ASTM C761-18

Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Uranium Hexafluoride

SIGNIFICANCE AND USE
4.1 Uranium hexafluoride is a basic material used to prepare nuclear reactor fuel. To be suitable for this purpose the material must meet criteria for uranium content, isotopic composition, metallic impurities, hydrocarbon and halohydrocarbon content. These test methods are designed to determine whether the material meets the requirements described in Specifications C787 and C996.
SCOPE
1.1 These test methods cover or give reference to procedures for subsampling and for chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of uranium hexafluoride (UF6). Most of these test methods are in routine use to determine conformance to UF6 specifications in the Enrichment and Conversion Facilities.  
1.2 The analytical procedures in this document appear in the following order:
Note 1: Subcommittee C26.05 will confer with C26.02 concerning the renumbered section in Test Methods C761 to determine how concerns with renumbering these sections are best addressed in subsequent publications as analytical methods are replaced with stand-alone analytical methods.    
Sections  
Subsampling of Uranium Hexafluoride  
8  
Gravimetric Determination of Uranium  
9 – 17  
Titrimetric Determination of Uranium  
18  
Preparation of High-Purity U3O8  
19  
Isotopic Analysis  
20  
Determination of Hydrocarbons, Chlorocarbons, and Partially Substituted Halohydrocarbons  
21 – 27  
Determination of Antimony  
28  
Determination of Bromine  
29  
Determination of Chlorine  
30 – 36  
Determination of Silicon and Phosphorus  
37 – 43  
Determination of Boron and Silicon  
44  
Determination of Ruthenium  
45  
Determination of Titanium and Vanadium  
46  
Spectrographic Determination of Metallic Impurities  
47  
Determination of Tungsten  
48  
Determination of Thorium and Rare Earths  
49  
Determination of Molybdenum  
50  
Atomic Absorption Determination of Metallic Impurities  
51 – 56  
Impurity Determination by Spark-Source Mass Spectrography  
57  
Determination of Boron-Equivalent Neutron Cross Section  
58  
Determination of Uranium-233 Abundance by Thermal Ionization Mass Spectrometry  
59  
Determination of Uranium-232 by Alpha Spectrometry  
60 – 66  
Determination of Fission Product Activity  
67  
Determination of Plutonium by Ion Exchange and Alpha Counting  
68 – 72  
Determination of Plutonium by Extraction and Alpha Counting  
73 – 80  
Determination of Neptunium by Extraction and Alpha Counting  
81 – 88  
Atomic Absorption Determination of Chromium Soluble In Uranium Hexafluoride  
89 – 95  
Atomic Absorption Determination of Chromium Insoluble In Uranium Hexafluoride  
101 – 102  
Determination of Technetium-99 In Uranium Hexafluoride  
103 – 110  
Method for the Determination of Gamma-Energy Emission Rate from Fission Products in Uranium Hexafluoride  
112  
Determination of Metallic Impurities by ICP-AES  
113 – 122  
Determination of Molybdenum, Niobium, Tantalum, Titanium, and Tungsten by ICP-AES  
123 – 132  
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. (For specific safeguard and safety consideration statements, see 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.

General Information

• Status: Published
• Publication Date: 31-Jan-2018
• 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 C1128-15 - Standard Guide for Preparation of Working Reference Materials for Use in Analysis of Nuclear Fuel Cycle Materials
• Effective Date: 01-Feb-2015
• 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 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
• Refers: ASTM C1474-19 - Standard Test Method for Analysis of Isotopic Composition of Uranium in Nuclear-Grade Fuel Material by Quadrupole Inductively Coupled Plasma-Mass Spectrometry
• Effective Date: 01-Feb-2019
• Refers: ASTM C859-14a - Standard Terminology Relating to Nuclear Materials
• Effective Date: 15-Jun-2014
• 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 C787-15 - Standard Specification for Uranium Hexafluoride for Enrichment
• Effective Date: 01-Jul-2015
• Refers: ASTM C996-15 - Standard Specification for Uranium Hexafluoride Enriched to Less Than 5 % ²³⁵U
• Effective Date: 01-Jul-2015
• Referred By: ASTM C1883-19 - Standard Practice for Sampling of Gaseous Enriched Uranium Hexafluoride
• Effective Date: 01-Feb-2018
• Referred By: ASTM C799-19 - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Uranyl Nitrate Solutions
• Effective Date: 01-Feb-2018
• Referred By: ASTM C1022-17(2022) - Standard Test Methods for Chemical and Atomic Absorption Analysis of Uranium-Ore Concentrate
• Effective Date: 01-Feb-2018
• Referred By: ASTM C1689-21 - Standard Practice for Subsampling of Uranium Hexafluoride
• Effective Date: 01-Feb-2018
• Referred By: ASTM C1346-19 - Standard Practice for Dissolution of UF<inf>6</inf> from P-10 Tubes
• Effective Date: 01-Feb-2018
• Referred By: ASTM C889-18 - Standard Test Methods for Chemical and Mass Spectrometric Analysis of Nuclear-Grade Gadolinium Oxide (Gd<inf>2</inf>O<inf>3</inf>) Powder
• Effective Date: 01-Feb-2018
• Referred By: ASTM C1233-15(2021) - Standard Practice for Determining Equivalent Boron Contents of Nuclear Materials
• Effective Date: 01-Feb-2018
• Referred By: ASTM C696-19 - Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Uranium Dioxide Powders and Pellets
• Effective Date: 01-Feb-2018
• Referred By: ASTM C1880-19 - Standard Practice for Sampling Gaseous Uranium Hexafluoride using Alumina Pellets
• Effective Date: 01-Feb-2018
• Referred By: ASTM C1703-18(2023) - Standard Practice for Sampling of Gaseous Uranium Hexafluoride for Enrichment
• Effective Date: 01-Feb-2018
• Referred By: ASTM C1842-16 - Standard Test Method for The Analysis of Boron and Silicon in Uranium Hexfluoride via Fourier-Transform Infrared (FTIR) Spectroscopy
• Effective Date: 01-Feb-2018
• Referred By: ASTM C787-20 - Standard Specification for Uranium Hexafluoride for Enrichment
• Effective Date: 01-Feb-2018
• Referred By: ASTM C1429-21 - Standard Test Method for Isotopic Analysis of Uranium Hexafluoride by Double-Standard Multi-Collector Gas Mass Spectrometer
• Effective Date: 01-Feb-2018
• Referred By: ASTM C996-20 - Standard Specification for Uranium Hexafluoride Enriched to Less Than 5&#x2009;%&#x2009;<sup > 235</sup>U
• Effective Date: 01-Feb-2018
• Referred By: ASTM C1477-19 - Standard Test Method for Isotopic Abundance Analysis of Uranium Hexafluoride and Uranyl Nitrate Solutions by Multi-Collector, Inductively Coupled Plasma-Mass Spectrometry
• Effective Date: 01-Feb-2018
• Referred By: ASTM C1508-18 - Standard Test Method for Determination of Bromine and Chlorine in UF<inf>6</inf> and Uranyl Nitrate by X-Ray Fluorescence (XRF) Spectroscopy
• Effective Date: 01-Feb-2018
• Referred By: 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-Feb-2018
• Referred By: ASTM C1517-16 - Standard Test Method for Determination of Metallic Impurities in Uranium Metal or Compounds by DC-Arc Emission Spectroscopy
• Effective Date: 01-Feb-2018

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:C761 −18
Standard Test Methods for
Chemical, Mass Spectrometric, Spectrochemical, Nuclear,
1
and Radiochemical Analysis of Uranium Hexafluoride
This standard is issued under the fixed designation C761; 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
Determination of Plutonium by Extraction and Alpha Counting 73 – 80
Determination of Neptunium by Extraction and Alpha Counting 81 – 88
1.1 These test methods cover or give reference to proce-
Atomic Absorption Determination of Chromium Soluble In 89 – 95
dures for subsampling and for chemical, mass spectrometric, Uranium Hexafluoride
Atomic Absorption Determination of Chromium Insoluble In 101 – 102
spectrochemical, nuclear, and radiochemical analysis of ura-
Uranium Hexafluoride
nium hexafluoride (UF ). Most of these test methods are in
6 Determination of Technetium-99 In Uranium Hexafluoride 103 – 110
routine use to determine conformance to UF specifications in Method for the Determination of Gamma-Energy Emission Rate 112
6
from Fission Products in Uranium Hexafluoride
the Enrichment and Conversion Facilities.
Determination of Metallic Impurities by ICP-AES 113 – 122
Determination of Molybdenum, Niobium, Tantalum, Titanium, 123 – 132
1.2 Theanalyticalproceduresinthisdocumentappearinthe
and Tungsten by ICP-AES
following order:
1.3 The values stated in SI units are to be regarded as
NOTE1—SubcommitteeC26.05willconferwithC26.02concerningthe
standard. No other units of measurement are included in this
renumbered section in Test Methods C761 to determine how concerns
standard.
with renumbering these sections are best addressed in subsequent publi-
cations as analytical methods are replaced with stand-alone analytical
1.4 This standard does not purport to address all of the
methods.
safety concerns, if any, associated with its use. It is the
Sections
responsibility of the user of this standard to establish appro-
Subsampling of Uranium Hexafluoride 8
priate safety, health, and environmental practices and deter-
Gravimetric Determination of Uranium 9 – 17
mine the applicability of regulatory limitations prior to use.
Titrimetric Determination of Uranium 18
Preparation of High-Purity U O 19
(Forspecificsafeguardandsafetyconsiderationstatements,see
3 8
Isotopic Analysis 20
Section 7.)
Determination of Hydrocarbons, Chlorocarbons, and Partially 21 – 27
1.5 This international standard was developed in accor-
Substituted Halohydrocarbons
Determination of Antimony 28
dance with internationally recognized principles on standard-
Determination of Bromine 29
ization established in the Decision on Principles for the
Determination of Chlorine 30 – 36
Development of International Standards, Guides and Recom-
Determination of Silicon and Phosphorus 37 – 43
Determination of Boron and Silicon 44
mendations issued by the World Trade Organization Technical
Determination of Ruthenium 45
Barriers to Trade (TBT) Committee.
Determination of Titanium and Vanadium 46
Spectrographic Determination of Metallic Impurities 47
2. Referenced Documents
Determination of Tungsten 48
Determination of Thorium and Rare Earths 49
2.1 The following documents of the issue in effect on date
Determination of Molybdenum 50
of material procurement form a part of this specification to the
Atomic Absorption Determination of Metallic Impurities 51 – 56
Impurity Determination by Spark-Source Mass Spectrography 57
extent referenced herein:
Determination of Boron-Equivalent Neutron Cross Section 58
2
Determination of Uranium-233 Abundance by Thermal Ionization 59
2.2 ASTM Standards:
Mass Spectrometry
C787Specification for Uranium Hexafluoride for Enrich-
Determination of Uranium-232 by Alpha Spectrometry 60 – 66
ment
Determination of Fission Product Activity 67
Determination of Plutonium by Ion Exchange and Alpha 68 – 72
C799Test Methods for Chemical, Mass Spectrometric,
Counting
Spectrochemical,Nuclear,andRadiochemicalAnalysisof
Nuclear-Grade Uranyl Nitrate Solutions
C859Terminology Relating to Nuclear Materials
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
2
Methods of Test. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Feb. 1, 2018. Published February 2018. Originally contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
approved in 1973. Last previous edition approv
...

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: C761 − 11 C761 − 18
Standard Test Methods for
Chemical, Mass Spectrometric, Spectrochemical, Nuclear,
1
and Radiochemical Analysis of Uranium Hexafluoride
This standard is issued under the fixed designation C761; 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 or give reference to procedures for subsampling and for chemical, mass spectrometric,
spectrochemical, nuclear, and radiochemical analysis of uranium hexafluoride (UF ). Most of these test methods are in routine use
6
to determine conformance to UF specifications in the Enrichment and Conversion Facilities.
6
1.2 The analytical procedures in this document appear in the following order:
NOTE 1—Subcommittee C26.05 will confer with C26.02 concerning the renumbered section in Test Methods C761 to determine how concerns with
renumbering these sections are best addressed in subsequent publications as analytical methods are replaced with stand-alone analytical methods.
Sections
Subsampling of Uranium Hexafluoride 7
Subsampling of Uranium Hexafluoride 8
Gravimetric Determination of Uranium 8 – 16
Gravimetric Determination of Uranium 9 – 17
Titrimetric Determination of Uranium 17
Titrimetric Determination of Uranium 18
Preparation of High-Purity U O 18
3 8
Preparation of High-Purity U O 19
3 8
Isotopic Analysis 19
Isotopic Analysis 20
Determination of Hydrocarbons, Chlorocarbons, and Partially 20–26
Substituted Halohydrocarbons
Determination of Hydrocarbons, Chlorocarbons, and Partially 21 – 27
Substituted Halohydrocarbons
Determination of Antimony 27
Determination of Antimony 28
Determination of Bromine 28
Determination of Bromine 29
Determination of Chlorine 29 – 35
Determination of Chlorine 30 – 36
Determination of Silicon and Phosphorus 36– 42
Determination of Silicon and Phosphorus 37 – 43
Determination of Boron and Silicon 43
Determination of Boron and Silicon 44
Determination of Ruthenium 44
Determination of Ruthenium 45
Determination of Titanium and Vanadium 45
Determination of Titanium and Vanadium 46
Spectrographic Determination of Metallic Impurities 46
Spectrographic Determination of Metallic Impurities 47
Determination of Tungsten 47
Determination of Tungsten 48
Determination of Thorium and Rare Earths 48
Determination of Thorium and Rare Earths 49
Determination of Molybdenum 49
Determination of Molybdenum 50
Atomic Absorption Determination of Metallic Impurities 50 – 55
Atomic Absorption Determination of Metallic Impurities 51 – 56
Impurity Determination by Spark-Source Mass Spectrography 56
Impurity Determination by Spark-Source Mass Spectrography 57
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 May 15, 2011Feb. 1, 2018. Published July 2011February 2018. Originally approved in 1973. Last previous edition approved in 20042011 as
ε1
C761 – 04C761 – 11. . DOI: 10.1520/C0761-11.10.1520/C0761-18.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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C761 − 18
Determination of Boron-Equivalent Neutron Cross Section 57
Determination of Boron-Equivalent Neutron Cross Section 58
Determination of Uranium-233 Abundance by Thermal Ionization 58
Mass Spectrometry
Determination of Uranium-233 Abundance by Thermal Ionization 59
Mass Spectrometry
Determination of Uranium-232 by Alpha Spectrometry 59 – 65
Determination of Uranium-232 by Alpha Spectrometry 60 – 66
Determination of Fission Product Activity 66
Determination of Fission Product Activity 67
Determination of Plutonium by Ion Exchange and Alpha 67 – 71
Counting
Determination of Plutonium by Ion Exchange and Alpha 68 – 72
Counting
Determination of Plutonium by Extraction and Alpha Counting 72 – 79
Determination of Plutonium by Extraction and Alpha Counting 73 – 80
Determination of Neptunium by Extraction and Alpha Counting 80 – 87
Determination of Neptunium by Extraction and Alpha Counting 81 – 88
Atomic Absorption Determination of Chromium Soluble In 88 – 94
Uranium Hexafluoride
Atomic Absorption Determination of Chromium Soluble In 89 – 95
Uranium Hexafluoride
Atomic Absorption Determination of Chromium Insolubl
...