ASTM C1411-08
(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
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 Specification C 833 and Specification C 1008. This standard 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.
In those facilities where perchloric acid use is tolerated, the separation in Test Method C 698 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 C 1625.
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 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 and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: C1411 − 08
StandardPractice 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 tions and Isotopic Abundances by Thermal Ionization
Mass Spectrometry
1.1 This practice is for the ion exchange separation of
uranium and plutonium from each other and from other
3. Terminology
impurities for subsequent isotopic analysis by thermal ioniza-
3.1 Definitions:For definitions of terms used in this
tion mass spectrometry. Plutonium–238 and uranium–238, and
standard, refer to C859.
plutonium–241 and americium–241, will appear as the same
mass peak and must be chemically separated prior to analysis.
4. Summary of Practice
Only high purity solutions can be analyzed reliably using
4.1 SolidsamplesaredissolvedaccordingtoPracticeC1168
thermal ionization mass spectrometry.
or other appropriate methods. The resulting solution is pro-
1.2 This standard may involve hazardous material,
cessed by this practice to prepare separate solutions of pluto-
operations, and equipment. This standard does not purport to
nium and uranium for mass spectrometric isotopic analysis
address all of the safety concerns, if any, associated with its
using Method C698, sections 112.4 through 114 or method
use. It is the responsibility of the user of this standard to
C1625.Appropriate aliquants are taken to provide up to 1 mg
consult and establish appropriate safety and health practices
ofplutoniumontheionexchangecolumntobeseparatedfrom
and determine the applicability of regulatory limitations prior
10 mg or less of uranium. Valence adjustment is obtained by
to use.
using one of two procedures as described in 4.1.1 and 4.1.2 or
by an alternative method demonstrated by the user to perform
2. Referenced Documents
3
the equivalent reduction/oxidation procedure.
2
2.1 ASTM Standards:
4.1.1 Foranysampletype,especiallythosecontaininglarge
C698Test Methods for Chemical, Mass Spectrometric, and
amounts of impurities, ferrous sulfate may be used for reduc-
Spectrochemical Analysis of Nuclear-Grade Mixed Ox-
tion.The aliquant is dissolved in 3 M HNO . Ferrous sulfate is
3
ides ((U, Pu)O )
2
added to reduce all plutonium (VI) to plutonium (III), then 16
C833Specification for Sintered (Uranium-Plutonium) Diox-
MHNO isaddedtooxidizeplutonium(III)toplutonium(IV),
3
ide Pellets
and to adjust the final acid concentration to8M HNO .
3
C859Terminology Relating to Nuclear Materials
4.1.2 A hydrogen peroxide reduction may be used for
C1008Specification for Sintered (Uranium-Plutonium) Di-
relatively pure samples which do not contain excessive
oxide Pellets—Fast Reactor Fuel
amounts of oxidizing impurities.The aliquant is dissolved in 8
C1168PracticeforPreparationandDissolutionofPlutonium
M HNO . Hydrogen peroxide is added to the aliquant prior to
3
Materials for Analysis
fuming to reduce plutonium (VI) to the lower oxidation states.
C1347Practice for Preparation and Dissolution of Uranium
The solution is warmed on a hot plate to destroy excess
Materials for Analysis 4,5
hydrogen peroxide and stabilize plutonium (IV) in solution.
C1625Test Method for Uranium and Plutonium Concentra-
4.2 After valence adjustment, the resulting solution is
passed through an anion exchange column in the nitrate form
which retains the plutonium; uranium and americium are not
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.
3
Current edition approved Jan. 1, 2008. Published February 2008. Originally Reduction of all higher plutonium oxidation states to plutonium (III) by the
approved in 1990. Last previous edition approved in 2001 as C1411–01. DOI: addition of hydroxylamine or NH CLO , followed by oxidation to plutonium (IV)
2 4
10.1520/C1411-08. by sodium nitrite and subsequent boiling to eliminate the nitrous fumes has been
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or foundtobeacceptable.ThismethodavoidstheadditionofFe,whichcouldinterfere
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM with electrodeposition of mass spectrometric samples.
4
Standards volume information, refer to the standard’s Document Summary page on I.V. Kressin and G.R. Waterbury, Anal. Chem. 34(12) , 1598 (1962).
5
the ASTM website. C.E. Pietri, B.P. Freeman, and J.R. Weiss, DOE/NBL-298 , September 1981.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:C1411–01 Designation:C1411–08
Standard Practice for
The Ion Exchange Separation of Uranium and Plutonium
1
Prior to Isotopic Analysis
This standard is issued under the fixed designation C 1411; 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 (e) 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–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 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 and health practices and determine the applicability of regulatory limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
C 698Standard Test Method Test Methods for Chemical, Mass Spectrometric, and SpectrochemicalAnalysis of Nuclear-Grade
Mixed Oxides ((U, Pu)O ), Sections 141-149. )
2
2
C 833Standard Specification for Sintered (Uranium, Plutonium) Dioxide Pellets. Specification for Sintered (Uranium-
Plutonium) Dioxide Pellets
C 859 Terminology Relating to Nuclear Materials
2
C 1008Standard Specification for Sintered (Uranium, Plutonium) Dioxide Pellets - Fast Reactor Fuel. Specification for
Sintered (Uranium-Plutonium) Dioxide PelletsFast Reactor Fuel
2
C 1168Standard Practice for Preparation and Dissolution of Plutonium Materials for Analysis.
E267Standard Test Method for Uranium and Plutonium Concentrations and IsotopicAbundances. Practice for Preparation and
Dissolution of Plutonium Materials for Analysis
C 1347 Practice for Preparation and Dissolution of Uranium Materials for Analysis
C 1625 Test Method for Uranium and Plutonium Concentrations and Isotopic Abundances by Thermal Ionization Mass
Spectrometry
3. Terminology
3.1 Definitions: For definitions of terms used in this standard, refer to C 859.
4. Summary of Practice
3.1Solid4.1 Solid samples are dissolved according to Practice C 1168 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
MethodC 698,seeSec.144sections112.4through145and147.4through149114oritsreplacement.methodC 1625.Appropriate
aliquants are taken to provide up to 1 mg of plutonium on the ion exchange column to be separated from 10 mg or less of uranium.
Valence adjustment is obtained by using one of two procedures as described in 3.1.14.1.1 and 3.1.2 4.1.2 or by an alternative
method demonstrated by the user to perform the equivalent reduction/oxidation procedure.
3
3.1.1
4.1.1 For any sample type, especially those containing large amounts of impurities, ferrous sulfate may be used for reduction.
The aliquant is dissolved in 3 M HNO . Ferrous sulfate is added to reduce all plutonium (VI) to plutonium (III), then 16 M HNO
3 3
is added to oxidize plutonium (III) to plutonium (IV), and to adjust the final acid concentration to8M HNO .
3
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. 10, 2001. Published March 2001. Originally published as C 1411–99. Last previous edition C 1411–99.
Current edition approved Jan. 1, 2008. Published February 2008. Originally approved in 1990. Last previous edition approved in 2001 as C 1411 – 01.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
, Vol 12.01.volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Annual Book of ASTM Standards, Vol 12.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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C1411–08
3.1.2
4.1.2 A hydrogen peroxide reduction may be used
...
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