ISO 19463:2018

INTERNATIONAL ISO
STANDARD 19463
First edition
2018-07
Microbeam analysis — Electron probe
microanalyser (EPMA) — Guidelines
for performing quality assurance
procedures
Analyse par microfaisceaux — Analyse par microsonde électronique
(microsonde de Castaing) — Lignes directrices pour la mise en œuvre
des procédures d'assurance qualité
Reference number
©
ISO 2018
© ISO 2018
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ii © ISO 2018 – All rights reserved

Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 General principles of electron probe microanalyser quality assurance (EPMA QA) .6
4.1 Objective . 6
4.2 Selection of challenge materials. 6
4.2.1 General. 6
4.2.2 General characteristics of analysed materials . 6
4.2.3 Specific characteristics of challenge materials . 7
4.3 QA measurement parameters . 7
4.3.1 General. 7
4.3.2 Laboratory environment preparation . 7
4.3.3 Instrument parameters . 8
4.4 Data acquisition .11
4.5 Frequency of QA diagnostic testing .12
5 Test report .12
6 Data analysis and performance tracking .13
6.1 General .13
6.2 Quantitative analysis of the challenge material .13
6.3 Calculation of means and standard deviations .13
6.4 Statistical tests performed on data .13
6.4.1 General.13
6.4.2 Normality test . .14
6.4.3 Variance test .14
Annex A (informative) Examples of challenge materials and reference materials for EPMA
WDS QA .15
Annex B (informative) Distinguishing specimen preparation effects from instrument
malfunction .17
Annex C (informative) Graphical rendering of data and control charting .21
Annex D (informative) Failure modes indicated by test results .26
Bibliography .30
Foreword
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This document was prepared by Technical Committee ISO/TC 202, Microbeam analysis, Subcommittee
SC 2, Electron probe microanalysis.
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iv © ISO 2018 – All rights reserved

Introduction
This document was developed to provide a general method for operators of electron probe
microanalysers (EPMA) to perform the most complete and reliable instrument diagnostic routine
possible in the smallest amount of operator time, instrument time and analysis time. Performing this
procedure on their instruments at regularly scheduled intervals will allow the operator to track the
quality of an instrument’s elemental qualitative and quantitative performance, and alert the operator of
the need for instrument service and calibration shortly after it fails to meet its operating specifications
for measurement uncertainty. With equal application of this document to the diagnostics procedure
of multiple instruments in a single laboratory, or even multiple instruments managed by different
operators in separate laboratories, analysis results can be normalized between instruments using the
performance comparison, facilitating analytical reproducibility.
The chief product of an analytical laboratory quality assurance (QA) program, ultimately, is confidence
– confidence that the analysis of any specimen sent to any laboratory participating in the program
will be consistent, correct within tolerance and interchangeable with equivalent analyses of related
specimens performed by any other laboratory in the program. In order to maximize confidence, the QA
tests and test materials chosen should evaluate the broadest possible range of instrument functionality.
In the context of EPMA, this means testing not only the stability of the electron gun and the function of
the photon counters, but also the functionality of every component of each wavelength spectrometer
mounted to the system. This includes the numerous types of diffracting crystals that disperse the
X-rays, the mechanical components that switch the spectrometer from one crystal to another, and the
drive mechanisms that scan the crystal through a spectral region of interest. Since these spectrometer
components can fail independently of the others, and many such failures will not be noticeable in all
measurements, a complete QA test will include materials that generate X-ray lines that span the range of
any diffracting crystal and methods to properly analyse them. It will therefore generate the maximum
possible information on the instrument’s functional integrity. From this information, instrument
performance can be optimized, thereby obtaining maximum analytical confidence. The procedures and
reference material attributes outlined in this document are designed to achieve these goals.
INTERNATIONAL STANDARD ISO 19463:2018(E)
Microbeam analysis — Electron probe microanalyser
(EPMA) — Guidelines for performing quality assurance
procedures
1 Scope
This document provides guidelines for performing routine diagnostics and quality assurance procedures
on electron probe microanalysers (EPMA). It is intended to be used periodically by an instrument’s
operator to confirm that the instrument is performing optimally, and to aid in troubleshooting if it is
not. It covers the properties of reference materials required and the analysis procedures necessary to
independently test and fully evaluate the functionality of the main components of an EPMA system.
The analytical procedure described herein is distinct from single-element diagnostic procedures, which
can be performed more rapidly. Such procedures are valid for the diffractor position and conditions
under which the test is performed, whereas the procedure described herein is intended to qualify an
instrument’s capabilities for exploratory analysis of unknowns, trace analysis and non-routine work
(such as peak interferences).
This document is applicable to EPMA and other wavelength dispersive spectrometer (WDS) systems in
which elemental identification and quantification are performed by analysis of the energy and intensity
of the characteristic X-ray lines observed in wavelength-dispersed X-ray spectra. It is not directly
applicable to elemental analysis using energy dispersive spectrometry (EDS).
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 3534-2, Statistics — Vocabulary and symbols — Part 2: Applied statistics
ISO 14595, Microbeam analysis — Electron probe microanalysis — Guidelines for the specification of
certified reference materials (CRMs)
ISO 22489, Microbeam analysis — Electron probe microanalysis — Quantitative point analysis for bulk
specimens using wavelength dispersive X-ray spectroscopy
ISO 23833, Microbeam analysis — Electron probe microanalysis (EPMA) — Vocabulary
ISO/IEC Guide 99, International vocabulary of metrology — Basic and general concepts and associated
terms (VIM)
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO/IEC Guide 99, ISO 3534-2,
ISO 23833 and the following apply.
ISO and IEC maintain terminologi
...