Significance and Use
Uranyl nitrate solution is used as a feed material for conversion to the hexafluoride as well as for direct conversion to the oxide. In order to be suitable for this purpose, the material must meet certain criteria for uranium content, isotopic composition, acidity, radioactivity, and impurity content. These methods are designed to show whether a given material meets the specifications for these items described in Specification C788.
An assay is performed to determine whether the material has the specified uranium content.
Determination of the isotopic content of the uranium is made to establish whether the effective fissile content is in accordance with the purchaser’s specifications.
Acidity, organic content, and alpha, beta, and gamma activity are measured to establish that they do not exceed their maximum limits.
Impurity content is determined to ensure that the maximum concentration limit of certain impurity elements is not exceeded. Impurity concentrations are also required for calculation of the equivalent boron content (EBC), and the total equivalent boron content (TEBC).
1. Scope
1.1 These test methods cover procedures for the chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade uranyl nitrate solution to determine compliance with specifications.
1.2 The analytical procedures appear in the following order:
| Sections |
| Determination of Uranium | 7 |
| Specific Gravity by Pycnometry | 15-20 |
| Free Acid by Oxalate Complexation | 21-27 |
| Determination of Thorium | 28 |
| Determination of Chromium | 29 |
| Determination of Molybdenum | 30 |
| Halogens Separation by Steam Distillation | 31-35 |
| Fluoride by Specific Ion Electrode | 36-42 |
Halogen Distillate Analysis: Chloride, Bromide, and Iodide by
Amperometric Microtitrimetry | 43 |
| Determination of Chloride and Bromide | 44 |
| Determination of Sulfur by X-Ray Fluorescence | 45 |
| Sulfate Sulfur by (Photometric) Turbidimetry | 46 |
| Phosphorus by the Molybdenum Blue (Photometric) Method | 54-61 |
| Silicon by the Molybdenum Blue (Photometric) Method | 62-69 |
| Carbon by Persulfate Oxidation-Acid Titrimetry | 70 |
| Conversion to U3O8 | 71-74 |
| Boron by Emission Spectrography | 75-81 |
| Impurity Elements by Spark Source Mass Spectrography | 82 |
| Isotopic Composition by Thermal Ionization Mass Spectrometry | 83 |
| Uranium-232 by Alpha Spectrometry | 84-90 |
| Total Alpha Activity by Direct Alpha Counting | 91-97 |
| Fission Product Activity by Beta Counting | 98-104 |
| Entrained Organic Matter by Infrared Spectrophotometry | 105 |
| Fission Product Activity by Gamma Counting | 106 |
| Determination of Arsenic | 107 |
| Determination of Impurities for the EBC Calculation | 108 |
| Determination of Technetium 99 | 109 |
| Determination of Plutonium and Neptunium | 110 |
1.3 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. Specific precautionary statements are given in Section 5.
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
C696 Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Uranium Dioxide Powders and Pellets
C761 Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Uranium Hexafluoride
C788 Specification for Nuclear-Grade Uranyl Nitrate Solution or Crystals
C1219 Test Methods for Arsenic in Uranium Hexafluoride
C1233 Practice for Determining Equivalent Boron Contents of Nuclear Materials
C1254 Test Method for Determination of Uranium in Mineral Acids by X-Ray Fluorescence
C1267 Test Method for Uranium by Iron (II) Reduction in Phosphoric Acid Followed by Chromium (VI) Titration in the Presence of Vanadium
C1287 Test Method for Determination of Impurities in Nuclear Grade Uranium Compounds by Inductively Coupled Plasma Mass Spectrometry
C1295 Test Method for Gamma Energy Emission from Fission Products in Uranium Hexafluoride and Uranyl Nitrate Solution
C1296 Test Method for Determination of Sulfur in Uranium Oxides and Uranyl Nitrate Solutions by X-Ray Fluorescence (XRF)
C1380 Test Method for the Determination of Uranium Content and Isotopic Composition by Isotope Dilution Mass Spectrometry
C1413 Test Method for Isotopic Analysis of Hydrolyzed Uranium Hexafluoride and Uranyl Nitrate Solutions by Thermal Ionization Mass Spectrometry
C1561 Guide for Determination of Plutonium and Neptunium in Uranium Hexafluoride and U-Rich Matrix by Alpha Spectrometry
D1193 Specification for Reagent Water
E12 Terminology Relating to Density and Specific Gravity of Solids, Liquids, and Gases
E60 Practice for Analysis of Metals, Ores, and Related Materials by Spectrophotometry
Other Documents
ISO7097 Determination of Uranium in Uranium Product Solutions and Solids with Cerium IV Oxidation Titrimetric Method Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http://www.ansi.org.
American Chemical Society Specification
Reagent Chemicals 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 Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
Keywords
impurity content; isotopic composition; stoichiometry; uranium content; uranyl nitrate ; Uranium-232 content; Uranium content; Uranyl nitrate solutions; Vanadium content; Volatile matter content--nuclear materials; Alpha (total) activity; Boron content--nuclear-grade materials; Bromine content; Carbon content--nuclear materials; Columbium content; Fission by-products; Free acid content; Impurities--nuclear materials; Mass spectrometry--nuclear materials/applications; Oxalatge complexation; Phosphorus content; Radiochemical analysis; Silicon content; Specific gravity; Spectrochemical analysis; Sulfate sulfur content; Tantalum (Ta) content; Titanium content; Trace elements--spectrochemical analysis; Tungsten content;
ICS Code
ICS Number Code 27.120.30 (Fissile materials and nuclear fuel technology)
DOI: 10.1520/C0799-12
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Citing ASTM Standards
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