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ASTM C799-99(2005)

(Test Method)

Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Uranyl Nitrate Solutions

Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Uranyl Nitrate Solutions

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 C 788.
3.1.1 An assay is performed to determine whether the material has the specified uranium content.
3.1.2 Determination of the isotopic content of the uranium is made to establish whether the effective fissile content is in accordance with the purchaser’specifications.
3.1.3 Acidity, organic content, and alpha, beta, and gamma activity are measured to establish that they do not exceed their maximum limits.
3.1.4 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).
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 Thorium28 Determination of Chromium29 Determination of Molybdenum30 Halogens Separation by Steam Distillation 31-35 Fluoride by Specific Ion Electrode 36-42 Halogen Distillate Analysis: Chloride, Bromide, and Iodide by
Amperometric Microtitrimetry43 Determination of Chloride and Bromide44 Determination of Sulfur by X-Ray Fluorescence45 Sulfate Sulfur by (Photometric) Turbidimetry46 Phosphorus by the Molybdenum Blue (Photometric) Method 54-61 Silicon by the Molybdenum Blue (Photometric) Method62-69 Carbon by Persulfate Oxidation-Acid Titrimetry70 Conversion to U3O871-74 Boron by Emission Spectrography75-81 Impurity Elements by Spark Source Mass Spectrography82 Isotopic Composition by Thermal Ionization Mass Spectrometry83 Uranium-232 by Alpha Spectrometry84-90 Total Alpha Activity by Direct Alpha Counting91-97 Fission Product Activity by Beta Counting98-104 Entrained Organic Matter by Infrared Spectrophotometry105 Fission Product Activity by Gamma Counting106 Determination of Arsenic107 Determination of Impurities for the EBC Calculation108 Determination of Technetium 99109 Determination of Plutonium and Neptunium110
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.  
7.1 Uranium can be determined using iron (II) reduction and dichromate titration. Test Method C1267 can be used.
7.2 Uranium can also be determined using cerium (IV) oxidation titrimetry. ISO 7097 Test Method can be used.  
7.3 Uranium can also be determined by X-Ray Fluorescence using Test Method C1254.
7.4 Previous sections have been deleted.  
8.1 This test method covers the determination of uranium in nuclear-grade uranyl nitrate solution. Appropriate size sample aliquots are chosen to obtain 5 to 10 g of U3O8.  
15.1 This test method covers the determination of the specific gravity of a solution of uranyl nitrate to ±0.0004.  
21.1 This test method covers the determination of the free acid content of uranyl nitrate solutions that may contain a ratio of up to 5 moles of acid to 1 mole of uranium.  
28.1 The determination of thorium by the arsenazo (III) (photometric) method has been discontinued, (see C79...

General Information

Status
Historical
Publication Date
31-May-2005
ICS
27.120.30 - Fissile materials and nuclear fuel technology
Technical Committee
C26 - Nuclear Fuel Cycle
Drafting Committee
C26.05 - Methods of Test
Current Stage
Ref Project

Relations

Replaces
ASTM C799-99e1 - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Uranyl Nitrate Solutions
Effective Date
01-Jun-2005
Referred By
ASTM C1462-21 - Standard Specification for Uranium Metal Enriched to Less Than 20 % <sup> 235</sup >U
Effective Date
01-Jun-2005
Referred By
ASTM C1267-17(2022) - Standard Test Method for Uranium by Iron (II) Reduction in Phosphoric Acid Followed by Chromium (VI) Titration in the Presence of Vanadium
Effective Date
01-Jun-2005
Referred By
ASTM C1334-05(2022) - Standard Specification for Uranium Oxides with a <sup>235</sup>U Content of Less Than 5 % for Dissolution Prior to Conversion to Nuclear-Grade Uranium Dioxide
Effective Date
01-Jun-2005
Referred By
ASTM C809-19 - Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Aluminum Oxide and Aluminum<brk/>Oxide-Boron Carbide Composite Pellets
Effective Date
01-Jun-2005
Referred By
ASTM C761-18 - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Uranium Hexafluoride
Effective Date
01-Jun-2005
Referred By
ASTM C788-03(2021) - Standard Specification for Nuclear-Grade Uranyl Nitrate Solution or Crystals
Effective Date
01-Jun-2005
Referred By
ASTM C1233-15(2021) - Standard Practice for Determining Equivalent Boron Contents of Nuclear Materials
Effective Date
01-Jun-2005

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ASTM C799-99(2005) - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Uranyl Nitrate SolutionsASTM C799-99(2005) - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Uranyl Nitrate Solutions
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ASTM C799-99(2005) - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Uranyl Nitrate Solutions
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Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:C799–99(Reapproved2005)
Standard Test Methods for
Chemical, Mass Spectrometric, Spectrochemical, Nuclear,
and Radiochemical Analysis of Nuclear-Grade Uranyl Nitrate
1
Solutions
This standard is issued under the fixed designation C799; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
2
1.1 These test methods cover procedures for the chemical, 2.1 ASTM Standards:
mass spectrometric, spectrochemical, nuclear, and radiochemi- C696 Test Methods for Chemical, Mass Spectrometric, and
cal analysis of nuclear-grade uranyl nitrate solution to deter- Spectrochemical Analysis of Nuclear-Grade Uranium Di-
mine compliance with specifications. oxide Powders and Pellets
1.2 Theanalyticalproceduresappearinthefollowingorder: C761 Test Methods for Chemical, Mass Spectrometric,
Spectrochemical, Nuclear, and RadiochemicalAnalysis of
Sections
Determination of Uranium 7
Uranium Hexafluoride
Specific Gravity by Pycnometry 15-20
C788 Specification for Nuclear-Grade Uranyl Nitrate Solu-
Free Acid by Oxalate Complexation 21-27
tion or Crystals
Determination of Thorium 28
Determination of Chromium 29
C1219 Test Methods for Arsenic in Uranium Hexafluoride
Determination of Molybdenum 30
C1233 PracticeforDeterminingEquivalentBoronContents
Halogens Separation by Steam Distillation 31-35
Fluoride by Specific Ion Electrode 36-42 of Nuclear Materials
Halogen Distillate Analysis: Chloride, Bromide, and Iodide by 43
C1254 Test Method for Determination of Uranium in Min-
Amperometric Microtitrimetry
eral Acids by X-Ray Fluorescence
Determination of Chloride and Bromide 44
Determination of Sulfur by X-Ray Fluorescence 45 C1267 Test Method for Uranium by Iron (II) Reduction in
Sulfate Sulfur by (Photometric) Turbidimetry 46
PhosphoricAcid Followed by Chromium (VI) Titration in
Phosphorus by the Molybdenum Blue (Photometric) Method 54-61
the Presence of Vanadium
Silicon by the Molybdenum Blue (Photometric) Method 62-69
Carbon by Persulfate Oxidation-Acid Titrimetry 70 C1287 Test Method for Determination of Impurities in
Conversion to U O 71-74
3 8
Nuclear Grade Uranium Compounds by Inductively
Boron by Emission Spectrography 75-81
Coupled Plasma Mass Spectrometry
Impurity Elements by Spark Source Mass Spectrography 82
Isotopic Composition by Thermal Ionization Mass Spectrometry 83 C1295 Test Method for Gamma Energy Emission from
Uranium-232 by Alpha Spectrometry 84-90
Fission Products in Uranium Hexafluoride and Uranyl
Total Alpha Activity by Direct Alpha Counting 91-97
Nitrate Solution
Fission Product Activity by Beta Counting 98-104
Entrained Organic Matter by Infrared Spectrophotometry 105 C1296 TestMethodforDeterminationofSulfurinUranium
Fission Product Activity by Gamma Counting 106
Oxides and Uranyl Nitrate Solutions by X-Ray Fluores-
Determination of Arsenic 107
3
cence (XRF)
Determination of Impurities for the EBC Calculation 108
Determination of Technetium 99 109
C1380 Test Method for the Determination of Uranium
Determination of Plutonium and Neptunium 110
Content and Isotopic Composition by Isotope Dilution
Mass Spectrometry
1.3 This standard does not purport to address all of the
C1413 Test Method for Isotopic Analysis of Hydrolyzed
safety concerns, if any, associated with its use. It is the
Uranium Hexafluoride and Uranyl Nitrate Solutions by
responsibility of the user of this standard to establish appro-
Thermal Ionization Mass Spectrometry
priate safety and health practices and determine the applica-
D1193 Specification for Reagent Water
bility of regulatory limitations prior to use. Specific precau-
E12 Terminology Relating to Density and Specific Gravity
tionary statements are given in Section 5.
1 2
These test methods are under the jurisdiction of ASTM Committee C26 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Nuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.05 on contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Methods of Test. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved June 1, 2005. Published October 2005. Originally the ASTM website.
e1 3
approved in 1975. Last previous edition approved in 1999 as C799–99 . DOI: Withdrawn. The last approved version of this historical standard is referenced
10.1520/C0799-99R05. on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
C799–99 (2005)
of Solids, Liquids, and Gases 5.2 T
...

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SIGNIFICANCE AND USE
5.1 This test method allows the determination of 241Am in a plutonium solution without separation of the americium from the plutonium. It is generally applicable to any solution containing 241Am.  
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Procedure Number  
Procedure Title  
Section  
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9  
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17  
10  
Open-Vessel (with Reflux Condenser) Dissolution of Mixed Oxide Pellets  
18  
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This specification covers finished sintered and ground (uranium-plutonium) dioxide pellets for use in thermal reactors. It applies to uranium-plutonium dioxide pellets containing plutonium additions up to 15 % weight. The diversity of manufacturing methods shall be recognized by which uranium-plutonium dioxide pellets are produced and the many special requirements for chemical and physical characterization that may be imposed by the operating conditions to which the pellets will be subjected in specific reactor systems. The following are different chemical requirements that shall be determined: uranium content, plutonium content, impurity content, stoichiometry, moisture content, gas content, and americium-241 content. Nuclear requirements such as isotopic content, plutonium equivalent at a given date, equivalent boron content, and reactivity shall also be determined. Physical properties of the pellets like dimensions, density, grain size, pore morphology, plutonium-oxide homogeneity, plutonium-oxide particle size, plutonium-oxide particle distribution, integrity, and surface cracks shall be determined as well. The surfaces of finished pellets shall be visually free of loose chips, oil, macroscopic inclusions, and foreign materials. An estimate of the fuel pellet irradiation stability shall be obtained unless adequate allowance for such effects are factored into the fuel rod design. The estimate of the stability shall consist of either conformance to the thermal stability test as specified in the or by adequate correlation of manufacturing process or microstructure to in-reactor behavior, or both.
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4.1 Materials handling equipment operability and long-term integrity are concerns that originate during the design and fabrication sequences. Such concerns are most efficiently addressed during one or the other of these stages. Equipment operability and integrity can be compromised during handling and installation sequences. For this reason, the subject equipment should be handled and installed under closely controlled and supervised conditions.  
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4.5.1 Boots and similar protective covers should not restrict movement of the equipment, should be properly sealed to the equipment and should withstand the radiation, cell atmosphere, dust, cell temperatures, chemical exposures, and cleaning and decontamination reagents, and also resist snags and tearing.  
4.5.2 Materials handling equipment should be capable of withstanding rigorous chemical cleaning and decontamination procedures.  
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1.1 Intent:  
1.1.1 This guide covers materials handling equipment used in hot cells (shielded cells) for the processing and handling of nuclear and radioactive materials. The intent of this guide is to aid in the selection and design of materials handling equipment for hot cells in order to minimize equipment failures and maximize the equipment utility.  
1.1.2 It is intended that this guide record the principles and caveats that experience has shown to be essential to the design, fabrication, installation, maintenance, repair, replacement, and decontamination and decommissioning of materials handling equipment capable of meeting the stringent demands of operating, dependably and safely, in a hot cell environment where operator visibility is limited due to the radiation exposure hazards.  
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1.1.4 This guide covers mechanical master-slave manipulators and electro-mechanical manipulators, but does not cover electro-hydraulic manipulators.  
1.2 Applicability:  
1.2.1 This guide is intended to be applicable to equipment used under one or more of the following conditions:
1.2.1.1 The materials handled or processed constitute a significant radiation hazard to man or to the environment.
1.2.1.2 The equipment will generally be used over a long-term life cycle (for example, in excess of two years), but equipment intended for use over a shorter life cycle is not excluded.
1.2.1.3 The equipment can neither be accessed directly for purposes of operation or maintenance, nor can the equipment be viewed directly, for example, without shielded viewing windows, periscopes, or a video monitoring system.  
1.3 User Caveats:  
1.3.1 This standard is not a substitute for applied engin...

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ASTM
ASTM C1703-18(2023)(Practice)
Standard Practice for Sampling of Gaseous Uranium Hexafluoride for Enrichment

SIGNIFICANCE AND USE
5.1 Uranium hexafluoride is normally produced and handled in large (typically 1 to 14-ton) quantities and must, therefore, be characterized by reference to representative samples (see ISO 7195). The samples are used to determine compliance with the applicable commercial specification C787. The quantities involved, physical properties, chemical reactivity, and hazardous nature of UF6 are such that for representative sampling, specially designed equipment must be used and operated in accordance with the most carefully controlled and stringent procedures. This practice can be used by UF6 converters to review the effectiveness of existing procedures or as a guide to the design of equipment and procedures for future use.  
5.2 The intention of this practice is to avoid liquid UF6 sampling once the cylinder has been filled. For safety reasons, manipulation of large quantities of liquid UF6 should be avoided when possible.  
5.3 It is emphasized that this practice is not meant to address conventional or nuclear criticality safety issues.
SCOPE
1.1 This practice covers methods for withdrawing representative sample(s) of uranium hexafluoride (UF6) during a transfer occurring in the gas phase. Such transfer in the gas phase can take place during the filling of a cylinder during a continuous production process, for example the distillation column in a conversion facility. Such sample(s) may be used for determining compliance with the applicable commercial specification, for example Specification C787.  
1.2 Since UF6 sampling is taken during the filling process, this practice does not address any special additional arrangements that may be agreed upon between the buyer and the seller when the sampled bulk material is being added to residues already present in a container (“heels recycle”). Such arrangements will be based on QA procedures such as traceability of cylinder origin (to prevent for example contamination with irradiated material).  
1.3 If the receiving cylinder is purged after filling and sampling, special verifications must be performed by the user to verify the representativity of the sample(s). It is then expected that the results found on volatile impurities with gas phase sampling may be conservative.  
1.4 This practice is only applicable when the transfer occurs in the gas phase. When the transfer is performed in the liquid phase, Practice C1052 should apply. This practice does not apply to gas sampling after the cylinder has been filled since the sample taken will not be representative of the cylinder.  
1.5 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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ASTM
ASTM C1347-08(2023)(Practice)
Standard Practice for Preparation and Dissolution of Uranium Materials for Analysis

SIGNIFICANCE AND USE
4.1 The materials covered that must meet ASTM specifications are uranium metal and uranium oxide.  
4.2 Uranium materials are used as nuclear reactor fuel. For this use, these materials must meet certain criteria for uranium content, uranium-235 enrichment, and impurity content, as described in Specifications C753 and C776. The material is assayed for uranium to determine whether the content is as specified.  
4.3 Uranium alloys, refractory uranium materials, and uranium containing scrap and ash are unique uranium materials for which the user must determine the applicability of this practice. In general, these unique uranium materials are dissolved with various acid mixtures or by fusion with various fluxes.
SCOPE
1.1 This practice covers dissolution treatments for uranium materials that are applicable to the test methods used for characterizing these materials for uranium elemental, isotopic, and impurities determinations. Dissolution treatments for the major uranium materials assayed for uranium or analyzed for other components are listed.  
1.2 The treatments, in order of presentation, are as follows:    
Procedure Title  
Section  
Dissolution of Uranium Metal and Oxide with Nitric Acid  
8.1  
Dissolution of Uranium Oxides with Nitric Acid and Residue
Treatment  
8.2  
Dissolution of Uranium-Aluminum Alloys in Hydrochloric Acid
with Residue Treatment  
8.3  
Dissolution of Uranium Scrap and Ash by Leaching with Nitric
Acid and Treatment of Residue by Carbonate Fusion  
8.4  
Dissolution of Refractory Uranium-Containing Material by
Carbonate Fusion  
8.5  
Dissolution of Uranium—Aluminum Alloys
Uranium Scrap and Ash, and Refractory
Uranium-Containing Materials by
Microwave Treatment  
8.6  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific hazards statements are given in Section 7.  
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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ASTM
ASTM C1165-23(Test Method)
Standard Test Method for Determining Plutonium by Controlled-Potential Coulometry in H2SO4 at a Platinum Working Electrode

SIGNIFICANCE AND USE
5.1 This test method is used to ascertain whether or not materials meet specifications for plutonium concentration or plutonium mass fraction.  
5.1.1 The materials (nuclear grade plutonium nitrate solutions, plutonium metal, plutonium oxide powder, and mixed oxide and carbide powders and pellets) to which this test method applies are subject to nuclear safeguards regulations governing their possession and use. However, adherence to this test method does not automatically guarantee regulatory acceptance of the resulting safeguards measurements. It remains the sole responsibility of the user of this test method to ensure that its application to safeguards has the approval of the proper regulatory authorities.  
5.1.2 When used in conjunction with appropriate certified reference materials (CRMs), this test method can demonstrate traceability to the international measurements system (SI).  
5.2 Fitness for Purpose of Safeguards and Nuclear Safety Application—Methods intended for use in safeguards and nuclear safety applications shall meet the requirements specified by Guide C1068 for use in such applications.  
5.3 A chemical calibration of the coulometer is necessary for accurate results.
FIG. 1 Example of a Cell Design Used at Los Alamos National Laboratory (LANL)
SCOPE
1.1 This test method covers the determination of milligram quantities of plutonium in unirradiated uranium-plutonium mixed oxide having a U/Pu ratio range of 0.1 to 10. This test method is also applicable to plutonium metal, plutonium oxide, uranium-plutonium mixed carbide, various plutonium compounds including fluoride and chloride salts, and plutonium solutions.  
1.2 The recommended amount of plutonium for each aliquant in the coulometric analysis is 5 mg to 10 mg. Precision worsens for lower amounts of plutonium, and elapsed time of electrolysis becomes impractical for higher amounts of plutonium.  
1.3 The quantity values stated in SI units are to be regarded as standard. The quantity values with non-SI units are given in parentheses 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 9.  
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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