Standard Guide for Elemental Analysis by Wavelength Dispersive X-Ray Fluorescence Spectrometry

SIGNIFICANCE AND USE
5.1 X-ray fluorescence spectrometry can provide an accurate determination of metallic and many non-metallic elements in a wide variety of solid and liquid materials. This guide covers the information that should be included in an X-ray spectrometric analytical method and provides direction to the user for determining the optimum conditions needed to achieve acceptable accuracy.  
5.2 The accuracy of a determination is a function of the calibration algorithm, the sample preparation, and the sample homogeneity. Close attention to all aspects of these areas is necessary to achieve acceptable results.  
5.3 All concepts discussed in this guide are explored in detail in a number of published texts and in the scientific literature.
SCOPE
1.1 This standard provides guidelines for developing and describing analytical procedures using a wavelength dispersive X-ray spectrometer for elemental analysis of solid metals, ores, and related materials. Material forms discussed herein include solids, powders, and solid forms prepared by chemical and physical processes such as borate fusion and pressing of briquettes.  
1.2 Liquids are not discussed in this guide because they are much less frequently encountered in metals and mining laboratories. However, aqueous liquids can be processed by borate fusion to create solid specimens, and X-ray spectrometers can be equipped to handle liquids directly.  
1.3 Some provisions of this guide may be applicable to the use of an energy dispersive X-ray spectrometer.  
1.4 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

Status
Published
Publication Date
14-Jun-2022
Current Stage
Ref Project

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: E1621 − 22
Standard Guide for
Elemental Analysis by Wavelength Dispersive X-Ray
1
Fluorescence Spectrometry
This standard is issued under the fixed designation E1621; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
2
2.1 ASTM Standards:
1.1 This standard provides guidelines for developing and
E135Terminology Relating to Analytical Chemistry for
describinganalyticalproceduresusingawavelengthdispersive
Metals, Ores, and Related Materials
X-rayspectrometerforelementalanalysisofsolidmetals,ores,
E1257Guide for Evaluating Grinding Materials Used for
and related materials. Material forms discussed herein include
Surface Preparation in Spectrochemical Analysis
solids, powders, and solid forms prepared by chemical and
E1329Practice forVerification and Use of Control Charts in
physical processes such as borate fusion and pressing of
3
Spectrochemical Analysis (Withdrawn 2019)
briquettes.
E1361Guide for Correction of Interelement Effects in
1.2 Liquids are not discussed in this guide because they are X-Ray Spectrometric Analysis
much less frequently encountered in metals and mining labo- E2857Guide for Validating Analytical Methods
E2972Guide for Production,Testing, andValueAssignment
ratories. However, aqueous liquids can be processed by borate
fusion to create solid specimens, and X-ray spectrometers can of In-House Reference Materials for Metals, Ores, and
Other Related Materials
be equipped to handle liquids directly.
4
2.2 ISO Standard:
1.3 Some provisions of this guide may be applicable to the
ISO17034:2016GeneralRequirementsfortheCompetence
use of an energy dispersive X-ray spectrometer.
of Reference Material Producers
1.4 Units—The values stated in SI units are to be regarded
asstandard.Nootherunitsofmeasurementareincludedinthis
3. Terminology
standard.
3.1 Definitions—For definitions of terms used in this guide,
refer to Terminology E135 and the terminology section of
1.5 This standard does not purport to address all of the
Guide E1361.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Guide
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
4.1 Important aspects of test equipment for wavelength
1.6 This international standard was developed in accor- dispersive X-ray fluorescence spectrometry are discussed in-
dance with internationally recognized principles on standard- cluding equipment components and accessories, reagents, and
ization established in the Decision on Principles for the materials.KeyaspectsoftheapplicationofX-rayspectrometry
to materials analysis are discussed including interferences and
Development of International Standards, Guides and Recom-
correction options, specimen preparation by a variety of
mendations issued by the World Trade Organization Technical
procedures, and materials and accessories for presentation of
Barriers to Trade (TBT) Committee.
specimens for measurement in spectrometers. Key elements of
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
1
This guide is under the jurisdiction of ASTM Committee E01 on Analytical the ASTM website.
3
ChemistryforMetals,Ores,andRelatedMaterialsandisthedirectresponsibilityof The last approved version of this historical standard is referenced on
Subcommittee E01.20 on Fundamental Practices. www.astm.org.
4
Current edition approved June 15, 2022. Published July 2022. Originally Available from International Organization for Standardization (ISO), ISO
approved in 1994. Last previous edition approved in 2021 as E1621–21. DOI: Central Secretariat, Chemin de Blandonnet 8, CP 401, 1214 Vernier, Geneva,
10.1520/E1621-22. Switzerland, https://www.iso.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
E1621 − 22
measurement procedures, calibration procedures, and result when the compositions of the calibrants used to prepare the
reporting are explained. calibrations are similar to the compositions of materials being
analyzed. This approach requires many more reference mate-
4.2 InanX-ray
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: E1621 − 21 E1621 − 22
Standard Guide for
Elemental Analysis by Wavelength Dispersive X-Ray
1
Fluorescence Spectrometry
This standard is issued under the fixed designation E1621; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This guidestandard provides guidelines for developing and describing analytical procedures using a wavelength dispersive
X-ray spectrometer for elemental analysis of solid metals, ores, and related materials. Material forms discussed herein include
solids, powders, and solid forms prepared by chemical and physical processes such as borate fusion and pressing of briquettes.
1.2 Liquids are not discussed in this guide because they are much less frequently encountered in metals and mining laboratories.
However, aqueous liquids can be processed by borate fusion to create solid specimens, and X-ray spectrometers can be equipped
to handle liquids directly.
1.3 Some provisions of this guide may be applicable to the use of an energy dispersive X-ray spectrometer.
1.4 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this
standard.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of
regulatory limitations prior to use.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2
2.1 ASTM Standards:
E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
E1257 Guide for Evaluating Grinding Materials Used for Surface Preparation in Spectrochemical Analysis
3
E1329 Practice for Verification and Use of Control Charts in Spectrochemical Analysis (Withdrawn 2019)
E1361 Guide for Correction of Interelement Effects in X-Ray Spectrometric Analysis
E2857 Guide for Validating Analytical Methods
1
This guide is under the jurisdiction of ASTM Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials and is the direct responsibility of
Subcommittee E01.20 on Fundamental Practices.
Current edition approved May 15, 2021June 15, 2022. Published June 2021July 2022. Originally approved in 1994. Last previous edition approved in 20132021 as
E1621 – 13.E1621 – 21. DOI: 10.1520/E1621-21.10.1520/E1621-22.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
The last approved version of this historical standard is referenced on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
E1621 − 22
E2972 Guide for Production, Testing, and Value Assignment of In-House Reference Materials for Metals, Ores, and Other
Related Materials
4
2.2 ISO Standard:
ISO 17034: 2016 General Requirements for the Competence of Reference Material Producers
3. Terminology
3.1 Definitions—For definitions of terms used in this guide, refer to TerminologiesTerminology E135 and the terminology
section of Guide E1361.
4. Summary of Guide
4.1 Important aspects of test equipment for wavelength dispersive X-ray fluorescence spectrometry are discussed including
equipment components and accessories, reagents, and materials. Key aspects of the application of X-ray spectrometry to materials
analysis are discussed including interferences and correction options, specimen preparation by a variety of procedures, and
materials and accessories for presentation of specimens for measurement in spectrometers. Key elements of measurement
procedures, calibrationscalibration procedures, and result reporting are explained.
4.2 In an X-ray spectrometric test method, the test specimen is prepared with a clean, uniform, flat surface. It
...

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