ASTM C791-12
(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 C750 and C751.
An assay is performed to determine whether the material has the specified boron content.
Determination of the isotopic content of the boron is made to establish whether the content is in compliance with the purchaser’s specifications.
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:
Sections Total Carbon by Combustion in an Inductive Furnace and Infrared Measurement 7-16 Total Boron by Titrimetry and ICP OES17-27 Isotopic Composition by Mass Spectrometry28-32 Pyrohydrolysis33-40 Chloride by Constant-Current Coulometry41-49 Chloride and Fluoride by Ion-Selective Electrode50-58 Water by Constant-Voltage Coulometry and Weight Loss on Drying59-62 Metallic Impurities63 and 64 Soluble Boron by Titrimetry and ICP OES65-79 Free Carbon by a Coulometric Method80-89
General Information
Relations
Buy Standard
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 − 12
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 3.1.2 Determination of the isotopic content of the boron is
madetoestablishwhetherthecontentisincompliancewiththe
1.1 These test methods cover procedures for the chemical,
purchaser’s specifications.
mass spectrometric, and spectrochemical analysis of nuclear-
3.1.3 Impurity content is determined to ensure that the
grade boron carbide powder and pellets to determine compli-
maximum concentration limit of certain impurity elements is
ance with specifications.
not exceeded.
1.2 Theanalyticalproceduresappearinthefollowingorder:
4. Reagents
Sections
Total Carbon by Combustion in an Inductive Furnace and 7–16
4.1 Purity of Reagents—Reagent grade chemicals shall be
Infrared Measurement
Total Boron by Titrimetry and ICP OES 17–27 used in all tests. Unless otherwise indicated, it is intended that
Isotopic Composition by Mass Spectrometry 28–32
all reagents shall conform to the specifications of the Commit-
Pyrohydrolysis 33–40
tee onAnalytical Reagents of theAmerican Chemical Society,
Chloride by Constant-Current Coulometry 41–49
3
Chloride and Fluoride by Ion-Selective Electrode 50–58 where such specifications are available. Other grades may be
Water by Constant-Voltage Coulometry and Weight Loss on 59–62
used, provided it is first ascertained that the reagent is of
Drying
sufficiently high purity to permit its use without lessening the
Metallic Impurities 63 and 64
Soluble Boron by Titrimetry and ICP OES 65–79 accuracy of the determination.
Free Carbon by a Coulometric Method 80–89
4.2 Purity of Water—Unless otherwise indicated, references
2. Referenced Documents
towatershallbeunderstoodtomeanreagentwaterconforming
2
to Specification D1193.
2.1 ASTM Standards:
C750Specification for Nuclear-Grade Boron Carbide Pow-
5. Safety Precautions
der
5.1 Many laboratories have established safety regulations
C751SpecificationforNuclear-GradeBoronCarbidePellets
governing the use of hazardous chemicals and equipment. The
D1193Specification for Reagent Water
users of these methods should be familiar with such safety
3. Significance and Use
practices.
3.1 Boron carbide is used as a control material in nuclear
6. Sampling
reactors. In order to be suitable for this purpose, the material
6.1 Criteria for sampling this material are given in Specifi-
must meet certain criteria for assay, isotopic composition, and
cations C750 and C751.
impuritycontent.Thesemethodsaredesignedtoshowwhether
or not a given material meets the specifications for these items
TOTAL CARBON BY COMBUSTION IN AN
as described in Specifications C750 and C751.
INDUCTIVE FURNACE AND INFRARED
3.1.1 An assay is performed to determine whether the
MEASUREMENT
material has the specified boron content.
7. Scope
1
These test methods are under the jurisdiction of ASTM Committee C26 on
7.1 This method covers the determination of total carbon in
Nuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.03 on
nuclear-grade boron carbide in either powder or pellet form.
Neutron Absorber Materials Specifications.
CurrenteditionapprovedJune1,2012.PublishedJuly2012.Originallyapproved
in 1975. Last previous edition approved in 2011 as C791–11. DOI: 10.1520/
3
C0791-12. Reagent Chemicals, American Chemical Society Specifications, American
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Chemical Society, Washington, DC. For suggestions on the testing of reagents not
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM listed by the American Chemical Society, see Analar Standards for Laboratory
Standards volume information, refer to the standard’s Document Summary page on Chemicals,BDHLtd.,Poole,Dorset,U.K.andthe United States Pharmacopeia and
the ASTM website. National Formulary,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 − 12
8. Summary of Test Method 11.1.4 Oxygen, purity ≥ 99.998% v/v.
11.1.5 Pneumatic gas, for example, nitrogen, purity
8.1 The sample and added combustion accelerators
≥99.9% v⁄v.
(mostly tungsten-and iron-granules) are heated in an inductive
furnace under oxygen atmosphere.The high-frequency field of
12. Sampling and Sample Preparation
thefurnacecoupleswithelectricallyconduct
...
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.
Designation:C791–11 Designation:C791–12
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
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:
Sections
Total Carbon by Combustion in an Inductive Furnace and 7-16
Infrared Measurement
Total Boron by Titrimetry and ICP OES 17-27
Isotopic Composition by Mass Spectrometry 28-32
Pyrohydrolysis 33-40
Chloride by Constant-Current Coulometry 41-49
Chloride and Fluoride by Ion-Selective Electrode 50-58
Water by Constant-Voltage Coulometry and Weight Loss on 59-62
Drying
Metallic Impurities 63 and 64
Soluble Boron by Titrimetry and ICP OES 65-79
Free Carbon by a Coulometric Method 80-89
2. Referenced Documents
2
2.1 ASTM Standards:
C750 Specification for Nuclear-Grade Boron Carbide Powder
C751 Specification for Nuclear-Grade Boron Carbide Pellets
D1193 Specification for Reagent Water
3. Significance and Use
3.1 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.
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’s specifications.
3.1.3 Impurity content is determined to ensure that the maximum concentration limit of certain impurity elements is not
exceeded.
4. Reagents
4.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
3
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
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 JulyJune 1, 2011.2012. Published December 2011.July 2012. Originally approved in 1975. Last previous edition approved in 20042011 as
C791–04.C791–11. DOI: 10.1520/C0791-112.
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by
the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K. and the United States Pharmacopeia and National
Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
C791–12
4.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to
Specification D1193.
5. Safety Precautions
5.1 Many laboratories have established safety regulations governing the use of hazardous chemicals and equipment. The users
of these methods should be familiar with such safety practices.
6. Sampling
6.1 Criteria for sampling this material are given in Specifications C750 and C751.
TOTAL CARBON BY COMBUSTION IN AN INDUCTIVE FURNACE AND INFRARED MEASUREMENT
7. Scope
7.1 This method covers the determination of total carbon in nuclear-grade boron carbide in either powder or pellet form.
8.
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.