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ASTM D8325-20

(Guide)

Standard Guide for Evaluation of Nuclear Graphite Surface Area and Porosity by Gas Adsorption Measurements

Standard Guide for Evaluation of Nuclear Graphite Surface Area and Porosity by Gas Adsorption Measurements

SCOPE
1.1 The purpose of this Guide is to provide methodologic information specific to highly graphitized, low surface area materials used in the nuclear industry. It applies to nitrogen adsorption measurements at 77 K for the characterization of graphite pore structure, such as: (1) specific surface area; (2) cumulative volume of open pores (for pore sizes less than about 300 nm); and (3) distribution of pore volumes as a function of pore sizes (for pore sizes less than about 30 nm). These properties are related to graphite’s reactivity in oxidative environments, graphite’s ability to retain fission products, and gas transport through graphite’s pore system.  
1.2 Characterization of surface area (also known as the Brunauer-Emmett-Teller “BET” method) and porosity in nuclear graphite by gas adsorption is challenged by nuclear graphite’s low specific surface area, weak adsorption interactions, and energetic and structural heterogeneity of surface sites in gas-accessible pores. This guide provides recommendations and practical information related to the nitrogen adsorption method, including guidance on specimen preparation, selection of experimental conditions, data processing, and interpretation of results.  
1.3 Other porosity characterization methods used for nuclear graphite, such as krypton adsorption at 77 K, argon adsorption at either 77 K or 87 K, helium pycnometry (Test Method B923), and mercury intrusion porosimetry, are not in the scope of this guide.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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.

General Information

Status
Published
Publication Date
31-May-2020
ICS
27.120.30 - Fissile materials and nuclear fuel technology
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.F0 - Manufactured Carbon and Graphite Products
Current Stage
Ref Project

Relations

Refers
ASTM C1274-12(2020) - Standard Test Method for Advanced Ceramic Specific Surface Area by Physical Adsorption
Effective Date
01-Apr-2020

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ASTM D8325-20 - Standard Guide for Evaluation of Nuclear Graphite Surface Area and Porosity by Gas Adsorption MeasurementsASTM D8325-20 - Standard Guide for Evaluation of Nuclear Graphite Surface Area and Porosity by Gas Adsorption Measurements
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ASTM D8325-20 - Standard Guide for Evaluation of Nuclear Graphite Surface Area and Porosity by Gas Adsorption Measurements
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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: D8325 − 20
Standard Guide for
Evaluation of Nuclear Graphite Surface Area and Porosity
1
by Gas Adsorption Measurements
This standard is issued under the fixed designation D8325; 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 1.6 This international standard was developed in accor-
dance with internationally recognized principles on standard-
1.1 The purpose of this Guide is to provide methodologic
ization established in the Decision on Principles for the
information specific to highly graphitized, low surface area
Development of International Standards, Guides and Recom-
materials used in the nuclear industry. It applies to nitrogen
mendations issued by the World Trade Organization Technical
adsorption measurements at 77K for the characterization of
Barriers to Trade (TBT) Committee.
graphite pore structure, such as: (1) specific surface area; (2)
cumulative volume of open pores (for pore sizes less than
2. Referenced Documents
about 300nm); and (3) distribution of pore volumes as a
2
2.1 ASTM Standards:
function of pore sizes (for pore sizes less than about 30nm).
C1274Test Method forAdvanced Ceramic Specific Surface
Thesepropertiesarerelatedtographite’sreactivityinoxidative
Area by Physical Adsorption
environments, graphite’s ability to retain fission products, and
D3663Test Method for Surface Area of Catalysts and
gas transport through graphite’s pore system.
Catalyst Carriers
1.2 Characterization of surface area (also known as the
D4641Practice for Calculation of Pore Size Distributions of
Brunauer-Emmett-Teller “BET” method) and porosity in
Catalysts and Catalyst Carriers from Nitrogen Desorption
nuclear graphite by gas adsorption is challenged by nuclear
Isotherms
graphite’s low specific surface area, weak adsorption
D4222Test Method for Determination of Nitrogen Adsorp-
interactions, and energetic and structural heterogeneity of
tion and Desorption Isotherms of Catalysts and Catalyst
surface sites in gas-accessible pores. This guide provides
Carriers by Static Volumetric Measurements
recommendations and practical information related to the
D6556Test Method for Carbon Black—Total and External
nitrogen adsorption method, including guidance on specimen
Surface Area by Nitrogen Adsorption
preparation, selection of experimental conditions, data
D6761Test Method for Determination of the Total Pore
processing, and interpretation of results.
Volume of Catalysts and Catalyst Carriers
B923Test Method for Metal Powder Skeletal Density by
1.3 Other porosity characterization methods used for
Helium or Nitrogen Pycnometry
nuclear graphite, such as krypton adsorption at 77K, argon
3
2.2 ISO Standards:
adsorption at either 77K or 87K, helium pycnometry (Test
ISO9227Determinationofthespecificsurfaceareaofsolids
Method B923), and mercury intrusion porosimetry, are not in
by gas adsorption–BET method (Second edition)
the scope of this guide.
1.4 The values stated in SI units are to be regarded as
3. Terminology
standard. No other units of measurement are included in this
3.1 Definitions of Terms Specific to This Standard:
standard.
3.1.1 adsorbate, n—the material retained by adsorption at
1.5 This standard does not purport to address all of the
the interface between a solid and a gas or liquid.
safety concerns, if any, associated with its use. It is the
3.1.2 adsorbent, n—a solid material able to concentrate
responsibility of the user of this standard to establish appro-
measurable quantities of other substances on its accessible
priate safety, health, and environmental practices and deter-
surface, either external or in pores.
mine the applicability of regulatory limitations prior to use.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
1
This guide is under the jurisdiction of ASTM Committee D02 on Petroleum Standards volume information, refer to the standard’s Document Summary page on
Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcom- the ASTM website.
3
mittee D02.F0 on Manufactured Carbon and Graphite Products. Available from International Organization for Standardization (ISO), ISO
Current edition approved June 1, 2020. Published July 2020. DOI: 10.1520/ Central Secretariat, BIBC II, Chemin de Blandonnet 8, CP 401, 1214 Vernier,
D8325-20. Geneva, Switzerland, http://www.iso.org.
Copyright © ASTM International
...

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Standard Test Method for Nondestructive Assay of Special Nuclear Material Holdup Using Gamma-Ray Spectroscopic Methods

SIGNIFICANCE AND USE
5.1 Measurement results from this test method assists in demonstrating regulatory compliance in such areas as safeguards SNM inventory control, criticality control, waste disposal, and decontamination and decommissioning (D&D). This test method can apply to the measurement of holdup in process equipment or discrete items whose gamma-ray absorption properties may be measured or estimated. This method may be adequate to accurately measure items with complex distributions of radioactive and attenuating material, however, the results are subject to larger measurement uncertainties than measurements of less complex distributions of radioactive material.  
5.2 Scan—A scan is used to provide a qualitative indication of the extent, location, and the relative quantity of holdup. It can be used to plan or supplement the quantitative measurements.  
5.3 Nuclide Mapping—Nuclide mapping measures the relative isotopic composition of the holdup at specific locations. It can also be used to detect the presence of radionuclides that emit radiation which could interfere with the assay. Nuclide mapping is best performed using a high resolution detector (such as HPGe) for best nuclide and interference detection. If the holdup is not isotopically homogeneous at the measurement location, that measured isotopic composition will not be a reliable estimate of the bulk isotopic composition.  
5.4 Quantitative Measurements—These measurements result in quantification of the mass of the measured nuclides in the holdup. They include all the corrections, such as attenuation, and descriptive information, such as isotopic composition, that are available  
5.4.1 High quality results require detailed knowledge of radiation sources and detectors, transmission of radiation, calibration, facility operations and error analysis. Judicious use of subject matter experts is required (Guide C1490).  
5.5 Holdup Monitoring—Periodic re-measurement of holdup at a defined point using the same technique and a...
SCOPE
1.1 This test method describes gamma-ray methods used to nondestructively measure the quantity of 235U or  239Pu present as holdup in nuclear facilities. Holdup may occur in any facility where nuclear material is processed, in process equipment, in exhaust ventilation systems and in building walls and floors.  
1.2 This test method includes information useful for management, planning, selection of equipment, consideration of interferences, measurement program definition, and the utilization of resources  (1, 2, 3, 4) .2  
1.3 The measurement of nuclear material hold up in process equipment requires a scientific knowledge of radiation sources and detectors, transmission of radiation, calibration, facility operations and uncertainty analysis. It is subject to the constraints of the facility, management, budget, and schedule; plus health and safety requirements. The measurement process includes defining measurement uncertainties and is sensitive to the form and distribution of the material, various backgrounds, and interferences. The work includes investigation of material distributions within a facility, which could include potentially large holdup surface areas. Nuclear material held up in pipes, ductwork, gloveboxes, and heavy equipment, is usually distributed in a diffuse and irregular manner. It is difficult to define the measurement geometry, to identify the form of the material, and to measure it without interference from adjacent sources of radiation.  
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.  
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles...

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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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