ASTM E3063-17
(Test Method)Test Method for Antimony Content Using Neutron Activation Analysis (NAA)
Test Method for Antimony Content Using Neutron Activation Analysis (NAA)
SIGNIFICANCE AND USE
5.1 High levels of antimony are commonly used in flame retardant formulations for various materials. NAA is a test method that can be useful for verifying these levels and, for other materials, NAA can also be useful in establishing the amount of low level contamination, if any, with high sensitivity and high precision.
5.2 Neutron activation analysis provides a rapid, highly sensitive, nondestructive procedure for antimony determination in a wide range of matrices. This test method is independent of the chemical form of the antimony.
5.3 This test method can be used for quality and process control in the petrochemical and other manufacturing industries, and for research purposes in a broad spectrum of applications.
SCOPE
1.1 This test method covers the measurement of antimony concentration in plastics or other hydrocarbon or organic matrix by using neutron activation analysis (NAA). The sample is activated by irradiation with neutrons from a research reactor and the subsequently emitted gamma-rays are detected with a germanium semiconductor detector. The same system may be used to determine antimony concentrations ranging from 1 ng/g to 10 000 μg/g with the lower end of the range limited by numerous interferences and the upper limit established by the demonstrated practical application of NAA.
1.2 This test method may be used on either solid or liquid samples, provided that they can be made to conform in size and shape during irradiation and counting to a standard sample of known antimony content using very simple sample preparation. Several variants of this method have been described in the technical literature. A monograph is available which provides a comprehensive description of the principles of neutron activation analysis using reactor neutrons (1).2
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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. Specific precautions are given in Section 9.
1.5 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.
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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: E3063 − 17
Standard Test Method for
1
Antimony Content Using Neutron Activation Analysis (NAA)
This standard is issued under the fixed designation E3063; 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
3
1.1 This test method covers the measurement of antimony 2.1 ASTM Standards:
concentration in plastics or other hydrocarbon or organic E170Terminology Relating to Radiation Measurements and
Dosimetry
matrix by using neutron activation analysis (NAA). The
sampleisactivatedbyirradiationwithneutronsfromaresearch E177Practice for Use of the Terms Precision and Bias in
ASTM Test Methods
reactor and the subsequently emitted gamma-rays are detected
with a germanium semiconductor detector. The same system E691Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
may be used to determine antimony concentrations ranging
4
from 1 ng/g to 10 000 µg/g with the lower end of the range
2.2 U.S. Government Document:
limited by numerous interferences and the upper limit estab-
Code of Federal Regulations, Title 10, Part 20
lished by the demonstrated practical application of NAA.
2.3 Joint Committee for Guides in Metrology (JCGM)
5
1.2 This test method may be used on either solid or liquid
Reports:
samples,providedthattheycanbemadetoconforminsizeand
JCGM 100:2008, GUM 1995, with minor corrections,
shape during irradiation and counting to a standard sample of
Evaluationofmeasurementdata—Guidetotheexpression
known antimony content using very simple sample prepara-
of uncertainty in measurement
tion.Severalvariantsofthismethodhavebeendescribedinthe
technicalliterature.Amonographisavailablewhichprovidesa
3. Terminology
comprehensive description of the principles of neutron activa-
2 3.1 Definitions: See also Terminology E170.
tion analysis using reactor neutrons (1).
3.1.1 comparator standard—a reference standard of known
1.3 The values stated in SI units are to be regarded as
antimony content whose specific activation and counting
−1
standard. No other units of measurement are included in this
sensitivity (counts (mg of antimony) ) may be used to
standard.
quantify the antimony content of a sample irradiated and
1.4 This standard does not purport to address all of the counted under the same conditions. Often, a comparator
safety concerns, if any, associated with its use. It is the standard is selected to have a matrix composition, physical
responsibility of the user of this standard to establish appro- size, density and shape very similar to the corresponding
priate safety, health, and environmental practices and deter- parameters of the sample to be analyzed. Differences in size,
mine the applicability of regulatory limitations prior to use. density, shape and matrix composition between sample and
Specific precautions are given in Section 9. standard may be corrected for using physical or empirical
1.5 This international standard was developed in accor- models.
dance with internationally recognized principles on standard-
3.1.2 gamma-ray spectrometer—a system comprising a de-
ization established in the Decision on Principles for the
tector which detects individual gamma-rays and converts their
Development of International Standards, Guides and Recom-
energyintoanelectronicpulsewhosevoltageisproportionalto
mendations issued by the World Trade Organization Technical
the energy deposited in the detector, and a multichannel
Barriers to Trade (TBT) Committee.
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
1
ThistestmethodisunderthejurisdictionofASTMCommitteeE10onNuclear contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Technology and Applications and is the direct responsibility of Subcommittee Standards volume information, refer to the standard’s Document Summary page on
E10.05 on Nuclear Radiation Metrology. the ASTM website.
4
Current edition approved Nov. 1, 2017. Published November 2017. Originally Available from the Superintendent of Documents, U.S. Government Printing
approved in 2016. Last previous edition approved in 2016 as E3063-16. DOI: Office, Washington, DC 20402.
5
10.1520/E3063-17. Document produced by Working Groups of the Joint Committee for Guides in
2
The boldface numbers in parentheses refer to a list of references at the end of Metrology (JCGM). Available free of charge at BIPM website (http://
this standard. www.bipm.or
...
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: E3063 − 16 E3063 − 17
Test Method for
1
Antimony Content Using Neutron Activation Analysis (NAA)
This standard is issued under the fixed designation E3063; 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 test method covers the measurement of antimony concentration in plastics or other hydrocarbon or organic matrix by
using neutron activation analysis (NAA). The sample is activated by irradiation with neutrons from a research reactor and the
subsequently emitted gamma-rays are detected with a germanium semiconductor detector. The same system may be used to
determine antimony concentrations ranging from 1 ng/g to 10 000 μg/g with the lower end of the range limited by numerous
interferences and the upper limit established by the demonstrated practical application of NAA.
1.2 This test method may be used on either solid or liquid samples, provided that they can be made to conform in size and shape
during irradiation and counting to a standard sample of known antimony content using very simple sample preparation. Several
variants of this method have been described in the technical literature. A monograph is available which provides a comprehensive
2
description of the principles of neutron activation analysis using reactor neutrons (1).
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. Specific precautions are given in Section 9.
1.5 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
3
2.1 ASTM Standards:
E170 Terminology Relating to Radiation Measurements and Dosimetry
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
4
2.2 U.S. Government Document:
Code of Federal Regulations, Title 10, Part 20
5
2.3 Joint Committee for Guides in Metrology (JCGM) Reports:
JCGM 100:2008, GUM 1995 , with minor corrections, Evaluation of measurement data—Guide to the expression of uncertainty
in measurement
3. Terminology
3.1 Definitions: See also Terminology E170.
3.1.1 comparator standard—a reference standard of known antimony content whose specific activation and counting sensitivity
−1
(counts (mg of antimony) ) may be used to quantify the antimony content of a sample irradiated and counted under the same
conditions. Often, a comparator standard is selected to have a matrix composition, physical size, density and shape very similar
1
This test method is under the jurisdiction of ASTM Committee E10 on Nuclear Technology and Applications and is the direct responsibility of Subcommittee E10.05
on Nuclear Radiation Metrology.
Current edition approved Oct. 1, 2016Nov. 1, 2017. Published October 2016November 2017. Originally approved in 2016. Last previous edition approved in 2016 as
E3063-16. DOI: 10.1520/E3063-16.10.1520/E3063-17.
2
The boldface numbers in parentheses refer to a list of references at the end of this standard.
3
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.
4
Available from the Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402.
5
Document produced by Working Groups of the Joint Committee for Guides in Metrology (JCGM). Available free of charge at BIPM website (http://www.bipm.org).
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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E3063 − 17
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