ASTM C1411-20
(Practice)Standard Practice for The Ion Exchange Separation of Uranium and Plutonium Prior to Isotopic Analysis
Standard Practice for The Ion Exchange Separation of Uranium and Plutonium Prior to Isotopic Analysis
SIGNIFICANCE AND USE
5.1 Uranium and plutonium are used in nuclear reactor fuel and must be analyzed to insure that they meet certain criteria for isotopic composition as described in Specifications C833 and C1008. This practice is used to chemically separate the same mass peak interferences from uranium and plutonium and from other impurities prior to isotopic abundance determination by thermal ionization mass spectrometry.
5.2 In those facilities where perchloric acid use is tolerated, the separation in Test Method C698 may be used prior to isotopic abundance determination. Uranium and plutonium concentrations as well as isotopic abundances using thermal ionization mass spectrometry can be determined using this separation and following Test Method C1625.
SCOPE
1.1 This practice is for the ion exchange separation of uranium and plutonium from each other and from other impurities for subsequent isotopic analysis by thermal ionization mass spectrometry. Plutonium-238 and uranium-238, and plutonium-241 and americium-241, will appear as the same mass peak and must be chemically separated prior to analysis. Only high purity solutions can be analyzed reliably using thermal ionization mass spectrometry.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.4 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: C1411 − 20
Standard Practice for
The Ion Exchange Separation of Uranium and Plutonium
1
Prior to Isotopic Analysis
This standard is issued under the fixed designation C1411; 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 C1008 Specification for Sintered (Uranium-Plutonium)
3
DioxidePellets—Fast Reactor Fuel (Withdrawn 2014)
1.1 This practice is for the ion exchange separation of
C1168PracticeforPreparationandDissolutionofPlutonium
uranium and plutonium from each other and from other
Materials for Analysis
impurities for subsequent isotopic analysis by thermal ioniza-
C1347Practice for Preparation and Dissolution of Uranium
tion mass spectrometry. Plutonium-238 and uranium-238, and
Materials for Analysis
plutonium-241 and americium-241, will appear as the same
C1625Test Method for Uranium and Plutonium Concentra-
mass peak and must be chemically separated prior to analysis.
tions and Isotopic Abundances by Thermal Ionization
Only high purity solutions can be analyzed reliably using
Mass Spectrometry
thermal ionization mass spectrometry.
D1193Specification for Reagent Water
1.2 The values stated in SI units are to be regarded as
3. Terminology
standard. No other units of measurement are included in this
standard.
3.1 Definitions:
1.3 This standard does not purport to address all of the 3.1.1 For definitions of terms used in this practice, refer to
safety concerns, if any, associated with its use. It is the
C859.
responsibility of the user of this standard to establish appro-
4. Summary of Practice
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use. 4.1 Solid samples are dissolved according to Practices
1.4 This international standard was developed in accor-
C1168, C1347, or other appropriate methods. The resulting
dance with internationally recognized principles on standard- solution is processed by this practice to prepare separate
ization established in the Decision on Principles for the
solutions of plutonium and uranium for mass spectrometric
Development of International Standards, Guides and Recom-
isotopic analysis using Test Method C698 or C1625. Appro-
mendations issued by the World Trade Organization Technical
priate aliquants are taken to provide up to 1 mg of plutonium
Barriers to Trade (TBT) Committee.
ontheionexchangecolumntobeseparatedfrom10mgorless
of uranium. Valence adjustment is obtained by using one of
2. Referenced Documents
two procedures as described in 4.1.1 and 4.1.2 or by an
2
alternative method demonstrated by the user to perform the
2.1 ASTM Standards:
equivalent reduction/oxidation procedure.
C698Test Methods for Chemical, Mass Spectrometric, and
Spectrochemical Analysis of Nuclear-Grade Mixed Ox-
NOTE 1—Reduction of all higher plutonium oxidation states to pluto-
ides ((U, Pu)O )
nium (III) by the addition of hydroxylamine or NH CLO , followed by
2
2 4
C833Specification for Sintered (Uranium-Plutonium) Diox- oxidation to plutonium (IV) by sodium nitrite and subsequent boiling to
eliminate the nitrous fumes has been found to be acceptable.This method
ide Pellets for Light Water Reactors
avoids the addition of Fe, which could interfere with electrodeposition of
C859Terminology Relating to Nuclear Materials
prior to mass spectrometry analysis samples.
4.1.1 Foranysampletype,especiallythosecontaininglarge
1
This practice is under the jurisdiction of ASTM Committee C26 on Nuclear amounts of impurities, ferrous sulfate may be used for reduc-
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
tion.The aliquant is dissolved in 3 M HNO . Ferrous sulfate is
3
Test.
added to reduce all plutonium (VI) to plutonium (III), then
CurrenteditionapprovedJuly1,2020.PublishedJuly2020.Originallyapproved
16 M HNO is added to oxidize plutonium (III) to plutonium
in 1990. Last previous edition approved in 2014 as C1411 – 14. DOI: 10.1520/
3
C1411-20.
(IV), and to adjust the final acid concentration to8M HNO .
3
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 The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA
...
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: C1411 − 14 C1411 − 20
Standard Practice for
The Ion Exchange Separation of Uranium and Plutonium
1
Prior to Isotopic Analysis
This standard is issued under the fixed designation C1411; 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 practice is for the ion exchange separation of uranium and plutonium from each other and from other impurities for
subsequent isotopic analysis by thermal ionization mass spectrometry. Plutonium–238Plutonium-238 and uranium–238,uranium-
238, and plutonium–241plutonium-241 and americium–241,americium-241, will appear as the same mass peak and must be
chemically separated prior to analysis. Only high purity solutions can be analyzed reliably using thermal ionization mass
spectrometry.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 This standard may involve hazardous material, operations, and equipment. 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 consult and establish
appropriate safety safety, health, and healthenvironmental practices and determine the applicability of regulatory limitations prior
to use.
1.4 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
2
2.1 ASTM Standards:
C698 Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Mixed Oxides ((U,
Pu)O )
2
C833 Specification for Sintered (Uranium-Plutonium) Dioxide Pellets for Light Water Reactors
C859 Terminology Relating to Nuclear Materials
3
C1008 Specification for Sintered (Uranium-Plutonium) DioxidePellets—Fast Reactor Fuel (Withdrawn 2014)
C1168 Practice for Preparation and Dissolution of Plutonium Materials for Analysis
C1347 Practice for Preparation and Dissolution of Uranium Materials for Analysis
C1625 Test Method for Uranium and Plutonium Concentrations and Isotopic Abundances by Thermal Ionization Mass
Spectrometry
D1193 Specification for Reagent Water
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in this practice, refer to C859.For definitions of terms used in this standard, refer to C859.
4. Summary of Practice
4.1 Solid samples are dissolved according to Practices C1168, C1347, or other appropriate methods. The resulting solution is
processed by this practice to prepare separate solutions of plutonium and uranium for mass spectrometric isotopic analysis using
Test Method C698 or Method C1625. Appropriate aliquants are taken to provide up to 1 mg of plutonium on the ion exchange
1
This practice 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, 2014July 1, 2020. Published February 2014July 2020. Originally approved in 1990. Last previous edition approved in 20082014 as
C1411 – 08.C1411 – 14. DOI: 10.1520/C1411-14.10.1520/C1411-20.
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
The last approved version of this historical standard is referenced on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
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C1411 − 20
column to be separated from 10 mg 10 mg or less of uranium. Valence adjustment is obtained by using one of two procedures as
described in 4.1.14.1.1 and 4.1.2 and 4.1.2or by an alternative method demonstrated by the user to perform the equivalent
reduction/oxidation procedure.
NOTE 1—Reduction of all higher plutonium oxidation states to plutonium (III) by the addition of hydroxylamine or NH CLO , followed by oxidation
2 4
to plutonium (IV) by sodium nitrite and subsequent boiling to eliminate the
...
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