GB/T 4930-2021Microbeam analysis - Electron probe microanalysis - Guidelines for the specification of certified reference materials(CRMs) (English PDF)

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 replaces GB/T 4930-2008 "Guidelines for the Technical Conditions of Microbeam Analysis Electron Probe Analysis Standard Samples", and

Compared with GB/T 4930-2008, in addition to editorial changes, the main technical changes are as follows.

a) "The amount of research material must be sufficient to prepare about.200 sets of standard samples" is changed to "The amount of research material should be sufficient for the standard sample

Preparation" (see 4.1, 4.1 of the.2008 edition);

b) Replace the note with the text. Delete the first paragraph "Based on these factors, there is no detailed regulation on the sampling sample size here, so that

Analysts flexibly design testing procedures" (see 5.2, 5.2 of the.2008 edition);

c) Added "(or a suitable and well-characterized composite sample, in which overlap will not cause problems)" (see 5.3);

d) "For an energy spectrometer, the dead time should be set at 30%" to "For an energy spectrometer, the dead time should be about 30%" (see

5.3, 5.3 of the.2008 edition);

e) "Background" is changed to "Background" (see 5.5, 5.5 of the.2008 edition);

f) In order to correct printing errors, the formula +/-2

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(See 5.6,.2008

Introduction

Electron probe microanalysis (EPMA) is a quantitative analysis method carried out by the comparative method. It has been widely used in the world and has a certificate.

Quasi-samples (CRMs) have a critical impact on the accuracy of quantitative analysis.

Therefore, the revision of this document is conducive to the international exchange of electron probe microanalysis and the compatibility of analysis data.

This document specifies how to evaluate and select reference materials (RMs)1), how to evaluate the inhomogeneity and stability of standard samples, and gives

The chemical composition determination method for the production of EPMA standard samples.

The first such standard in the world is GB 4930-1985 "General Technical Conditions for Electron Probe Analysis Standard Samples", which is composed of

Drafted by Liu Yongkang, Lin Zhuoran and Zhang Yi, approved by the National Standardization Technical Committee for Electron Probe Analysis Standard Samples (National Standardization Technology for Microbeam Analysis)

The predecessor of the Technical Committee) reviewed and passed the report to the National Bureau of Standards (CBS) (the CSBTS of the National Bureau of Technical Supervision and the China National Standardization Committee)

The predecessor of SAC) was approved for release and implemented in 1985.This standard was revised for the first time and formed GB/T 4930-1993.The drafters Liu Yongkang,

Zhang Yi, Lin Zhuoran, Suo Zhicheng, reviewed by the National Microbeam Analysis Standardization Technical Committee, approved by the State Technical Supervision Bureau, August.1993

Promulgated on the 30th and implemented on July 1,.1994.

In.1993, Lin Zhuoran translated GB/T 4930-1993 into English, and was approved by the China Committee of the International Organization for Standardization (ISO /CS, namely

CSBTS) applied to the Electronic Probe Branch of the Microbeam Analysis Technical Committee of the International Organization for Standardization (ISO /TC202/SC2) for the establishment of international standards.

After many revisions by domestic and foreign peer experts, it was submitted to ISO for approval, and finally formed ISO 14595.2003 Microbeamanalysis-Electron

probemicroanalysis-Guidelinesforthespecificationofcertifiedreferencematerials(CRMs). according to

The provisions of GB/T 20000.2-2001 are equivalent to using ISO 14595 to replace GB/T 4930-1993, which is equivalent to a revision of the original standard.

GB/T 4930-2008 was drafted by Liu Yongkang, Wan Guangquan, Liang Xirong, Yang Qiujian, and was reviewed and approved by the National Microbeam Analysis Standardization Technical Committee.

It was reported to SAC for approval and implemented on October 1,.2008.

In.2014, the ISO 14595.2003 edition was revised, and finally the ISO 14595.2014 "Microbeamanalysis-Electron

probemicroanalysis-Guidelinesforthespecificationofcertifiedreferencematerials(CRMs)". according to

According to the provisions of GB/T 20000.2-2009, this document is equivalent to ISO 14595.2014 instead of GB/T 4930-2008, which is equivalent to

Revision of GB/T 4930-2008.

1) Reference material (RM) according to the relevant definition in JJF1001-2011.a substance with sufficiently uniform and stable specific characteristics,

Its characteristics have been confirmed to be suitable for the intended use in the measurement or in the inspection of the nominal characteristics.

Microbeam analysis electron probe microanalysis

Guidelines for Technical Conditions of Standard Samples

1 Scope

This document applies to single-phase standard samples (certified reference materials, CRMs) used in electron probe microanalysis (EPMA), and gives

The guidelines for the use of standard samples for microanalysis of flat and polished surfaces are introduced. This document does not apply to organic and biological standard samples.

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 15000.4-2019 Work Guidelines for Standard Samples Part 4.Contents of Certificates, Labels and Attached Documents (ISO Guide

31.2015, IDT)

3 Terms and definitions

The following terms and definitions apply to this document.

3.1

Heterogeneity

The change in elemental composition value measured from a set of samples.

Note. The non-uniformity comes from the measurement between the sample and the sample, the measurement between the micrometer scale in each sample, and the uncertainty of the testing process itself

Fixed degree.

3.2

Researchmaterial

The physical and chemical characteristics meet the requirements of standard samples, but the details (including chemical composition,

Stability and micro-area and macro-inhomogeneity) materials for testing.

3.3

Stability

< General> The ability of the sample to resist chemical and physical changes when stored for a long time under normal temperature and pressure.

3.4

Stability

\u003cEPMA\u003eThe ability of the material to resist changes in chemical composition when bombarded by an electron beam, that is, the phase resistance observed during the exposure of the sample to the electron beam

The ability to change the intensity of characteristic X-rays.

3.5

Uncertainty

It characterizes the parameters that are reasonably assigned to the dispersion of the measured value and are related to the measurement result.