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).
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 | |
| 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.
