ASTM C1411-14
(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 Specification C833 and Specification C1008. 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.
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 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 − 14
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 C1347Practice for Preparation and Dissolution of Uranium
Materials for Analysis
1.1 This practice is for the ion exchange separation of
C1625Test Method for Uranium and Plutonium Concentra-
uranium and plutonium from each other and from other
tions and Isotopic Abundances by Thermal Ionization
impurities for subsequent isotopic analysis by thermal ioniza-
Mass Spectrometry
tion mass spectrometry. Plutonium–238 and uranium–238, and
D1193Specification for Reagent Water
plutonium–241 and americium–241, will appear as the same
mass peak and must be chemically separated prior to analysis.
3. Terminology
Only high purity solutions can be analyzed reliably using
3.1 Definitions: For definitions of terms used in this
thermal ionization mass spectrometry.
standard, refer to C859.
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
4. Summary of Practice
standard.
4.1 Solid samples are dissolved according to Practices
1.3 This standard may involve hazardous material,
C1168, C1347, or other appropriate methods. The resulting
operations, and equipment. This standard does not purport to
solution is processed by this practice to prepare separate
address all of the safety concerns, if any, associated with its
solutions of plutonium and uranium for mass spectrometric
use. It is the responsibility of the user of this standard to
isotopic analysis using Method C698 or Method C1625.
consult and establish appropriate safety and health practices
Appropriate aliquants are taken to provide up to 1 mg of
and determine the applicability of regulatory limitations prior
plutoniumontheionexchangecolumntobeseparatedfrom10
to use.
mgorlessofuranium.Valenceadjustmentisobtainedbyusing
one of two procedures as described in 4.1.1 and 4.1.2 or by an
2. Referenced Documents
alternative method demonstrated by the user to perform the
2
3
2.1 ASTM Standards:
equivalent reduction/oxidation procedure.
C698Test Methods for Chemical, Mass Spectrometric, and
4.1.1 Foranysampletype,especiallythosecontaininglarge
Spectrochemical Analysis of Nuclear-Grade Mixed Ox-
amounts of impurities, ferrous sulfate may be used for reduc-
ides ((U, Pu)O )
tion.The aliquant is dissolved in 3 M HNO . Ferrous sulfate is
2
3
C833Specification for Sintered (Uranium-Plutonium) Diox-
added to reduce all plutonium (VI) to plutonium (III), then 16
ide Pellets
MHNO isaddedtooxidizeplutonium(III)toplutonium(IV),
3
C859Terminology Relating to Nuclear Materials
and to adjust the final acid concentration to8M HNO .
3
C1008Specification for Sintered (Uranium-Plutonium) Di-
4.1.2 A hydrogen peroxide reduction may be used for
oxide Pellets—Fast Reactor Fuel
relatively pure samples which do not contain excessive
C1168PracticeforPreparationandDissolutionofPlutonium
amounts of oxidizing impurities.The aliquant is dissolved in 8
Materials for Analysis
M HNO . Hydrogen peroxide is added to the aliquant prior to
3
fuming to reduce plutonium (VI) to the lower oxidation states.
The solution is warmed on a hot plate to destroy excess
1
This practice is under the jurisdiction of ASTM Committee C26 on Nuclear
4,5
hydrogen peroxide and stabilize plutonium (IV) in solution.
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
Test.
Current edition approved Jan. 1, 2014. Published February 2014. Originally
3
approved in 1990. Last previous edition approved in 2008 as C1411–08. DOI: Reduction of all higher plutonium oxidation states to plutonium (III) by the
10.1520/C1411-14. addition of hydroxylamine or NH CLO , followed by oxidation to plutonium (IV)
2 4
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or by sodium nitrite and subsequent boiling to eliminate the nitrous fumes has been
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM foundtobeacceptable.ThismethodavoidstheadditionofFe,whichcouldinterfere
Standards volume information, refer to the standard’s Document Summary page on with electrodeposition of prior to mass spectrometry analysis samples.
4
the ASTM website. I.V. Kressin and G.R. Waterbury, Anal. Chem. 34(12) , 1598 (1962).
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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C1411 − 1
...
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 − 08 C1411 − 14
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–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 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:
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
C859 Terminology Relating to Nuclear Materials
C1008 Specification for Sintered (Uranium-Plutonium) Dioxide Pellets—Fast Reactor Fuel
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: For definitions of terms used in this standard, refer to C859.
4. Summary of Practice
4.1 Solid samples are dissolved according to PracticePractices 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 Method C698, sections 112.4 through 114 or method or Method C1625. 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 4.1.1 and 4.1.2 or by an alternative method demonstrated by the user to perform
3
the equivalent reduction/oxidation procedure.
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, 2008Jan. 1, 2014. Published February 2008February 2014. Originally approved in 1990. Last previous edition approved in 20012008 as
C1411 – 01.C1411 – 08. DOI: 10.1520/C1411-08.10.1520/C1411-14.
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.
3
Reduction of all higher plutonium oxidation states to plutonium (III) by the addition of hydroxylamine or NH CLO , followed by oxidation to plutonium (IV) by sodium
2 4
nitrite and subsequent boiling to eliminate the nitrous fumes has been found to be acceptable. This method avoids the addition of Fe, which could interfere with
electrodeposition of mass spectrometric prior to mass spectrometry analysis samples.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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---------------------- Page: 1 ----------------------
C1411 − 14
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 to 8 M HNO .
3
4.1.2 A hyd
...
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