ASTM C1206-02

Standard Test Method for Plutonium by Iron (II)/Chromium (VI) Amperometric Titration

SIGNIFICANCE AND USE
All plutonium materials covered in this test method are used in the preparation of nuclear-reactor fuels. In order to be suitable for this purpose, the materials must meet specified criteria for plutonium content. This test method is used to verify the plutonium content.
A primary standard dichromate such as that available from National Institute of Standards and Technology (NIST) or a dichromate traceable to a primary standard such as New Brunswick Laboratory (NBL) plutonium standard, is required for this technique.
SCOPE
1.1 This test method covers the determination of plutonium in unirradiated nuclear-grade plutonium dioxide, uranium-plutonium mixed oxides with uranium (U)/plutonium (Pu) ratios up to 21, plutonium metal, and plutonium nitrate solutions. Optimum quantities of plutonium to measure are 7 to 15 mg.
1.2 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-2002
• 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 C1206-91(1996) - Standard Test Method for Plutonium by Iron (II)/Chromium (VI) Amperometric Titration
• Effective Date: 10-Jan-2002
• Replaced By: ASTM C1206-02(2010) - Standard Test Method for Plutonium by Iron (II)/Chromium (VI) Amperometric Titration (Withdrawn 2015)
• Effective Date: 01-Jan-2010
• Referred By: ASTM C759-18 - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Plutonium Nitrate Solutions
• Effective Date: 10-Jan-2002
• Referred By: ASTM C758-18 - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Plutonium Metal
• Effective Date: 10-Jan-2002
• Referred By: 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: 10-Jan-2002
• Referred By: ASTM C697-16 - Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Plutonium Dioxide Powders and Pellets
• Effective Date: 10-Jan-2002

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:C1206–02
Standard Test Method for
Plutonium by Iron (II)/Chromium (VI) Amperometric
1
Titration
This standard is issued under the fixed designation C1206; 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 its application to safeguards has the approval of the proper
regulatory authorities.
1.1 This test method covers the determination of plutonium
in unirradiated nuclear-grade plutonium dioxide, uranium-
4. Summary of Test Method
plutonium mixed oxides with uranium (U)/plutonium (Pu)
4.1 Amperometric titrations are based on the measured
ratios up to 21, plutonium metal, and plutonium nitrate
change in the current flow between two electrodes, held at
solutions.Optimumquantitiesofplutoniumtomeasureare7to
constant potential, when a titrant is added. The plutonium is
15 mg.
first oxidized to the +6 oxidation state in a dilute sulfuric acid
1.2 This standard does not purport to address all of the
solution with argentic oxide. The excess oxidant is destroyed
safety concerns, if any, associated with its use. It is the
by heating, and the Pu(VI) is then reduced to Pu(IV) by excess
responsibility of the user of this standard to establish appro-
Fe(II) during the titration. The excess Fe(II) is titrated by
priate safety and health practices and determine the applica-
Cr(VI), and the Pu determined by difference from the quanti-
bility of regulatory limitations prior to use.
ties of the two titrants.
2. Referenced Documents 4.2 Oxide and metal samples are prepared to produce final
2
solutions as a soluble sulfate. Plutonium-nitrate solutions can
2.1 ASTM Standards:
beintroduceddirectlyatthebeginningoftheprocedureandare
C1168 Practice for Preparation and Dissolution of Pluto-
later diluted with sulfuric acid. Chlorides must be removed.
nium Materials for Analysis
5. Significance and Use
3. Committee C-26 Safeguards Statement
5.1 All plutonium materials covered in this test method are
3.1 The materials [nuclear-grade mixed oxides (U, Pu)O
2
used in the preparation of nuclear-reactor fuels. In order to be
powders,pellets,Pumetal,Puoxides,andPunitrates]towhich
suitable for this purpose, the materials must meet specified
this test method applies, are subject to nuclear safeguards
criteria for plutonium content. This test method is used to
regulations governing their possession and use. This analytical
verify the plutonium content.
test method has been designated as technically acceptable for
5.2 A primary standard dichromate such as that available
generating safeguards accountability measurement data for
fromNationalInstituteofStandardsandTechnology(NIST)or
plutonium.
a dichromate traceable to a primary standard such as New
3.2 When used in conjunction with appropriate standard
Brunswick Laboratory (NBL) plutonium standard, is required
referencematerialthistestmethodcandemonstratetraceability
for this technique.
to the national measurement base. However, adherence to this
testmethoddoesnotautomaticallyguaranteeregulatoryaccep-
6. Interferences
tance of the resulting safeguards measurements. It remains the
6.1 Interference is caused by ions that are oxidized by
sole responsibility of the user of this test method to ensure that
argentic oxide and reduced by ferrous ion in sulfuric-acid
solution. Elements that may be present in plutonium materials
1
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear
and that will produce quantitative positive errors include
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
vanadium (V), chromium (Cr), and manganese (Mn). Correc-
Test.
tion can be made for these elements by calculation when they
Current edition approved Jan. 10, 2002. Published April 2002. Originally
do not individually exceed 200 µg impurity elements per gram
published as C1206–91. Last previous edition C1206–91(1996). DOI: 10.1520/
C1206-02.
of plutonium.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
6.2 Other elements that will cause positive errors include
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
cerium (Ce), ruthenium (Ru), gold (Au), rhodium (Rh), plati-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. num (Pt), lead (Pb), and neptunium (Np). Americium (Am)
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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C1206–02
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does not interfere because it is not oxidized to higher valency such specifications are available.
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