ASTM C758-04(2010)
(Test Method)Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Plutonium Metal
Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Plutonium Metal
SIGNIFICANCE AND USE
These test methods are designed to show whether a given material meets the purchaser's specifications.
An assay is performed to determine whether the material has the specified plutonium content.
Determination of the isotopic content of the plutonium is made to establish whether the effective fissile content is in compliance with the purchaser's specifications.
Impurity content is verified by a variety of methods to ensure that the maximum concentration limit of specified impurities is not exceeded. Determination of impurities is also required for calculation of the equivalent boron content (EBC).
SCOPE
1.1 These test methods cover procedures for the chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade plutonium metal to determine compliance with specifications.
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: C758 − 04 (Reapproved 2010)
Standard Test Methods for
Chemical, Mass Spectrometric, Spectrochemical, Nuclear,
and Radiochemical Analysis of Nuclear-Grade Plutonium
Metal
This standard is issued under the fixed designation C758; 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 1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 These test methods cover procedures for the chemical,
responsibility of the user of this standard to establish appro-
mass spectrometric, spectrochemical, nuclear, and radiochemi-
priate safety and health practices and determine the applica-
cal analysis of nuclear-grade plutonium metal to determine
bility of regulatory limitations prior to use. For specific
compliance with specifications.
safeguard and safety hazards statements, see Section 6.
1.2 Theanalyticalproceduresappearinthefollowingorder:
Sections 2. Referenced Documents
Dissolution Procedure
2.1 ASTM Standards:
Plutonium by Controlled-Potential Coulometry
Plutonium by Amperometric Titration with Iron (II)
C697Test Methods for Chemical, Mass Spectrometric, and
Plutonium by Ceric Sulfate Titration Test Method
Spectrochemical Analysis of Nuclear-Grade Plutonium
Plutonium by Diode Array Spectrophotometry
Dioxide Powders and Pellets
Uranium by Arsenazo I Spectrophotometric Test Method 8–10
Thorium by Thorin Spectrophotometric Test Method 11–13
C698Test Methods for Chemical, Mass Spectrometric, and
Iron by 1,10-Phenanthroline Spectrophotometric Test Method 14–16
Spectrochemical Analysis of Nuclear-Grade Mixed Ox-
Iron by 2,2-Bipyridyl Spectrophotometric Test Method 17–23
ides ((U, Pu)O )
Impurities by ICP-AES
Chloride by the Thiocyanate Spectrophotometric Test Method 24–26
C759Test Methods for Chemical, Mass Spectrometric,
Fluoride by Distillation-Spectrophotometric Test Method 27–28
Spectrochemical,Nuclear,andRadiochemicalAnalysisof
Nitrogen by Distillation-Nessler Reagent Spectrophotometric Test 29–30
Nuclear-Grade Plutonium Nitrate Solutions
Method
Carbon by the Direct Combustion-Thermal Conductivity Test 31–33
C852Guide for Design Criteria for Plutonium Gloveboxes
Method
C1009Guide for Establishing and Maintaining a Quality
Sulfur by Distillation-Spectrophotometric Test Method 34–36
AssuranceProgramforAnalyticalLaboratoriesWithinthe
Isotopic Composition by Mass Spectrometry 37 and
Nuclear Industry
Plutonium-238 Isotopic Abundance by Alpha Spectrometry
C1068Guide for Qualification of Measurement Methods by
Americium-241 by Extraction and Gamma Counting 39–41
Americium-241 by Gamma Counting a Laboratory Within the Nuclear Industry
Gamma-Emitting Fission Products, Uranium, and Thorium by 42–49
C1108Test Method for Plutonium by Controlled-Potential
Gamma-Ray Spectroscopy
Coulometry
Rare Earths by Copper Spark Spectrochemical Test Method 50–52
Tungsten, Niobium (Columbium), and Tantalum by Spectro- 53–55 C1128Guide for Preparation of Working Reference Materi-
chemical Test Method
als for Use in Analysis of Nuclear Fuel Cycle Materials
Sample Preparation for Spectrographic Analysis for Trace Impuri 56–60
C1156Guide for Establishing Calibration for a Measure-
ties
ment Method Used toAnalyze Nuclear Fuel Cycle Mate-
1.3 The values stated in SI units are to be regarded as
rials
standard. No other units of measurement are included in this
C1165 Test Method for Determining Plutonium by
standard.
Controlled-Potential Coulometry in H SO at a Platinum
2 4
Working Electrode
C1168PracticeforPreparationandDissolutionofPlutonium
These test methods are under the jurisdiction of ASTM Committee C26 on
Materials for Analysis
Nuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.05 on
Methods of Test.
Current edition approved Jan. 1, 2010. Published February 2010. Originally
approved in 1973. Last previous edition approved in 2004 as C758–04. DOI: For referenced ASTM Standards, visit the ASTM website, www.astm.org, or
10.1520/C0758-10. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Discontinued as of February 10, 1998. Standardsvolume information, refer to the standard’s Document Summary page on
Discontinued as of November 15, 1992 the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C758 − 04 (2010)
C1206Test Method for Plutonium by Iron (II)/Chromium 5. Reagents and Materials
(VI) Amperometric Titration (Withdrawn 2015)
5.1 Purity of Reagents—Reagent grade chemicals shall be
C1210Guide for Establishing a Measurement System Qual-
used in all test methods. Unless otherwise indicated, it is
ity Control Program for Analytical Chemistry Laborato-
intended that all reagents shall conform to the specifications of
ries Within the Nuclear Industry
theCommitteeonAnalyticalReagentsoftheAmericanChemi-
C1235 Test Method for Plutonium by Titanium(III)/
cal Society, where such specifications are available. Other
Cerium(IV) Titration (Withdrawn 2005)
grades may be used, provided it is first ascertained that the
C1268 Test Method for Quantitative Determination of
reagent is of sufficient high purity to permit its use without
Am in Plutonium by Gamma-Ray Spectrometry
lessening the accuracy of the determination.
C1297Guide for Qualification of Laboratory Analysts for
5.2 Purity of Water—Unless otherwise indicated, reference
the Analysis of Nuclear Fuel Cycle Materials
towatershallbeunderstoodtomeanreagentwaterconforming
C1307Test Method for PlutoniumAssay by Plutonium (III)
to Specification D1193.
Diode Array Spectrophotometry
C1415Test Method for Pu Isotopic Abundance By Alpha
6. Safety Hazards
Spectrometry
6.1 Since plutonium bearing materials are radioactive and
C1432Test Method for Determination of Impurities in
toxic,adequatelaboratoryfacilities,glovedboxes,fumehoods,
Plutonium: Acid Dissolution, Ion Exchange Matrix
etc., along with safe techniques, must be used in handling
Separation, and Inductively Coupled Plasma-Atomic
samplescontainingthesematerials.Adetaileddiscussionofall
Emission Spectroscopic (ICP/AES) Analysis
the precautions necessary is beyond the scope of these test
D1193Specification for Reagent Water
methods; however, personnel who handle these materials
should be familiar with such safe handling practices as are
3. Significance and Use
given in Guide C852 and in Refs. (1-3).
3.1 These test methods are designed to show whether a
given material meets the purchaser’s specifications.
7. Sampling
3.1.1 An assay is performed to determine whether the
7.1 In the absence of ASTM test methods for sampling
material has the specified plutonium content.
plutonium metal, alternative techniques are recommended
3.1.2 Determinationoftheisotopiccontentoftheplutonium
(3-6).
is made to establish whether the effective fissile content is in
7.2 Cognizance shall be taken of the fact that various
compliance with the purchaser’s specifications.
3.1.3 Impurity content is verified by a variety of methods to impuritiescanbeintroducedintosamplesduringtheprocessof
sampling. The particular impurities introduced are a function
ensure that the maximum concentration limit of specified
impurities is not exceeded. Determination of impurities is also of the method of sampling (for example, iron and alloying
elementsindrillturning,oxygenorcomponentsofcoolingoil,
requiredforcalculationoftheequivalentboroncontent(EBC).
or both, from lathe turnings, etc.). It is necessary for the
4. Committee C-26 Safeguards Statement
purchaser and the seller to recognize this possibility for
contaminationduringsamplingandmutuallyagreeonthemost
4.1 The material (plutonium metal) to which these test
suitable method.
methods apply is subject to nuclear safeguards regulations
governing its possession and use. The following analytical
7.3 Samplesizeshallbesufficienttoperformthefollowing:
procedures in these test methods have been designed as
7.3.1 Quality verification tests at the seller’s plant,
technicallyacceptableforgeneratingsafeguardsaccountability
7.3.2 Acceptance tests at the purchaser’s plant, and
measurement data: Plutonium by Controlled-Potential Cou-
7.3.3 Referee tests in the event these become necessary.
lometry; Plutonium by Ceric Sulfate Titration; Plutonium by
7.4 All samples shall be identified clearly by the seller’s
Amperometric Titration with Iron(II); Plutonium by Diode
button number and by the lot number, and all pieces of metal
Array Spectrophotometry and Isotopic Composition by Mass
in that lot shall be identified clearly by the lot number and the
Spectrometry.
piece number.
4.2 When used in conjunction with appropriate Certified
7.4.1 Alotisdefinedasasinglebutton,fractionofabutton,
Reference Materials (CRMs), these procedures can demon-
or multiple castings from a single melt of plutonium metal.
strate traceability to the national measurement base. However,
Buttons, fractions of buttons, or multiple castings are usually
adherence to these procedures does not automatically guaran-
supplied in pieces of not less than 50 g. All pieces shall be
tee regulatory acceptance of the resulting safeguards measure-
identified positively as coming from a particular button,
ments.Itremainsthesoleresponsibilityoftheuserofthesetest
fraction of a button, or casting.
methods to assure that their application to safeguards has the
approval of the proper regulatory authorities.
Reagent Chemicals, American Chemical Society Specifications,” American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
The last approved version of this historical standard is referenced on Chemicals,BDHLtd.,Poole,Dorset,U.K.,andthe Unites States Pharmacopeia and
www.astm.org. National Foundary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
6 8
Based upon Committee C-26 Safeguards Matrix (C1009, C1068, C1128, Theboldfacenumbersinparenthesesrefertothelistofreferencesattheendof
C1156, C1210, C1297). these test methods.
C758 − 04 (2010)
ing the uranium concentration must be substituted for the equation given
7.4.2 A lot shall normally not be less than 1800 g of
in 28.1 of Test Methods C759:
plutonium, except as necessary to meet some special require-
ment. The maximum size of a lot will depend on equipment R 5 Y 2 B D/AW (1)
~ !
size of the producer and criticality considerations.
where:
DISSOLUTION PROCEDURE R = micrograms U per gram Pu,
A, B = constants in linear calibration equation,
(This practice is replaced by Standard Practice C1168).
D = dilution factor= V/E
PLUTONIUM BY CONTROLLED-POTENTIAL
where:
COULOMETRY
V = volume in which sample solution was diluted, mL, and
(This test method was discontinued in 1992 and replaced by
E = volume of aliquot of V used for uranium determination,
Test Method C1165)
mL,
PLUTONIUM BY CONTROLLED-POTENTIAL
where:
COULOMETRY
W = weight of test portion of Pu metal sample, g, and
(With appropriate sample preparation, controlled-potential
Y = a− b=corrected absorbance of sample,
coulometric measurement as described in Test Method C1108
may be used for plutonium determination.)
where:
a = absorbance of sample solution, and
PLUTONIUM BY AMPEROMETRIC TITRATION
b = average absorbance of duplicate calibration blanks.
WITH IRON(II)
(This test method was discontinued in 1992 and replaced by
THORIUM BY THORIN SPECTROPHOTOMETRIC
Test Method C1206)
TEST METHOD
PLUTONIUM BY CERIC SULFATE TITRATION TEST
11. Scope
METHOD
(This test method is replaced by Test Method C1235.)
11.1 This test method covers the determination of thorium
intherangefrom10to150µg/gofplutoniuminnuclear-grade
TEST METHOD FOR PLUTONIUM ASSAY BY
plutonium metal.
PLUTONIUM(III) DIODE ARRAY
SPECTROPHOTOMETRY
12. Summary of Test Method
(With appropriate sample preparation, the measurement
described in Test Method C1307 may be used for plutonium
12.1 To an acid solution of plutonium metal, lanthanum is
determination.)
added as a carrier and is precipitated along with thorium as
insolublefluoride,whiletheplutoniumremainsinsolutionand
URANIUM BY ARSENAZO I
isdecantedaftercentrifugationofthesample.Thethoriumand
SPECTROPHOTOMETRIC TEST METHOD
lanthanumfluorideprecipitatesaredissolvedinperchloricacid
andtheabsorbanceofthethorium-Thorincomplexismeasured
8. Scope
at a wavelength of 545 nm versus a reference solution. The
8.1 Thistestmethodcoversthedeterminationofuraniumin
molar absorptivity of the colored complex is of 15 600 for
the range from 300 to 3000 µg/g of plutonium.
thorium concentration in the range from 5 to 70 µg Th/10 mL
of solution.
9. Summary of Test Method
13. Procedure
9.1 Plutonium metal dissolved in 6 N HCl is reduced to
Pu(III) with hydroxylamine hydrochloride. The uranium and
13.1 Transfer an aliquot of solution of plutonium metal,
plutonium are separated by anion exchange; then the uranium
prepared in accordance with Sections 6 and 7 of these test
is determined by measuring the absorbance of the U(VI)-
methods, that contains from 10 to 70 µg of thorium and no
Arsenazo I complex in a 1-cm cell at a wavelength of 600 nm
greater than 500 mg of plutonium, into a 20-mL beaker.
versus a reagent blank.
13.2 Determine the thorium concentration in accordance
10. Procedure with the appropriate sections of Test Methods C759.
10.1 Transfer an aliquot of sample solution, prepared in
NOTE 2—Since the starting sample is plutonium metal the following
accordance with Practice C1168, that contains approximately equation for calculating the thorium concentration must be substituted for
the equation given in 49.3 of Test Methods C759:
70 mg of plutonium, to a 50-mLbeaker and add 1 mLof nitric
acid (sp gr 1.42) and heat to boiling. Proceed with the
Th, µg/g ofPu 5 Y 2 B D/AW (2)
~ !
determination of uranium in accordance with the appropriate
where:
sections of Test Methods C759.
A, B = constants in the linear calibration equation,
NOTE 1—Since the sample starts as plutonium metal and is then
W = sample weight, g,
dissolved in acid and diluted to volume and an aliquot of this solution
D = dilution factor= V/E
taken for the uranium determination, the following equation for calculat-
C758 − 04 (2010)
where: 19. Apparatus
V = volume to which dissolved plutonium metal is diluted,
19.1 Spectrophotometer, visible range.
mL, and
19.2 Extraction Bottles, glass-stopped, 125-mL volume.
E = volume of aliquot of V taken for
...
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