ASTM C1168-01
(Practice)Standard Practice for Preparation and Dissolution of Plutonium Materials for Analysis
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 TitleSectionDissolution of Plutonium Metal with Hydrochloric Acid7.1Dissolution of Plutonium Metal with Sulfuric Acid7.2Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed Oxide by the Sealed-Reflux Technique7.3Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed Oxides by Sodium Bisulfate Fusion7.4Dissolution of Uranium-Plutonium Mixed Oxides and Low-Fired Plutonium Oxide in Beakers7.5
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
Relations
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: C 1168 – 01
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 3. Summary of Dissolution Methods
1.1 This practice is a compilation of dissolution techniques 3.1 Most plutonium-containing samples are dissolved with
for plutonium materials that are applicable to the test methods various mineral acids and, except for plutonium metal, with
used for characterizing these materials. Dissolution treatments applied heat. Dissolution-resistant materials are dissolved in
for the major plutonium materials assayed for plutonium or heated and sealed containers in which pressurization provides
analyzed for other components are listed. Aliquants of the a higher temperature than is attained at ambient pressure.
dissolved samples are dispensed on a weight basis when one of 3.2 Another dissolution technique is fusion of refractory
the analyses must be highly reliable, such as plutonium assay; plutonium oxide with sodium bisulfate.
otherwise they are dispensed on a volume basis. 3.3 The dissolved materials are quantitatively transferred to
1.2 The treatments, in order of presentation, are as follows: ataredpolyethylenedispensingbottleforsubsequentdeliveries
of weight aliquants for high-precision analysis methods, such
Procedure Title Section
as assays, or to a volumetric flask for deliveries of volume
Dissolution of Plutonium Metal with Hydrochloric Acid 7.1
aliquants for less precise analysis methods, such as impurity
Dissolution of Plutonium Metal with Sulfuric Acid 7.2
Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed 7.3
analyses. Acids, usually 1 M, are used as rinses to effect
Oxide by the Sealed-Reflux Technique
quantitative transfers and as diluents in the polyethylene
Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed 7.4
dispensing bottles and volumetric flasks. The use of water for
Oxides by Sodium Bisulfate Fusion
Dissolution of Uranium-Plutonium Mixed Oxides and Low-Fired 7.5
these purposes can, in some cases, result in hydrolysis of
Plutonium Oxide in Beakers
plutonium to produce polymers that, although soluble, are
1.3 The values stated in SI units are to be regarded as
nonreactive in separation treatments or in plutonium assay
standard. methods that have no pretreatments, such as fuming with acid.
1.4 This standard does not purport to address all of the 3.4 Plutonium metal is dissolved with hydrochloric acid or
safety concerns, if any, associated with its use. It is the with sulfuric acid.
responsibility of the user of this standard to establish appro- 3.5 Plutonium oxide, calcined at about 1000°C or lower, is
priate safety and health practices and determine the applica- dissolved with a mixture of hydrochloric, nitric, and hydrof-
3
bility of regulatory limitations prior to use. luoric acids using the sealed-reflux techniques (1). More
refractory plutonium oxide is dissolved with a fusion using
2. Referenced Documents
sodium bisuflate (2). Low-fired (<650°C) plutonium oxide can
2.1 ASTM Standards:
also be dissolved in a mixture of nitric and hydrofluoric acids
C 757 Specification for Nuclear-Grade Plutonium Dioxide in beakers. Plutonium oxide fired at temperatures above 650°C
2
Powder, Sinterable
may also be dissolved in beakers using a mixture of nitric and
C 833 Specification for Sintered (Uranium-Plutonium) Di- hydrofluoric acids when complete dissolution can be demon-
2
oxide Pellets
strated.
C 1008 Specification for Sintered (Uranium-Plutonium) Di- 3.6 Uranium-plutonium mixed oxide is dissolved in either
2
oxide Pellets—Fast Reactor Fuel
of three ways: sodium bisulfate fusion, a heated mixture of
nitric and hydrofluoric acids in a beaker, or a mixture of
hydrochloric,nitric,andhydrofluoricacidsbythesealed-reflux
1
This practice is under the jurisdiction of ASTM Committee C26 on Nuclear
technique.
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
3
published as C 1168–90. Last previous edition C 1168–90(1995). The boldface numbers in parentheses refer to a list of references at the end of
2
Annual Book of ASTM Standards, Vol 12.01. this practice.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
C 1168
3.7 Combinations of these dissolution techniques described
in 3.4 to 3.6 are sometimes used on di
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.