Standard Practice for Preparation of Plutonium Materials by Pyrohydrolysis for Determination of Fluoride, Chloride, or Both

SIGNIFICANCE AND USE
5.1 This practice provides a means of collecting fluoride and chloride from plutonium test materials for analysis by ISE or IC. The results can be used to determine whether the material meets the requirements of Specifications C757 or C833, or other specification agreed by a supplier and customer, for fluoride or chloride content, or both.
SCOPE
1.1 This practice provides a procedure for the preparation of samples of plutonium (Pu) materials, using pyrohydrolysis, for subsequent measurement of fluoride, chloride, or both, by ion chromatography (IC) or ion-selective electrode (ISE).  
1.2 This practice utilizes a sample size of 0.3 ± 0.1 g and is therefore suitable when the larger sample size used in Test Methods C697 and C698 is not available.  
1.3 Test materials within the scope of this practice include plutonium dioxide powder and mixed (U, Pu) oxide powder. Pellets of plutonium dioxide and mixed (U, Pu) oxide may also be treated after pulverization and with use of an accelerant. Samples of neptunium oxide may also be prepared using this practice.  
1.4 Full recovery may not be achieved for levels above 50 μg/g fluoride or 50 μg/g chloride (1).2 At higher levels precipitation may occur in the reaction vessel or condenser, or both. The user should validate suitability of the method above these levels.  
1.5 The procedure described in this practice may be applicable to other plutonium materials, such as plutonium compounds and scrap metals. The user must determine the safety and applicability of this practice to such materials.  
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.7 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.8 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

Status
Published
Publication Date
14-Feb-2021
Technical Committee
Drafting Committee
Current Stage
Ref Project

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: C1907 − 21
Standard Practice for
Preparation of Plutonium Materials by Pyrohydrolysis for
1
Determination of Fluoride, Chloride, or Both
This standard is issued under the fixed designation C1907; 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 ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
1.1 Thispracticeprovidesaprocedureforthepreparationof
mendations issued by the World Trade Organization Technical
samples of plutonium (Pu) materials, using pyrohydrolysis, for
Barriers to Trade (TBT) Committee.
subsequent measurement of fluoride, chloride, or both, by ion
chromatography (IC) or ion-selective electrode (ISE).
2. Referenced Documents
1.2 This practice utilizes a sample size of 0.3 6 0.1 g and is
3
2.1 ASTM Standards:
therefore suitable when the larger sample size used in Test
C697 Test Methods for Chemical, Mass Spectrometric, and
Methods C697 and C698 is not available.
Spectrochemical Analysis of Nuclear-Grade Plutonium
1.3 Test materials within the scope of this practice include
Dioxide Powders and Pellets
plutonium dioxide powder and mixed (U, Pu) oxide powder.
C698 Test Methods for Chemical, Mass Spectrometric, and
Pellets of plutonium dioxide and mixed (U, Pu) oxide may also
Spectrochemical Analysis of Nuclear-Grade Mixed Ox-
be treated after pulverization and with use of an accelerant.
ides ((U, Pu)O )
2
Samples of neptunium oxide may also be prepared using this
C757 Specification for Nuclear-Grade Plutonium Dioxide
practice.
Powder for Light Water Reactors
C833 Specification for Sintered (Uranium-Plutonium) Diox-
1.4 Full recovery may not be achieved for levels above
2
ide Pellets for Light Water Reactors
50 µg⁄g fluoride or 50 µg/g chloride (1). At higher levels
C852/C852M Guide for Design Criteria for Plutonium
precipitation may occur in the reaction vessel or condenser, or
Gloveboxes
both. The user should validate suitability of the method above
C859 Terminology Relating to Nuclear Materials
these levels.
C1068 Guide for Qualification of Measurement Methods by
1.5 The procedure described in this practice may be appli-
a Laboratory Within the Nuclear Industry
cable to other plutonium materials, such as plutonium com-
C1502 Test Method for Determination of Total Chlorine and
pounds and scrap metals. The user must determine the safety
Fluorine in Uranium Dioxide and Gadolinium Oxide
and applicability of this practice to such materials.
D1193 Specification for Reagent Water
1.6 The values stated in SI units are to be regarded as
D4327 Test Method for Anions in Water by Suppressed Ion
standard. No other units of measurement are included in this
Chromatography
standard.
3. Terminology
1.7 This standard does not purport to address all of the
3.1 Except as otherwise defined herein, definitions of terms
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- are as given in Terminology C859.
priate safety, health, and environmental practices and deter-
3.2 Definitions:
mine the applicability of regulatory limitations prior to use.
3.2.1 accelerant, n—a chemical compound or a flux that
1.8 This international standard was developed in accor-
will decrease the reaction time or pyrohydrolysis time. C1502
dance with internationally recognized principles on standard-
3.2.2 pyrohydrolysis, n—treatment involving heating of a
sample in a stream of moist argon or oxygen at a temperature
of 900 to 1000 °C.
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.
3
Current edition approved Feb. 15, 2021. Published May 2021. DOI: 10.1520/ For referenced ASTM standards, visit the ASTM website, www.astm.org, or
C1907-21. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
2
The boldface numbers in parentheses refer to a list of references at the end of Standards volume information, refer to the standard’s Document Summary page on
this standard. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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C1907 − 21
3.3 Definitions of Terms Specific to This Standard: 6.3 UraniumOxide(U O )—Halogen-freepowderusedasa
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3.3.1 test material, n—material being t
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