ASTM C759

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 in the plutonium-nitrate solution is made to establish whether the effective fissile content is in compliance with the purchaser's specifications.

Impurity content is determined 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).

1. Scope

1.1 These test methods cover procedures for the chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade plutonium nitrate solutions to determine compliance with specifications.

1.2 The analytical procedures appear in the following order:

	Sections

Plutonium by Controlled-Potential Coulometry
Plutonium by Amperometric Titration with Iron(II)
Plutonium by Diode Array Spectrophotometry
Free Acid by Titration in an Oxalate Solution	8 to 15
Free Acid by Iodate Precipitation-Potentiometric Titration Test Method	16 to 22
Uranium by Arsenazo I Spectrophotometric Test Method	23 to 33
Thorium by Thorin Spectrophotometric Test Method	34 to 42
Iron by 1,10-Phenanthroline Spectrophotometric Test Method	43 to 50
Impurities by ICP-AES
Chloride by Thiocyanate Spectrophotometric Test Method	51 to 58
Fluoride by Distillation-Spectrophotometric Test Method	59 to 66
Sulfate by Barium Sulfate Turbidimetric Test Method	67 to 74
Isotopic Composition by Mass Spectrometry	75 to 76
Plutonium 238 Isotopic Abundance by Alpha Spectrometry
Americium-241 by Extraction and Gamma Counting	77 to 85
Americium-241 by Gamma Counting	86 to 94
Gamma-Emitting Fission Products, Uranium, and Thorium by Gamma-Ray Spectroscopy	94 to 102
Rare Earths by Copper Spark Spectrochemical Test Method	103 to 105
Tungsten, Niobium (Columbium), and Tantalum by Spectro chemical Test Method	106 to 114
Sample Preparation for Spectrographic Analysis for General Impurities	115 to 118

1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.

1.4 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. For specific safeguard and safety hazard statements, see Section 6.

8.1 This test method covers the determination of free acid in plutonium nitrate solutions (4, 5).

16.1 This test method covers the determination of free acid in strong acid solutions of plutonium nitrate.

23.1 This test method covers the determination of uranium in the range from 300 to 3000 μg/g of plutonium in plutonium nitrate solutions.

34.1 This test method covers the determination of 10 to 150 μg of thorium per gram of plutonium in plutonium nitrate solutions.

43.1 This test method covers the determination of microgram quantities of iron in plutonium nitrate solutions.

51.1 This test method (9) is used to determine chloride in plutonium nitrate solution.

59.1 This test method covers the determination of microquantities of fluoride in plutonium nitrate solutions.

67.1 This test procedure covers the determination of the sulfate concentration in plutonium nitrate solutions in the range from 50 to 700 μg/g of plutonium.

75.1 This test method covers the determination of the isotopic content of nuclear-grade plutonium nitrate solutions.

77.1 This test method covers the determination of americium-241 in plutonium nitrate solutions.

86.1 This test method covers the determination of americium-241 in plutonium nitrate solutions that do not contain significant amounts of other radioactive fission products or high specific-activity gamma emitters.

95.1 This test method covers the determination of gamma-emitting fission products (for example, ⁹⁵Zr-⁹⁵Nb, ¹⁰³Ru, ¹⁰⁶Rh, and ¹³⁷Cs-^137mBa) and actinide impurities (²³²Th, ²³⁵U, and ²³⁸U) in plutonium nitrate. Test portions of plutonium nitrate are prepared to contain from 0.1 to 1.0 g of plutonium. The age of the plutonium after the last separation from actinides must be considered in calculating the actinide contents.

103.1 This test method covers the determination of rare earths in plutonium nitrate solutions in the range from 10 to 200 μg/g of plutonium.

106.1 This test method covers the determination of tungsten, niobium, and tantalum in plutonium nitrate solutions.

115.1 This test method covers the sample preparation for spectrographic analysis of plutonium nitrate for general metallic impurities by the carrier distillation test method.

2. Referenced Documents (purchase separately) The documents listed below are referenced within the subject standard but are not provided as part of the standard.

ASTM Standards

C697 Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Plutonium Dioxide Powders and Pellets

C852 Guide for Design Criteria for Plutonium Gloveboxes

C1009 Guide for Establishing a Quality Assurance Program for Analytical Chemistry Laboratories Within the Nuclear Industry

C1068 Guide for Qualification of Measurement Methods by a Laboratory Within the Nuclear Industry

C1108 Test Method for Plutonium by Controlled-Potential Coulometry

C1128 Guide for Preparation of Working Reference Materials for Use in Analysis of Nuclear Fuel Cycle Materials

C1156 Guide for Establishing Calibration for a Measurement Method Used to Analyze Nuclear Fuel Cycle Materials

C1165 Test Method for Determining Plutonium by Controlled-Potential Coulometry in H2SO4 at a Platinum Working Electrode

C1206 Test Method for Plutonium by Iron (II)/Chromium (VI) Amperometric Titration

C1210 Guide for Establishing a Measurement System Quality Control Program for Analytical Chemistry Laboratories Within the Nuclear Industry

C1235 Test Method for Plutonium by Titanium(III)/Cerium(IV) Titration

C1268 Test Method for Quantitative Determination of Americium 241 in Plutonium by Gamma-Ray Spectrometry

C1297 Guide for Qualification of Laboratory Analysts for the Analysis of Nuclear Fuel Cycle Materials

C1307 Test Method for Plutonium Assay by Plutonium (III) Diode Array Spectrophotometry

C1415 Test Method for 238Pu Isotopic Abundance By Alpha Spectrometry

C1432 Test Method for Determination of Impurities in Plutonium: Acid Dissolution, Ion Exchange Matrix Separation, and Inductively Coupled Plasma-Atomic Emission Spectroscopic (ICP/AES) Analysis

D1193 Specification for Reagent Water

E50 Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials

E115 Practice for Photographic Processing in Optical Emission Spectrographic Analysis

E116 Practice for Photographic Photometry in Spectrochemical Analysis

Keywords

impurity content; isotopic composition; plutonium content; plutonium nitrate; Actinide impurities content; Americium-241 (²⁴¹Am) content; Chloride analysis--nuclear applications; Columbium content; Fission by-products--gamma emitting; Fluoride content; Free acid content; Gamma radiation; Iron content; Isotopic analysis; Mass spectrometry--nuclear materials/applications; Plutonium--isotopic analysis; Plutonium solutions; Radiochemical analysis; Rare earth content; Spectrochemical analysis; Tantalum (Ta) content; Thorium-232 content; Thorium content; Trace elements--spectrochemical analysis; Tungsten content; Uranium-235; Uranium-238; Uranium content ;

ICS Code

ICS Number Code 27.120.30 (Fissile materials and nuclear fuel technology)

DOI: 10.1520/C0759-10

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ASTM C759 (Nuclear Technology Standards)

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ASTM C759 - 10

ASTM C759 - 10 Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Plutonium Nitrate Solutions

ASTM C759 (Nuclear Technology Standards)