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.

General Information

Status
Historical
Publication Date
31-May-2015
Technical Committee
Drafting Committee
Current Stage
Ref Project

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ASTM C1816-15 - Standard Practice for The Ion Exchange Separation of Small Volume Samples Containing Uranium, Americium, and Plutonium Prior to Isotopic Abundance and Content Analysis
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Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: C1816 − 15
StandardPractice 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 Spectrochemical Analysis of Nuclear-Grade Mixed Ox-
ides ((U, Pu)O )
2
1.1 This practice is an alternative to Practice C1411 for the
C833Specification for Sintered (Uranium-Plutonium) Diox-
ion exchange separation in small mass samples (~5 µg of
ide Pellets
plutoniumandupto0.5mgofuraniumin1mLofsolution)of
C859Terminology Relating to Nuclear Materials
uranium and plutonium from each other and from other
C1008 Specification for Sintered (Uranium-Plutonium)
impurities for subsequent isotopic abundance and content
3
DioxidePellets—Fast Reactor Fuel (Withdrawn 2014)
analysis by thermal ionization mass spectrometry (TIMS). In
C1168PracticeforPreparationandDissolutionofPlutonium
addition to being adapted to smaller sample sizes, this practice
Materials for Analysis
alsoavoidstheuseofhydrochloricacid(HCl)andhydrofluoric
C1347Practice for Preparation and Dissolution of Uranium
acid (HF) and does not require the use of two anion exchange
Materials for Analysis
columns as required in Practice C1411.
C1411Practice for The Ion Exchange Separation of Ura-
1.2 In chemically unseparated samples isobaric nuclides at
nium and Plutonium Prior to Isotopic Analysis
238 238 241 241
238
mass 238 ( U and Pu), and mass 241 ( Pu and Am)
C1415Test Method for Pu Isotopic Abundance By Alpha
will be measured together thus compromising the accuracy of
Spectrometry
the results of isotopic composition of Pu. Therefore, chemical
C1625Test Method for Uranium and Plutonium Concentra-
separation of elements is essential prior to isotopic analyses.
tions and Isotopic Abundances by Thermal Ionization
Concentrationsandvolumesgivenintheparagraphsbelowcan
Mass Spectrometry
be modified for larger sample sizes, different types of anion
C1672Test Method for Determination of Uranium or Pluto-
exchange resin, etc.
nium Isotopic Composition or Concentration by the Total
Evaporation Method Using a Thermal Ionization Mass
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this Spectrometer
D1193Specification for Reagent Water
standard.
1.4 This standard does not purport to address all of the
3. Terminology
safety concerns, if any, associated with its use. It is the
3.1 Definitions—For definitions of terms used in this
responsibility of the user of this standard to establish appro-
practice, refer to Terminology C859.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
4. Summary of Practice
2. Referenced Documents
4.1 Solid samples are dissolved according to Practices
2
C1168 or C1347 or other appropriate methods. The resulting
2.1 ASTM Standards:
solution is processed by this practice to prepare separate
C698Test Methods for Chemical, Mass Spectrometric, and
solutions of plutonium and uranium for mass spectrometric
isotopic abundance analysis using Test Method C698, C1625,
1
This practice is under the jurisdiction of ASTM Committee C26 on Nuclear or C1672.Appropriate portions are taken to provide up to 5 µg
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
ofplutoniumontheionexchangecolumntobeseparatedfrom
Test.
0.5mgorlessofuranium.Alldilutionsshouldbeperformedby
Current edition approved June 1, 2015. Published July 2015. DOI: 10.1520/
mass to ensure the smallest uncertainty possible. This practice
C1816-15.
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

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C1816 − 15
canbeusedforhigheruraniumtoplutoniumratios,butcolumn abundance determination. Uranium and plutonium content as
rinsing volumes should be adjusted accordingly (see 10.1.3.8). well as isotopic abundances usingTIMS can be determined by
Using the volumes proposed in this practice leads to a using this separation practice and by following Test Methods
separationefficiencyofatleast99.999%betweenura
...

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