Standard Test Method for Plutonium Assay by Plutonium (III) Diode Array Spectrophotometry

SIGNIFICANCE AND USE
5.1 This test method is designed to determine whether a given material meets the purchaser's specification for plutonium content.
SCOPE
1.1 This test method describes the determination of total plutonium as plutonium(III) in nitrate and chloride solutions. The technique is applicable to solutions of plutonium dioxide powders and pellets (Test Methods C697), nuclear grade mixed oxides (Test Methods C698), plutonium metal (Test Methods C758), and plutonium nitrate solutions (Test Methods C759). Solid samples are dissolved using the appropriate dissolution techniques described in Practice C1168. The use of this technique for other plutonium-bearing materials has been reported (1-5), but final determination of applicability must be made by the user. The applicable concentration range for plutonium sample solutions is 10–200 g Pu/L.2  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 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-2014
Technical Committee
Drafting Committee
Current Stage
Ref Project

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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: C1307 − 15
Standard Test Method for
Plutonium Assay by Plutonium (III) Diode Array
1
Spectrophotometry
This standard is issued under the fixed designation C1307; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope Spectrochemical Analysis of Nuclear-Grade Mixed Ox-
ides ((U, Pu)O )
2
1.1 This test method describes the determination of total
C757Specification for Nuclear-Grade Plutonium Dioxide
plutonium as plutonium(III) in nitrate and chloride solutions.
Powder, Sinterable
The technique is applicable to solutions of plutonium dioxide
C758Test Methods for Chemical, Mass Spectrometric,
powdersandpellets(TestMethodsC697),nucleargrademixed
Spectrochemical,Nuclear,andRadiochemicalAnalysisof
oxides (Test Methods C698), plutonium metal (Test Methods
Nuclear-Grade Plutonium Metal
C758), and plutonium nitrate solutions (Test Methods C759).
C759Test Methods for Chemical, Mass Spectrometric,
Solid samples are dissolved using the appropriate dissolution
Spectrochemical,Nuclear,andRadiochemicalAnalysisof
techniques described in Practice C1168. The use of this
Nuclear-Grade Plutonium Nitrate Solutions
technique for other plutonium-bearing materials has been
C833Specification for Sintered (Uranium-Plutonium) Diox-
reported (1-5), but final determination of applicability must be
ide Pellets
made by the user. The applicable concentration range for
2
C859Terminology Relating to Nuclear Materials
plutonium sample solutions is 10–200 g Pu/L.
C1168PracticeforPreparationandDissolutionofPlutonium
1.2 The values stated in SI units are to be regarded as
Materials for Analysis
standard. No other units of measurement are included in this
3. Terminology
standard.
3.1 Definitions:
1.3 This standard does not purport to address all of the
3.1.1 For definitions of terms related to nuclear materials,
safety concerns, if any, associated with its use. It is the
refer to Terminology C859.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
4. Summary of Method
bility of regulatory limitations prior to use.
4.1 In a diode array spectrophotometric measurement, as in
aconventionalspectrophotometricmeasurement,thesubstance
2. Referenced Documents
being determined absorbs light at frequencies characteristic of
3
2.1 ASTM Standards:
that substance. The amount of light absorbed at each wave-
C697Test Methods for Chemical, Mass Spectrometric, and
length is directly proportional to the concentration of the
Spectrochemical Analysis of Nuclear-Grade Plutonium
speciesofinterest.Theabsorptionisafunctionoftheoxidation
Dioxide Powders and Pellets
state and the complexation obtained in the solution matrix
C698Test Methods for Chemical, Mass Spectrometric, and
selected for measurement. Beer’s Law permits quantifying the
species of interest relative to a traceable standard when both
solutionsaremeasuredunderthesameconditions.Thearrayof
1
photosensitive diodes permits the (virtually) simultaneous
ThistestmethodisunderthejurisdictionofASTMCommitteeC26onNuclear
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
collection of spectral information over the entire range of the
Test.
instrument, for example, 190–820 nm (or any selected portion
Current edition approved Jan. 1, 2015. Published January 2015. Originally
oftherange).Anentireabsorptionspectrumcanbeobtainedin
approved in 1995. Last previous edition approved in 2014 as C1307–14. DOI:
10.1520/C1307-15. 0.1 s; however, optimum precision is obtained from multiple
2
Forsolidsamples,selectthesamplesizeanddissolvedsolutionweighttoyield
spectra collected over a 4-s period.
sample solutions in the 10–30 g Pu/L range. With special preparation and spectral
4.2 Reduction to plutonium(III) is accomplished by the
analysis techniques, the method has been applied to nitrate solutions in the 0.1–10
g Pu/L range.
addition of a measured quantity of reductant solution to the
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
sample aliquant.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
4.2.1 For nitrate solutions, ferrous sulfamate is the recom-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. mended reductant. Aliquants (1 mL or less) of the sample
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
C1307 − 15
solution are diluted with 10 mL of a ferrous reductant/matrix minimum, sam
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM 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: C1307 − 14 C1307 − 15
Standard Test Method for
Plutonium Assay by Plutonium (III) Diode Array
1
Spectrophotometry
This standard is issued under the fixed designation C1307; 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
1.1 This test method describes the determination of total plutonium as plutonium(III) in nitrate and chloride solutions. The
technique is applicable to solutions of plutonium dioxide powders and pellets (Test Methods C697), nuclear grade mixed oxides
(Test Methods C698), plutonium metal (Test Methods C758), and plutonium nitrate solutions (Test Methods C759). Solid samples
are dissolved using the appropriate dissolution techniques described in Practice C1168. The use of this technique for other
plutonium-bearing materials has been reported (1-5), but final determination of applicability must be made by the user. The
2
applicable concentration range for plutonium sample solutions is 10–200 g Pu/L.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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
3
2.1 ASTM Standards:
C697 Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Plutonium Dioxide
Powders and Pellets
C698 Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Mixed Oxides ((U,
Pu)O )
2
C757 Specification for Nuclear-Grade Plutonium Dioxide Powder, Sinterable
C758 Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-
Grade Plutonium Metal
C759 Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-
Grade Plutonium Nitrate Solutions
C833 Specification for Sintered (Uranium-Plutonium) Dioxide Pellets
C859 Terminology Relating to Nuclear Materials
C1168 Practice for Preparation and Dissolution of Plutonium Materials for Analysis
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms related to nuclear materials, refer to Terminology C859.
4. Summary of Method
4.1 In a diode array spectrophotometric measurement, as in a conventional spectrophotometric measurement, the substance
being determined absorbs light at frequencies characteristic of that substance. The amount of light absorbed at each wavelength
is directly proportional to the concentration of the species of interest. The absorption is a function of the oxidation state and the
1
This test method 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 June 1, 2014Jan. 1, 2015. Published June 2014January 2015. Originally approved in 1995. Last previous edition approved in 20082014 as
C1307 – 02 (2008).C1307 – 14. DOI: 10.1520/C1307-14.10.1520/C1307-15.
2
For solid samples, select the sample size and dissolved solution weight to yield sample solutions in the 10–30 g Pu/L range. With special preparation and spectral analysis
techniques, the method has been applied to nitrate solutions in the 0.1–10 g Pu/L range.
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
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

---------------------- Page: 1 ----------------------
C1307 − 15
complexation obtained in the solution matrix selected for measurement. Beer’s Law permits quantifying the species of interest
relative to a traceable standard when both solutions are measured under the same conditions. The array of photosensitive diodes
permits the (virtually) simultaneous collection of spectral information over the entire range of the instrument, for example,
190–820 nm (or any selected portion of the range). An entire absorption spectrum can
...

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