ASTM C1268-15
(Test Method)Standard Test Method for Quantitative Determination of 241Am in Plutonium by Gamma-Ray Spectrometry
Standard Test Method for Quantitative Determination of <sup>241</sup>Am in Plutonium by Gamma-Ray Spectrometry
SIGNIFICANCE AND USE
5.1 This test method allows the determination of 241Am in a plutonium solution without separation of the americium from the plutonium. It is generally applicable to any solution containing 241Am.
5.2 The 241Am in solid plutonium materials may be determined when these materials are dissolved (see Practice C1168).
5.3 When the plutonium solution contains unacceptable levels of fission products or other materials, this method may be used following a tri-n-octylphosphine oxide (TOPO) extraction, ion exchange or other similar separation techniques (see Test Methods C758 and C759).
5.4 This test method is less subject to interferences from plutonium than alpha counting since the energy of the gamma ray used for the analysis is better resolved from other gamma rays than the alpha particle energies used for alpha counting.
5.5 The minimal sample preparation reduces the amount of sample handling and exposure to the analyst.
5.6 This test method is applicable only to homogeneous solutions. This test method is not suitable for solutions containing solids.
5.7 Solutions containing as little as 1 × 10 −5 g/L 241Am may be analyzed using this method. The lower limit depends on the detector used and the counting geometry. Solutions containing high concentrations may be analyzed following an appropriate dilution.
SCOPE
1.1 This test method covers the quantitative determination of 241Am by gamma-ray spectrometry in plutonium nitrate solution samples that do not contain significant amounts of radioactive fission products or other high specific activity gamma-ray emitters.
1.2 This test method can be used to determine the 241Am in samples of plutonium metal, oxide and other solid forms, when the solid is appropriately sampled and dissolved.
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.
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Designation: C1268 − 15
Standard Test Method for
241
Quantitative Determination of Am in Plutonium by
1
Gamma-Ray Spectrometry
This standard is issued under the fixed designation C1268; 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 C1592/C1592MGuide for Making Quality Nondestructive
Assay Measurements
1.1 This test method covers the quantitative determination
241 E181Test Methods for Detector Calibration andAnalysis of
of Am by gamma-ray spectrometry in plutonium nitrate
Radionuclides
solution samples that do not contain significant amounts of
radioactive fission products or other high specific activity 2.2 U.S. Nuclear Regulatory Commission Regulatory
3
gamma-ray emitters. Guides:
241 Regulatory Guide 5.9,Rev. 2—Guidelines for Germanium
1.2 This test method can be used to determine the Am in
Spectroscopy Systems for Measurement of Special
samplesofplutoniummetal,oxideandothersolidforms,when
Nuclear Materials
the solid is appropriately sampled and dissolved.
Regulatory Guide 5.53,Rev. 1—Qualification, Calibration,
3
1.3 The values stated in SI units are to be regarded as
and Error Estimation Methods for NondestructiveAssay
standard. No other units of measurement are included in this
standard.
3. Terminology
1.4 This standard does not purport to address all of the
3.1 Except as otherwise defined herein, definitions of terms
safety concerns, if any, associated with its use. It is the
are as given in Terminology C859.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
4. Summary of Test Method
bility of regulatory limitations prior to use.
4.1 An aliquot of the sample that contains about 10 to 100
241
2. Referenced Documents ng of Am is analyzed by measuring the intensity of the
241
2 characteristic 59.5 keV gamma ray emitted by Am.
2.1 ASTM Standards:
C758Test Methods for Chemical, Mass Spectrometric,
4.2 Multiple sample geometries may be used if an appro-
Spectrochemical,Nuclear,andRadiochemicalAnalysisof priate calibration for each geometry is made.
Nuclear-Grade Plutonium Metal
4.3 The sample geometry must be reproducible. This in-
C759Test Methods for Chemical, Mass Spectrometric,
cludes the physical characteristics of the sample container, the
Spectrochemical,Nuclear,andRadiochemicalAnalysisof
positioningofthesample,andthevolumeofsampleviewedby
Nuclear-Grade Plutonium Nitrate Solutions
the gamma-ray detector.
C859Terminology Relating to Nuclear Materials
4.4 Electronic corrections are made, if required, for the
C1009Guide for Establishing and Maintaining a Quality
effectsofpulsepile-upanddeadtimelossesduetotheactivity
AssuranceProgramforAnalyticalLaboratoriesWithinthe
of the sample. The necessity of dead time and pulse pile-up
Nuclear Industry
corrections can be reduced by sample dilution to control count
C1168PracticeforPreparationandDissolutionofPlutonium
rates.
Materials for Analysis
4.5 Acorrectionismadeforthecontributiontothe59.5keV
237
intensity due to gamma rays produced in the decay of U.
1
ThistestmethodisunderthejurisdictionofASTMCommitteeC26onNuclear
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
4.6 The relationship between the measured gamma-ray
Test. 241
intensity and the Am content is determined by the use of
CurrenteditionapprovedJune1,2015.PublishedJuly2015.Originallyapproved
appropriate standards.
in 1994. Last previous edition approved in 2008 as C1268–94(2008). DOI:
10.1520/C1268-15.
2
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
3
Standards volume information, refer to the standard’s Document Summary page on Available from U.S. Nuclear Regulatory Commission, One White Flint North,
the ASTM website. 11555 Rockville Pike, Rockville, MD 20852. Also through www.nrc.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
C1268 − 15
5. Significance and Use 7.1.1 Germanium Photon Detector with Integral
241 Preamplifier—A coaxial type detector should typically have a
5.1 Thistestmethodallowsthedeterminationof Amina
fullwidthathalfmaximumresolutionof850eVorlessat122
plutonium solution without separation of the americium from
keV and 2.0 keV or less at 1332 keV. A planar type detector
the plutonium. I
...
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: C1268 − 94 (Reapproved 2008) C1268 − 15
Standard Test Method for
241
Quantitative Determination of Americium 241 Am in
1
Plutonium by Gamma-Ray Spectrometry
This standard is issued under the fixed designation C1268; 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
241
1.1 This test method covers the quantitative determination of americium 241 Am by gamma-ray spectrometry in plutonium
nitrate solution samples that do not contain significant amounts of radioactive fission products or other high specific activity
gamma-ray emitters.
241
1.2 This test method can be used to determine the americium 241 Am in samples of plutonium metal, oxide and other solid
forms, when the solid is appropriately sampled and dissolved.
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.
2. Referenced Documents
2
2.1 ASTM Standards:
C758 Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-
Grade Plutonium Metal
C759 Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-
Grade Plutonium Nitrate Solutions
C859 Terminology Relating to Nuclear Materials
3
C982 Guide for Selecting Components for Energy-Dispersive X-Ray Fluorescence (XRF) Systems (Withdrawn 2008)
C1009 Guide for Establishing and Maintaining a Quality Assurance Program for Analytical Laboratories Within the Nuclear
Industry
C1168 Practice for Preparation and Dissolution of Plutonium Materials for Analysis
C1592/C1592M Guide for Making Quality Nondestructive Assay Measurements
E181 Test Methods for Detector Calibration and Analysis of Radionuclides
4
2.2 ANSI Standards:
ANSI N15.20 Guide to Calibrating Nondestructive Assay Systems
4
ANSI N15.35 Guide to Preparing Calibration Material for Nondestructive Assay Systems that Count Passive Gamma Rays
4
ANSI N15.37 Guide to the Automation of Nondestructive Assay Systems for Nuclear Material Control
3
2.2 U.S. Nuclear Regulatory Commission Regulatory Guides:
Regulatory Guide 5.9, Rev. 2—Guidelines for Germanium Spectroscopy Systems for Measurement of Special Nuclear Materials
3
Regulatory Guide 5.53, Rev. 1—Qualification, Calibration, and Error Estimation Methods for Nondestructive Assay
3. Terminology
3.1 Except as otherwise defined herein, definitions of terms are as given in Terminology C859.
1
This test method is under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of Test.
Current edition approved Jan. 1, 2008June 1, 2015. Published February 2008July 2015. Originally approved in 1994. Last previous edition approved in 20002008 as
C1268 – 94 (2000).(2008). DOI: 10.1520/C1268-94R08.10.1520/C1268-15.
2
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.
3
Available from U.S. Nuclear Regulatory Commission, 1717 H ST., NW, Washington, DC 20555.One White Flint North, 11555 Rockville Pike, Rockville, MD 20852.
Also through www.nrc.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
C1268 − 15
4. Summary of Test Method
241
4.1 An aliquot of the sample that contains about 10 to 100 ng of americium 241 Am is analyzed by measuring the intensity
241
of the characteristic 59.5 keV gamma ray emitted by americium 241.Am.
4.2 Multiple sample geometries may be used if an appropriate calibration for each geometry is made.
4.3 The sample geometry must be reproducible. This includes the physical characteristics of the sample container, the
positioning of the sample, and the volume of sample viewed by the gamma-ray detector.
4.4 Electronic corrections are made, if required, for the effe
...
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: C1268 − 15
Standard Test Method for
241
Quantitative Determination of Am in Plutonium by
1
Gamma-Ray Spectrometry
This standard is issued under the fixed designation C1268; 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 C1592/C1592M Guide for Making Quality Nondestructive
Assay Measurements
1.1 This test method covers the quantitative determination
241 E181 Test Methods for Detector Calibration and Analysis of
of Am by gamma-ray spectrometry in plutonium nitrate
Radionuclides
solution samples that do not contain significant amounts of
radioactive fission products or other high specific activity 2.2 U.S. Nuclear Regulatory Commission Regulatory
3
gamma-ray emitters. Guides:
241 Regulatory Guide 5.9, Rev. 2—Guidelines for Germanium
1.2 This test method can be used to determine the Am in
Spectroscopy Systems for Measurement of Special
samples of plutonium metal, oxide and other solid forms, when
Nuclear Materials
the solid is appropriately sampled and dissolved.
Regulatory Guide 5.53, Rev. 1—Qualification, Calibration,
3
1.3 The values stated in SI units are to be regarded as
and Error Estimation Methods for Nondestructive Assay
standard. No other units of measurement are included in this
standard.
3. Terminology
1.4 This standard does not purport to address all of the
3.1 Except as otherwise defined herein, definitions of terms
safety concerns, if any, associated with its use. It is the
are as given in Terminology C859.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
4. Summary of Test Method
bility of regulatory limitations prior to use.
4.1 An aliquot of the sample that contains about 10 to 100
241
2. Referenced Documents ng of Am is analyzed by measuring the intensity of the
241
2
characteristic 59.5 keV gamma ray emitted by Am.
2.1 ASTM Standards:
C758 Test Methods for Chemical, Mass Spectrometric, 4.2 Multiple sample geometries may be used if an appro-
Spectrochemical, Nuclear, and Radiochemical Analysis of
priate calibration for each geometry is made.
Nuclear-Grade Plutonium Metal
4.3 The sample geometry must be reproducible. This in-
C759 Test Methods for Chemical, Mass Spectrometric,
cludes the physical characteristics of the sample container, the
Spectrochemical, Nuclear, and Radiochemical Analysis of
positioning of the sample, and the volume of sample viewed by
Nuclear-Grade Plutonium Nitrate Solutions
the gamma-ray detector.
C859 Terminology Relating to Nuclear Materials
4.4 Electronic corrections are made, if required, for the
C1009 Guide for Establishing and Maintaining a Quality
effects of pulse pile-up and dead time losses due to the activity
Assurance Program for Analytical Laboratories Within the
of the sample. The necessity of dead time and pulse pile-up
Nuclear Industry
corrections can be reduced by sample dilution to control count
C1168 Practice for Preparation and Dissolution of Plutonium
rates.
Materials for Analysis
4.5 A correction is made for the contribution to the 59.5 keV
237
intensity due to gamma rays produced in the decay of U.
1
This test method is under the jurisdiction of ASTM Committee C26 on Nuclear
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
4.6 The relationship between the measured gamma-ray
Test. 241
intensity and the Am content is determined by the use of
Current edition approved June 1, 2015. Published July 2015. Originally approved
appropriate standards.
in 1994. Last previous edition approved in 2008 as C1268 – 94 (2008). DOI:
10.1520/C1268-15.
2
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
3
Standards volume information, refer to the standard’s Document Summary page on Available from U.S. Nuclear Regulatory Commission, One White Flint North,
the ASTM website. 11555 Rockville Pike, Rockville, MD 20852. Also through www.nrc.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
C1268 − 15
5. Significance and Use 7.1.1 Germanium Photon Detector with Integral
241 Preamplifier—A coaxial type detector should typically have a
5.1 This test method allows the determination of Am in a
full width at half maximum resolution of 850 eV or less at 122
plutonium solution without separation of the americium from
keV and 2.0 keV or less at 1332 keV. A planar type detector
the plutonium. It is generally applicable t
...
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