ASTM C1168-08

Standard Practice for Preparation and Dissolution of Plutonium Materials for Analysis

SIGNIFICANCE AND USE
The materials covered are plutonium metal, plutonium oxide, and uranium-plutonium mixed oxide, including those that must meet ASTM product specifications.  
Plutonium and uranium mixtures are used as nuclear reactor fuels. For use as a nuclear reactor fuel, the material must meet certain criteria for combined uranium and pluto-
nium content, effective fissile content, and impurity content as described in Specifications C 757, C 833, and C 1008. The material is assayed for plutonium and uranium to determine if the content is correct as specified by the purchaser.
The materials not covered are unique plutonium materials, including alloys, compounds, and scrap materials. The user must determine the applicability of this practice to these other materials. In general, these unique plutonium materials are dissolved with various acid mixtures or by fusion with various fluxes. Many plutonium salts are soluble in hydrochloric acid.
SCOPE
1.1 This practice is a compilation of dissolution techniques for plutonium materials that are applicable to the test methods used for characterizing these materials. Dissolution treatments for the major plutonium materials assayed for plutonium or analyzed for other components are listed. Aliquants of the dissolved samples are dispensed on a weight basis when one of the analyses must be highly reliable, such as plutonium assay; otherwise they are dispensed on a volume basis.
1.2 The treatments, in order of presentation, are as follows:
  Procedure TitleSection Dissolution of Plutonium Metal with Hydrochloric Acid9.1 Dissolution of Plutonium Metal with Sulfuric Acid9.2 Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed
Oxide by the Sealed-Reflux Technique9.3 Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed
Oxides by Sodium Bisulfate Fusion9.4 Dissolution of Uranium-Plutonium Mixed Oxides and Low-Fired
Plutonium Oxide in Beakers9.5
1.3 The values stated in SI units are to be regarded as 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-Dec-2007
• 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 C1168-01 - Standard Practice for Preparation and Dissolution of Plutonium Materials for Analysis
• Effective Date: 01-Jan-2008
• Replaced By: ASTM C1168-15 - Standard Practice for Preparation and Dissolution of Plutonium Materials for Analysis
• Effective Date: 01-Sep-2015
• Referred By: ASTM C1415-18 - Standard Test Method for ²³⁸Pu Isotopic Abundance By Alpha Spectrometry
• Effective Date: 01-Jan-2008
• Referred By: ASTM C1204-14(2023) - Standard Test Method for Uranium in Presence of Plutonium by Iron(II) Reduction in Phosphoric Acid Followed by Chromium(VI) Titration
• Effective Date: 01-Jan-2008
• Referred By: ASTM C1221-10(2018) - Standard Test Method for Nondestructive Analysis of Special Nuclear Materials in Homogeneous Solutions by Gamma-Ray Spectrometry
• Effective Date: 01-Jan-2008
• Referred By: ASTM C1347-08(2023) - Standard Practice for Preparation and Dissolution of Uranium Materials for Analysis
• Effective Date: 01-Jan-2008
• Referred By: ASTM C1625-19 - Standard Test Method for Uranium and Plutonium Concentrations and Isotopic Abundances by Thermal Ionization Mass Spectrometry
• Effective Date: 01-Jan-2008
• Referred By: ASTM C1307-21 - Standard Test Method for Plutonium Assay by Plutonium (III) Diode Array Spectrophotometry
• Effective Date: 01-Jan-2008
• Referred By: ASTM C1637-21 - Standard Test Method for Determination of Impurities in Plutonium Materials—Acid Digestion and Inductively Coupled Plasma-Mass Spectroscopy (ICP-MS) Analysis
• Effective Date: 01-Jan-2008
• Referred By: ASTM E321-20 - Standard Test Method for Atom Percent Fission in Uranium and Plutonium Fuel (Neodymium-148 Method)
• Effective Date: 01-Jan-2008
• Referred By: ASTM C1432-15 - Standard Test Method for Determination of Impurities in Plutonium: Acid Dissolution, Ion Exchange Matrix Separation, and Inductively Coupled Plasma-Atomic Emission Spectroscopic (ICP/AES) Analysis
• Effective Date: 01-Jan-2008
• Referred By: ASTM C1855-18 - Standard Test Method for Determination of Uranium and Plutonium Concentration in Aqueous Solutions Using Hybrid K-Edge Densitometry and X-Ray Fluorescence
• Effective Date: 01-Jan-2008
• Referred By: ASTM C1411-20 - Standard Practice for The Ion Exchange Separation of Uranium and Plutonium Prior to Isotopic Analysis
• Effective Date: 01-Jan-2008
• Referred By: ASTM C1647-20 - Standard Practice for Removal of Uranium or Plutonium, or both, for Impurity Assay in Uranium or Plutonium Materials
• Effective Date: 01-Jan-2008
• Referred By: ASTM C1268-15 - Standard Test Method for Quantitative Determination of ²⁴¹Am in Plutonium by Gamma-Ray Spectrometry
• Effective Date: 01-Jan-2008

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:C1168 −08
StandardPractice for
Preparation and Dissolution of Plutonium Materials for
1
Analysis
This standard is issued under the fixed designation C1168; 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 C1008 Specification for Sintered (Uranium-Plutonium)
3
DioxidePellets—Fast Reactor Fuel (Withdrawn 2014)
1.1 This practice is a compilation of dissolution techniques
for plutonium materials that are applicable to the test methods
3. Terminology
used for characterizing these materials. Dissolution treatments
3.1 Definitions—For definitions of terms used in this
for the major plutonium materials assayed for plutonium or
standard, refer to C859.
analyzed for other components are listed. Aliquants of the
dissolved samples are dispensed on a weight basis when one of
4. Summary of Dissolution Methods
the analyses must be highly reliable, such as plutonium assay;
otherwise they are dispensed on a volume basis. 4.1 Most plutonium-containing samples are dissolved with
various mineral acids and, except for plutonium metal, with
1.2 The treatments, in order of presentation, are as follows:
applied heat. Dissolution-resistant materials are dissolved in
Procedure Title Section
heated and sealed containers in which pressurization provides
Dissolution of Plutonium Metal with Hydrochloric Acid 9.1
Dissolution of Plutonium Metal with Sulfuric Acid 9.2 a higher temperature than is attained at ambient pressure.
Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed 9.3
4.2 Another dissolution technique is fusion of refractory
Oxide by the Sealed-Reflux Technique
Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed 9.4
plutonium oxide with sodium bisulfate flux.
Oxides by Sodium Bisulfate Fusion
4.3 The dissolved materials are quantitatively transferred to
Dissolution of Uranium-Plutonium Mixed Oxides and Low-Fired 9.5
Plutonium Oxide in Beakers
ataredpolyethylenedispensingbottleforsubsequentdeliveries
1.3 The values stated in SI units are to be regarded as of weight aliquants for high-precision analysis methods, such
standard.
as assays, or to a volumetric flask for deliveries of volume
aliquants for less precise analysis methods, such as impurity
1.4 This standard does not purport to address all of the
analyses. Acids, usually 1 M, are used as rinses to effect
safety concerns, if any, associated with its use. It is the
quantitative transfers and as diluents in the polyethylene
responsibility of the user of this standard to establish appro-
dispensing bottles and volumetric flasks. The use of water for
priate safety and health practices and determine the applica-
these purposes can, in some cases, result in hydrolysis of
bility of regulatory limitations prior to use.
plutonium to produce polymers that, although soluble, are
2. Referenced Documents nonreactive in separation treatments or in plutonium assay
2
methods that have no pretreatments, such as fuming with acid.
2.1 ASTM Standards:
C757 Specification for Nuclear-Grade Plutonium Dioxide 4.4 Plutonium metal is dissolved with hydrochloric acid or
Powder, Sinterable
with sulfuric acid.
C833 Specification for Sintered (Uranium-Plutonium) Diox-
4.5 Plutonium oxide, calcined at about 1000°C or lower, is
ide Pellets
dissolved with a mixture of hydrochloric, nitric, and hydroflu-
C859 Terminology Relating to Nuclear Materials
4
oric acids using the sealed-reflux techniques (1). More refrac-
tory plutonium oxide is dissolved with a fusion using sodium
1
bisuflate flux (2). Low-fired (<650°C) plutonium oxide can
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
also be dissolved in a mixture of nitric and hydrofluoric acids
Test.
in beakers. Plutonium oxide fired at temperatures above 650°C
Current edition approved Jan. 1, 2008. Published February 2008. Originally
approved in 1990. Last previous edition approved in 2001 as C1168 – 01. DOI:
10.1520/C1168-08.
2 3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or The last approved version of this historical standard is referenced on
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM www.astm.org.
4
Standards volume information, refer to the standard’s Document Summary page on The boldface numbers in parentheses refer to a list of references at the end of
the ASTM website. this practice.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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C11
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This document is not anASTM standard and is intended only to provide the user of anASTM 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:C1168–01 Designation: C 1168 – 08
Standard Practice for
Preparation and Dissolution of Plutonium Materials for
1
Analysis
This standard is issued under the fixed designation C 1168; 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
1.1 This practice is a compilation of dissolution techniques for plutonium materials that are applicable to the test methods used
for characterizing these materials. Dissolution treatments for the major plutonium materials assayed for plutonium or analyzed for
other components are listed. Aliquants of the dissolved samples are dispensed on a weight basis when one of the analyses must
be highly reliable, such as plutonium assay; otherwise they are dispensed on a volume basis.
1.2 The treatments, in order of presentation, are as follows:
Procedure Title Section
Dissolution of Plutonium Metal with Hydrochloric Acid 7.1
Dissolution of Plutonium Metal with Hydrochloric Acid 9.1
Dissolution of Plutonium Metal with Sulfuric Acid 7.2
Dissolution of Plutonium Metal with Sulfuric Acid 9.2
Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed 7.3
Oxide by the Sealed-Reflux Technique
Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed 9.3
Oxide by the Sealed-Reflux Technique
Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed 7.4
Oxides by Sodium Bisulfate Fusion
Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed 9.4
Oxides by Sodium Bisulfate Fusion
Dissolution of Uranium-Plutonium Mixed Oxides and Low-Fired 7.5
Plutonium Oxide in Beakers
Dissolution of Uranium-Plutonium Mixed Oxides and Low-Fired 9.5
Plutonium Oxide in Beakers
1.3 The values stated in SI units are to be regarded as 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:
C 757 Specification for Nuclear-Grade Plutonium Dioxide Powder, Sinterable
2
C 833Specification for Sintered (Uranium-Plutonium) Dioxide Pellets Specification for Sintered (Uranium-Plutonium)
Dioxide Pellets
C 859 Terminology Relating to Nuclear Materials
C 1008 Specification for Sintered (Uranium-Plutonium) Dioxide Pellets—Fast Reactor Fuel
3. Terminology
3.1 Definitions: For definitions of terms used in this standard, refer to C 859.
4. Summary of Dissolution Methods
3.1Most4.1 Most plutonium-containing samples are dissolved with various mineral acids and, except for plutonium metal, with
appliedheat.Dissolution-resistantmaterialsaredissolvedinheatedandsealedcontainersinwhichpressurizationprovidesahigher
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. 10, 2001. Published March 2001. Originally published as C 1168–90. Last previous edition C 1168–90(1995).
Current edition approved Jan. 1, 2008. Published February 2008. Originally approved in 1990. Last previous edition approved in 2001 as C 1168 – 01.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
, Vol 12.01.volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

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C1168–08
temperature than is attained at ambient pressure.
34.2 Another dissolution technique is fusion of refractory plutonium oxide with sodium bisulfate flux.
3.3The4.3 The dissolved materials are quantitatively transferred to a tared polyethylene dispensing bottle for subsequent
deliveries of weight aliquants for high-precision analysis methods, such as assays, or to a volumetric flask for deliveries of volume
aliquants for less precise analysis methods, such as impurity analyses.Acids, usually 1 M, are used as rinses to effect quantitative
transfers and as diluents in the polyethylene dispensing bottles and volumetric flasks. The use of water for these purposes can, in
some cases, result in hyd
...