Standard Guide for X-Ray Emission Spectrometric Analysis

SIGNIFICANCE AND USE
X-ray fluorescence spectrometry can provide an accurate and precise determination of metallic and many non-metallic elements. 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.
The accuracy of an analysis 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 the best results.
SCOPE
1.1 This guide covers guidelines for developing and describing analytical procedures using a wavelength-dispersive X-ray spectrometer.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 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.

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Historical
Publication Date
14-Jul-2005
Current Stage
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ASTM E1621-05 - Standard Guide for X-Ray Emission Spectrometric Analysis
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: E1621 − 05
StandardGuide for
1
X-Ray Emission Spectrometric Analysis
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 4. Summary of Guide
1.1 This guide covers guidelines for developing and de- 4.1 Thetestspecimenispreparedwithaclean,uniform,flat
scribing analytical procedures using a wavelength-dispersive surface. It may be prepared by grinding, polishing, or lathing a
metalsurfaceorbyfusingorbriquettingapowder.Thissurface
X-ray spectrometer.
is irradiated with a primary source of X rays.The secondary X
1.2 The values stated in SI units are to be regarded as
rays produced in the specimen are dispersed according to their
standard. No other units of measurement are included in this
wavelengthbymeansofcrystalsorsyntheticmultilayers.Their
standard.
intensities are measured by suitable detectors at selected
1.3 This standard does not purport to address all of the
wavelengths and converted to counts by the detector. Concen-
safety concerns, if any, associated with its use. It is the
trations of the elements are determined from the measured
responsibility of the user of this standard to establish appro-
intensities of analyte X-ray lines using analytical curves
priate safety and health practices and determine the applica-
prepared with suitable reference materials. Either a fixed
bility of regulatory limitations prior to use.
multi-channel simultaneous system or a sequential monochro-
mator system may be used to provide determinations of the
2. Referenced Documents
elements.
2
2.1 ASTM Standards:
5. Significance and Use
E135Terminology Relating to Analytical Chemistry for
Metals, Ores, and Related Materials 5.1 X-ray fluorescence spectrometry can provide an accu-
E305Practice for Establishing and Controlling Atomic rate and precise determination of metallic and many non-
Emission Spectrochemical Analytical Curves metallic elements. This guide covers the information that
E1257Guide for Evaluating Grinding Materials Used for shouldbeincludedinanX-rayspectrometricanalyticalmethod
Surface Preparation in Spectrochemical Analysis and provides direction to the analyst for determining the
E1329PracticeforVerificationandUseofControlChartsin optimum conditions needed to achieve acceptable accuracy.
Spectrochemical Analysis
5.2 The accuracy of an analysis is a function of the
E1361Guide for Correction of Interelement Effects in
calibration scheme, the sample preparation, and the sample
X-Ray Spectrometric Analysis
homogeneity. Close attention to all aspects of these areas is
E1601Practice for Conducting an Interlaboratory Study to
necessary to achieve the best results.
Evaluate the Performance of an Analytical Method
6. Interferences
3. Terminology
6.1 Lineoverlaps,eithertotalorpartial,mayoccurforsome
3.1 Definitions—For definitions of terms used in this guide, elements.Fundamentalparameterequationsrequirethatthenet
refer to Terminologies E135 and the terminology section of
intensities be free from line overlap effects. Some empirical
E1361.
schemesincorporatelineoverlapcorrectionsintheirequations.
See Appendix X1 for correction of line overlap effects.
6.2 Interelementeffectsormatrixeffectsmayexistforsome
1
This guide is under the jurisdiction of ASTM Committee E01 on Analytical
elements.An empirical way to compensate for these effects is
ChemistryforMetals,Ores,andRelatedMaterialsandisthedirectresponsibilityof
to prepare a series of calibration curves that cover the desig-
Subcommittee E01.20 on Fundamental Practices.
nated concentration ranges to be analyzed. A large suite of
Current edition approved July 15, 2005. Published August 2005. Originally
carefully designed reference materials is necessary for this
approved in 1994. Last previous edition approved in 1999 as E1621–94(1999).
DOI: 10.1520/E1621-05.
procedure. A series of samples in which all elements are
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
relativelyconstant,exceptfortheanalyte,isnecessaryforeach
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
analyte that can be affected by other elements in the matrix. In
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. addition, several series for the same analyte may be necessary,
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E1621 − 05
if the analyte is subject to large effects from some other assembly that pr
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