ASTM C1816-16
(Practice)Standard Practice for The Ion Exchange Separation of Small Volume Samples Containing Uranium, Americium, and Plutonium Prior to Isotopic Abundance and Content Analysis
Standard Practice for The Ion Exchange Separation of Small Volume Samples Containing Uranium, Americium, and Plutonium Prior to Isotopic Abundance and Content Analysis
SIGNIFICANCE AND USE
5.1 Uranium and plutonium are used in nuclear reactor fuel and must be analyzed to ensure that they meet acceptance criteria for isotopic composition as described in Specifications C833 and C1008. The criteria are set by mutual agreement between the manufacturer and end user (or between buyer and seller). This standard practice is used to separate chemically the isobaric interferences from 238U and 238Pu and from 241Am and 241Pu, and from other impurities prior to isotopic abundance determination by TIMS.
5.2 In facilities where perchloric acid use is authorized, the separation in Test Method C698 may be used prior to isotopic abundance determination. Uranium and plutonium content as well as isotopic abundances using TIMS can be determined by using this separation practice and by following Test Methods C698, C1625, or C1672.
SCOPE
1.1 This practice is an alternative to Practice C1411 for the ion exchange separation in small mass samples (~5 μg of plutonium and up to 0.5 mg of uranium in 1 mL of solution) of uranium and plutonium from each other and from other impurities for subsequent isotopic abundance and content analysis by thermal ionization mass spectrometry (TIMS). In addition to being adapted to smaller sample sizes, this practice also avoids the use of hydrochloric acid (HCl) and hydrofluoric acid (HF) and does not require the use of two anion exchange columns as required in Practice C1411.
1.2 In chemically unseparated samples isobaric nuclides at mass 238 (238U and 238Pu), and mass 241 (241Pu and 241Am) will be measured together thus compromising the accuracy of the results of isotopic composition of Pu. Therefore, chemical separation of elements is essential prior to isotopic analyses. Concentrations and volumes given in the paragraphs below can be modified for larger sample sizes, different types of anion exchange resin, etc.
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: C1816 − 16
Standard Practice for
The Ion Exchange Separation of Small Volume Samples
Containing Uranium, Americium, and Plutonium Prior to
1
Isotopic Abundance and Content Analysis
This standard is issued under the fixed designation C1816; 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 C698Test Methods for Chemical, Mass Spectrometric, and
Spectrochemical Analysis of Nuclear-Grade Mixed Ox-
1.1 This practice is an alternative to Practice C1411 for the
ides ((U, Pu)O )
2
ion exchange separation in small mass samples (~5 µg of
C833Specification for Sintered (Uranium-Plutonium) Diox-
plutoniumandupto0.5mgofuraniumin1mLofsolution)of
ide Pellets
uranium and plutonium from each other and from other
C859Terminology Relating to Nuclear Materials
impurities for subsequent isotopic abundance and content
C1008 Specification for Sintered (Uranium-Plutonium)
analysis by thermal ionization mass spectrometry (TIMS). In
3
DioxidePellets—Fast Reactor Fuel (Withdrawn 2014)
addition to being adapted to smaller sample sizes, this practice
C1168PracticeforPreparationandDissolutionofPlutonium
alsoavoidstheuseofhydrochloricacid(HCl)andhydrofluoric
Materials for Analysis
acid (HF) and does not require the use of two anion exchange
C1347Practice for Preparation and Dissolution of Uranium
columns as required in Practice C1411.
Materials for Analysis
1.2 In chemically unseparated samples isobaric nuclides at
C1411Practice for The Ion Exchange Separation of Ura-
238 238 241 241
mass 238 ( U and Pu), and mass 241 ( Pu and Am)
nium and Plutonium Prior to Isotopic Analysis
238
will be measured together thus compromising the accuracy of
C1415Test Method for Pu Isotopic Abundance By Alpha
the results of isotopic composition of Pu. Therefore, chemical
Spectrometry
separation of elements is essential prior to isotopic analyses.
C1625Test Method for Uranium and Plutonium Concentra-
Concentrationsandvolumesgivenintheparagraphsbelowcan
tions and Isotopic Abundances by Thermal Ionization
be modified for larger sample sizes, different types of anion
Mass Spectrometry
exchange resin, etc.
C1672Test Method for Determination of Uranium or Pluto-
nium Isotopic Composition or Concentration by the Total
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this Evaporation Method Using a Thermal Ionization Mass
Spectrometer
standard.
D1193Specification for Reagent Water
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
3. Terminology
responsibility of the user of this standard to establish appro-
3.1 Definitions—For definitions of terms used in this
priate safety and health practices and determine the applica-
practice, refer to Terminology C859.
bility of regulatory limitations prior to use.
4. Summary of Practice
2. Referenced Documents
2
4.1 Solid samples are dissolved according to Practices
2.1 ASTM Standards:
C1168 or C1347 or other appropriate methods. The resulting
solution is processed by this practice to prepare separate
solutions of plutonium and uranium for mass spectrometric
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 isotopic abundance analysis using Test Method C698, C1625,
Test.
or C1672.Appropriate portions are taken to provide up to 5 µg
Current edition approved Jan. 15, 2016. Published February 2016. Originally
ofplutoniumontheionexchangecolumntobeseparatedfrom
approved in 2015. Last previous edition approved in 2015 as C1816–15. DOI:
0.5mgorlessofuranium.Alldilutionsshouldbeperformedby
10.1520/C1816-16.
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 19428-2959. United States
1
---------------------- Page: 1 ----------------------
C1816 − 16
mass to ensure the smallest uncertainty possible. This practice 5.2 In facilities where perchloric acid use is authorized, the
canbeusedforhigheruraniumtoplutoniumratios,butcolumn separation in Test Method C698 may b
...
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: C1816 − 15 C1816 − 16
Standard Practice for
The Ion Exchange Separation of Small Volume Samples
Containing Uranium, Americium, and Plutonium Prior to
1
Isotopic Abundance and Content Analysis
This standard is issued under the fixed designation C1816; 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 an alternative to Practice C1411 for the ion exchange separation in small mass samples (~5 μg of plutonium
and up to 0.5 mg of uranium in 1 mL of solution) of uranium and plutonium from each other and from other impurities for
subsequent isotopic abundance and content analysis by thermal ionization mass spectrometry (TIMS). In addition to being adapted
to smaller sample sizes, this practice also avoids the use of hydrochloric acid (HCl) and hydrofluoric acid (HF) and does not require
the use of two anion exchange columns as required in Practice C1411.
238 238 241 241
1.2 In chemically unseparated samples isobaric nuclides at mass 238 ( U and Pu), and mass 241 ( Pu and Am) will
be measured together thus compromising the accuracy of the results of isotopic composition of Pu. Therefore, chemical separation
of elements is essential prior to isotopic analyses. Concentrations and volumes given in the paragraphs below can be modified for
larger sample sizes, different types of anion exchange resin, etc.
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:
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
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
C1411 Practice for The Ion Exchange Separation of Uranium and Plutonium Prior to Isotopic Analysis
238
C1415 Test Method for Pu Isotopic Abundance By Alpha Spectrometry
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 Definitions—For definitions of terms used in this practice, refer to Terminology C859.
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 June 1, 2015Jan. 15, 2016. Published July 2015February 2016. Originally approved in 2015. Last previous edition approved in 2015 as
C1816 – 15. DOI: 10.1520/C1816-15.10.1520/C1816-16.
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
---------------------- Page: 1 ----------------------
C1816 − 16
4. Summary of Practice
4.1 Solid samples are dissolved according to Practices C1168 or 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 abundance
analysis using Test Method C698, C1625, or C1672. Appropriate portions are taken to provide up to 5 μg of plutonium on the ion
exchange column to be separated from 0.5 mg or less of uranium. All dilutions should be
...
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