Standard Practice for Testing Homogeneity of a Metal Lot or Batch in Solid Form by Spark Atomic Emission Spectrometry

SIGNIFICANCE AND USE
The purpose of this practice is to evaluate the homogeneity of a lot of material selected as a candidate for development as a reference material or certified reference material, or for a L/B selected for some other purpose (see Appendix X1-Appendix X4 for examples).
This practice is applicable to the testing of samples taken at various stages during production. For example, continuous cast materials, ingots, rolled bars, wire, etc., could be sampled at various stages during the production process and tested.
SCOPE
1.1 This practice is suitable for testing the homogeneity of a metal lot or batch (L/B) in solid form by spark atomic emission spectrometry (Spark-AES). It is compliant with ISO Guide 35—Certification of Reference Materials: General and Statistical Principles. It is primarily intended for use in the development of reference materials but may be used in any other application where a L/B is to be tested for homogeneity. It is designed to provide a combined study of within-unit and between-unit homogeneity of such a L/B.
1.2 This practice is designed primarily to test for elemental homogeneity of a metal L/B by Spark-AES. However, it can be adapted for use with other instrumental techniques such as X-ray fluorescence spectrometry (XRF) or atomic absorption spectrometry (AAS).
Note 1—This practice is not limited to elemental analysis or techniques. This practice can be applied to any property that can be measured, for example, the property of hardness as measured by the Rockwell technique.
1.3 The criteria for acceptance of the test specimens must be previously determined. That is, the maximum acceptable level of heterogeneity must be determined on the basis of the intended use of the L/B.
1.4 It is assumed that the analyst is trained in Spark-AES techniques including the specimen preparation procedures needed to make specimens ready for measurements. It is further assumed that the analyst is versed in and has access to computer-based data capture and analysis. The methodology of this practice is best utilized in a computer based spreadsheet.
1.5 This practice can be applied to one or more elements in a specimen provided the signal-to-background ratio is not a limiting factor.
1.6 This practice includes methods to correct for systematic drift of the instrument with time. (Warning—If drift occurs, erroneous conclusions will be obtained from the data analysis.)
1.7 This practice also includes methods to refine estimates of composition and uncertainty through the use of a type standard or multiple calibrants.
1.8 It further provides a means of reducing a nonhomogeneous set to a homogeneous subset.
1.9 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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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: E826 − 08
StandardPractice for
Testing Homogeneity of a Metal Lot or Batch in Solid Form
1
by Spark Atomic Emission Spectrometry
This standard is issued under the fixed designation E826; 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 1.7 This practice also includes methods to refine estimates
of composition and uncertainty through the use of a type
1.1 Thispracticeissuitablefortestingthehomogeneityofa
standard or multiple calibrants.
metallotorbatch(L/B)insolidformbysparkatomicemission
spectrometry (Spark-AES). It is compliant with ISO Guide
1.8 It further provides a means of reducing a nonhomoge-
35—Certification of Reference Materials: General and Statis-
neous set to a homogeneous subset.
tical Principles. It is primarily intended for use in the devel-
1.9 This standard does not purport to address all of the
opment of reference materials but may be used in any other
safety concerns, if any, associated with its use. It is the
application where a L/B is to be tested for homogeneity. It is
responsibility of the user of this standard to establish appro-
designed to provide a combined study of within-unit and
priate safety and health practices and determine the applica-
between-unit homogeneity of such a L/B.
bility of regulatory limitations prior to use.
1.2 This practice is designed primarily to test for elemental
homogeneityofametalL/BbySpark-AES.However,itcanbe
2. Referenced Documents
adapted for use with other instrumental techniques such as
2
X-ray fluorescence spectrometry (XRF) or atomic absorption
2.1 ASTM Standards:
spectrometry (AAS).
E135Terminology Relating to Analytical Chemistry for
NOTE 1—This practice is not limited to elemental analysis or tech-
Metals, Ores, and Related Materials
niques.Thispracticecanbeappliedtoanypropertythatcanbemeasured,
E177Practice for Use of the Terms Precision and Bias in
for example, the property of hardness as measured by the Rockwell
technique. ASTM Test Methods
E178Practice for Dealing With Outlying Observations
1.3 Thecriteriaforacceptanceofthetestspecimensmustbe
E634Practice for Sampling of Zinc and Zinc Alloys by
previously determined. That is, the maximum acceptable level
Spark Atomic Emission Spectrometry
of heterogeneity must be determined on the basis of the
E716Practices for Sampling and Sample Preparation of
intended use of the L/B.
Aluminum and Aluminum Alloys for Determination of
1.4 It is assumed that the analyst is trained in Spark-AES
Chemical Composition by Spectrochemical Analysis
techniques including the specimen preparation procedures
E1329PracticeforVerificationandUseofControlChartsin
needed to make specimens ready for measurements. It is
Spectrochemical Analysis
further assumed that the analyst is versed in and has access to
E1601Practice for Conducting an Interlaboratory Study to
computer-baseddatacaptureandanalysis.Themethodologyof
Evaluate the Performance of an Analytical Method
this practice is best utilized in a computer based spreadsheet.
E1806Practice for Sampling Steel and Iron for Determina-
1.5 This practice can be applied to one or more elements in
tion of Chemical Composition
a specimen provided the signal-to-background ratio is not a
3
2.2 ISO Standard:
limiting factor.
ISO Guide 35Certification of Reference Materials: General
1.6 This practice includes methods to correct for systematic
and Statistical Principles
drift of the instrument with time. (Warning—If drift occurs,
erroneousconclusionswillbeobtainedfromthedataanalysis.)
1 2
This practice is under the jurisdiction ofASTM Committee E01 on Analytical For referenced ASTM standards, visit the ASTM website, www.astm.org, or
ChemistryforMetals,Ores,andRelatedMaterialsandisthedirectresponsibilityof contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Subcommittee E01.22 on Laboratory Quality. Standardsvolumeinformation,refertothestandard’sDocumentSummarypageon
Current edition approved May 1, 2008. Published June 2008. Originally the ASTM website.
ϵ1 3
approved in 1981. Last previous edition approved in 1996 as E826–81(1996) , Available from International Organization for Standardization (ISO), 1, ch. de
whichwaswithdrawnApril2004andreinstatedinMay2008.DOI:10.1520/E0826- la Voie-Creuse, Case postale 56, CH-1211, Geneva 20, Switzerland, http://
08. www.iso.ch.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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E826 − 08
3. Terminology 4.4 This practice requires that there be an absence of
outliers in the data (Pra
...

This document is not anASTM standard and is intended only to provide the user of anASTM 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.
e1
Designation:E826–85 (Reapproved 1996) Designation: E 826 – 08
Standard Practice for
Testing Homogeneity of Materials for Development of
Reference MaterialsTesting Homogeneity of a Metal Lot or
Batch in Solid Form by Spark Atomic Emission
1
Spectrometry
This standard is issued under the fixed designation E826; 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
e NOTE—Section 12 was added editorially in June 1996.
1. Scope
1.1This practice is suitable for testing the homogeneity of metals, either in solid or powdered form, and finely ground oxide
materials that are intended for use as reference materials in X-ray emission, or optical emission spectroscopy, or both.The criteria
for acceptance of the test specimens as reference materials, however, must be previously determined by the user for meeting his
specific requirements.
1.2TheprocedureisdesignedprimarilyfortestingspecimensbyX-rayemissionspectrometryoropticalemissionspectroscopy,
or both. However, the practice could be easily adapted for use with other instrumental techniques such as atomic absorption
spectrophotometry.
1.3Thisprocedurecanbeappliedtooneormoreelementsinaspecimenprovidedthesignal-to-backgroundratioisnotalimiting
factor.
1.4This practice includes one method, if desired, to correct for systematic or periodic (sinusoidal) drift in the instrument with
time through the use of a control reference material.
1.1 This practice is suitable for testing the homogeneity of a metal lot or batch (L/B) in solid form by spark atomic emission
spectrometry (Spark-AES). It is compliant with ISO Guide 35—Certification of Reference Materials: General and Statistical
Principles.Itisprimarilyintendedforuseinthedevelopmentofreferencematerialsbutmaybeusedinanyotherapplicationwhere
a L/B is to be tested for homogeneity. It is designed to provide a combined study of within-unit and between-unit homogeneity
of such a L/B.
1.2 This practice is designed primarily to test for elemental homogeneity of a metal L/B by Spark-AES. However, it can be
adapted for use with other instrumental techniques such as X-ray fluorescence spectrometry (XRF) or atomic absorption
spectrometry (AAS).
NOTE1—Caution: If serious drift occurs (for example, unstable power supply, X-ray tube, etc.) erroneous conclusions may be obtained from the data
analysis.
1.5 1—This practice is not limited to elemental analysis or techniques. This practice can be applied to any property that can
be measured, for example, the property of hardness as measured by the Rockwell technique.
1.3 The criteria for acceptance of the test specimens must be previously determined. That is, the maximum acceptable level of
heterogeneity must be determined on the basis of the intended use of the L/B.
1.4 It is assumed that the analyst is trained in Spark-AES techniques including the specimen preparation procedures needed to
make specimens ready for measurements. It is further assumed that the analyst is versed in and has access to computer-based data
capture and analysis. The methodology of this practice is best utilized in a computer based spreadsheet.
1.5 Thispracticecanbeappliedtooneormoreelementsinaspecimenprovidedthesignal-to-backgroundratioisnotalimiting
factor.
1.6 This practice includes methods to correct for systematic drift of the instrument with time. (Warning—If drift occurs,
erroneous conclusions will be obtained from the data analysis.)
1
This practice is under the jurisdiction of ASTM Committee E-1 on Analytical Chemistry for Metals, Ores and Related Materials and is the direct responsibility of
Subcommittee E01.22 on Statistics and Quality Control.
Current edition approved June 28, 1985. Published October 1985. Originally published as E826–81. Last previous edition E826–81.
1
This practice is under the jurisdiction of ASTM Committee E01 on Analytical Chemistry for Metals, Ores and Related Materials and is the direct responsibility of
Subcommittee E01.22 on Laboratory Quality.
´1
Current edition approved May 1, 2008. Published June 2008. Originally approved in 1981. Last previous edition approved in 1996 as E826–81(1996) , which was
withdrawn April 2004 and reinstated in May 2008.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

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