ASTM C1415-14
(Test Method)Standard Test Method for 238Pu Isotopic Abundance By Alpha Spectrometry
Standard Test Method for <sup>238</sup>Pu Isotopic Abundance By Alpha Spectrometry
SIGNIFICANCE AND USE
5.1 This test method is used when the determination of 238Pu isotopic abundance is required for plutonium samples.
SCOPE
1.1 This test method covers the use of alpha spectrometry for determining the 238Pu isotopic abundance in plutonium samples. It is particularly useful for samples in which the 238Pu content is less than 1 % of the total plutonium content. For such samples, mass spectrometric results are vulnerable to bias because of potential interference from any 238U isobar remaining after ion exchange.
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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Designation: C1415 − 14
Standard Test Method for
238 1
Pu Isotopic Abundance By Alpha Spectrometry
This standard is issued under the fixed designation C1415; 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 3. Terminology
1.1 This test method covers the use of alpha spectrometry
3.1 For definitions of pertinent terms not listed here, see
238
for determining the Pu isotopic abundance in plutonium
Terminology C859.
238
samples. It is particularly useful for samples in which the Pu
contentislessthan1 %ofthetotalplutoniumcontent.Forsuch
4. Summary of Test Method
samples, mass spectrometric results are vulnerable to bias
238
4.1 Thisdeterminationmethodinvolvesthemeasurementof
because of potential interference from any U isobar remain-
238 239 240
the alpha-activity ratio of Pu and Pu + Pu. The
ing after ion exchange.
238
isotopic analysis of plutonium for the Pu isotope requires
1.2 The values stated in SI units are to be regarded as the
the prior separation of potentially interfering species. After
standard. The values given in parentheses are for information
dissolution of the sample (see Practice C1168), the plutonium
only.
is separated from interferences by an anion-exchange purifica-
1.3 This standard does not purport to address all of the
tion technique. Nitric acid (HNO ) is used to adsorb the
3
safety concerns, if any, associated with its use. It is the
plutonium fraction on the resin. Interfering ions, principally
responsibility of the user of this standard to establish appro-
uranium and americium, are not adsorbed. The plutonium is
priate safety and health practices and determine the applica-
then eluted with dilute HNO (0.1 M). Because an alpha-
3
bility of regulatory limitations prior to use.
activity ratio is used, quantitative recovery of the plutonium is
not required. The alpha spectrum in the 5 to 6-MeV region is
2. Referenced Documents 238 239 240
obtained. The total counts in the Pu and the Pu + Pu
238
2
peaks are obtained and corrected for background. The Pu
2.1 ASTM Standards:
C697 Test Methods for Chemical, Mass Spectrometric, and abundance is calculated from the ratio of the alpha activity due
238 239 240 239
to Pu and that due to Pu + Pu. The abundance of Pu
Spectrochemical Analysis of Nuclear-Grade Plutonium
240
Dioxide Powders and Pellets and Pu is determined by mass spectrometry (see Test
Methods C697, C1625,or C1672) on a separate portion of the
C859 Terminology Relating to Nuclear Materials
C1168 PracticeforPreparationandDissolutionofPlutonium purified sample.
Materials for Analysis
C1625 Test Method for Uranium and Plutonium Concentra- 5. Significance and Use
tions and Isotopic Abundances by Thermal Ionization
5.1 This test method is used when the determination of
Mass Spectrometry
238
Pu isotopic abundance is required for plutonium samples.
C1672 Test Method for Determination of Uranium or Pluto-
nium Isotopic Composition or Concentration by the Total
6. Interferences
Evaporation Method Using a Thermal Ionization Mass
241
Spectrometer
6.1 Am-241 is always present as a result of Pu decay and
D1193 Specification for Reagent Water
is a direct interference that must be removed prior to the
238 230
determination of Pu. The very small amount of Th and
232
Th which could be present causes insignificant interference
238
1
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear
with the determination of Pu at the level of uncertainty of
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
this test method. Other nuclides that could interfere, such as
Test.
238 243 245 249
U, Am, Cm, and Bk, are removed by the anion-
CurrenteditionapprovedJune1,2014.PublishedJuly2014.Originallyapproved
exchange separation. Any residual uranium, while it does not
in 1999. Last previous edition approved in 2007 as C1415 – 01a (2007). DOI:
10.1520/C1415-14.
directly interfere with the alpha-pulse height determination,
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
can raise the salt content of the sample.Ahigh salt content can
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
decrease the resolution of the alpha spectra, and, consequently,
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. decrease the accuracy of the test method.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
C1415 − 14
7. Apparatus 8.5 Nitric acid, 0.1 M.Add6.2mL
...
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: C1415 − 01a (Reapproved 2007) C1415 − 14
Standard Test Method for
238 1
Pu Isotopic Abundance By Alpha Spectrometry
This standard is issued under the fixed designation C1415; 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
238
1.1 This test method covers the use of alpha spectrometry for determining the Pu isotopic abundance in plutonium samples.
238
It is particularly useful for samples in which the Pu content is less than 1 % of the total plutonium content. For such samples,
mass spectrometric results are less reliable than those from alpha spectrometry because of vulnerable to bias because of potential
238
interference from any U isobar remaining after ion exchange.
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.
2. Referenced Documents
2
2.1 ASTM Standards:
C697 Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Plutonium Dioxide
Powders and Pellets
C859 Terminology Relating to Nuclear Materials
C1168 Practice for Preparation and Dissolution of Plutonium Materials for Analysis
C1625 Test Method for Uranium and Plutonium Concentrations and Isotopic Abundances by Thermal Ionization Mass
Spectrometry
C1672 Test Method for Determination of Uranium or Plutonium Isotopic Composition or Concentration by the Total
Evaporation Method Using a Thermal Ionization Mass Spectrometer
D1193 Specification for Reagent Water
3. Terminology
3.1 For definitions of pertinent terms not listed here, see Terminology C859.
4. Summary of Test Method
238 239 240
4.1 This determination method involves the measurement of the alpha-activity ratio of Pu and Pu + Pu. The isotopic
238
analysis of plutonium for the Pu isotope requires the prior separation of interferences. potentially interfering species. After
dissolution of the sample (see Practice C1168), the plutonium is separated from interferences by an anion-exchange purification
technique. Nitric acid (HNO ) is used to adsorb the plutonium fraction on the resin. Interfering ions, principally uranium and
3
americium, are not adsorbed. The plutonium is then eluted with dilute HNO (0.1 M). Because an alpha-activity ratio is used,
3
quantitative recovery of the plutonium is not required. The alpha spectrum in the 5 to 6-MeV region is obtained. The total counts
238 239 240 238
in the Pu and the Pu + Pu peaks are obtained and corrected for background. The Pu abundance is calculated from the
238 239 240 239 240
ratio of the alpha activity due to Pu and that due to Pu + Pu. The abundance of Pu and Pu is determined by mass
spectrometry (see Test Methods C697, C1625, or C1672) on a separate portion of the purified sample.
5. Significance and Use
238
5.1 This test method is used when the determineddetermination of Pu isotopic abundance is required for plutonium samples.
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 Feb. 15, 2007June 1, 2014. Published April 2007July 2014. Originally approved in 1999. Last previous edition approved in 20012007 as
C1415 – 01a.C1415 – 01a (2007). DOI: 10.1520/C1415-01AR07.10.1520/C1415-14.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
C1415 − 14
6. Interferences
241 241
6.1 AmAm-241 is always present as a result of Pu decay and is a direct interference that must be removed prior to the
238 230 232
determination of Pu. The very small amount of Th and Th which could be present causes insignificant interference with
238
the determination of Pu at the leve
...
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