ASTM C791-19
(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
4.1 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 C750 and C751.
4.1.1 An assay is performed to determine whether the material has the specified boron and carbon content.
4.1.2 Determination of the isotopic content of the boron and the free carbon content is made to establish whether the content is in compliance with the purchaser’s specifications.
4.1.3 Impurity content is determined to ensure that the maximum concentration limit of certain impurities (chloride, fluoride, water, metallic impurities, soluble boron) 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 values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 The analytical procedures appear in the following order:
Sections
Total Carbon by Combustion in an Inductive Furnace and
Infrared Measurement
8 – 17
Total Boron by Titrimetry and ICP OES
18 – 28
Isotopic Composition by Mass Spectrometry
29 – 33
Pyrohydrolysis
34 – 41
Chloride by Constant-Current Coulometry
42 – 50
Chloride and Fluoride by Ion-Selective Electrode
51 – 59
Water by Constant-Voltage Coulometry and Weight Loss on
Drying
60 – 63
Metallic Impurities by DCArc OES and wet chemical methods
64 and 65
Soluble Boron by Titrimetry and ICP OES
66 – 80
Free Carbon by a Coulometric Method
81 – 90
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 for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
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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: C791 − 19
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 2. Referenced Documents
2
2.1 ASTM Standards:
1.1 These test methods cover procedures for the chemical,
mass spectrometric, and spectrochemical analysis of nuclear- C750Specification for Nuclear-Grade Boron Carbide Pow-
der
grade boron carbide powder and pellets to determine compli-
ance with specifications. C751SpecificationforNuclear-GradeBoronCarbidePellets
C859Terminology Relating to Nuclear Materials
1.2 The values stated in SI units are to be regarded as the
C1128Guide for Preparation of Working Reference Materi-
standard. The values given in parentheses are for information
als for Use in Analysis of Nuclear Fuel Cycle Materials
only.
D1193Specification for Reagent Water
1.3 Theanalyticalproceduresappearinthefollowingorder:
E969Specification for Glass Volumetric (Transfer) Pipets
Sections
3. Terminology
Total Carbon by Combustion in an Inductive Furnace and 8–17
Infrared Measurement
3.1 Definitions—For definitions of terms relating to nuclear
Total Boron by Titrimetry and ICP OES 18–28
Isotopic Composition by Mass Spectrometry 29–33 materials, refer to Terminology C859.
Pyrohydrolysis 34–41
3.2 Definitions of Terms Specific to This Standard:
Chloride by Constant-Current Coulometry 42–50
Chloride and Fluoride by Ion-Selective Electrode 51–59
3.2.1 analyte—the constituent determined by a chemical
Water by Constant-Voltage Coulometry and Weight Loss on 60–63
measurement process.
Drying
Metallic Impurities by DCArc OES and wet chemical meth- 64 and 65
3.2.2 analytical or emission line—the particular wavelength
ods
of electromagnetic radiation used in determining the presence
Soluble Boron by Titrimetry and ICP OES 66–80
or concentration of an element.
Free Carbon by a Coulometric Method 81–90
1.4 This standard does not purport to address all of the 3.2.3 background—spectral intensity that would be mea-
safety concerns, if any, associated with its use. It is the
suredatthewavelengthoftheemissionlineiftheemissionand
responsibility of the user of this standard to establish appro- overlapping lines were not present.
priate safety, health, and environmental practices and deter-
3.2.4 calibration—the act, process, or result of establishing
mine the applicability of regulatory limitations prior to use.
the relationship between the response of an instrument and the
1.5 This international standard was developed in accor-
amount of analyte present.
dance with internationally recognized principles on standard-
3.2.5 calibration function—the graphical or mathematical
ization established in the Decision on Principles for the
representation of the relationship between the response of an
Development of International Standards, Guides and Recom-
instrument and the concentration or mass of the analyte.
mendations issued by the World Trade Organization Technical
3.2.6 calibration samples or solutions—samples or solu-
Barriers to Trade (TBT) Committee.
tions with known analyte contents or analyte concentrations,
respectively, to establish the relationship between the response
of an instrument and the amount of analyte.
1
These test methods are under the jurisdiction of ASTM Committee C26 on
Nuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.03 on
2
Neutron Absorber Materials Specifications. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Feb. 1, 2019. Published March 2019. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1975. Last previous edition approved in 2012 as C791–12. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/C0791-19. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
C791 − 19
3.2.7 certified reference material (CRM)—a reference or not a given material meets the specifications for these items
material, accompanied by a certificate, one or more of whose as described in Specifications C750 and C751.
property values are certified by a procedure which establishes 4.1.1 An assay is performed to determine whether th
...
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: C791 − 12 C791 − 19
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. 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, and spectrochemical analysis of nuclear-grade
boron carbide powder and pellets to determine compliance with specifications.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 The analytical procedures appear in the following order:
Sections
Total Carbon by Combustion in an Inductive Furnace and 7 – 16
Infrared Measurement
Total Carbon by Combustion in an Inductive Furnace and 8 – 17
Infrared Measurement
Total Boron by Titrimetry and ICP OES 17 – 27
Total Boron by Titrimetry and ICP OES 18 – 28
Isotopic Composition by Mass Spectrometry 28 – 32
Isotopic Composition by Mass Spectrometry 29 – 33
Pyrohydrolysis 33 – 40
Pyrohydrolysis 34 – 41
Chloride by Constant-Current Coulometry 41 – 49
Chloride by Constant-Current Coulometry 42 – 50
Chloride and Fluoride by Ion-Selective Electrode 50 – 58
Chloride and Fluoride by Ion-Selective Electrode 51 – 59
Water by Constant-Voltage Coulometry and Weight Loss on 59 – 62
Drying
Water by Constant-Voltage Coulometry and Weight Loss on 60 – 63
Drying
Metallic Impurities 63 and 64
Metallic Impurities by DCArc OES and wet chemical meth- 64 and 65
ods
Soluble Boron by Titrimetry and ICP OES 65 – 79
Soluble Boron by Titrimetry and ICP OES 66 – 80
Free Carbon by a Coulometric Method 80 – 89
Free Carbon by a Coulometric Method 81 – 90
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 for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2
2.1 ASTM Standards:
C750 Specification for Nuclear-Grade Boron Carbide Powder
C751 Specification for Nuclear-Grade Boron Carbide Pellets
1
These test methods are under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.03 on Neutron
Absorber Materials Specifications.
Current edition approved June 1, 2012Feb. 1, 2019. Published July 2012March 2019. Originally approved in 1975. Last previous edition approved in 20112012 as
C791 – 11.C791 – 12. DOI: 10.1520/C0791-12.10.1520/C0791-19.
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 Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
C791 − 19
C859 Terminology Relating to Nuclear Materials
C1128 Guide for Preparation of Working Reference Materials for Use in Analysis of Nuclear Fuel Cycle Materials
D1193 Specification for Reagent Water
E969 Specification for Glass Volumetric (Transfer) Pipets
3. Terminology
3.1 Definitions—For definitions of terms relating to nuclear materials, refer to Terminology C859.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 analyte—the constituent determined by a chemical measurement process.
3.2.2 analytical or emission line—the particular wavelength of electromagnetic radiation used in determining the presence or
concentration of an element.
3.2.3 background—spectral intensity that would be measured at the wavelength of the emission line if the emission and
overlapping lines were not present.
3.2.4 calibration—the act, process, or result of establishing the relationship between the response of an instrument and the
amount of analyte present.
3.2.5 calibration f
...
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