ASTM C1411-01

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 ion exchange separation procedure in Test Method E 267 may be used prior to isotopic abundance determination. Also, in those facilities where perchloric acid use is tolerated and when uranium and plutonium concentrations are to be determined as well as isotopic abundances using the thermal ionization mass spectrometer, the ion exchange separation procedure in Test Method E 267 may be used.
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 establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 09-Jan-2001
• 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 C1411-99 - Standard Practice for the Ion Exchange Separation of Uranium and Plutonium Prior to Isotopic Analysis
• Effective Date: 10-Jan-2001
• Replaced By: ASTM C1411-08 - Standard Practice for The Ion Exchange Separation of Uranium and Plutonium Prior to Isotopic Analysis
• Effective Date: 01-Jan-2008
• Referred By: ASTM C1871-22 - Standard Test Method for Determination of Uranium Isotopic Composition by the Double Spike Method Using a Thermal Ionization Mass Spectrometer
• Effective Date: 10-Jan-2001
• Referred By: ASTM C1832-23 - Standard Test Method for Determination of Uranium Isotopic Composition by Modified Total Evaporation (MTE) Method Using Thermal Ionization Mass Spectrometer
• Effective Date: 10-Jan-2001
• Referred By: ASTM C1590-21 - Standard Practice for Alternate Actinide Calibration for Inductively Coupled Plasma-Mass Spectrometry
• Effective Date: 10-Jan-2001
• Referred By: ASTM C1672-17 - Standard Test Method for Determination of Uranium or Plutonium Isotopic Composition or Concentration by the Total Evaporation Method Using a Thermal Ionization Mass Spectrometer
• Effective Date: 10-Jan-2001
• Referred By: ASTM C1625-19 - Standard Test Method for Uranium and Plutonium Concentrations and Isotopic Abundances by Thermal Ionization Mass Spectrometry
• Effective Date: 10-Jan-2001
• Referred By: ASTM E321-20 - Standard Test Method for Atom Percent Fission in Uranium and Plutonium Fuel (Neodymium-148 Method)
• Effective Date: 10-Jan-2001
• Referred By: ASTM C1816-16 - Standard Practice for The Ion Exchange Separation of Small Volume Samples Containing Uranium, Americium, and Plutonium Prior to Isotopic Abundance and Content Analysis
• Effective Date: 10-Jan-2001
• Referred By: ASTM C1415-18 - Standard Test Method for ²³⁸Pu Isotopic Abundance By Alpha Spectrometry
• Effective Date: 10-Jan-2001

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:C1411–01
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 processed by this practice to prepare separate solutions of
plutonium and uranium for mass spectrometric isotopic analy-
1.1 This practice is for the ion exchange separation of
sis using Method C 698, see Sec. 144 through 145 and 147.4
uranium and plutonium from each other and from other
through149oritsreplacement.Appropriatealiquantsaretaken
impurities for subsequent isotopic analysis by thermal ioniza-
to provide up to 1 mg of plutonium on the ion exchange
tion mass spectrometry. Plutonium–238 and uranium–238, and
columntobeseparatedfrom10mgorlessofuranium.Valence
plutonium–241 and americium–241, will appear as the same
adjustment is obtained by using one of two procedures as
mass peak and must be chemically separated prior to analysis.
described in 3.1.1 and 3.1.2 or by an alternative method
Only high purity solutions can be analyzed reliably using
demonstrated by the user to perform the equivalent reduction/
thermal ionization mass spectrometry.
4
oxidation procedure.
1.2 This standard may involve hazardous material, opera-
3.1.1 For any sample type, especially those containing large
tions, and equipment. This standard does not purport to
amounts of impurities, ferrous sulfate may be used for reduc-
address all of the safety concerns, if any, associated with its
tion. The aliquant is dissolved in 3 M HNO . Ferrous sulfate is
3
use. It is the responsibility of the user of this standard to
added to reduce all plutonium (VI) to plutonium (III), then 16
consult and establish appropriate safety and health practices
M HNO is added to oxidize plutonium (III) to plutonium (IV),
3
and determine the applicability of regulatory limitations prior
and to adjust the final acid concentration to8M HNO .
3
to use.
3.1.2 A hydrogen peroxide reduction may be used for
2. Referenced Documents relatively pure samples which do not contain excessive
amounts of oxidizing impurities. The aliquant is dissolved in 8
2.1 ASTM Standards:
M HNO . Hydrogen peroxide is added to the aliquant prior to
C 698 Standard Test Method for Chemical, Mass Spectro- 3
fuming to reduce plutonium (VI) to the lower oxidation states.
metric, and Spectrochemical Analysis of Nuclear-Grade
2
The solution is warmed on a hot plate to destroy excess
Mixed Oxides ((U, Pu)O ), Sections 141-149.
2
,
5 6
hydrogen peroxide and stabilize plutonium (IV) in solution.
C 833 Standard Specification for Sintered (Uranium, Pluto-
2
3.2 After valence adjustment, the resulting solution is
nium) Dioxide Pellets.
passed through an anion exchange column in the nitrate form
C 1008 Standard Specification for Sintered (Uranium, Plu-
2
which retains the plutonium; uranium and americium are not
tonium) Dioxide Pellets - Fast Reactor Fuel.
absorbed. The adsorbed plutonium is washed with additional 8
C 1168 StandardPracticeforPreparationandDissolutionof
2
M nitric acid (HNO ) to remove impurities and then stripped
Plutonium Materials for Analysis. 3
fromthecolumnwith 0.36 M hydrochloric acid(HCl)and 0.01
E 267 Standard Test Method for Uranium and Plutonium
3
M hydrofluoric acid (HF). The effluent containing the uranium
Concentrations and Isotopic Abundances.
andamericiumisconvertedtoaHClmedium,andthissolution
3. Summary of Practice
is passed through an anion exchange column in the chloride
form which retains the uranium. The adsorbed uranium is
3.1 Solid samples are dissolved according to Practice
C 1168 or other appropriate methods. The resulting solution is
1 4
This practice is under the jurisdiction of ASTM Committee C26 on Nuclear Reduction of all higher plutonium oxidation states to plutonium (III) by the
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of addition of hydroxylamine or NH CLO , followed by oxidation to plutonium (IV)
2 4
Test. by sodium nitrite and subsequent boiling to eliminate the nitrous fumes has been
Current edition approved Jan. 10, 2001. Published March 2001. Originally foundtobeacceptable.ThismethodavoidstheadditionofFe,whichcouldinterfere
published as C 1411–99. Last previous edition C 1411–99. with electrodeposition of mass spectrometric samples.
2 5
Annual Book of ASTM Standards, Vol 12.01. I.V. Kressin and G.R. Waterbury, Anal. Chem. 34(12), 1598 (1962).
3 6
Annual Book of ASTM Standards, Vol 12.02. C.E. Pietri, B.P. Freeman, and J.R. Weiss, DOE/NBL-298, September 1981.
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