ASTM C791-11
(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
7.1 This method covers the determination of total carbon in nuclear-grade boron carbide in either powder or pellet form.
17.1 This method covers the determination of total boron in samples of boron carbide powder and pellets by titrimetry and ICP OES. The recommended amount of boron for each titration is 100 ± 10 mg.
28.1 This method covers the determination of the isotopic composition of boron in nuclear-grade boron carbide, in powder and pellet form, containing natural to highly enriched boron.
33.1 This method covers the separation of up to 100 μg of halides per gram of boron carbide. The separated halides are measured using other methods found in this standard. It also covers the sample preparation for the determination of isotopic composition by ICP MS.
41.1 This method covers the measurement of chloride after separation from boron carbide by pyrohydrolysis. The lower limit of the method is about 2 μg of chloride per titration.
50.1 This method covers the measurement of chloride and fluoride after separation from boron carbide by pyrohydrolysis. The limit of detection for chloride and fluoride in the boron carbide sample is 3 mg/kg and 2 mg/kg, respectively.
60.1 This method covers the determination of water in boron carbide in either powder or pellet form. The lower limit of the method is 5 μg of water. The lower limit of the weight loss on drying method is 20 mg/kg for a sample mass of 5 g.
65.1 This method covers the determination of soluble boron in boron carbide. Soluble boron is defined as that boron dissolved under the conditions of the test.
80.1 This method covers the determination of free carbon (also called soluble carbon) in boron carbide powders and shaped or sintered bodies of boron carbide after crushing. This method is applicable to mass fractions of free carbon of 0.01 % to 10 %.
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Designation:C791–11
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 or not a given material meets the specifications for these items
as described in Specifications C750 and C751.
1.1 These test methods cover procedures for the chemical,
3.1.1 An assay is performed to determine whether the
mass spectrometric, and spectrochemical analysis of nuclear-
material has the specified boron content.
grade boron carbide powder and pellets to determine compli-
3.1.2 Determination of the isotopic content of the boron is
ance with specifications.
madetoestablishwhetherthecontentisincompliancewiththe
1.2 Theanalyticalproceduresappearinthefollowingorder:
purchaser’s specifications.
Sections
3.1.3 Impurity content is determined to ensure that the
Total Carbon by Combustion in an Inductive Furnace and 7-16
Infrared Measurement
maximum concentration limit of certain impurity elements is
Total Boron by Titrimetry and ICP OES 17-27
not exceeded.
Isotopic Composition by Mass Spectrometry 28-32
Pyrohydrolysis 33-40
4. Reagents
Chloride by Constant-Current Coulometry 41-49
Chloride and Fluoride by Ion-Selective Electrode 50-58
4.1 Purity of Reagents—Reagent grade chemicals shall be
Water by Constant-Voltage Coulometry and Weight Loss on 59-62
used in all tests. Unless otherwise indicated, it is intended that
Drying
Metallic Impurities 63 and 64
all reagents shall conform to the specifications of the Commit-
Soluble Boron by Titrimetry and ICP OES 65-79
tee onAnalytical Reagents of theAmerican Chemical Society,
Free Carbon by a Coulometric Method 80-89
3
where such specifications are available. Other grades may be
2. Referenced Documents
used, provided it is first ascertained that the reagent is of
2
sufficiently high purity to permit its use without lessening the
2.1 ASTM Standards:
accuracy of the determination.
C750 Specification for Nuclear-Grade Boron Carbide Pow-
4.2 Purity of Water—Unlessotherwiseindicated,references
der
towatershallbeunderstoodtomeanreagentwaterconforming
C751 Specification for Nuclear-Grade Boron Carbide Pel-
to Specification D1193.
lets
D1193 Specification for Reagent Water
5. Safety Precautions
3. Significance and Use
5.1 Many laboratories have established safety regulations
governing the use of hazardous chemicals and equipment. The
3.1 Boron carbide is used as a control material in nuclear
users of these methods should be familiar with such safety
reactors. In order to be suitable for this purpose, the material
practices.
must meet certain criteria for assay, isotopic composition, and
impuritycontent.Thesemethodsaredesignedtoshowwhether
6. Sampling
6.1 Criteria for sampling this material are given in Specifi-
1
These test methods are under the jurisdiction of ASTM Committee C26 on
cations C750 and C751.
Nuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.03 on
Neutron Absorber Materials Specifications.
Current edition approved July 1, 2011. Published December 2011. Originally
approved in 1975. Last previous edition approved in 2004 as C791–04. DOI:
3
10.1520/C0791-11. 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
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C791–11
tungstengranulesbytingranules.Tungsten/tin-mixturesarecommercially
TOTAL CARBON BY COMBUSTION IN AN
available.
INDUCTIVE FURNACE AND INFRARED
MEASUREMENT
11.1.2 Iron granules
11.1.3 Calibration samples, with defined carbon content,
7. Scope
preferably certified reference materials with composition and
7.1 This method covers the determination of total carbon in
carbon content similar to the analyzed material. Also suitable
nuclear-grade boron carbide in either powder or pellet form.
are primary substances preferably carbonates.
11.1.4 Oxygen, purity$ 99.998% v/
...
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:C791–04 Designation:C791–11
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 and Gravimetry 7-17
Total Carbon by Combustion in an Inductive Furnace and 7-16
Infrared Measurement
Total Boron by Titrimetry 18-28
Total Boron by Titrimetry and ICP OES 17-27
Isotopic Composition by Mass Spectrometry 29-38
Isotopic Composition by Mass Spectrometry 28-32
Chloride and Fluoride Separation by Pyrohydrolysis 39-45
Pyrohydrolysis 33-40
Chloride by Constant-Current Coulometry 46-54
Chloride by Constant-Current Coulometry 41-49
Fluoride by Ion-Selective Electrode 55-63
Chloride and Fluoride by Ion-Selective Electrode 50-58
Water by Constant-Voltage Coulometry 64-72 Water by Constant-
Voltage Coulometry and
Weight Loss on Drying
Impurities by Spectrochemical Analysis 73-81 Metallic Impurities
Soluble Boron by Titrimetry 82-95
Soluble Boron by Titrimetry and ICP OES 65-79
Soluble Carbon by a Manometric Measurement 96-105
Free Carbon by a Coulometric Method 96-105
Metallic Impurities by a Direct Reader Spectrometric 106-114
Method
Metallic Impurities by a Direct Reader Spectrometric 106-11480-89
Method
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
E115Practice for Photographic Processing in Optical Emission Spectrographic Analysis
E116Practice for Photographic Photometry in Spectrochemical Analysis
E130Practice for Designation of Shapes and Sizes of Graphite Electrodes 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.
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 JuneJuly 1, 2004.2011. Published July 2004.December 2011. Originally approved in 1975. Last previous edition approved in 20002004 as
C791–83(2000)C791–04. DOI: 10.1520/C0791-04.10.1520/C0791-11.
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.ForAnnualBookofASTMStandards
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 ----------------------
C791–11
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.
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 establi
...
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