Significance and Use
Plutonium dioxide is used in mixtures with uranium dioxide as a nuclear-reactor fuel. In order to be suitable for this purpose, the material must meet certain criteria for plutonium content, isotopic composition, and impurity content. These test methods are designed to show whether or not a given material meets the specifications for these items as described in Specification C757.
An assay is performed to determine whether the material has the minimum plutonium content specified on a dry weight basis.
Determination of the isotopic content of the plutonium in the plutonium dioxide powder is made to establish whether the effective fissile content is in compliance with the purchaser's specifications.
Impurity content is determined to ensure that the maximum concentration limit of certain impurity elements 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, and spectrochemical analysis of nuclear-grade plutonium dioxide powders and pellets to determine compliance with specifications.
1.2 The analytical procedures appear in the following order:
| Sections |
| Plutonium Sample Handling | 8 to 10 |
| Plutonium by Controlled-Potential Coulometry | |
| Plutonium by Ceric Sulfate Titration | |
| Plutonium by Amperometric Titration with Iron(II) | |
| Plutonium by Diode Array Spectrophotometry | |
Nitrogen by Distillation Spectrophotometry Using Nessler
Reagent | 11 to 18 |
| Carbon (Total) by Direct Combustion–Thermal Conductivity | 19 to 30 |
| Total Chlorine and Fluorine by Pyrohydrolysis | 31 to 38 |
| Sulfur by Distillation Spectrophotometry | 39 to 47 |
| Plutonium Isotopic Analysis by Mass Spectrometry | |
| Rare Earth Elements by Spectroscopy | 48 to 55 |
| Trace Elements by Carrier–Distillation Spectroscopy | 56 to 63 |
| Impurities by ICP-AES | |
| Impurity Elements by Spark-Source Mass Spectrography | 64 to 70 |
| Moisture by the Coulometric Electrolytic Moisture Analyzer | 71 to 78 |
| Total Gas in Reactor-Grade Plutonium Dioxide Pellets | 79 to 86 |
| Plutonium-238 Isotopic Abundance by Alpha Spectrometry | |
| Americium-241 in Plutonium by Gamma-Ray Spectrometry | |
| Rare Earths By Copper Spark-Spectroscopy | 87 to 96 |
| Plutonium Isotopic Analysis by Mass Spectrometry | 97 to 105 |
| Oxygen-To-Metal Atom Ratio by Gravimetry | 106 to 114 |
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 precautionary statements, see Sections 6, 15, 24, 111, and 52.9 and 101.5.1 . 8.1 This test method covers the conditions necessary to preserve the integrity of plutonium dioxide samples. Conditions listed here are directed toward the analytical chemist. However, they are just as applicable to any group handling the material.
11.1 This test method covers the determination of 5 to 100 μg/g of nitride nitrogen in 1-g samples of nuclear-grade plutonium dioxide.
19.1 This test method covers the determination of 10 to 200 μg of residual carbon in nuclear-grade plutonium dioxide.
31.1 This test method covers the determination of 5 to 100 μg/g of chlorine and 1 to 100 μg/g of fluorine in 1-g samples of nuclear-grade plutonium dioxide.
39.1 This test method coves the determination of sulfur in the concentration range from 10 to 600 μg/g for samples of nuclear-grade plutonium dioxide powders or pellets.
48.1 This test method covers the determination of dysprosium, europium, gadolinium, and samarium in plutonium dioxide (PuO2) in concentrations of 0.1 to 10 μg/g of PuO2.
FIG. 5 Schematic Diagram of Atmosphere Chamber
56.1 This test method covers the determination of 36 impurity elements in nuclear-grade plutonium dioxide (PuO2). The concentration ranges covered by the method and the analytical lines used for each element are listed in Table 1.
TABLE 1 Impurity Elements, Lines, and Concentration Limits
| Element | Wavelength, Å | Concentration
Range, ppm |
|---|
| Al | 2567.99A | 10–500 |
| Al | 3082.68A | |
| Ag | 3280.68 | 1–250 |
| As | 2349.84 | 10–250 |
| Au | 2427.95 | 2.5–50 |
| B | 2497.73 | 1–50 |
| Ba | 4554.03 | 2.5–100 |
| (first order) | |
| Be | 2348.61 | 0.5–25 |
| Bi | 3067.72 | 2.5–100 |
| Ca | 3933.67 | 10–1000 |
| Cd | 2288.02 | 1–100 |
| Co | 2407.25 | 10–1000 |
| Co | 3044.00 | |
| Cu | 3247.54 | 1–250 |
| Cr | 2835.63A | 5–500 |
| Fe | 2983.57A | 10–1000 |
| Ga | 2450.07A | 1–500 |
| Ga | 2943.64 | |
| In | 3039.36 | 2.5–100 |
| K | 7664.91 | 3–1000 |
| (first order) | |
| Mg | 2802.70 | 1–1000 |
| Mn | 2798.27 | 5–250 |
| MoB | 3132.59 | 5–250 |
| Ni | 3002.49A | 10–1000 |
| P | 2553.28 | 100–1000 |
| Pb | 2614.18 | 5–100 |
| Pd | 3242.70 | 2.5–100 |
| Sb | 2598.05 | 2.5–100 |
| Si | 2514.32A | 10–300 |
| Sn | 2863.33 | 2.5–100 |
| Sr | 4607.33 | 5–100 |
| (first order) | |
| Ti | 3223.52 | 5–100 |
| VB | 3183.98A | 5–100 |
| WB | 2724.35A | 20–200 |
| Zn | 3345.02 | 10–250 |
| Zr | 3438.23 | 5–100 |
A These elements are determined with the aid of a microphotometer.
B These elements are analyzed by using a AgCl carrier and PdCl2 as an internal standard. Mix 20 mg of PdCl2 with 10.0 g of AgCl. Add 80 mg of this mixture to 120 mg of PuO2 sample-blend before loading 50-mg charges in a graphite electrode ASTM-Type-S-4 (follow 96.2.2).
71.1 This test method covers the determination of moisture in plutonium dioxide samples. Detection limits are as low as 10 μg.
79.1 This test method covers the measurement of volatiles other than water in reactor-grade plutonium dioxide pellets (16). The lower limit of the test method using the described equipment and a sample of approximately 1 g is 0.01 cm3 per gram of sample at STP conditions.
87.1 This test method covers the determination of rare earths in plutonium dioxide over the range from 10 to 200 μg/g.
97.1 This test method covers the determination of the isotopic composition of plutonium in nuclear-grade plutonium dioxide powders and pellets.
106.1 This test method is applicable to the determination of the oxygen-to-metal atom ratio (O/M) in plutonium dioxide pellets and powders.
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
C757 Specification for Nuclear-Grade Plutonium Dioxide Powder, Sinterable
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
C1168 Practice for Preparation and Dissolution of Plutonium Materials for Analysis
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
E60 Practice for Analysis of Metals, Ores, and Related Materials by Molecular Absorption Spectrometry
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 dioxide pellets; plutonium dioxide powders;
ICS Code
ICS Number Code 27.120.30 (Fissile materials and nuclear fuel technology)
DOI: 10.1520/C0697-10
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Citing ASTM Standards
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