ASTM C758-98
(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
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.
1.2 The analytical procedures appear in the following order: Sections Dissolution Procedure 7 to 12 Plutonium by Controlled-Potential Coulometry 2 Plutonium by Amperometric Titration with Iron (II) 2 Plutonium by Ceric Sulfate Titration Test Method 17 to 19 Uranium by Arsenazo I Spectrophotometric Test Method 20 to 22 Thorium by Thorin Spectrophotometric Test Method 23 to 25 Iron by 1,10-Phenanthroline Spectrophotometric Test Method 26 to 28 Iron by 2,2[prime]-Bipyridyl Spectrophotometric Test Method 29 to 35 Chloride by the Thiocyanate Spectrophotometric Test Method 36 to 38 Fluoride by Distillation-Spectrophotometric Test Method 39 to 40 Nitrogen by Distillation-Nesaler Reagent Spectrophotometric Test Method 41 to 42 Carbon by the Direct Combustion-Thermal Conductivity Test Method 43 to 45 Sulfur by Distillation-Spectrophotometric Test Method 46 to 48 Isotopic Composition by Mass Spectrometry 49 to 50 Americium-241 by Extraction and Gamma Counting 51 to 53 Americium-241 by Gamma Counting 54 to 56 Gamma-Emitting Fission Products, Uranium, and Thorium by 57 to 64 Gamma-Ray Spectroscopy Rare Earths by Copper Spark Spectrochemical Test Method 65 to 67 Tungsten, Niobium (Columbium), and Tantalum by Spectro-chemical Test Method 68 to 70 Sample Preparation for Spectrographic Analysis for Trace Impurities 71 to 75
1.3 This standard does not purport to address all of the safety problems, 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. For specific safeguard and safety hazards statements, see Section 5.
General Information
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Standards Content (Sample)
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Designation: C 758 – 98
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 C 758; 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 697 Test Methods for Chemical, Mass Spectrometric, and
Spectrochemical Analysis of Nuclear-Grade Plutonium
1.1 These test methods cover procedures for the chemical,
Dioxide Powders and Pellets
mass spectrometric, spectrochemical, nuclear, and radiochemi-
C 698 Test Methods for Chemical, Mass Spectrometric, and
cal analysis of nuclear-grade plutonium metal to determine
Spectrochemical Analysis of Nuclear-Grade Mixed Oxides
compliance with specifications.
((U, Pu)O )
1.2 The analytical procedures appear in the following order: 2
C 759 Test Methods for Chemical, Mass Spectrometric,
Sections
Spectrochemical, Nuclear, and Radiochemical Analysis of
Dissolution Procedure
Plutonium by Controlled-Potential Coulometry
Nuclear-Grade Plutonium Nitrate Solutions
Plutonium by Amperometric Titration with Iron (II)
C 852 Guide for Design Criteria for Plutonium Glove-
Plutonium by Ceric Sulfate Titration Test Method
boxes
Plutonium by Diode Array Spectrophotometry
Uranium by Arsenazo I Spectrophotometric Test Method 8-10
C 1009 Guide for Establishing a Quality Assurance Pro-
Thorium by Thorin Spectrophotometric Test Method 11-13
gram for Analytical Chemistry Laboratories Within the
Iron by 1,10-Phenanthroline Spectrophotometric Test Method 14-16
Nuclear Industry
Iron by 2,28-Bipyridyl Spectrophotometric Test Method 17-23
Chloride by the Thiocyanate Spectrophotometric Test Method 24-26
C 1068 Guide for Qualification of Measurement Methods
Fluoride by Distillation-Spectrophotometric Test Method 27 and 28
by a Laboratory Within the Nuclear Industry
Nitrogen by Distillation-Nessler Reagent Spectrophotometric Test 29 and 30
Method C 1108 Test Method for Plutonium by Controlled-Potential
Carbon by the Direct Combustion-Thermal Conductivity Test 31-33
Coulometry
Method
C 1128 Guide for Preparation of Working Reference Mate-
Sulfur by Distillation-Spectrophotometric Test Method 34-36
Isotopic Composition by Mass Spectrometry 37 and 38 rials for Use in the Analysis of Nuclear Fuel Cycle
Americium-241 by Extraction and Gamma Counting 39-41
Materials
Americium-241 by Gamma Counting
C 1156 Guide for Establishing Calibration for a Measure-
Gamma-Emitting Fission Products, Uranium, and Thorium by 42-49
Gamma-Ray Spectroscopy ment Method Used to Analyze Nuclear Fuel Cycle Mate-
Rare Earths by Copper Spark Spectrochemical Test Method 50-52
rials
Tungsten, Niobium (Columbium), and Tantalum by Spectro- 53-55
C 1165 Test Method for Determining Plutonium by
chemical Test Method
Sample Preparation for Spectrographic Analysis for Trace Impuri 56-60 Controlled-Potential Coulometry in H SO at a Platinum
2 4
ties 2
Working Electrode
C 1168 Practice for Preparation and Dissolution of Pluto-
1.3 This standard does not purport to address all of the
nium Materials for Analysis
safety concerns, if any, associated with its use. It is the
C 1206 Test Method for Plutonium by Iron (II)/Chromium
responsibility of the user of this standard to establish appro-
(VI) Amperometric Titration
priate safety and health practices and determine the applica-
C 1210 Guide for Establishing a Measurement System
bility of regulatory limitations prior to use. For specific
Quality Control Program for Analytical Chemistry Labo-
safeguard and safety hazards statements, see Section 6.
ratories Within the Nuclear Industry
2. Referenced Documents
C 1235 Standard Test Method for Plutonium by
2.1 ASTM Standards: Titanium(III)/Cerium(IV) Titration
C 1268 Test Method for Quantitative Determination of
Americium 241 in Plutonium by Gamma-Ray Spectrom-
These test methods are under the jurisdiction of ASTM Committee C-26 on
etry
Nuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.05 on
Methods of Test.
C 1297 Guide for Qualification of Laboratory Analysts for
Current edition approved Feb. 10, 1998. Published May 1998. Originally
the Analysis of Nuclear Fuel Cycle Materials
published as C 758 – 73. Last previous edition C 758 – 92.
Annual Book of ASTM Standards, Vol 12.01.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
C 758
C 1307 Test Method for Plutonium Assay by Plutonium(III) 6. Safety Hazards
Diode Array Spectrophotometry
6.1 Since plutonium bearing materials are radioactive and
D 1193 Specification for Reagent Water
toxic, adequate laboratory facilities, gloved boxes, fume hoods,
etc., along with safe techniques, must be used in handling
3. Significance and Use
samples containing these materials. A detailed discussion of all
3.1 These test methods are designed to show whether a the precautions necessary is beyond the scope of these test
given material meets the purchaser’s specifications. methods; however, personnel who handle these materials
3.1.1 An assay is performed to determine whether the should be familiar with such safe handling practices as are
material has the specified plutonium content. given in Guide C 852 and in Refs. (1-3).
3.1.2 Determination of the isotopic content of the plutonium
7. Sampling
is made to establish whether the effective fissile content is in
compliance with the purchaser’s specifications. 7.1 In the absence of ASTM test methods for sampling
3.1.3 Impurity content is verified by a variety of methods to plutonium metal, alternative techniques are recommended
ensure that the maximum concentration limit of specified (3-6).
impurities is not exceeded. Determination of impurities is also 7.2 Cognizance shall be taken of the fact that various
required for calculation of the equivalent boron content (EBC). impurities can be introduced into samples during the process of
sampling. The particular impurities introduced are a function
4. Committee C-26 Safeguards Statement of the method of sampling (for example, iron and alloying
elements in drill turning, oxygen or components of cooling oil,
4.1 The material (plutonium metal) to which these test
or both, from lathe turnings, etc.). It is necessary for the
methods apply is subject to nuclear safeguards regulations
purchaser and the seller to recognize this possibility for
governing its possession and use. The following analytical
contamination during sampling and mutually agree on the most
procedures in these test methods have been designed as
suitable method.
technically acceptable for generating safeguards accountability
7.3 Sample size shall be sufficient to perform the following:
measurement data: Plutonium by Controlled-Potential Cou-
7.3.1 Quality verification tests at the seller’s plant,
lometry; Plutonium by Ceric Sulfate Titration; Plutonium by
7.3.2 Acceptance tests at the purchaser’s plant, and
Amperometric Titration with Iron(II); Plutonium by Diode
7.3.3 Referee tests in the event these become necessary.
Array Spectrophotometry and Isotopic Composition by Mass
7.4 All samples shall be identified clearly by the seller’s
Spectrometry.
button number and by the lot number, and all pieces of metal
4.2 When used in conjunction with appropriate Certified
in that lot shall be identified clearly by the lot number and the
Reference Materials (CRMs), these procedures can demon-
piece number.
strate traceability to the national measurement base. However,
7.4.1 A lot is defined as a single button, fraction of a button,
adherence to these procedures does not automatically guaran-
or multiple castings from a single melt of plutonium metal.
tee regulatory acceptance of the resulting safeguards measure-
Buttons, fractions of buttons, or multiple castings are usually
ments. It remains the sole responsibility of the user of these test
supplied in pieces of not less than 50 g. All pieces shall be
methods to assure that their application to safeguards has the
identified positively as coming from a particular button,
approval of the proper regulatory authorities.
fraction of a button, or casting.
7.4.2 A lot shall normally not be less than 1800 g of
5. Reagents and Materials
plutonium, except as necessary to meet some special require-
5.1 Purity of Reagents—Reagent grade chemicals shall be
ment. The maximum size of a lot will depend on equipment
used in all test methods. Unless otherwise indicated, it is
size of the producer and criticality considerations.
intended that all reagents shall conform to the specifications of
the Committee on Analytical Reagents of the American Chemi-
DISSOLUTION PROCEDURE
cal Society, where such specifications are available. Other
(This practice is replaced by Standard Practice C 1168).
grades may be used, provided it is first ascertained that the
reagent is of sufficient high purity to permit its use without
PLUTONIUM BY CONTROLLED-POTENTIAL
lessening the accuracy of the determination.
COULOMETRY
5.2 Purity of Water—Unless otherwise indicated, reference
(This test method was discontinued in 1992 and replaced by
to water shall be understood to mean reagent water conforming
Test Method C 1165)
to Specification D 1193.
PLUTONIUM BY CONTROLLED-POTENTIAL
COULOMETRY
(With appropriate sample preparation, controlled-potential
Annual Book of ASTM Standards, Vol 11.01.
Based upon Committee C-26 Safeguards Matrix (C 1009, C 1068, C 1128,
coulometric measurement as described in Test Method C 1108
C 1156, C 1210, C 1297).
may be used for plutonium determination.)
“Reagent Chemicals, American Chemical Society Specifications,” Am. Chemi-
cal Soc., Washington, DC. For suggestions on the testing of reagents not listed by
the American Chemical Society, see “Reagent Chemicals and Standards,” by Joseph
Rosin, D. Van Nostrand Co., Inc., New York, NY, and the “United States The boldface numbers in parentheses refer to the list of references at the end of
Pharmacopeia.” these test methods.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
C 758
PLUTONIUM BY AMPEROMETRIC TITRATION
W 5 weight of test portion of Pu metal sample, g, and
WITH IRON(II)
Y 5 a − b 5 corrected absorbance of sample,
(This test method was discontinued in 1992 and replaced by
where:
Test Method C 1206)
a 5 absorbance of sample solution, and
b 5 average absorbance of duplicate calibration
PLUTONIUM BY CERIC SULFATE TITRATION TEST
blanks.
METHOD
(This test method is replaced by Test Method C 1235.)
THORIUM BY THORIN SPECTROPHOTOMETRIC
TEST METHOD
TEST METHOD FOR PLUTONIUM ASSAY BY
PLUTONIUM(III) DIODE ARRAY
11. Scope
SPECTROPHOTOMETRY
11.1 This test method covers the determination of thorium
(With appropriate sample preparation, the measurement
in the range from 10 to 150 μg/g of plutonium in nuclear-grade
described in Test Method C 1307 may be used for plutonium
plutonium metal.
determination.)
URANIUM BY ARSENAZO I
12. Summary of Test Method
SPECTROPHOTOMETRIC TEST METHOD
12.1 To an acid solution of plutonium metal, lanthanum is
added as a carrier and is precipitated along with thorium as
8. Scope
insoluble fluoride, while the plutonium remains in solution and
8.1 This test method covers the determination of uranium in
is decanted after centrifugation of the sample. The thorium and
the range from 300 to 3000 μg/g of plutonium.
lanthanum fluoride precipitates are dissolved in perchloric acid
and the absorbance of the thorium-Thorin complex is measured
9. Summary of Test Method
at a wavelength of 545 nm versus a reference solution. The
9.1 Plutonium metal dissolved in 6 N HCl is reduced to
molar absorptivity of the colored complex is of 15 600 for
Pu(III) with hydroxylamine hydrochloride. The uranium and
thorium concentration in the range from 5 to 70 μg Th/10 mL
plutonium are separated by anion exchange; then the uranium
of solution.
is determined by measuring the absorbance of the U(VI)-
Arsenazo I complex in a 1-cm cell at a wavelength of 600 nm
13. Procedure
versus a reagent blank.
13.1 Transfer an aliquot of solution of plutonium metal,
10. Procedure
prepared in accordance with Sections 6 and 7 of these test
10.1 Transfer an aliquot of sample solution, prepared in methods, that contains from 10 to 70 μg of thorium and no
accordance with Practice C 1168, that contains approximately
greater than 500 mg of plutonium, into a 20-mL beaker.
70 mg of plutonium, to a 50-mL beaker and add 1 mL of nitric
13.2 Determine the thorium concentration in accordance
acid (sp gr 1.42) and heat to boiling. Proceed with the
with the appropriate sections of Test Methods C 759.
determination of uranium in accordance with the appropriate
NOTE 2—Since the starting sample is plutonium metal the following
sections of Test Methods C 759.
equation for calculating the thorium concentration must be substituted for
the equation given in 49.3 of Test Methods C 759:
NOTE 1—Since the sample starts as plutonium metal and is then
dissolved in acid and diluted to volume and an aliquot of this solution
Th, μg/g of Pu 5 Y 2 B!D/AW (2)
~
taken for the uranium determination, the following equation for calculat-
ing the uranium concentration must be substituted for the equation given
where:
in 28.1 of Test Methods C 759:
A, B 5 constants in the linear calibration equation,
W 5 sample weight, g,
R 5 ~Y 2 B!D/AW (1)
D 5 dilution factor 5 V/E
where:
R 5 micrograms U per gram Pu, where:
A, B 5 constants in linear calibration equation, V 5 volume to which dissolved plutonium metal
D 5 dilution factor 5 V/E is diluted, mL, and
E 5 volume of aliquot of V taken for determina-
where:
tion, mL,
V 5 volume in which sample solution was di-
luted, mL, and
E 5 volume of aliquot of V used for uranium
Y 5 a − b 5 corrected absorbance of sample solution
determination, mL,
where:
a 5 absorbance of sample solution, and
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
C 758
20. Reagents and Materials
b 5 average absorbance from the duplicate re-
agent blanks (see section 47.2.1 of Test
20.1 Chloroform.
Method
...
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