ASTM C799-19

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

SIGNIFICANCE AND USE
4.1 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.  
4.1.1 An assay is performed to determine whether the material has the specified uranium content.  
4.1.2 Determination of the isotopic content of the uranium is made to establish whether the effective fissile content is in accordance with the purchaser’s specifications.  
4.1.3 Acidity, organic content, and alpha, beta, and gamma activity are measured to establish that they do not exceed their maximum limits.  
4.1.4 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  
8  
Specific Gravity by Pycnometry  
16 – 21  
Free Acid by Oxalate Complexation  
22 – 28  
Determination of Thorium  
29  
Determination of Chromium  
30  
Determination of Molybdenum  
31  
Halogens Separation by Steam Distillation  
32 – 36  
Fluoride by Specific Ion Electrode  
37 – 43  
Halogen Distillate Analysis: Chloride, Bromide, and Iodide by
Amperometric Microtitrimetry  
44  
Determination of Chloride and Bromide  
45  
Determination of Sulfur by X-Ray Fluorescence  
46  
Sulfate Sulfur by (Photometric) Turbidimetry  
47  
Phosphorus by the Molybdenum Blue (Photometric) Method  
55 – 62  
Silicon by the Molybdenum Blue (Photometric) Method  
63 – 70  
Carbon by Persulfate Oxidation-Acid Titrimetry  
71  
Conversion to U3O8  
72 – 75  
Boron by Emission Spectrography  
A  
Impurity Elements by Spark Source Mass Spectrography  
77  
Isotopic Composition by Thermal Ionization Mass Spectrometry  
78  
Uranium-232 by Alpha Spectrometry  
79 – 85  
Total Alpha Activity by Direct Alpha Counting  
86 – 92  
Fission Product Activity by Beta Counting  
93 – 99  
Entrained Organic Matter by Infrared Spectrophotometry  
100  
Fission Product Activity by Gamma Counting  
101  
Determination of Arsenic  
102  
Determination of Impurities for the EBC Calculation  
103  
Determination of Technetium 99  
104  
Determination of Plutonium and Neptunium  
105  
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 precautionary statements are given in Section 6.  
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.

General Information

• Status: Published
• Publication Date: 30-Jun-2019
• ICS: 27.120.30 - Fissile materials and nuclear fuel technology
• Technical Committee: C26 - Nuclear Fuel Cycle
• Drafting Committee: C26.05 - Methods of Test

Relations

• Refers: ASTM C1295-14 - Standard Test Method for Gamma Energy Emission from Fission and Decay Products in Uranium Hexafluoride and Uranyl Nitrate Solution
• Effective Date: 15-Jun-2014
• Refers: ASTM C761-18 - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Uranium Hexafluoride
• Effective Date: 01-Feb-2018
• Refers: ASTM C1871-18 - Standard Test Method for Determination of Uranium Isotopic Composition by the Double Spike Method Using a Thermal Ionization Mass Spectrometer
• Effective Date: 01-Feb-2018
• Refers: ASTM C1254-18 - Standard Test Method for Determination of Uranium in Mineral Acids by X-Ray Fluorescence
• Effective Date: 01-Oct-2018
• Refers: ASTM C1413-18 - Standard Test Method for Isotopic Analysis of Hydrolyzed Uranium Hexafluoride and Uranyl Nitrate Solutions by Thermal Ionization Mass Spectrometry
• Effective Date: 01-Nov-2018
• Refers: ASTM C696-19 - Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Uranium Dioxide Powders and Pellets
• Effective Date: 01-Nov-2019
• Refers: ASTM C859-14a - Standard Terminology Relating to Nuclear Materials
• Effective Date: 15-Jun-2014
• Refers: ASTM C1295-15 - Standard Test Method for Gamma Energy Emission from Fission and Decay Products in Uranium Hexafluoride and Uranyl Nitrate Solution
• Effective Date: 01-Jun-2015
• Refers: ASTM C1517-16 - Standard Test Method for Determination of Metallic Impurities in Uranium Metal or Compounds by DC-Arc Emission Spectroscopy
• Effective Date: 01-Apr-2016
• Refers: ASTM C1561-10(2016) - Standard Guide for Determination of Plutonium and Neptunium in Uranium Hexafluoride and U-Rich Matrix by Alpha Spectrometry
• Effective Date: 01-Jun-2016
• Refers: ASTM C1287-18 - Standard Test Method for Determination of Impurities in Nuclear Grade Uranium Compounds by Inductively Coupled Plasma Mass Spectrometry
• Effective Date: 01-Jan-2018
• Referred By: ASTM C788-03(2021) - Standard Specification for Nuclear-Grade Uranyl Nitrate Solution or Crystals
• Effective Date: 01-Jul-2019
• Referred By: ASTM C1334-05(2022) - Standard Specification for Uranium Oxides with a ²³⁵U Content of Less Than 5 % for Dissolution Prior to Conversion to Nuclear-Grade Uranium Dioxide
• Effective Date: 01-Jul-2019
• 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-Jul-2019
• 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-Jul-2019
• Referred By: ASTM C1233-15(2021) - Standard Practice for Determining Equivalent Boron Contents of Nuclear Materials
• Effective Date: 01-Jul-2019
• Referred By: ASTM C1462-21 - Standard Specification for Uranium Metal Enriched to Less Than 20 % <sup> 235</sup >U
• Effective Date: 01-Jul-2019

Standards Content (Sample)

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.
Designation: C799 − 19
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 1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 These test methods cover procedures for the chemical,
responsibility of the user of this standard to establish appro-
mass spectrometric, spectrochemical, nuclear, and radiochemi-
priate safety, health, and environmental practices and deter-
cal analysis of nuclear-grade uranyl nitrate solution to deter-
mine the applicability of regulatory limitations prior to use.
mine compliance with specifications.
Specific precautionary statements are given in Section 6.
1.2 Theanalyticalproceduresappearinthefollowingorder:
1.5 This international standard was developed in accor-
Sections
dance with internationally recognized principles on standard-
Determination of Uranium 8
ization established in the Decision on Principles for the
Specific Gravity by Pycnometry 16–21
Development of International Standards, Guides and Recom-
Free Acid by Oxalate Complexation 22–28
Determination of Thorium 29
mendations issued by the World Trade Organization Technical
Determination of Chromium 30
Barriers to Trade (TBT) Committee.
Determination of Molybdenum 31
Halogens Separation by Steam Distillation 32–36
2. Referenced Documents
Fluoride by Specific Ion Electrode 37–43
Halogen Distillate Analysis: Chloride, Bromide, and Iodide by 44
2
2.1 ASTM Standards:
Amperometric Microtitrimetry
Determination of Chloride and Bromide 45 C696Test Methods for Chemical, Mass Spectrometric, and
Determination of Sulfur by X-Ray Fluorescence 46
SpectrochemicalAnalysis of Nuclear-Grade Uranium Di-
Sulfate Sulfur by (Photometric) Turbidimetry 47
oxide Powders and Pellets
Phosphorus by the Molybdenum Blue (Photometric) Method 55–62
Silicon by the Molybdenum Blue (Photometric) Method 63–70
C761Test Methods for Chemical, Mass Spectrometric,
Carbon by Persulfate Oxidation-Acid Titrimetry 71
Spectrochemical,Nuclear,andRadiochemicalAnalysisof
Conversion to U O 72–75
3 8
A
Uranium Hexafluoride
Boron by Emission Spectrography
Impurity Elements by Spark Source Mass Spectrography 77
C788Specification for Nuclear-Grade Uranyl Nitrate Solu-
Isotopic Composition by Thermal Ionization Mass Spectrometry 78
tion or Crystals
Uranium-232 by Alpha Spectrometry 79–85
C859Terminology Relating to Nuclear Materials
Total Alpha Activity by Direct Alpha Counting 86–92
Fission Product Activity by Beta Counting 93–99 C1219Test Methods for Arsenic in Uranium Hexafluoride
Entrained Organic Matter by Infrared Spectrophotometry 100 3
(Withdrawn 2015)
Fission Product Activity by Gamma Counting 101
C1233Practice for Determining Equivalent Boron Contents
Determination of Arsenic 102
Determination of Impurities for the EBC Calculation 103
of Nuclear Materials
Determination of Technetium 99 104
C1254Test Method for Determination of Uranium in Min-
Determination of Plutonium and Neptunium 105
eral Acids by X-Ray Fluorescence
A
C1267Test Method for Uranium by Iron (II) Reduction in
Discontinued July 2019.
PhosphoricAcid Followed by Chromium (VI)Titration in
1.3 The values stated in SI units are to be regarded as
the Presence of Vanadium
standard. No other units of measurement are included in this
C1287Test Method for Determination of Impurities in
standard.
Nuclear Grade Uranium Compounds by Inductively
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 [e-mail]. For Annual Book of ASTM
Methods of Test. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved July 1, 2019. Published August 2019. Originally the ASTM website.
3
approved in 1975. Last previous edition approved in 2012 as C799–12. DOI: The last approved version of this historical standard is referenced on
10.1520/C0799-19. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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C799
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: C799 − 12 C799 − 19
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. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
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
Determination of Uranium 8
Specific Gravity by Pycnometry 15 – 20
Specific Gravity by Pycnometry 16 – 21
Free Acid by Oxalate Complexation 21 – 27
Free Acid by Oxalate Complexation 22 – 28
Determination of Thorium 28
Determination of Thorium 29
Determination of Chromium 29
Determination of Chromium 30
Determination of Molybdenum 30
Determination of Molybdenum 31
Halogens Separation by Steam Distillation 31 – 35
Halogens Separation by Steam Distillation 32 – 36
Fluoride by Specific Ion Electrode 36 – 42
Fluoride by Specific Ion Electrode 37 – 43
Halogen Distillate Analysis: Chloride, Bromide, and Iodide by 43
Amperometric Microtitrimetry
Halogen Distillate Analysis: Chloride, Bromide, and Iodide by 44
Amperometric Microtitrimetry
Determination of Chloride and Bromide 44
Determination of Chloride and Bromide 45
Determination of Sulfur by X-Ray Fluorescence 45
Determination of Sulfur by X-Ray Fluorescence 46
Sulfate Sulfur by (Photometric) Turbidimetry 46
Sulfate Sulfur by (Photometric) Turbidimetry 47
Phosphorus by the Molybdenum Blue (Photometric) Method 54 – 61
Phosphorus by the Molybdenum Blue (Photometric) Method 55 – 62
Silicon by the Molybdenum Blue (Photometric) Method 62 – 69
Silicon by the Molybdenum Blue (Photometric) Method 63 – 70
Carbon by Persulfate Oxidation-Acid Titrimetry 70
Carbon by Persulfate Oxidation-Acid Titrimetry 71
Conversion to U O 71 – 74
3 8
Conversion to U O 72 – 75
3 8
Boron by Emission Spectrography 75 – 81
A
Boron by Emission Spectrography
Impurity Elements by Spark Source Mass Spectrography 82
Impurity Elements by Spark Source Mass Spectrography 77
Isotopic Composition by Thermal Ionization Mass Spectrometry 83
Isotopic Composition by Thermal Ionization Mass Spectrometry 78
Uranium-232 by Alpha Spectrometry 84 – 90
Uranium-232 by Alpha Spectrometry 79 – 85
1
These test methods are under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.05 on Methods
of Test.
Current edition approved Jan. 1, 2012July 1, 2019. Published February 2012August 2019. Originally approved in 1975. Last previous edition approved in 20052012 as
C799 – 99C799 – 12.(2005). DOI: 10.1520/C0799-12.10.1520/C0799-19.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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C799 − 19
Total Alpha Activity by Direct Alpha Counting 91 – 97
Total Alpha Activity by Direct Alpha Counting 86 – 92
Fission Product Activity by Beta Counting 98 – 104
Fission Product Activity by Beta Counting 93 – 99
Entrained Organic Matter by Infrared Spectrophotometry 105
Entrained Organic Matter by Infrared Spectrophotometry 100
Fission Product Activity by Gamma Counting 106
Fission Product Activity by Gamma Counting 101
Determination of Arsenic 107
Determination of Arsenic 102
Determination of Impurities for the EBC Calculation 108
Determination of Impurities for the EBC Calculation 103
Determination of Technetium 99 109
Determination of Technetium 99 104
Determination of Plutonium and Neptunium 110
Determination of Plutonium and Neptunium 105
A
Discontinued July 2019.
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 56.
1.5 This inter
...