ASTM C1411-20

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.

General Information

• Status: Published
• Publication Date: 30-Jun-2020
• ICS: 27.120.30 - Fissile materials and nuclear fuel technology
• Technical Committee: C26 - Nuclear Fuel Cycle
• Drafting Committee: C26.05 - Methods of Test

Relations

• Replaces: ASTM C1411-14 - Standard Practice for The Ion Exchange Separation of Uranium and Plutonium Prior to Isotopic Analysis
• Effective Date: 01-Jul-2020
• Refers: ASTM C859-24 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Jan-2024
• Refers: ASTM C1168-23 - Standard Practice for Preparation and Dissolution of Plutonium Materials for Analysis
• Effective Date: 01-Oct-2023
• Refers: ASTM C1625-19 - Standard Test Method for Uranium and Plutonium Concentrations and Isotopic Abundances by Thermal Ionization Mass Spectrometry
• Effective Date: 15-Sep-2019
• Refers: ASTM C698-16 - Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Mixed Oxides ((U, Pu)O<inf>2</inf>)
• Effective Date: 01-Jun-2016
• Refers: ASTM C1168-15 - Standard Practice for Preparation and Dissolution of Plutonium Materials for Analysis
• Effective Date: 01-Sep-2015
• Refers: ASTM C859-14a - Standard Terminology Relating to Nuclear Materials
• Effective Date: 15-Jun-2014
• Refers: ASTM C859-14 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 15-Jan-2014
• Refers: ASTM C859-13a - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Jun-2013
• Refers: ASTM C859-13 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-May-2013
• Refers: ASTM C833-13 - Standard Specification for Sintered (Uranium-Plutonium) Dioxide Pellets
• Effective Date: 01-Jan-2013
• Refers: ASTM C1625-12 - Standard Test Method for Uranium and Plutonium Concentrations and Isotopic Abundances by Thermal Ionization Mass Spectrometry
• Effective Date: 01-Jun-2012
• Refers: ASTM C859-10b - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Nov-2010
• Refers: ASTM C859-10a - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Aug-2010
• Refers: ASTM C698-10 - Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Mixed Oxides ((U, Pu)O₂)
• Effective Date: 01-Jun-2010

Overview

ASTM C1411-20: Standard Practice for The Ion Exchange Separation of Uranium and Plutonium Prior to Isotopic Analysis provides a comprehensive procedure for the chemical separation of uranium and plutonium before their isotopic analysis using thermal ionization mass spectrometry (TIMS). This practice addresses the challenge of mass peak interferences between uranium, plutonium, and americium isotopes, ensuring high-purity sample solutions essential for reliable isotopic measurements. Institutions involved in nuclear fuel analysis, quality control, and research rely on this standard to achieve conformance with fuel isotopic composition requirements as defined in ASTM Specifications C833 and C1008.

Key Topics

• Ion Exchange Separation: Detailed guidance on using ion exchange columns to separate uranium and plutonium, thereby removing impurities and isobaric interferences such as uranium-238, plutonium-238, plutonium-241, and americium-241.
• Sample Preparation: Stepwise procedures for dissolving solid nuclear material samples and preparing aliquots using specific acid mixtures, ensuring complete dissolution and accurate subsequent analysis.
• Valence Adjustment: Recommendations for adjusting oxidation states using ferrous sulfate or hydrogen peroxide, which is critical to successful ion exchange separation and precludes interferences from transition metals such as iron.
• Purity and Interferences: Emphasis on the necessity for high chemical purity in separated samples. Discusses the potential impacts of organic and elemental impurities, as well as methods to destroy residue organics following separation.
• Safety Considerations: Highlights the use of strong acids and the need for appropriate laboratory safety practices, especially when handling hazardous chemicals such as hydrofluoric acid.

Applications

The practices described in ASTM C1411-20 are essential in several nuclear science and industry contexts:

• Nuclear Fuel Analysis: Supports determination of uranium and plutonium isotopic compositions in nuclear-grade mixed oxide fuels used in light water and fast reactors.
• Quality Control: Ensures compliance with reactor fuel specifications, providing reliable data for regulatory and operational certification.
• Research Laboratories: Used in specialty isotope laboratories to prepare high-purity uranium and plutonium specimens for detailed isotopic analysis by TIMS.
• Safeguards and Non-Proliferation: Facilitates accurate tracking of nuclear materials by enabling precise isotopic fingerprinting, which is critical for non-proliferation monitoring and treaty verification.

Related Standards

ASTM C1411-20 is used in conjunction with several other key ASTM standards related to nuclear materials and their analysis:

• ASTM C698: Test methods for chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade mixed oxides.
• ASTM C833: Specification for sintered (uranium-plutonium) dioxide pellets for light water reactors.
• ASTM C1008: Specification for sintered (uranium-plutonium) dioxide pellets for fast reactor fuel.
• ASTM C1168: Practice for preparation and dissolution of plutonium materials for analysis.
• ASTM C1347: Practice for preparation and dissolution of uranium materials for analysis.
• ASTM C1625: Test method for uranium and plutonium concentrations and isotopic abundances by TIMS.
• ASTM D1193: Specification for reagent water used in laboratory settings.

Practical Value

Implementing ASTM C1411-20 improves laboratory consistency, accuracy, and safety in the analysis of uranium and plutonium isotopic compositions. It is highly recommended for nuclear laboratories, fuel manufacturers, and regulatory bodies aiming to perform reliable mass spectrometric analysis and maintain compliance with international nuclear standards.

Keywords: ion exchange, uranium separation, plutonium separation, isotopic analysis, thermal ionization mass spectrometry (TIMS), nuclear fuel, ASTM C1411-20, sample purity, nuclear material analysis.

Standards Content (Sample)

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
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)
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
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 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
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
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/
C1411-20.
(IV), and to adjust the final acid concentration to8M HNO .
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
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
C1411 − 20
4.1.2 A hydrogen peroxide reduction may be used for 6.4 Elemental impurities, especially alkali elements, tend to
relatively pure samples which do not contain excessive produce unstable ion emission and alter observed ratios in an
amounts of oxidizing impurities. The aliquant is dissolved in unpredictable manner.
8MHNO .Hydrogenperoxideisaddedtothealiquantpriorto
6.5 Isobaric impurities or contaminants will alter the ob-
fuming to reduce plutonium (VI) to the lower oxidation states.
served isotopic ratios; most notable of these for plutonium are
The solution is warmed on a hot plate to destroy excess
americium-241 and uranium-238; the most notable isobaric
4,5
hydrogen peroxide and stabilize plutonium (IV) in solution.
impurity for uranium is plutonium-238.
4.2 After valence adjustment, the resulting solution is
6.6 Extreme care must be taken to avoid contamination of
passed through an anion exchange column in the nitrate form
the sample by environmental uranium. The level of uranium
which retains the plutonium; uranium and americium are not
contamination should be measured by analyzing an aliquant of
absorbed. The adsorbed plutonium is washed with additional
8MHNO reagentasablanktakenthroughthesamechemical
8 M nitric acid(HNO )toremoveimpuritiesandthenstripped
processing as the sample and computing the amount of
from the column with 0.36 M hydrochloric acid (HCl) and
uranium it contains.
0.01 M hydrofluoric acid (HF). The effluent containing the
uraniumandamericiumisconvertedtoaHClmedium,andthis 7. Apparatus
solution is passed through an anion exchange column in the
7.1 Ion Exchange Columns—Disposable, 0.9 cm id×3cm
chloride form which retains the uranium. The adsorbed ura-
with a 15 mL reservoir.
nium is washed with additional 9 M HCl to remove the
7.2 Beakers or Alternate Acceptable Containers—
impurities and then stripped from the column with 0.1 M HCl.
Pretreated, 20 to 30 mL, borosilicate glass. To avoid cross
5. Significance and Use contamination, use only new borosilicate glass containers
pretreated by heating in 4 M HNO to leach uranium, rinsed in
5.1 Uranium and plutonium are used in nuclear reactor fuel
deionized water, and air or oven dried prior to use.
and must be analyzed to insure that they meet certain criteria
for isotopic composition as described in Specifications C833 7.3 Infrared Heating Lamps or Hot Plate, with adjustable
and C1008. This practice is used to chemically separate the low and high heat settings.
samemasspeakinterferencesfromuraniumandplutoniumand
7.4 Transfer Pipets—Disposable.
from other impurities prior to isotopic abundance determina-
tion by thermal ionization mass spectrometry.
8. Reagents
5.2 In those facilities where perchloric acid use is tolerated, 8.1 Reagent grade or better chemicals should be used.
the separation in Test Method C698 may be used prior to
Unless otherwise indicated, it is intended that all reagents
isotopic abundance determination. Uranium and plutonium conform to the specifications of the Committee on Analytical
concentrations as well as isotopic abundances using thermal
Reagents of the American Chemical Society where such
ionization mass spectrometry can be determined using this specifications are available. Other grades of reagents may be
separation and following Test Method C1625. used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
6. Interferences
accuracy of measurements made on the prepared materials.
6.1 The separated heavy element fractions placed on mass Store solutions in appropriate polyethylene or glass bottles
except as noted.
spectrometric filaments must be very pure. The quantity
required depends upon the sensitivity of the instrument detec-
8.2 Purity of Water—Unless otherwise indicated, references
tion system. Chemical purity of the sample becomes more
to water shall be understood to mean laboratory accepted
important as the sample size decreases, because the ion
demineralized or deionized water conforming to Specification
emission of the sample is repressed by impurities.
D1193.
6.2 Organicsfromionexchangeresindegradationproducts,
8.3 Nitric Acid (sp gr 1.42), 16 M—Concentratednitricacid
if present, could affect the response of the mass spectrometer
(HNO ).
during the plutonium and uranium isotopic abundance mea-
8.4 Nitric Acid, 8 M—Add500mLofHNO (spgr1.42)to
surements.Evaporationofthesampleswithconcentratednitric
about 400 mL of water and dilute to 1 L.
acid after the ion exchange separation has been found to
destroy any resin degradation products. Organics from extrac- 8.5 Nitric Acid, 4 M—Add250mLofHNO (spgr1.42)to
tion resins may not be destroyed by this process, and will about 700 mL of water and dilute to 1 L with water.
require a perchloric acid treatment, heating in a furnace at
8.6 Nitric Acid, 3 M—Add187mLofHNO (spgr1.42)to
500 °C, or both.
about 750 mL of water and dilute to 1 L with water.
6.3 The use of hydrogen peroxide for valence adjustment,
whenpossible,avoidstheadditionofiron,anelementwhichis
Reagent Chemicals, American Chemical Society Specifications, American
not cleanly removed from uranium by HCl ion exchange.
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Kressin, I.V. and Waterbury, G.R., Anal. Chem. Vol 34, No. 12, p. 1598, 1962. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Pietri, C.E., Freeman, B.P., and Weiss, J.R.,
...

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
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
2.1 ASTM Standards:
C698 Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Mixed Oxides ((U,
Pu)O )
C833 Specification for Sintered (Uranium-Plutonium) Dioxide Pellets for Light Water Reactors
C859 Terminology Relating to Nuclear Materials
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
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.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
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
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 nitrous fumes has been found to be acceptable. This method avoids the
addition of Fe, which could interfere with electrodeposition of prior to mass spectrometry analysis samples.
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 16 M
HNO is added to oxidize plutonium (III) to plutonium (IV), and to adjust the final acid concentration to 8 M HNO .
3 3
4.1.2 A hydrogen peroxide reduction may be used for relatively pure samples which do not contain excessive amounts of
oxidizing impurities. The aliquant is dissolved in 8 M8 M HNO . Hydrogen peroxide is added to the aliquant prior to fuming to
reduce plutonium (VI) to the lower oxidation states. The solution is warmed on a hot plate to destroy excess hydrogen peroxide
4,5
and stabilize plutonium (IV) in solution.
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 absorbed. The adsorbed plutonium is washed with additional 8 M 8 M nitric
acid (HNO ) to remove impurities and then stripped from the column with 0.36 M hydrochloric acid (HCl) and 0.01 M 0.01 M
hydrofluoric acid (HF). The effluent containing the uranium and americium is converted to a HCl medium, and this solution is
passed through an anion exchange column in the chloride form which retains the uranium. The adsorbed uranium is washed with
additional 9 M HCl to remove the impurities and then stripped from the column with 0.1 M HCl.
5. 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 SpecificationSpecifications 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.
6. Interferences
6.1 The separated heavy element fractions placed on mass spectrometric filaments must be very pure. The quantity required
depends upon the sensitivity of the instrument detection system. Chemical purity of the sample becomes more important as the
sample size decreases, because the ion emission of the sample is repressed by impurities.
6.2 Organics from ion exchange resin degradation products, if present, could affect the response of the mass spectrometer during
the plutonium and uranium isotopic abundance measurements. Evaporation of the samples with concentrated nitric acid after the
ion exchange separation has been found to destroy any resin degradation products. Organics from extraction resins may not be
destroyed by this process, and will require a perchloric acid treatment, heating in a furnace at 500°C,500 °C, or both.
6.3 The use of hydrogen peroxide for valence adjustment, when possible, avoids the addition of iron, an element which is not
cleanly removed from uranium by HCl ion exchange.
6.4 Elemental impurities, especially alkali elements, tend to produce unstable ion emission and alter observed ratios in an
unpredictable manner.
6.5 Isobaric impurities or contaminants will alter the observed isotopic ratios; most notable of these for plutonium are
americium-241 and uranium-238; the most notable isobaric impurity for uranium is plutonium-238.
6.6 Extreme care must be taken to avoid contamination of the sample by environmental uranium. The level of uranium
contamination should be measured by analyzing an aliquant of 8 M HNO reagent as a blank taken through the same chemical
processing as the sample and computing the amount of uranium it contains.
7. Apparatus
7.1 Ion Exchange Columns—Disposable, 0.9 cm id × 3 cm with a 15 mL reservoir.
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 prior to mass spectrometry analysis samples.
Kressin, I.V. Kressin and G.R. Waterbury, G.R., Anal. Chem. 34(12) , 1598 (1962).Vol 34, No. 12, p. 1598, 1962.
C.E. Pietri, B.P.C.E., Freeman, B.P., and J.R. Weiss, J.R., DOE/NBL-298DOE/NBL-298, , September Sept. 1981.
C1411 − 20
7.2 Beakers or Alternate Acceptable Containers—pretreated, 20-30 Pretreated, 20 to 30 mL, borosilicate glass. To avoid cross
contamination, use only new borosilicate glass containers pretreated by heating in 4 M HNO to leach uranium, rinsed in deionized
water, and air or oven dried prior to use.
7.3 Infrared Heating Lamps or Hot Plate, Infrared Heating Lamps or Hot Plate with adjustable low and high heat settings.
7.4 Transfer Pipets—Transfer Pipets—Disposable.Disposable.
8. Reagents
8.1 Reagent grade or better chemicals should be used. Unless otherwise indicated, it is intended that all reagents conform to the
specifications of the Committee on Analytical Reagents of the American Chemical Society where such specifications are available.
Other grades of reagents may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use
without lessening the accuracy of measurements made on the prepared materials. Store solutions in appropriate polyethylene or
glass bottles except as noted.
8.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean laboratory accepted
demineralized or deionized water conforming to Specification D1193.
8.3 Nitric Acid (sp gr 1.42), 16 M—concentratedConcentrated nitric acid (HNO ).
8.4 Nitric Acid, 8 M— Add 500 mL of HNO (sp gr 1.42) to about 400 mL of water and dilute to 1 L.
8.5 Nitric Acid, 4 M— Add 250 mL of HNO (sp gr 1.42) to about 700 mL of water and dilute to 1 L with water.
8.6 Nitric Acid, 3 M— Add 187 mL of HNO (sp gr 1.42) to about 750 mL of water and dilute to 1 L with water.
8.7 Hydrochloric Acid (sp gr 1.19), 12 M—concentratedConcentrated hydrochloric acid (HCl).
8.8 Hydrochloric Acid, 9M—Add 750 mlmL of HCl (sp. gr.(sp gr 1.19) to about 250 mlmL of water and dilute to 1 L.
8.9 Hydrofluoric Acid (sp gr 1.18), 29 M—concentratedConcentrated hydrofluoric acid (HF).
8.10 Hydrochloric Acid, 0.1 M—Add 8 mL of HCl (sp gr 1.1
...