ASTM E1621-13

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 and precise 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 analyst for determining the optimum conditions needed to achieve acceptable accuracy.  
5.2 The accuracy of a determination is a function of the calibration scheme, 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 guide 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 solids 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 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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 30-Sep-2013
• ICS: 71.040.50 - Physicochemical methods of analysis
• Technical Committee: E01 - Analytical Chemistry for Metals, Ores, and Related Materials
• Drafting Committee: E01.20 - Fundamental Practices

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: E1621 − 13
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 Spectrochemical Analysis
E1361Guide for Correction of Interelement Effects in
1.1 This guide provides guidelines for developing and
X-Ray Spectrometric Analysis
describinganalyticalproceduresusingawavelengthdispersive
E1601Practice for Conducting an Interlaboratory Study to
X-rayspectrometerforelementalanalysisofsolidmetals,ores,
Evaluate the Performance of an Analytical Method
and related materials. Material forms discussed herein include
E2857Guide for Validating Analytical Methods
solids, powders, and solid forms prepared by chemical and
physical processes such as borate fusion and pressing of
3. Terminology
briquettes.
3.1 Definitions—For definitions of terms used in this guide,
1.2 Liquids are not discussed in this guide because they are
refer to Terminologies E135 and the terminology section of
much less frequently encountered in metals and mining labo-
E1361.
ratories. However, aqueous liquids can be processed by borate
fusiontocreatesolidsspecimens,andX-rayspectrometerscan
4. Summary of Guide
be equipped to handle liquids directly.
4.1 Important aspects of test equipment for wavelength
1.3 Some provisions of this guide may be applicable to the
dispersive X-ray fluorescence spectrometry are discussed in-
use of an energy dispersive X-ray spectrometer.
cluding equipment components and accessories, reagents, and
materials.KeyaspectsoftheapplicationofX-rayspectrometry
1.4 The values stated in SI units are to be regarded as
to materials analysis are discussed including interferences and
standard. No other units of measurement are included in this
correction options, specimen preparation by a variety of
standard.
procedures, and materials and accessories for presentation of
1.5 This standard does not purport to address all of the
specimens for measurement in spectrometers. Key elements of
safety concerns, if any, associated with its use. It is the
measurement procedures, calibrations procedures, and result
responsibility of the user of this standard to establish appro-
reporting are explained.
priate safety and health practices and determine the applica-
4.2 InanX-rayspectrometrictestmethod,thetestspecimen
bility of regulatory limitations prior to use.
is prepared with a clean, uniform, flat surface. It may be
2. Referenced Documents prepared by grinding, polishing, or lathing a metal surface or
2 by fusing or briquetting a powder. This surface is irradiated
2.1 ASTM Standards:
with a primary source of X-rays. The secondary X-rays
E135Terminology Relating to Analytical Chemistry for
produced in the specimen are dispersed according to their
Metals, Ores, and Related Materials
wavelengthbymeansofcrystalsorsyntheticmultilayers.Their
E1257Guide for Evaluating Grinding Materials Used for
count rates at selected wavelengths, hereinafter called
Surface Preparation in Spectrochemical Analysis
intensities, are measured by suitable detector systems.
E1329PracticeforVerificationandUseofControlChartsin
Amounts of the elements are determined from the measured
intensities using analytical curves prepared with suitable cali-
brants.
1
This guide is under the jurisdiction of ASTM Committee E01 on Analytical
ChemistryforMetals,Ores,andRelatedMaterialsandisthedirectresponsibilityof
4.3 Importantaspectsofbackgroundestimationarecovered
Subcommittee E01.20 on Fundamental Practices.
in an appendix to the guide.
Current edition approved Oct. 1, 2013. Published November 2013. Originally
approved in 1994. Last previous edition approved in 2005 as E1621–05. DOI:
5. Significance and Use
10.1520/E1621-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
5.1 X-ray fluorescence spectrometry can provide an accu-
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
rate and precise determination of metallic and many non-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. metallic elements in a wide variety of solid and liquid
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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E1621 − 13
sate for these effects. Reference materials that were not used in the
materials. This guide covers the information that should be
calibration should be analyzed as unknowns to verify the calibration.
included
...

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 − 05 E1621 − 13
Standard Guide for
X-Ray Emission Spectrometric AnalysisElemental Analysis
by Wavelength Dispersive X-Ray Fluorescence
1
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 guide coversprovides guidelines for developing and describing analytical procedures using a wavelength-dispersive
X-ray spectrometer. 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 solids 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 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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
E305 Practice for Establishing and Controlling Atomic Emission Spectrochemical Analytical Curves
E1257 Guide for Evaluating Grinding Materials Used for Surface Preparation in Spectrochemical Analysis
E1329 Practice for Verification and Use of Control Charts in Spectrochemical Analysis
E1361 Guide for Correction of Interelement Effects in X-Ray Spectrometric Analysis
E1601 Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Method
E2857 Guide for Validating Analytical Methods
3. Terminology
3.1 Definitions—For definitions of terms used in this guide, refer to Terminologies E135 and the terminology section of 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, calibrations procedures, and result reporting are explained.
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 July 15, 2005Oct. 1, 2013. Published August 2005November 2013. Originally approved in 1994. Last previous edition approved in 19992005
as E1621 – 94 (1999).E1621 – 05. DOI: 10.1520/E1621-05.10.1520/E1621-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
E1621 − 13
4.2 The test In an X-ray spectrometric test method, the test specimen is prepared with a clean, uniform, flat surface. It may be
prepared by grinding, polishing, or lathing a metal surface or by fusing or briquetting a powder. This surface is irradiated with a
primary source of X rays. X-rays. The secondary X rays X-rays produced in the specimen are dispersed according to their
wavelength by means of crystals or synthetic multilayers. Their intensities count rates at selected wavelengths, hereinafter called
intensities, are measured by
...