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ASTM C791-04

(Test Method)

Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Boron Carbide

Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Boron Carbide

SIGNIFICANCE AND USE
Boron carbide is used as a control material in nuclear reactors. In order to be suitable for this purpose, the material must meet certain criteria for assay, isotopic composition, and impurity content. These methods are designed to show whether or not a given material meets the specifications for these items as described in Specifications C 750 and C 751.
3.1.1 An assay is performed to determine whether the material has the specified boron content.
3.1.2 Determination of the isotopic content of the boron is made to establish whether the content is in compliance with the purchaser’specifications.
3.1.3 Impurity content is determined to ensure that the maximum concentration limit of certain impurity elements is not exceeded.
SCOPE
1.1 These test methods cover procedures for the chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade boron carbide powder and pellets to determine compliance with specifications.
1.2 The analytical procedures appear in the following order:SectionsTotal Carbon by Combustion and Gravimetry7-17Total Boron by Titrimetry18-28Isotopic Composition by Mass Spectrometry29-38Chloride and Fluoride Separation by Pyrohydrolysis39-45Chloride by Constant-Current Coulometry46-54Fluoride by Ion-Selective Electrode55-63Water by Constant-Voltage Coulometry64-72Impurities by Spectrochemical Analysis73-81Soluble Boron by Titrimetry82-95Soluble Carbon by a Manometric Measurement96-105Metallic Impurities by a Direct Reader Spectrometric Method106-114

General Information

Status
Historical
Publication Date
31-May-2004
ICS
27.120.30 - Fissile materials and nuclear fuel technology
Technical Committee
C26 - Nuclear Fuel Cycle
Drafting Committee
C26.03 - Neutron Absorber Materials Specifications
Current Stage
Ref Project

Relations

Replaces
ASTM C791-83(2000) - Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Boron Carbide
Effective Date
01-Jun-2004
Replaced By
ASTM C791-11 - Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Boron Carbide
Effective Date
01-Jul-2011
Referred By
ASTM C750-18 - Standard Specification for Nuclear-Grade Boron Carbide Powder
Effective Date
01-Jun-2004
Referred By
ASTM C751-20 - Standard Specification for Nuclear-Grade Boron Carbide Pellets
Effective Date
01-Jun-2004
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-2004
Referred By
ASTM C1671-20a - Standard Practice for Qualification and Acceptance of Boron Based Metallic Neutron Absorbers for Nuclear Criticality Control for Dry Cask Storage Systems and Transportation Packaging
Effective Date
01-Jun-2004

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ASTM C791-04 - Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Boron CarbideASTM C791-04 - Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Boron Carbide
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ASTM C791-04 - Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Boron Carbide
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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: C791 – 04
Standard Test Methods for
Chemical, Mass Spectrometric, and Spectrochemical
1
Analysis of Nuclear-Grade Boron Carbide
This standard is issued under the fixed designation C791; 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 3. Significance and Use
1.1 These test methods cover procedures for the chemical, 3.1 Boron carbide is used as a control material in nuclear
mass spectrometric, and spectrochemical analysis of nuclear- reactors. In order to be suitable for this purpose, the material
grade boron carbide powder and pellets to determine compli- must meet certain criteria for assay, isotopic composition, and
ance with specifications. impuritycontent.Thesemethodsaredesignedtoshowwhether
1.2 Theanalyticalproceduresappearinthefollowingorder: or not a given material meets the specifications for these items
as described in Specifications C750 and C751.
Sections
Total Carbon by Combustion and Gravimetry 7-17
3.1.1 An assay is performed to determine whether the
Total Boron by Titrimetry 18-28
material has the specified boron content.
Isotopic Composition by Mass Spectrometry 29-38
3.1.2 Determination of the isotopic content of the boron is
Chloride and Fluoride Separation by Pyrohydrolysis 39-45
Chloride by Constant-Current Coulometry 46-54
madetoestablishwhetherthecontentisincompliancewiththe
Fluoride by Ion-Selective Electrode 55-63
purchaser’s specifications.
Water by Constant-Voltage Coulometry 64-72
Impurities by Spectrochemical Analysis 73-81 3.1.3 Impurity content is determined to ensure that the
Soluble Boron by Titrimetry 82-95
maximum concentration limit of certain impurity elements is
Soluble Carbon by a Manometric Measurement 96-105
not exceeded.
Metallic Impurities by a Direct Reader Spectrometric 106-114
Method
4. Reagents
2. Referenced Documents
4.1 Purity of Reagents—Reagent grade chemicals shall be
2
2.1 ASTM Standards:
used in all tests. Unless otherwise indicated, it is intended that
C750 Specification for Nuclear-Grade Boron Carbide Pow-
all reagents shall conform to the specifications of the Commit-
der
tee onAnalytical Reagents of theAmerican Chemical Society,
4
C751 Specification for Nuclear-Grade Boron Carbide Pel-
where such specifications are available. Other grades may be
lets
used, provided it is first ascertained that the reagent is of
D1193 Specification for Reagent Water
sufficiently high purity to permit its use without lessening the
E115 PracticeforPhotographicProcessinginOpticalEmis-
accuracy of the determination.
3
sion Spectrographic Analysis
4.2 PurityofWater—Unlessotherwiseindicated,references
E116 Practice for Photographic Photometry in Spectro-
towatershallbeunderstoodtomeanreagentwaterconforming
3
chemical Analysis
to Specification D1193.
E130 Practice for Designation of Shapes and Sizes of
5. Safety Precautions
Graphite Electrodes
5.1 Many laboratories have established safety regulations
governing the use of hazardous chemicals and equipment.The
1
These test methods are under the jurisdiction of ASTM Committee C26 on
users of these methods should be familiar with such safety
Nuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.03 on
Neutron Absorber Materials Specifications. practices.
CurrenteditionapprovedJune1,2004.PublishedJuly2004.Originallyapproved
in 1975. Last previous edition approved in 2000 as C791–83(2000) DOI:
10.1520/C0791-04.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
4
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Reagent Chemicals, American Chemical Society Specifications, American
Standards volume information, refer to the standard’s Document Summary page on Chemical Society, Washington, DC. For suggestions on the testing of reagents not
the ASTM website. listed by the American Chemical Society, see Analar Standards for Laboratory
3
Withdrawn. The last approved version of this historical standard is referenced Chemicals,BDHLtd.,Poole,Dorset,U.K.andtheUnitedStatesPharmacopeiaand
on www.astm.org. NationalFormulary,U.S.PharmacopeialConvention,Inc.(USPC),Rockville,MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
C791 – 04
13
6. Sampling 10.6.2 Drying Tube (B), filled with magnesium perchlo-
16
rate,anhydrouscalciumsulfate,andsodiumhydrate-asbestos
6.1 Criteria for sampling this material are given in Specifi-
to prevent any back-diffusion of water and carbon dioxide into
cations C750 and C751.
the absorption bulb.
17
10.6.3 Flowmete
...

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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.  
4.5.3 Materials handling equipment should be designed and fabricated to remain dimensionally stable throughout its life cycle.  
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1.1 Intent:  
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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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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.  
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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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    6 pages
    English language
    sale 15% off