ASTM C1206-91(1996)

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

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

• Replaced By: ASTM C1206-02 - Standard Test Method for Plutonium by Iron (II)/Chromium (VI) Amperometric Titration
• 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NOTICE: This standard has either been superseded and replaced by a new version or
withdrawn.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: C 1206 – 91 (Reapproved 1996)
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Plutonium by Iron (II)/Chromium (VI) Amperometric
1
Titration
This standard is issued under the fixed designation C 1206; 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 regulations governing their possession and use. This analytical
test method has been designated as technically acceptable for
1.1 This test method covers the determination of plutonium
generating safeguards accountability measurement data for
in unirradiated nuclear-grade plutonium dioxide, uranium-
plutonium.
plutonium mixed oxides with uranium (U)/plutonium (Pu)
3.2 When used in conjunction with appropriate standard
ratios up to 21, plutonium metal, and plutonium nitrate
reference material this test method can demonstrate traceability
solutions. Optimum quantities of plutonium to measure are 7 to
to the national measurement base. However, adherence to this
15 mg.
test method does not automatically guarantee regulatory accep-
1.2 This standard does not purport to address all of the
tance of the resulting safeguards measurements. It remains the
safety concerns, if any, associated with its use. It is the
sole responsibility of the user of this test method to ensure that
responsibility of the user of this standard to establish appro-
its application to safeguards has the approval of the proper
priate safety and health practices and determine the applica-
regulatory authorities.
bility of regulatory limitations prior to use.
4. Summary of Test Method
2. Referenced Documents
4.1 Amperometric titrations are based on the measured
2.1 ASTM Standards:
change in the current flow between two electrodes, held at
C 697 Test Methods for Chemical, Mass Spectrometric, and
constant potential, when a titrant is added. The plutonium is
Spectrochemical Analysis of Nuclear-Grade Plutonium
2
first oxidized to the +6 oxidation state in a dilute sulfuric acid
Dioxide Powders and Pellets
solution with argentic oxide. The excess oxidant is destroyed
C 698 Test Methods for Chemical, Mass Spectrometric, and
by heating, and the Pu(VI) is then reduced to Pu(IV) by excess
Spectrochemical Analysis of Nuclear-Grade Mixed Oxides
2
Fe(II) during the titration. The excess Fe(II) is titrated by
((U, Pu)O )
2
Cr(VI), and the Pu determined by difference from the quanti-
C 757 Specification for Nuclear-Grade Plutonium Dioxide
2 ties of the two titrants.
Powder, Sinterable
4.2 Oxide and metal samples are prepared to produce final
C 758 Test Methods for Chemical, Mass Spectrometric,
solutions as a soluble sulfate. Plutonium-nitrate solutions can
Spectrochemical, Nuclear, and Radiochemical Analysis of
2
be introduced directly at the beginning of the procedure and are
Nuclear-Grade Plutonium Metal
later diluted with sulfuric acid. Chlorides must be removed.
C 759 Test Methods for Chemical, Mass Spectrometric,
Spectrochemical, Nuclear, and Radiochemical Analysis of
5. Significance and Use
2
Nuclear-Grade Plutonium Nitrate Solutions
5.1 All plutonium materials covered in this test method are
C 833 Specification for Sintered (Uranium-Plutonium) Di-
2 used in the preparation of nuclear-reactor fuels. In order to be
oxide Pellets
suitable for this purpose, the materials must meet specified
C 1168 Practice for Preparation and Dissolution of Pluto-
2 criteria for plutonium content. This test method is used to
nium Materials for Analysis
verify the plutonium content.
3. Committee C-26 Safeguards Statement 5.2 A primary standard dichromate or a dichromate trace-
able to a primary standard such as a National Institute of
3.1 The materials [nuclear-grade mixed oxides (U, Pu)O
2
Standards and Technology (NIST) plutonium standard is re-
powders, pellets, Pu metal, Pu oxides, and Pu nitrates] to which
quired for this technique.
this test method applies, are subject to nuclear safeguards
6. Interferences
1
6.1 Interference is caused by ions that are oxidized by
This test method is under the jurisdiction of ASTM Committee C-26 on Nuclear
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
argentic oxide and reduced by ferrous ion in sulfuric-acid
Test.
solution. Elements that may be present in plutonium materials
Current edition approved Nov. 15, 1991. Published June 1992.
2 and that will produce quantitative positive errors include
Annual Book of ASTM Standards, Vol 12.01.
1

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