SIST-TP CEN/TR 10377:2023
(Main)Guidelines for the preparation of standard routine methods with wavelength-dispersive X-ray fluorescence spectrometry
Guidelines for the preparation of standard routine methods with wavelength-dispersive X-ray fluorescence spectrometry
X-ray Fluorescence Spectrometry (XRF) has been used for several decades as an important analytical tool for production analysis. XRF is characterised by its speed and high precision over a wide concentration range and since the technique in most cases is used as an relative method the limitations are often connected to the quality of the calibration samples. The technique is well established and most of its physical properties are well known.
Lignes directrices pour la préparation de méthodes de routine utilisant la spectrométrie de fluorescence X à dispersion de longueur d'onde
Le présent document est destiné à être utilisé pour l'analyse des métaux et des alliages (principalement les aciers), mais il est également applicable à d'autres matériaux bien que les techniques de préparation des échantillons soient diffèrentes. L'objet du présent document est de décrire les concepts et les modes opératoires généraux pour l'étalonnage et l'analyse par XRF.
Navodilo za pripravo standardnih postopkov z valovno-disperzno rentgensko fluorescenčno spektrometrijo
Fluorescenčna spektrometrija (XRF) se že več desetletij uporablja kot pomembno analitično orodje za analizo proizvodnje. Za fluorescenčno spektrometrijo je značilno, da je z njo mogoče hitro in zelo natančno analizirati širok razpon koncentracij. Ker se ta tehnika večinoma uporablja kot relativna metoda, so njene omejitve pogosto povezane s kakovostjo vzorcev za umerjanje. Ta tehnika je dobro uveljavljena, večina njenih fizičnih lastnosti pa je dobro znana.
General Information
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Standards Content (Sample)
SLOVENSKI STANDARD
01-september-2023
Navodilo za pripravo standardnih postopkov z valovno-disperzno rentgensko
fluorescenčno spektrometrijo
Guidelines for the preparation of standard routine methods with wavelength-dispersive
X-ray fluorescence spectrometry
Ta slovenski standard je istoveten z: CEN/TR 10377:2023
ICS:
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
77.040.30 Kemijska analiza kovin Chemical analysis of metals
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
CEN/TR 10377
TECHNICAL REPORT
RAPPORT TECHNIQUE
June 2023
TECHNISCHER REPORT
ICS 77.040.30 Supersedes CR 10299:1998
English Version
Guidelines for the preparation of standard routine
methods with wavelength-dispersive X-ray fluorescence
spectrometry
This Technical Report was approved by CEN on 12 June 2023. It has been drawn up by the Technical Committee CEN/TC 459/SC
2.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2023 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TR 10377:2023 E
worldwide for CEN national Members.
Contents Page
European foreword . 4
Introduction . 5
1 Scope . 6
2 Normative references . 6
3 Terms and definitions . 6
4 Principle . 8
5 Instruments. 8
5.1 General. 8
5.2 Tubes . 9
5.3 Vacuum system . 10
5.4 Sample spinner . 10
5.5 Filters . 10
5.6 Collimators . 10
5.7 Crystals . 11
5.8 Detectors . 11
5.9 Sequential- simultaneous instruments . 12
6 Sampling and sample preparation . 12
7 Evaluation methods . 13
7.1 Dead time correction . 13
7.2 Background correction . 13
7.3 Line interference, correction models . 13
7.4 Inter-element effects, correction models . 14
8 Calibration strategy . 15
8.1 General. 15
8.2 Optimizing 2Θ . 15
8.3 Selecting the optimum conditions for detectors . 15
8.4 Selecting the optimum tube voltage and current . 15
8.5 Selecting the minimum measuring times . 15
8.6 Selecting the calibration samples . 15
8.7 Selecting the recalibration samples . 16
8.8 Measuring of calibration samples . 16
8.9 Regression calculations . 16
9 Validation of method (trueness and precision) . 17
10 Performance criteria . 17
10.1 General. 17
10.2 Checking the precision . 17
10.3 Performance monitoring . 17
10.4 Maintenance . 18
11 Radiation protection . 18
Annex A (informative) Example of assessment of Sensitivity (S), Background Equivalent
Concentration (BEC), Background (Bg), Limit of Detection (LOD), Limit of
Quantification (LOQ) and Lower Limit of Detection (LLD) . 19
Annex B (informative) Example of an assessment of line interference . 21
Annex C (informative) Example of performance criteria obtained under repeatability
conditions . 22
Bibliography . 23
European foreword
This document (CEN/TR 10377:2023) has been prepared by Technical Committee CEN/TC 459/SC 2
“Methods of chemical analysis for iron and steel”, the secretariat of which is held by SIS.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes CR 10299:1999.
In comparison with the previous edition, the following modifications have been made:
— Conversion of the document from a CEN Report (CR) to a Technical Report (TR);
— Title: reworded;
— Clause 1, “Purpose of the guideline” split in “Introduction” and “Scope”;
— Definition 3.3, deleted;
— Definition 3.4, deleted;
— Definition 3.9, updated;
— Definition 3.10, updated;
— Definition 3.11, updated;
— Definition 3.12, updated;
— Renumbering of Clauses 2, 4, 5, 6, 7, 8, 9 and 10;
— Annex A updated and became “Bibliography”;
— Annex B, became Annex A;
— Annex C, became Annex B;
— Annex D, became Annex C;
— Annex E, withdrawn.
Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.
Introduction
X-ray Fluorescence Spectrometry (XRF) has been used for several decades as an important analytical
tool for routine analysis. XRF is characterized by its speed and high precision over wide content ranges.
Since the technique in most cases is used as a relative method, its limitations are often connected to
the quality of the calibration samples.
The technique is well established and most of its physical properties are well known.
1 Scope
This document is intended to be used for the analysis of metals and alloys (namely steels), but it can
also be applicable to other materials although the sample preparation techniques differ. The purpose
of this document is to describe general concepts and the procedures for calibration and analysis by
XRF.
2 Normative references
There are no normative references in this document.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
• IEC Electropedia: available at https://www.electropedia.org/
• ISO Online browsing platform: available at https://www.iso.org/obp
3.1
calibration
calculation of the best fit of net intensities and contents from a number of calibration samples to a
calibration curve
3.2
recalibration
calculation of new calibration constants with a few number of samples, selected from the calibration
samples
Note 1 to entry: Calibration samples using the apparent contents calculated in 3.1
Note 2 to entry: To compensate for the day-to-day variations of the instrument a set of recalibration samples is
measured; either one with a low and one with a high content for each element (two-point recalibration) or one
with a high content only for each element (one-point recalibration). The intensities are compared to the initial
intensities recorded during the calibration procedure and recalibration coefficients are calculated. Calibration
constants are not changed.
3.3
background equivalent concentration
BEC
quantity of analyte which, when subjected to excitation, provides a net intensity equal to the spectral
background
3.4
limit of detection
LOD
minimum content at which the signal generated by a given element can be positively recognised above
any background signals with a specified degree of certainty
3.5
lower limit of detection
LLD
minimum content at which the signal generated by a given element can be positively recognised above
any background signals with a specified degree of certainty
Note 1 to entry: The related calculations are based only on the counting statistical error
3.7
limit of quantification
LOQ
smallest content that can be determined with a specified degree of certainty
3.8
repeatability conditions
conditions where independent test results are obtained with the same method on identical test items
in the same laboratory by the same operator using the same equipment within short intervals of time
[SOURCE: ISO 5725-1:1994]
3.9
reproducibility conditions
conditions where test results are obtained with the same method on identical test items in different
laboratories with different operators using different equipment
[SOURCE: ISO 5725-1:1994]
3.10
accuracy
closeness of agreement between test result and accepted reference value
Note 1 to entry: The term accuracy, when applied to a set of test results, involves a combination of random
components and a common systematic error or bias component.
[SOURCE: ISO 5725-1:1994]
3.11
trueness
closeness of agreement between the average value obtained from a large series of test results and an
accepted reference value
Note 1 to entry: The measure of trueness is usually expressed in terms of bias.
Note 2 to entry: Trueness has been referred to as “accuracy of the mean”. This usage is not recommended.
[SOURCE: ISO 5725-1:1994]
3.12
sensitivity, S
difference in intensities between a sample with a high content and one with a low content divided by
the difference in content
Note 1 to entry: Sensitivity is expressed as counts per second per percent.
4 Principle
The sample is prepared to a clean uniform surface and then irradiated by an X-ray beam of high energy.
The secondary X-rays produced are dispersed by means of crystals and the intensities are measured
by detectors at selected characteristic wavelengths. The measuring time is set to reach below a
specified statistical counting error.
Contents of the elements are calculated by relating the measured i
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