ASTM C1307-02
(Test Method)Standard Test Method for Plutonium Assay by Plutonium (III) Diode Array Spectrophotometry
Standard Test Method for Plutonium Assay by Plutonium (III) Diode Array Spectrophotometry
SIGNIFICANCE AND USE
This test method is designed to determine whether a given material meets the purchaser’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 C 697), nuclear grade mixed oxides (Test Methods C 698), plutonium metal (Test Methods C 758), and plutonium nitrate solutions (Test Methods C 759). Solid samples are dissolved using the appropriate dissolution techniques described in Practice C 1168. 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.
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.
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Designation:C1307–02
Standard Test Method for
Plutonium Assay by Plutonium (III) Diode Array
1
Spectrophotometry
This standard is issued under the fixed designation C 1307; 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 C 759 Test Methods for Chemical, Mass Spectrometric,
Spectrochemical, Nuclear, and Radiochemical Analysis of
1.1 This test method describes the determination of total
3
Nuclear-Grade Plutonium Nitrate Solutions
plutonium as plutonium(III) in nitrate and chloride solutions.
C 833 Specification for Sintered (Uranium-Plutonium) Di-
The technique is applicable to solutions of plutonium dioxide
3
oxide Pellets
powders and pellets (Test Methods C 697), nuclear grade
C 1168 Practice for Preparation and Dissolution of Pluto-
mixed oxides (Test Methods C 698), plutonium metal (Test
3
nium Materials for Analysis
Methods C 758), and plutonium nitrate solutions (Test Meth-
ods C 759). Solid samples are dissolved using the appropriate
3. Summary of Method
dissolutiontechniquesdescribedinPracticeC 1168.Theuseof
3.1 In a diode array spectrophotometric measurement, as in
this technique for other plutonium-bearing materials has been
aconventionalspectrophotometricmeasurement,thesubstance
reported (1-5), but final determination of applicability must be
being determined absorbs light at frequencies characteristic of
made by the user. The applicable concentration range for
2 that substance. The amount of light absorbed at each wave-
plutonium sample solutions is 10–200 g Pu/L.
length is directly proportional to the concentration of the
1.2 This standard does not purport to address all of the
speciesofinterest.Theabsorptionisafunctionoftheoxidation
safety concerns, if any, associated with its use. It is the
state and the complexation obtained in the solution matrix
responsibility of the user of this standard to establish appro-
selected for measurement. Beer’s Law permits quantifying the
priate safety and health practices and determine the applica-
species of interest relative to a traceable standard when both
bility of regulatory limitations prior to use.
solutionsaremeasuredunderthesameconditions.Thearrayof
2. Referenced Documents photosensitive diodes permits the (virtually) simultaneous
collection of spectral information over the entire range of the
2.1 ASTM Standards:
instrument, for example, 190–820 nm (or any selected portion
C 697 Test Methods for Chemical, Mass Spectrometric, and
of the range).An entire absorption spectrum can be obtained in
Spectrochemical Analysis of Nuclear-Grade Plutonium
3 0.1 s; however, optimum precision is obtained from multiple
Dioxide Powders and Pellets
spectra collected over a 4-s period.
C 698 Test Methods for Chemical, Mass Spectrometric, and
3.2 Reduction to plutonium(III) is accomplished by the
SpectrochemicalAnalysis of Nuclear-Grade Mixed Oxides
3
addition of a measured quantity of reductant solution to the
((U, Pu)O )
2
sample aliquant.
C 757 Specification for Nuclear-Grade Plutonium Dioxide
3
3.2.1 For nitrate solutions, ferrous sulfamate is the recom-
Powder, Sinterable
mended reductant. Aliquants (1 mL or less) of the sample
C 758 Test Methods for Chemical, Mass Spectrometric,
solution are diluted with 10 mL of a ferrous reductant/matrix
Spectrochemical, Nuclear, and Radiochemical Analysis of
3
solution to 1 g Pu/L, and measured.
Nuclear-Grade Plutonium Metal
3.2.2 For chloride solutions, ascorbic acid is the recom-
mended reductant. Aliquants of the sample solution, each
1
ThistestmethodisunderthejurisdictionofASTMCommitteeC-26onNuclear
containing 50–100 mg of plutonium, are diluted with 2 mL of
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
zirconium solution to complex fluoride ions, 2 mL ascorbic
Test.
acid reductant solution, and 1.0 M HCl to a total volume of 25
Current edition approved Jan. 10, 2002. Published May 2002. Originally
mL, yielding 2–4 g Pu/L solutions for measurement.
published as C1307–95. Last previous edition C1307–95.
2
For solid samples, select the sample size and dissolved solution weight to yield
3.3 Plutonium concentration is determined from light ab-
sample solutions in the 10–30 g Pu/L range. With special preparation and spectral
sorption measurements taken on the sample solution in the
analysis techniques, the method has been applied to nitrate solutions in the 0.1–10
blue-green region from 516 to 640 nm where a broad doublet
g Pu/L range.
3
Annual Book of ASTM Standards, Vol 12.01. band is observed. Spectral quantifying software capable of
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