ASTM E3063-16

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 and health practices and determine the applicability of regulatory limitations prior to use. Specific precautions are given in Section 9.

General Information

• Status: Historical
• Publication Date: 30-Sep-2016
• ICS: 71.040.40 - Chemical analysis
• Technical Committee: E10 - Nuclear Technology and Applications
• Drafting Committee: E10.05 - Nuclear Radiation Metrology

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: E3063 − 16
Test Method for
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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
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2.1 ASTM Standards:
1.1 This test method covers the measurement of antimony
E170Terminology Relating to Radiation Measurements and
concentration in plastics or other hydrocarbon or organic
Dosimetry
matrix by using neutron activation analysis (NAA). The
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sampleisactivatedbyirradiationwithneutronsfromaresearch
2.2 U.S. Government Document:
reactor and the subsequently emitted gamma-rays are detected
Code of Federal Regulations, Title 10, Part 20
with a germanium semiconductor detector. The same system
2.3 Joint Committee for Guides in Metrology (JCGM)
may be used to determine antimony concentrations ranging
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Reports:
from 1 ng/g to 10 000 µg/g with the lower end of the range
JCGM 100:2008, GUM 1995, with minor corrections,
limited by numerous interferences and the upper limit estab-
Evaluationofmeasurementdata—Guidetotheexpression
lished by the demonstrated practical application of NAA.
of uncertainty in measurement
1.2 This test method may be used on either solid or liquid
samples,providedthattheycanbemadetoconforminsizeand 3. Terminology
shape during irradiation and counting to a standard sample of
3.1 Definitions: See also Terminology E170.
known antimony content using very simple sample prepara-
3.1.1 comparator standard—a reference standard of known
tion.Severalvariantsofthismethodhavebeendescribedinthe
antimony content whose specific activation and counting
technicalliterature.Amonographisavailablewhichprovidesa −1
sensitivity (counts (mg of antimony) ) may be used to
comprehensive description of the principles of neutron activa-
quantify the antimony content of a sample irradiated and
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tion analysis using reactor neutrons (1).
counted under the same conditions. Often, a comparator
standard is selected to have a matrix composition, physical
1.3 The values stated in SI units are to be regarded as
size, density and shape very similar to the corresponding
standard. No other units of measurement are included in this
parameters of the sample to be analyzed. Differences in size,
standard.
density, shape and matrix composition between sample and
1.4 This standard does not purport to address all of the
standard may be corrected for using physical or empirical
safety concerns, if any, associated with its use. It is the
models.
responsibility of the user of this standard to establish appro-
3.1.2 gamma-ray spectrometer—a system comprising a de-
priate safety and health practices and determine the applica-
tector which detects individual gamma-rays and converts their
bility of regulatory limitations prior to use. Specific precau-
energyintoanelectronicpulsewhosevoltageisproportionalto
tions are given in Section 9.
the energy deposited in the detector, and a multichannel
1.5 This international standard was developed in accor-
pulse-height analyzer which measures the pulse heights, as-
dance with internationally recognized principles on standard-
signs a digital value and stores the individual counts in the
ization established in the Decision on Principles for the
channels of a gamma-ray spectrum according to the digital
Development of International Standards, Guides and Recom-
values assigned.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
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For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
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ThistestmethodisunderthejurisdictionofASTMCommitteeE10onNuclear Standards volume information, refer to the standard’s Document Summary page on
Technology and Applications and is the direct responsibility of Subcommittee the ASTM website.
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E10.05 on Nuclear Radiation Metrology. Available from the Superintendent of Documents, U.S. Government Printing
Current edition approved Oct. 1, 2016. Published October 2016. DOI: 10.1520/ Office, Washington, DC 20402.
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E3063-16. Document produced by Working Groups of the Joint Committee for Guides in
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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.org).
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E3063 − 16
3.1.3 intensity—the probability of emission
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