahlung radiation, certified reference material, electron probe microanalysis, fluorescence correction, incident were deleted
Terms and definitions of electron beam energy, EDS quantitative analysis, traceability, and X-ray absorption (see 3:1, 3:4, 3:7,:2012 edition
3:8, 3:12, 3:15, 3:17, 3:24, 3:32, 3:35);
b) Changed the terms and definitions of energy resolution and spatial resolution (see 3:21, 3:22, 3:28, 3:29 of the:2012 edition);
c) Changed the requirements for sample uniformity (see 4:2, 4:2 of the:2012 edition);
d) Changed the requirements for removing contaminants on the surface of the specimen (see 4:3, 4:3 of the:2012 edition);
e) Changed the requirements for sample preparation (see 4:5, 4:5 of the:2012 edition);
f) Changed the requirements for sample conductivity (see 4:6,:2012 version of 4:6);
g) Changed the requirements for reference materials (see 4:8, 4:8 of the:2012 edition);
h) Changed the requirements for detectors (see 5:5,:2012 version of 5:5);
i) The requirements for accelerating voltage have been changed (see 6:1, 6:1 of the:2012 edition);
j) Changed the requirements for the system count rate range (see 6:2, 6:2 of the:2012 version);
k) Changed the requirements for selecting the analysis location (see 6:5, 6:5 of the:2012 version);
l) Changed the requirements for peak identification (see 7:2,:2012 version of 7:2);
m) Changed the requirements for reference material application (see 7:6,:2012 version of 7:6);
n) Changed the requirements for validation of analytical methods (see 7:8:2,:2012 version of 7:8:2);
o) Changed the requirements for normalization of analysis results [see 7:9j),:2012 version of 7:9j)]:
This document is modified to adopt ISO 22309:2011 "Microbeam analysis of elements with atomic number greater than or equal to 11 (Na) by energy spectrometry:
Analysis":
Compared with ISO 22309:2011, this document has made the following structural adjustments:
---The order of the appendices has been adjusted according to the order in which they are mentioned in the text:
The technical differences between this document and ISO 22309:2011 and their reasons are as follows:
---Replaced ISO 15632:2002 (see 5:1, 5:4, 5:5) with the normatively quoted GB/T 20726-2015 to adapt to my country's
Technical conditions to increase operability;
---Replaced ISO /IEC 17025:2005 (see 7:9) with normatively quoted GB/T 27025-2019 to adapt to my country's technology
technical conditions to increase operability;
---Replaced ISO 14594 [see 6:1c)] with normatively cited GB/T 30705 to adapt to my country's technical conditions and increase the availability
operability;
---Replaced ISO 16700 (see 6:3) with normatively quoted GB/T 27788 to adapt to my country's technical conditions and increase operability
work nature;
---Deleted the words "absorption correction, atomic number correction, Bremsstrahlung radiation, certified reference materials, electron probe microanalysis,
Fluorescence correction, incident electron beam energy, EDS quantitative analysis, traceability, X-ray absorption" terms and definitions to comply with our country's
Standard writing rules;
---Modify the terms and definitions of energy resolution and spatial resolution to make it more clearly distinguish between energy resolution and spatial resolution:
rate (see 3:20, 3:21):
The following editorial changes have been made to this document:
---Deleted the note of ISO 22309:20113:16 (see 3:10):
Please note that some content in this document may be subject to patents: The publisher of this document assumes no responsibility for identifying patents:
This document is proposed and coordinated by the National Microbeam Analysis Standardization Technical Committee (SAC/TC38):
This document was drafted by: Beijing Institute of Geology of Nuclear Industry, Institute of Mineral Resources, Chinese Academy of Geological Sciences, Chinese Academy of Geology and Geology
Institute of Geophysical Physics, Industrial Analysis and Testing Center of Guangdong Academy of Sciences:
The main drafters of this document: Fan Guang, Ge Xiangkun, Chen Zhenyu, Yu Apeng, Mao Qian, and Wu Chaoqun:
This document was first published in:2012 and this is the first revision:
Introduction
The high-energy electron beam acts on the sample to produce X-rays, which have different characteristics depending on the chemical composition (atom type) in the sample:
And have different energies (wavelengths): The X-ray intensity of each element is related to the content of that element in the sample: If it were possible to measure this
These X-ray intensities are compared with the X-ray intensities of an appropriate reference material or a group of reference materials, and are calibrated using appropriate methods:
Yes, then the content of each element can be measured: The "no standard sample" program can also provide quantitative results of the sample, but it must be stored in the software:
A previously measured reference X-ray intensity in the package or a theoretically calculated X-ray intensity is compared to this: This is based on some false
The test accuracy of the designed procedure is bound to be lower than the test accuracy of the reference material method (see references [1]~[8]): Detect featureX
There are two common methods of ray analysis: wave spectroscopy (WDX) and energy spectroscopy (EDS): The method used in this paper is energy spectroscopy:
When analyzed by energy spectroscopy, the quantitative analysis of light elements [elements with atomic number Z < 11 (Na)] is more complicated: This paper discusses a
some issues related to this aspect:
Microbeam analysis of elements with atomic number no less than 11
Quantitative analysis by energy spectroscopy
1 Scope
This document describes the use of an energy spectrometer mounted on a scanning electron microscope (SEM) or electron microprobe (EPMA) to analyze specific points or specific
Methods for quantitative analysis of areas: Quantitative analysis refers to expressing the content of elements in mass fraction (percentage): Correctly identify all the
Elements are an essential part of quantitative analysis, therefore, this document also covers this aspect: This document describes various energy spectroscopy methods
Quantitative analysis methods:
This document is applicable to the analysis of elements with a mass fraction higher than 1% and atomic number Z >10 using reference materials or the "no standard sample" procedure:
Quantitative analysis:
This document also gives information on analytical methods for light elements with atomic numbers less than 11:
Note: When there are no overlapping peaks and the corresponding characteristic X-rays are strongly excited, the energy spectrometer can also measure elements with mass fractions at the 0:1% level: Book
The document is mainly used for quantitative analysis of samples with flat surfaces: The basic method is also suitable for the analysis of samples with uneven surfaces, but it will introduce additional uncertainties:
Quantity:
There is currently no recognized accurate energy spectroscopy (EDS) quantitative analysis method for light elements: The following are several commonly used methods for light element analysis:
EDS method:
a) Measure peak areas and compare peak intensities: For reasons stated in Appendix A, the uncertainty of this method in light element analysis results
Larger than heavier elements:
b) When it is known that the light element in the sample is combined with the heavy element (Z >10) in a stoichiometric manner, the concentration of the light element can be determined by
Determined by relative concentration ratios to other elements: This method is usually used for the determination of oxygen in silicate mineral samples:
c) Calculate the concentration by the difference method, that is, subtract the total percentage of analyzable elements from 100% to obtain the percentage of light elements: This kind of
The method can only be applied under the conditions of good beam stability and independent measurement of at least one reference sample, and also requires
To accurately determine other elements in the sample:
Appendix A summarizes issues in the quantitative analysis of light elements in the presence of heavy elements: If an energy spectrometer and wave spectrometer are installed on the instrument
(WDS), WDS can be used to overcome the low-energy peak overlap problem in EDS analysis: However, many other issues arise for both technologies
Technically speaking, they are all common:
2 Normative reference documents
The contents of the following documents constitute essential provisions of this document through normative references in the text: Among them, the dated quotations
For undated referenced documents, only the version corresponding to that date applies to this document; for undated referenced documents, the latest version (including all amendments) applies to
this document:
GB/T 27025-2019 General requirements for testing and calibration laboratory capabilities (ISO /IEC 17025:2017, IDT)
GB/T 20726-2015 Main performance parameters and verification methods of X-ray energy spectrometer for microbeam analysis, electron probe microanalysis
(ISO 15632:2012,IDT)
GB/T 27788 Microbeam analysis scanning electron microscope image magnification calibration guidelines (GB/T 27788-2020, ISO 16700:
2016,IDT)
GB/T 30705 Guidelines for determination of experimental parameters of microbeam analysis electron probe microanalysis spectrometry (GB/T 30705-2014,
ISO 14594:2009,MOD)
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