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

SCOPE
1.1 These test methods cover 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, as analytical methods are replaced with stand-alone analytical methods, are best addressed in subsequent publications.
SectionsSubsampling of Uranium Hexafluoride7 - 10Gravimetric Determination of Uranium11 - 19Titrimetric Determination of Uranium20 Preparation of High-Purity U3O 821Isotopic Analysis22Isotopic Analysis by Double-Standard Mass-Spectrometer Method23 - 29Determination of Hydrocarbons, Chlorocarbons, and Partially Substituted Halohydrocarbons29-36Atomic Absorption Determination of Antimony36Spectrophotometric Determination of Bromine37Titrimetric Determination of Chlorine38-44Determination of Silicon and Phosphorus45-51Determination of Boron and Silicon52-59 Determination of Ruthenium60 Determination of Titanium and Vanadium61Spectrographic Determination of Metallic Impurities 62Determination of Tungsten63Determination of Thorium and Rare Earths64-69Determination of Molybdenum70Atomic Absorption Determination of Metallic Impurities71-76Impurity Determination by Spark-Source Mass Spectrography77Determination of Boron-Equivalent Neutron Cross Section78Determination of Uranium-233 Abundance by Thermal Ionization Mass Spectrometry79Determination of Uranium-232 by Alpha Spectrometry80-86Determination of Fission Product Activity87Determination of Plutonium by Ion Exchange and Alpha Counting88-92Determination of Plutonium by Extraction and Alpha Counting93-100Determination of Neptunium by Extraction and Alpha Counting101-108Atomic Absorption Determination of Chromium Soluble In Uranium Hexafluoride109-115Atomic Absorption Determination of Chromium Insoluble In Uranium Hexafluoride116-122Determination of Technetium-99 In Uranium Hexafluoride123-131Method for the Determiation of Gamma-Energy Emission Rate from Fission Products in Uranium Hexafluoride132Determination of Metallic Impurities by ICP-AES133-142Determination of Molybdenum, Niobium, Tantalum, Titanium, and Tungsten by ICP-AES143-152
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. (For specific safeguard and safety consideration statements, see Section 6.)

General Information

Status
Historical
Publication Date
14-May-2011
Technical Committee
Drafting Committee
Current Stage
Ref Project

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ASTM C761-11 - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Uranium Hexafluoride
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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:C761 −11
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 72 – 79
Determination of Neptunium by Extraction and Alpha Counting 80 – 87
1.1 These test methods cover or give reference to proce-
Atomic Absorption Determination of Chromium Soluble In 88–94
dures for subsampling and for chemical, mass spectrometric, Uranium Hexafluoride
Atomic Absorption Determination of Chromium Insoluble In 95 – 101
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 102 – 110
routine use to determine conformance to UF specifications in Method for the Determiation of Gamma-Energy Emission Rate 111
6
from Fission Products in Uranium Hexafluoride
the Enrichment and Conversion Facilities.
Determination of Metallic Impurities by ICP-AES 112 – 121
Determination of Molybdenum, Niobium, Tantalum, Titanium, 122 – 131
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
with renumbering these sections are best addressed in subsequent publi- standard.
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 7
Gravimetric Determination of Uranium 8 – 16
priate safety and health practices and determine the applica-
Titrimetric Determination of Uranium 17
bility of regulatory limitations prior to use. (For specific
Preparation of High-Purity U O 18
3 8
Isotopic Analysis 19
safeguard and safety consideration statements, see Section 6.)
Determination of Hydrocarbons, Chlorocarbons, and Partially 20–26
Substituted Halohydrocarbons
2. Referenced Documents
Determination of Antimony 27
Determination of Bromine 28
Determination of Chlorine 29 – 35 2.1 The following documents of the issue in effect on date
Determination of Silicon and Phosphorus 36– 42
of material procurement form a part of this specification to the
Determination of Boron and Silicon 43
extent referenced herein:
Determination of Ruthenium 44
Determination of Titanium and Vanadium 45
2
Spectrographic Determination of Metallic Impurities 46 2.2 ASTM Standards:
Determination of Tungsten 47
C787Specification for Uranium Hexafluoride for Enrich-
Determination of Thorium and Rare Earths 48
ment
Determination of Molybdenum 49
Atomic Absorption Determination of Metallic Impurities 50 – 55
C799Test Methods for Chemical, Mass Spectrometric,
Impurity Determination by Spark-Source Mass Spectrography 56
Spectrochemical,Nuclear,andRadiochemicalAnalysisof
Determination of Boron-Equivalent Neutron Cross Section 57
Determination of Uranium-233 Abundance by Thermal Ionization 58 Nuclear-Grade Uranyl Nitrate Solutions
Mass Spectrometry
C859Terminology Relating to Nuclear Materials
Determination of Uranium-232 by Alpha Spectrometry 59 – 65
C996Specification for Uranium Hexafluoride Enriched to
Determination of Fission Product Activity 66
235
Determination of Plutonium by Ion Exchange and Alpha 67–71 Less Than 5% U
Counting
C1128Guide for Preparation of Working Reference Materi-
als for Use in Analysis of Nuclear Fuel Cycle 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 May 15, 2011. Published July 2011. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
ε1
approved in 1973. Last previous edition approved in 2004 as C761–04 . DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/C0761-11. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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C
...

This document is not anASTM standard and is intended only to provide the user of anASTM 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.
´1
Designation:C761–04 Designation: C761 – 11
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.
This standard has been approved for use by agencies of the Department of Defense.
1
´ NOTE—Two versions of Table 1 appeared in this standard. The incorrect version was editorially deleted.
1. Scope
1.1 These test methods cover or give reference to procedures for subsampling and for chemical, mass spectrometric,
spectrochemical,nuclear,andradiochemicalanalysisofuraniumhexafluoride(UF ).Mostofthesetestmethodsareinroutineuse
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
renumberingthesesections,sectionsarebestaddressedinsubsequentpublicationsasanalyticalmethodsarereplacedwithstand-aloneanalyticalmethods,
are best addressed in subsequent publications.
methods.
Sections
Subsampling of Uranium Hexafluoride 7–10
Subsampling of Uranium Hexafluoride 7
Gravimetric Determination of Uranium 11–19
Gravimetric Determination of Uranium 8–16
Titrimetric Determination of Uranium 20
Titrimetric Determination of Uranium 17
Preparation of High-Purity U O 21
3 8
Preparation of High-Purity U O 18
3 8
Isotopic Analysis 22
Isotopic Analysis 19
Isotopic Analysis by Double-Standard Mass-Spectrometer 23 - 29
Method
Determination of Hydrocarbons, Chlorocarbons, and Partially 29–36
Substituted Halohydrocarbons
Determination of Hydrocarbons, Chlorocarbons, and Partially 20–26
Substituted Halohydrocarbons
Atomic Absorption Determination of Antimony 36
Determination of Antimony 27
Spectrophotometric Determination of Bromine 37
Determination of Bromine 28
Titrimetric Determination of Chlorine 38–44
Determination of Chlorine 29–35
Determination of Silicon and Phosphorus 45–51
Determination of Silicon and Phosphorus 36– 42
Determination of Boron and Silicon 52–59
Determination of Boron and Silicon 43
Determination of Ruthenium 60
Determination of Ruthenium 44
Determination of Titanium and Vanadium 61
Determination of Titanium and Vanadium 45
Spectrographic Determination of Metallic Impurities 62
Spectrographic Determination of Metallic Impurities 46
Determination of Tungsten 63
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 June 15, 2006. Published August 2004. Originally approved in 1973. Last previous edition approved in 2001 as C761–01. DOI:
10.1520/C0761-04E01.
e1
Current edition approved May 15, 2011. Published July 2011. Originally approved in 1973. Last previous edition approved in 2004 as C761–04 . DOI:
10.1520/C0761-11.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
C761 – 11
Determination of Tungsten 47
Determination of Thorium and Rare Earths 64–69
Determination of Thorium and Rare Earths 48
Determination of Molybdenum 70
Determination of Molybdenum 49
Atomic Absorption Determination of Metallic Impurities 71–76
Atomic Absorption Determination of Metallic Impurities 50–55
Impurity Determination by Spark-Source Mass Spectrography 77
Impurity Determination by Spark-Source Mass Spectrography 56
Determination of Boron-Equivalent Neutron Cross Section 78
Determination of Boron-Equivalent Neutron Cross Section 57
Determination of Uranium-233 Abundance by Thermal Ionization 79
Mass Spectrometry
Determination of Uranium-233 Abundance by Thermal Ionization 58
Mass Spectrometry
Determination of Uranium-232 by Alpha Spectrometry 80–86
Determination of Uranium-232 by Alpha Spectrometry 59–65
Determination of Fission Product Activity 87
Determination of Fission Product Activity 66
Determination of Plutonium by Ion Exchange and Alpha Count- 88–92
ing
Determination of Plutonium by Ion Exchange and Alpha Count- 67–71
ing
Determination of Plutonium by Extraction
...

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