ASTM C809-94(2007)
(Test Method)Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Aluminum Oxide and Aluminum
Oxide-Boron Carbide Composite Pellets
Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Aluminum Oxide and Aluminum<br> Oxide-Boron Carbide Composite Pellets
SIGNIFICANCE AND USE
Aluminum oxide pellets are used in a reactor core as filler or spacers within fuel, burnable poison, or control rods. In order to be suitable for this purpose, the material must meet certain criteria for impurity content. These test methods are designed to show whether or not a given material meets the specifications for these items as described in Specification C 785.
3.1.1 Impurity content is determined to ensure that the maximum concentration limit of certain impurity elements is not exceeded.
Aluminum oxide-boron carbide composite pellets are used in a reactor core as a component in neutron absorber rods. In order to be suitable for this purpose, the material must meet certain criteria for boron content, isotopic composition, and impurity content as described in Specification C 784.
3.2.1 The material is assayed for boron to determine whether the boron content is as specified by the purchaser.
3.2.2 Determination of the isotopic content of the boron is made to establish whether the 10B concentration is in compliance with the purchaser’specifications.
3.2.3 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 aluminum oxide and aluminum oxide-boron carbide composite pellets to determine compliance with specifications.
1.2 The analytical procedures appear in the following order:
Sections Boron by Titrimetry 7 to 13 Separation of Boron for Mass Spectrometry14 to 19 Isotopic Composition by Mass Spectrometry20 to 23 Separation of Halides by Pyrohydrolysis24 to 27 Fluoride by Ion-Selective Electrode28 to 30 Chloride, Bromide, and Iodide by Amperometric Microtitrimetry31 to 33 Trace Elements by Emission Spectroscopy34 to 46
1.3 The values stated in SI units are to be regarded as the 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 and health practices and determine the applicability of regulatory limitations prior to use. (For specific precautionary statements, see Section 5.)
7.1 This test method covers the determination of boron in aluminum oxide-boron carbide composites. As an alternative, the procedure for total boron by titrimetry detailed in Test Methods C791 may be used.
14.1 This test method covers the separation of boron from aluminum and other impurities. The isotopic composition of the separated boron is measured using another test method found herein.
20.1 This test method covers the determination of the isotopic composition of boron in nuclear-grade aluminum oxide/boron carbide composite pellets containing natural to highly enriched boron.
24.1 This test method covers the separation of up to 100 μg of halides per gram of sample. The separated halides are measured using other test methods found herein.
28.1 This test method can determine as low as 2-μg of F/g sample in condensate containing all the halogens.
31.1 This test method covers the determination of halogens, except fluorine, as separated by pyrohydrolysis. The detection limit is 1.5 μg Cl/g sample.
34.1 This spectrochemical test method provides for the determination of 14 impurity elements. The elements and concentration ranges are as follows:
ElementsConcentration Range, ppm Boron10 to 10 000 Calcium 10 to 10 000 Chromium10 to 10 000 Dysprosium30 to 10 000 Europium10 to 10 000 Gadolinium30 to 10 000 Hafnium 30 to 10 000 Iron 10 to 10 000 Magnesium10 to 10 000 Nickel 10 to 10 000 Samarium10 to 10 000 Silicon 10 to 10 000 Sodium 10 to 10 000 Titanium10 to 10 000
34.2 The test method can also be extended to cover the determination of other elements of interest.
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Designation: C809 − 94 (Reapproved 2007)
StandardTest Methods for
Chemical, Mass Spectrometric, and Spectrochemical
Analysis of Nuclear-Grade Aluminum Oxide and Aluminum
Oxide-Boron Carbide Composite Pellets
This standard is issued under the fixed designation C809; 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 C799Test Methods for Chemical, Mass Spectrometric,
Spectrochemical,Nuclear,andRadiochemicalAnalysisof
1.1 These test methods cover procedures for the chemical,
Nuclear-Grade Uranyl Nitrate Solutions
mass spectrometric, and spectrochemical analysis of nuclear-
D1193Specification for Reagent Water
grade aluminum oxide and aluminum oxide-boron carbide
E115Practice for Photographic Processing in Optical Emis-
composite pellets to determine compliance with specifications.
sion Spectrographic Analysis (Withdrawn 2002)
1.2 Theanalyticalproceduresappearinthefollowingorder:
E116Practice for Photographic Photometry in Spectro-
Sections
chemical Analysis (Withdrawn 2002)
Boron by Titrimetry 7 to 13
3. Significance and Use
Separation of Boron for Mass Spectrometry 14 to 19
Isotopic Composition by Mass Spectrometry 20 to 23
3.1 Aluminum oxide pellets are used in a reactor core as
Separation of Halides by Pyrohydrolysis 24 to 27
fillerorspacerswithinfuel,burnablepoison,orcontrolrods.In
Fluoride by Ion-Selective Electrode 28 to 30
Chloride, Bromide, and Iodide by Amperometric Microtitrimetry 31 to 33
order to be suitable for this purpose, the material must meet
Trace Elements by Emission Spectroscopy 34 to 46
certain criteria for impurity content. These test methods are
1.3 The values stated in SI units are to be regarded as the
designed to show whether or not a given material meets the
standard.
specifications for these items as described in Specification
C785.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 3.1.1 Impurity content is determined to ensure that the
maximum concentration limit of certain impurity elements is
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- not exceeded.
bility of regulatory limitations prior to use. (For specific
3.2 Aluminum oxide-boron carbide composite pellets are
precautionary statements, see Section 5.)
usedinareactorcoreasacomponentinneutronabsorberrods.
In order to be suitable for this purpose, the material must meet
2. Referenced Documents
certain criteria for boron content, isotopic composition, and
2.1 ASTM Standards:
impurity content as described in Specification C784.
C784Specification for Nuclear-Grade Aluminum Oxide-
3.2.1 The material is assayed for boron to determine
Boron Carbide Composite Pellets
whether the boron content is as specified by the purchaser.
C785SpecificationforNuclear-GradeAluminumOxidePel-
3.2.2 Determination of the isotopic content of the boron is
lets 10
made to establish whether the B concentration is in compli-
C791Test Methods for Chemical, Mass Spectrometric, and
ance with the purchaser’s specifications.
Spectrochemical Analysis of Nuclear-Grade Boron Car-
3.2.3 Impurity content is determined to ensure that the
bide
maximum concentration limit of certain impurity elements is
not exceeded.
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
4. Reagents
Neutron Absorber Materials Specifications.
Current edition approved July 1, 2007. Published August 2007. Originally 4.1 Purity of Reagents—Reagent grade chemicals shall be
approved in 1980. Last previous edition approved in 2000 as C809–94(2000).
used in all tests. Unless otherwise indicated, it is intended that
DOI: 10.1520/C0809-94R07.
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 last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C809 − 94 (Reapproved 2007)
all reagents shall conform to the specifications of the Commit- 9.3 Sieve, No. 100 (150-µm) U.S. Standard Sieve Series,
tee onAnalytical Reagents of theAmerican Chemical Society, 76-mm diameter, brass or stainless steel.
where such specifications are available. Other grades may be
9.4 Glass Boats, borosilicate, 4-mm wide, 3-mm deep,
used, provided it is first ascertained that the reagent is of
40-mm long.
sufficiently high purity to permit its use without lessening the
9.5 Glass Tubing, heavy-wall borosilicate, 5-mm inside
accuracy of the determination.
diameter by 250-mm long, sealed at one end.
4.2 Purity of Water—Unless otherwise indicated, reference
9.6 Mixer, vortex type.
towatershallbeunderstoodtomeanreagentwaterconforming
to Specification D1193, Type III.
9.7 Glass Blower’s Torch.
9.8 Iron Pipe,12.7by254-mmlongwiththreadedendcaps.
5. Safety Precautions
9.9 Muffle Furnace, capable of operation at 300°C. The
5.1 Many laboratories have established safety regulations
heated area must be of sufficient size to hold the capped iron
governing the use of hazardous chemicals and equipment. The
pipe.
users of these test methods should be familiar with such safety
practices. 9.10 pH Meter, with pH electrodes and magnetic stirrer.
9.11 Steam Bath.
6. Sampling
9.12 Hot Plate.
6.1 Criteria for sampling aluminum oxide pellets are given
9.13 Filter Paper, 11 cm, ashless slow filtering for fine
in Specification C785.
precipitates.
6.2 Criteria for sampling aluminum oxide-boron carbide
9.14 Buret, Class A, 25-mL.
composite pellets are given in Specification C784.
BORON BY TITRIMETRY
10. Reagents
10.1 Boric Acid, NIST SRM 951 or its replacement.
7. Scope
10.2 Hydrochloric Acid (HCl), 1 N.
7.1 This test method covers the determination of boron in
aluminum oxide-boron carbide composites. As an alternative,
10.3 Hydrochloric Acid (HCl), 0.1 N.
the procedure for total boron by titrimetry detailed in Test
10.4 Mannitol.
Methods C791 may be used.
10.5 Nitric Acid (sp gr 1.42)—Concentrated Nitric Acid
8. Summary of Test Method
(HNO ).
8.1 The sample is crushed, passed through a 100-mesh 10.6 Sodium Hydroxide (NaOH) Solution, 1 N, carbonate-
screen, weighed in a glass boat, and introduced into a heavy-
free.
wallglasstube.Nitricacidisaddedtothetubeandthecontents
10.7 Sodium Hydroxide (NaOH) Solution,0.1 N,carbonate-
mixed using a vortex mixer. The tube is sealed, placed into a
free.
safety container, heated for 6 h, cooled to room temperature,
10.8 Sodium Hydroxide (NaOH) Solution, 0.025 N,
opened,andthecontentswashedintoabeaker. Thesolutionis
carbonate-free, standardized against NIST SRM 951.
adjusted to pH 9.0 and filtered, then adjusted to pH 3.5 and
boiled to remove CO . Substantially, a pure boric acid is
11. Procedure
obtainedwhichcanbetitratedinthepresenceofmannitolwith
6,7
a standard solution of sodium hydroxide. 11.1 Crush the aluminum oxide/boron carbide composite
pellet using a diamond mortar until all the sample is passed
9. Apparatus
through a No. 100 (150-µm) screen.
9.1 Analytical Balance, capable of weighing to 60.1 mg.
11.2 Weigh a 250-mg sample into a glass boat.
9.2 Mortar, diamond (Plattner) (or equivalent).
11.3 Introduce the boat and sample into a heavy-wall glass
tube, being very careful to prevent any of the sample from
4 adhering to the wall of the tube near the open end.
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
11.4 Introduce 0.5 mLof concentrated HNO into the glass
listed by the American Chemical Society, see Analar Standards for Laboratory
tube.
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
11.5 Mix the sample and acid using the vortex mixer.
MD.
Wichers,E.,Schlecht,W.G.,andGordon,C.L.,“PreparingRefractoryOxides,
11.6 Flame the glass tube to remove the moisture from the
Silicates,andCeramicMaterialsforAnalysisbyHeatingwithAcidsinSealedTubes
walls.
atElevatedTemperatures,” Journal of Research of the National Bureau of Standards
, Vol 33, 1944, p. 451.
11.7 Seal the glass tube. There are two methods available:
Lerner, M. W., The Analysis of Elemental Boron, New Brunswick Laboratory,
11.7.1 Sealing the glass tube may be accomplished by
U. S.Atomic Energy Commission, TID-25190, November 1970.
constriction, then drawing off a short piece of the tube, then
Rodden, C. J., Analysis of Essential Nuclear Reactor Materials, U.S. Atomic
Energy Commission, Washington, DC, Government Printing Office, 1964. working down the sealed end.
C809 − 94 (Reapproved 2007)
11.7.2 Aseal can be made by allowing the open end of the
B = millilitres of NaOH solution used in titration of the
tubetoflowtogetherbyheatingandrevolvingthetubeslowly.
blank,
While the tube is red with heat, the tube is warmed enough to
N = normality of the NaOH solution,
blow out the seal to a rounded shape. A = atomicweightofboroncomputedforthesamplebased
upon the measured isotopic composition, and
11.8 Place the glass tube into a safety container which
W = milligrams of sample weight.
consists of a 12.7-mm inside diameter black iron pipe with
screw caps on each end.The caps can be tightened with finger
13. Precision
tip control.
13.1 The limit of error at the 95% confidence level for a
11.9 Insert the assembly into a 300°C muffle furnace with
single determination is 60.10% absolute.
the top end of the assembly elevated and heat for 6 h.
SEPARATION OF BORON FOR MASS
11.10 Remove the assembly from the muffle furnace and
SPECTROMETRY
place into a tray, keeping the same end of the assembly
elevated.
14. Scope
11.11 Allow the assembly to cool to room temperature.
14.1 This test method covers the separation of boron from
11.12 Withdrawtheglasstubefromthesafetycontainerand
aluminum and other impurities. The isotopic composition of
file a notch about 13 mm from one end of the tube.
the separated boron is measured using another test method
found herein.
NOTE 1—Contents of the tube may be under pressure.
11.13 Heat a glass rod to red heat, then place the rod on the
15. Summary of Test Method
notch.Thisactionshouldcracktheglasstube;however,alight
15.1 Boron is put into solution using a sealed-tube dissolu-
tap may be needed to complete the break.
tion method. It is separated from aluminum and other impuri-
11.14 Wash the contents from the glass tube into a 250-mL
ties by solvent extraction and ion exchange.
beaker;however,ifthealuminumoxideisstucktothewallsof
16. Interferences
the tube, shake on a vortex mixer.
16.1 There are no known interferences not eliminated by
NOTE 2—The matrixAl O does not completely dissolve, but all of the
2 3
this separation test method.
boron is in solution.
11.15 Precipitate the iron and the aluminum by using 1 N
17. Apparatus
sodium hydroxide solution to adjust the pH to 9.0.
17.1 Separatory Funnel, 60-mL with TFE-fluorocarbon
11.16 Place the beaker on a steam bath and digest for 1 h.
stopcock.
11.17 Filter the sample through the filter paper (9.13) and
17.2 Mixer, vortex type.
wash the precipitate with several portions of hot deionized
17.3 Filter Paper, ashless, slow filtering for fine precipi-
water.
tates.
11.18 Adjust the pH between 3.5 and 4.0 using 1 N HCl.
17.4 Ion Exchange Column, borosilicate glass, 5-mm inside
11.19 Cover the solution with a flat watch glass, then place
diameter, 100-mm long with a TFE-fluorocarbon stopcock.
the beaker on a hot plate and boil for about 5 min to remove
17.5 Beaker, 50-mL, quartz or TFE-fluorocarbon.
carbon dioxide.
11.20 Remove the sample from the hot plate and cool to
18. Reagents
room temperature in a water bath.
18.1 Cation Exchange Resin, 80 to 100 mesh. Prepare the
11.21 Adjust the pH of the sample to 5.6 to 5.7 using 0.1 N
resin by treatment with 3 N HCl followed by water wash until
NaOH solution and 0.1 N HCl. Add 1 to3gof mannitol.
the effluent is neutral to pH paper.
11.22 Titrate the sample to pH 8.0 using a 0.025 N NaOH
18.2 Chloroform (CHCl ).
solution.
18.3 2-Ethyl-1,3Hexanediol Solution, 5 volume% in chlo-
11.23 Determine a blank by performing 11.3-11.22 without
roform.
the sample.
18.4 Nitric Acid (HNO ), 2 M.
18.5 Sodium carbonate (Na CO ), powder.
12. Calculation
2 3
18.6 Sodium Hydroxide(NaOH) Solution,0.1 N,carbonate-
12.1 Calculate the percent boron in the sample as follows:
free. Store in a plastic bottle.
~V 2 B!~N!~A!~100!
B,% 5 (1)
W
19. Procedure
where:
19.1 Prepare an aliquot of sample by following 11.1-11.13.
V = millilitres of NaOH solution used in titration of the
sample,
Dowex 50×8 (or equivalent).
C809 − 94 (Reapproved 2007)
19.2 Pipet 4 mL of water into the glass tube and mix using 22. Interferences
a vortex mixer.
22.1 Impurity elements, at the specification limits usually
established for nuclear-grade composites, do not interfere.
19.3 Filterthesolutionthroughfilterpaper(15.3).Catchthe
Strontium is a potential interference and it is an impurity
filtrate in a 60-mL separatory funnel.
element in the tantalum filament material. At the temperature
19.4 Wash the paper with 15-mL of 2 M HNO . Catch the
used to ionize sodium borate, however, the strontium impurity
wash in the separatory funnel.
in the filament does not volatilize to cause a high bias at mass
19.5 Add 10 mL of 5% 2-ethyl-1,3 hexanediol solution to 88.
the separatory funnel and shake for 2 min.
23. Procedure
19.6 Drain the organic (lower) layer into a clean 100-mL
23.1 Continue with the determination of the isotopic com-
beaker.
position in accordance with the relevant sections of Test
19.7 Repeat 19.5 and 19.6. Methods C791.
19.8 Transfer the 2-ethyl-1,3 hexanediol solution to a clean
SEPARATION OF HALIDES BY PYROHYDROLYSIS
60-mL separatory funnel.
24. Scope
19.9 Extract the boron by shaking for 2-min with a NaOH
24.1 This test method covers the separation of up to 100 µg
solution containing the amount of sodium calculated to give a
of halides per gram of sample. The separated halides are
B/Na ratio of two and a volume sufficient to give 1 mg B/mL.
measured using other test methods found herein.
19.10 Discard the organic phase.
25. Summary of Test
...
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:C 809–94 Designation:C809–94(Reapproved2007)
Standard Test Methods for
Chemical, Mass Spectrometric, and Spectrochemical
Analysis of Nuclear-Grade Aluminum Oxide and Aluminum
Oxide-Boron Carbide Composite Pellets
This standard is issued under the fixed designation C809; 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
aluminum oxide and aluminum oxide-boron carbide composite pellets to determine compliance with specifications.
1.2 The analytical procedures appear in the following order:
Sections
Boron by Titrimetry 7to13
Separation of Boron for Mass Spectrometry 14 to 19
Isotopic Composition by Mass Spectrometry 20 to 23
Separation of Halides by Pyrohydrolysis 24 to 27
Fluoride by Ion-Selective Electrode 28 to 30
Chloride, Bromide, and Iodide by Amperometric Microtitrimetry 31 to 33
Trace Elements by Emission Spectroscopy 34 to 46
1.3 The values stated in SI units are to be regarded as the 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 and health practices and determine the applicability of regulatory
limitations prior to use. (For specific precautionary statements, see Section 5.)
2. Referenced Documents
2.1 ASTM Standards:
C784 Specification for Nuclear-Grade Aluminum Oxide-Boron Carbide Composite Pellets
C785 Specification for Nuclear-Grade Aluminum Oxide Pellets
C791 Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Boron Carbide
C799 Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-
Grade Uranyl Nitrate Solutions
D1193 Specification for Reagent Water
E115 Practice for Photographic Processing in Optical Emission Spectrographic Analysis
E116 Practice for Photographic Photometry in Spectrochemical Analysis
3. Significance and Use
3.1 Aluminum oxide pellets are used in a reactor core as filler or spacers within fuel, burnable poison, or control rods. In order
tobesuitableforthispurpose,thematerialmustmeetcertaincriteriaforimpuritycontent.Thesetestmethodsaredesignedtoshow
whether or not a given material meets the specifications for these items as described in Specification C 785C785.
3.1.1 Impurity content is determined to ensure that the maximum concentration limit of certain impurity elements is not
exceeded.
3.2Aluminum3.2 Aluminum oxide-boron carbide composite pellets are used in a reactor core as a component in neutron
absorber rods. In order to be suitable for this purpose, the material must meet certain criteria for boron content, isotopic
ThesetestmethodsareunderthejurisdictionofASTMCommitteeC-26C26onNuclearFuelCycleandarethedirectresponsibilityofSubcommitteeC26.03onNeutron
Absorbers Materials Specifications .
Current edition approved Oct. 15, 1994. Published December 1994. Originally published as C 809–80. Last previous edition C 809–80.on Neutron Absorber Materials
Specifications.
Current edition approved July 1, 2007. Published August 2007. Originally approved in 1980. Last previous edition approved in 2000 as C809–94(2000). DOI:
10.1520/C0809-94R07.
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.ForAnnualBookofASTMStandards
, Vol 12.01.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.
C809–94 (2007)
composition, and impurity content as described in Specification C 784C784.
3.2.1 The material is assayed for boron to determine whether the boron content is as specified by the purchaser.
3.2.2 Determinationoftheisotopiccontentoftheboronismadetoestablishwhetherthe Bconcentrationisincompliancewith
the purchaser’s specifications.
3.2.3 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
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, reference to water shall be understood to mean reagent water conforming to
Specification D 1193D1193, Type III.
5. Safety Precautions
5.1 Many laboratories have established safety regulations governing the use of hazardous chemicals and equipment. The users
of these test methods should be familiar with such safety practices.
6. Sampling
6.1 Criteria for sampling aluminum oxide pellets are given in Specification C 785C785.
6.2 Criteria for sampling aluminum oxide-boron carbide composite pellets are given in Specification C 784C784.
BORON BY TITRIMETRY
7. Scope
7.1 This test method covers the determination of boron in aluminum oxide-boron carbide composites. As an alternative, the
procedure for total boron by titrimetry detailed in Test Methods C 791C791 may be used.
8. Summary of Test Method
8.1 The sample is crushed, passed through a 100-mesh screen, weighed in a glass boat, and introduced into a heavy-wall glass
tube.Nitricacidisaddedtothetubeandthecontentsmixedusingavortexmixer.Thetubeissealed,placedintoasafetycontainer,
heated for 6 h, cooled to room temperature, opened, and the contents washed into a beaker. The solution is adjusted to pH 9.0
and filtered, then adjusted to pH 3.5 and boiled to remove CO . Substantially, a pure boric acid is obtained which can be titrated
,
in the presence of mannitol with a standard solution of sodium hydroxide.
9. Apparatus
9.1 Analytical Balance, capable of weighing to 60.1 mg.
9.2 Mortar, diamond (Plattner) (or equivalent).
9.3 Sieve, No. 100 (150-µm) U.S. Standard Sieve Series, 76-mm diameter, brass or stainless steel.
9.4 Glass Boats, borosilicate, 4-mm wide, 3-mm deep, 40-mm long.
9.5 Glass Tubing, heavy-wall borosilicate, 5-mm inside diameter by 250-mm long, sealed at one end.
9.6 Mixer, vortex type.
9.7 Glass Blower’s Torch.
9.8 Iron Pipe, 12.7 by 254-mm long with threaded end caps.
9.9 Muffle Furnace, capable of operation at 300°C. The heated area must be of sufficient size to hold the capped iron pipe.
9.10 pH Meter, with pH electrodes and magnetic stirrer.
Annual Book of ASTM Standards, Vol 11.01.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.
Annual Book of ASTM Standards, Vol 03.05.
Wichers, E., Schlecht, W. G., and Gordon, C. L., “Preparing Refractory Oxides, Silicates, and Ceramic Materials for Analysis by Heating with Acids in Sealed Tubes
at Elevated Temperatures,” Journal of Research of the National Bureau of Standards , Vol 33, 1944, p. 451.
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. Pharmaceutical Convention, Inc. (USPC), Rockville, MD.
Lerner, M. W., The Analysis of Elemental Boron, New Brunswick Laboratory, U. S. Atomic Energy Commission, TID-25190, November 1970.
Wichers, E., Schlecht, W. G., and Gordon, C. L., “Preparing Refractory Oxides, Silicates, and Ceramic Materials for Analysis by Heating with Acids in Sealed Tubes
at Elevated Temperatures,” Journal of Research of the National Bureau of Standards, Vol 33, 1944, p. 451.
Rodden, C. J., Analysis of Essential Nuclear Reactor Materials, U.S. Atomic Energy Commission, Washington, DC, Government Printing Office, 1964.
C809–94 (2007)
9.11 Steam Bath.
9.12 Hot Plate.
9.13 Filter Paper, 11 cm, ashless slow filtering for fine precipitates.
9.14 Buret, Class A, 25-mL.
10. Reagents
10.1 Boric Acid, NIST SRM 951 or its replacement.
10.2 Hydrochloric Acid (HCl),1 N.
10.3 Hydrochloric Acid (HCl), 0.1 N.
10.4 Mannitol.
10.5 Nitric Acid (sp gr 1.42)—Concentrated Nitric Acid (HNO ).
10.6 Sodium Hydroxide (NaOH) Solution,1 N, carbonate-free.
10.7 Sodium Hydroxide (NaOH) Solution, 0.1 N, carbonate-free.
10.8 Sodium Hydroxide (NaOH) Solution, 0.025 N, carbonate-free, standardized against NIST SRM 951.
11. Procedure
11.1 Crush the aluminum oxide/boron carbide composite pellet using a diamond mortar until all the sample is passed through
a No. 100 (150-µm) screen.
11.2 Weigh a 250-mg sample into a glass boat.
11.3 Introducetheboatandsampleintoaheavy-wallglasstube,beingverycarefultopreventanyofthesamplefromadhering
to the wall of the tube near the open end.
11.4 Introduce 0.5 mL of concentrated HNO into the glass tube.
11.5 Mix the sample and acid using the vortex mixer.
11.6 Flame the glass tube to remove the moisture from the walls.
11.7 Seal the glass tube. There are two methods available:
11.7.1 Sealing the glass tube may be accomplished by constriction, then drawing off a short piece of the tube, then working
down the sealed end.
11.7.2 Asealcanbemadebyallowingtheopenendofthetubetoflowtogetherbyheatingandrevolvingthetubeslowly.While
the tube is red with heat, the tube is warmed enough to blow out the seal to a rounded shape.
11.8 Place the glass tube into a safety container which consists of a 12.7-mm inside diameter black iron pipe with screw caps
on each end. The caps can be tightened with finger tip control.
11.9 Insert the assembly into a 300°C muffle furnace with the top end of the assembly elevated and heat for 6 h.
11.10 Remove the assembly from the muffle furnace and place into a tray, keeping the same end of the assembly elevated.
11.11 Allow the assembly to cool to room temperature.
11.12 Withdraw the glass tube from the safety container and file a notch about 13 mm from one end of the tube.
NOTE 1—Contents of the tube may be under pressure.
11.13 Heat a glass rod to red heat, then place the rod on the notch. This action should crack the glass tube; however, a light
tap may be needed to complete the break.
11.14 Wash the contents from the glass tube into a 250-mLbeaker; however, if the aluminum oxide is stuck to the walls of the
tube, shake on a vortex mixer.
NOTE 2—The matrix Al O does not completely dissolve, but all of the boron is in solution.
2 3
11.15 Precipitate the iron and the aluminum by using 1 N sodium hydroxide solution to adjust the pH to 9.0.
11.16 Place the beaker on a steam bath and digest for 1 h.
11.17 Filter the sample through the filter paper (9.13) and wash the precipitate with several portions of hot deionized water.
11.18 Adjust the pH between 3.5 and 4.0 using 1 N HCl.
11.19 Coverthesolutionwithaflatwatchglass,thenplacethebeakeronahotplateandboilforabout5mintoremovecarbon
dioxide.
11.20 Remove the sample from the hot plate and cool to room temperature in a water bath.
11.21 Adjust the pH of the sample to 5.6 to 5.7 using 0.1 N NaOH solution and 0.1 N HCl. Add 1 to3gof mannitol.
11.22 Titrate the sample to pH 8.0 using a 0.025 N NaOH solution.
11.23 Determine a blank by performing 11.3-11.22 without the sample.
12. Calculation
12.1 Calculate the percent boron in the sample as follows:
~V–B!~N!~A!~100!
B,% 5
W
(1)
C809–94 (2007)
where:
V = millilitres of NaOH solution used in titration of the sample,
B = millilitres of NaOH solution used in titration of the blank,
N = normality of the NaOH solution,
A = atomic weight of boron computed for the sample based upon the measured isotopic composition, and
W = milligrams of sample weight.
13. Precision
13.1 The limit of error at the 95% confidence level for a single determination is 60.10% absolute.
SEPARATION OF BORON FOR MASS SPECTROMETRY
14. Scope
14.1 This test method covers the separation of boron from aluminum and other impurities. The isotopic composition of the
separated boron is measured using another test method found herein.
15. Summary of Test Method
15.1 Boron is put into solution using a sealed-tube dissolution method. It is separated from aluminum and other impurities by
solvent extraction and ion exchange.
16. Interferences
16.1 There are no known interferences not eliminated by this separation test method.
17. Apparatus
17.1 Separatory Funnel, 60-mL with TFE-fluorocarbon stopcock.
17.2 Mixer, vortex type.
17.3 Filter Paper, ashless, slow filtering for fine precipitates.
17.4 Ion Exchange Column, borosilicate glass, 5-mm inside diameter, 100-mm long with a TFE-fluorocarbon stopcock.
17.5 Beaker, 50-mL, quartz or TFE-fluorocarbon.
18. Reagents
18.1 Cation Exchange Resin, 80 to 100 mesh. Prepare the resin by treatment with 3 N HCl followed by water wash until the
effluent is neutral to pH paper.
18.2 Chloroform (CHCl ).
18.3 2-Ethyl-1,3Hexanediol Solution, 5 volume% in chloroform.
18.4 Nitric Acid (HNO ), 2 M.
18.5 Sodium carbonate (Na CO ), powder.
2 3
18.6 Sodium Hydroxide (NaOH) Solution, 0.1 N , carbonate-free. Store in a plastic bottle.
19. Procedure
19.1 Prepare an aliquot of sample by following 11.1-11.13.
19.2 Pipet 4 mL of water into the glass tube and mix using a vortex mixer.
19.3 Filter the solution through filter paper (15.3). Catch the filtrate in a 60-mL separatory funnel.
19.4 Wash the paper with 15-mL of 2 M HNO . Catch the wash in the separatory funnel.
19.5 Add 10 mL of 5% 2-ethyl-1,3 hexanediol solution to the separatory funnel and shake for 2 min.
19.6 Drain the organic (lower) layer into a clean 100-mL beaker.
19.7 Repeat 19.5 and 19.6.
19.8 Tr
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