ASTM C1267-11
(Test Method)Standard Test Method for Uranium by Iron (II) Reduction in Phosphoric Acid Followed by Chromium (VI) Titration in the Presence of Vanadium
Standard Test Method for Uranium by Iron (II) Reduction in Phosphoric Acid Followed by Chromium (VI) Titration in the Presence of Vanadium
SIGNIFICANCE AND USE
Factors governing selection of a method for the determination of uranium include available quantity of sample, homogeneity of material sampled, sample purity, desired level of reliability, and facility available equipment.
This uranium assay method is referenced in the Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Uranium Dioxide Powders and Pellets (Test Methods C696) and in the Test Methods for Chemical, Mass Spectrometric, and Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Uranyl Nitrate Solutions (Test Methods C799). This uranium assay method may also be used for uranium hexafluoride and uranium ore concentrate. This test method determines 20 to 200 mg of uranium; is applicable to product, fuel, and scrap material after the material is dissolved; is tolerant towards most metallic impurity elements usually specified in product and fuel; and uses no special equipment.
The ruggedness of the titration method has been studied for both the volumetric (6) and the weight (7) titration of uranium with dichromate.
Committee C26 Safeguards Statement:
The materials (nuclear grade uranium in product, fuel, and scrap) to which this test method applies are subject to nuclear safeguard regulations governing their possession and use. The analytical method in this standard meets U.S. Department of Energy guidelines for acceptability of a measurement method for generation of safeguards accountability measurement data.
When used in conjunction with the appropriate certified reference materials (SRM or CRM), this procedure can demonstrate traceability to the national measurement base. However, use of the 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 assure that its application to safeguards has the approval of the proper regulatory authorities.
SCOPE
1.1 This test method, commonly referred to as the Modified Davies and Gray technique, covers the titration of uranium in product, fuel, and scrap materials after the material is dissolved. The test method is versatile and has been ruggedness tested. With appropriate sample preparation, this test method can give precise and unbiased uranium assays over a wide variety of material types (1, 2). Details of the titration procedure in the presence of plutonium with appropriate modifications are given in Test Method C1204.
1.2 Uranium levels titrated are usually 20 to 50 mg, but up to 200 mg uranium can be titrated using the reagent volumes stated in this test method.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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 safeguard and safety precaution statements, see Section 4.
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Designation: C1267 − 11
Standard Test Method for
Uranium by Iron (II) Reduction in Phosphoric Acid Followed
1
by Chromium (VI) Titration in the Presence of Vanadium
This standard is issued under the fixed designation C1267; 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 Nuclear-Grade Uranyl Nitrate Solutions
C1128Guide for Preparation of Working Reference Materi-
1.1 This test method, commonly referred to as the Modified
als for Use in Analysis of Nuclear Fuel Cycle Materials
Davies and Gray technique, covers the titration of uranium in
C1204Test Method for Uranium in Presence of Plutonium
product, fuel, and scrap materials after the material is dis-
by Iron(II) Reduction in Phosphoric Acid Followed by
solved. The test method is versatile and has been ruggedness
Chromium(VI) Titration
tested. With appropriate sample preparation, this test method
,
C1346Practice for Dissolution of UF from P-10 Tubes
6
can give precise and unbiased uranium assays over a wide
2 C1347Practice for Preparation and Dissolution of Uranium
variety of material types (1, 2). Details of the titration
Materials for Analysis
procedure in the presence of plutonium with appropriate
4
2.2 NIST Standard:
modifications are given in Test Method C1204.
SRM 136ePotassium Dichromate (Oxidimetric Standard)
1.2 Uranium levels titrated are usually 20 to 50 mg, but up
5
2.3 NBL Standard:
to 200 mg uranium can be titrated using the reagent volumes
CRM 112AUranium Metal Standard
stated in this test method.
1.3 The values stated in SI units are to be regarded as
3. Summary of Test Method
standard. No other units of measurement are included in this
3.1 Samples are prepared by dissolution techniques detailed
standard.
in Practices C1346, C1347, or Refs (2), (3), and (4). Appro-
1.4 This standard does not purport to address all of the
priate uncertainties for sampling and weight determination
safety concerns, if any, associated with its use. It is the
should be applied to the overall precision and bias calculations
responsibility of the user of this standard to establish appro-
for the final result. Aliquants containing 20 to 200 mg of
priate safety and health practices and determine the applica-
uranium are prepared by weight. The sample is fumed to
bility of regulatory limitations prior to use. For specific
dryness after the appropriate acid treatment. The sample is
safeguard and safety precaution statements, see Section 4.
dissolved in dilute nitric acid or water prior to titration.
2. Referenced Documents 3.2 Uraniumisreducedtouranium(IV)byexcessiron(II)in
3 concentrated phosphoric acid (H PO ) containing sulfamic
3 4
2.1 ASTM Standards:
acid. The excess iron(II) is selectively oxidized by nitric acid
C696Test Methods for Chemical, Mass Spectrometric, and
(HNO ) in the presence of a molybdenum(VI) catalyst. After
3
SpectrochemicalAnalysis of Nuclear-Grade Uranium Di-
the addition of a vanadium(IV) solution, the uranium(IV) is
oxide Powders and Pellets
titrated with chromium(VI) to a potentiometric end point.
C799Test Methods for Chemical, Mass Spectrometric,
Spectrochemical,Nuclear,andRadiochemicalAnalysisof 3.3 Thechromium(VI)titrantmaybedeliveredmanuallyon
a weight or on a volumetric basis as specified by the facility
titration procedure.
1
ThistestmethodisunderthejurisdictionofASTMCommitteeC26onNuclear
3.3.1 If the titrant is delivered on a volumetric basis,
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
correctionstothevolumeoftitrantmaybeneededtoadjustfor
Test.
the difference between the temperature of preparation and the
Current edition approved June 1, 2011. Published June 2011. Originally
approved in 1994. Last previous edition approved in 2006 as C1267–06. DOI:
ambient temperature.
10.1520/C1267-11.
2
Theboldfacenumbersinparenthesesrefertothelistofreferencesattheendof
this standard.
3 4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Available from National Institute of Standards and Technology (NIST), 100
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http://www.nist.gov.
5
Standards volume information, refer to the standard’s Document Summary page on NewBrunswickLaboratory(NBL)CertifiedReferenceMaterialsCatalog(U.S.
the ASTM website. Department of Energy), http://www.nbl.doe.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
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C1267 − 11
3.3.2 Automated titrators are fac
...
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:C1267–06 Designation: C1267 – 11
Standard Test Method for
Uranium by Iron (II) Reduction in Phosphoric Acid Followed
1
by Chromium (VI) Titration in the Presence of Vanadium
This standard is issued under the fixed designation C1267; 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 This test method, commonly referred to as the Modified Davies and Gray technique, covers the titration of uranium in
product,fuel,andscrapmaterialsafterthematerialisdissolved.Thetestmethodisversatileandhasbeenruggednesstested.With
appropriatesamplepreparation,thistestmethodcangivepreciseandunbiaseduraniumassaysoverawidevarietyofmaterialtypes
2
(1, 2). Details of the titration procedure in the presence of plutonium with appropriate modifications are given in Test Method
C1204.
1.2 Uranium levels titrated are usually 20 to 50 mg, but up to 200 mg uranium can be titrated using the reagent volumes stated
in this test method.
1.3
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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 safeguard and safety precaution statements, see Section 4.
2. Referenced Documents
3
2.1 ASTM Standards:
C696 Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Uranium Dioxide
Powders and Pellets
C799 Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-
Grade Uranyl Nitrate Solutions
C1128 Guide for Preparation of Working Reference Materials for Use in Analysis of Nuclear Fuel Cycle Materials
C1204 Test Method for Uranium in Presence of Plutonium by Iron(II) Reduction in Phosphoric Acid Followed by
Chromium(VI) Titration
,
C1346 Practice for Dissolution of UF from P-10 Tubes
6
C1347 Practice for Preparation and Dissolution of Uranium Materials for Analysis
4
2.2 NIST Standard:
SRM 136e Potassium Dichromate (Oxidimetric Standard)
5
2.3 NBL Standard:
CRM 112A Uranium Metal Standard
3. Summary of Test Method
3.1 Samples are prepared by dissolution techniques detailed in Practices C1346, C1347, or Refs (2), (3), and (4).Appropriate
uncertainties for sampling and weight determination should be applied to the overall precision and bias calculations for the final
result.Aliquantscontaining20to200mgofuraniumarepreparedbyweight.Thesampleisfumedtodrynessaftertheappropriate
acid treatment. The sample is dissolved in dilute nitric acid or water prior to titration.
3.2 Uranium is reduced to uranium(IV) by excess iron(II) in concentrated phosphoric acid (H PO ) containing sulfamic acid.
3 4
The excess iron(II) is selectively oxidized by nitric acid (HNO ) in the presence of a molybdenum(VI) catalyst.After the addition
3
1
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods ofTest.
Current edition approved JulyJune 1, 2006.2011. Published July 2006.June 2011. Originally approved in 1994. Last previous edition approved in 20002006 as
C1267–006. DOI: 10.1520/C1267-06.10.1520/C1267-11.
2
The boldface numbers in parentheses refer to the list of references at the end of this standard.
3
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.
4
Available from National Institute of Standards and Technology (NIST), 100 Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http://www.nist.gov.
5
New Brunswick Laboratory (NBL) Certified Reference Materials Catalog (U.S. Department of Energy), http://www.nbl.doe.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
C1267 – 11
of a vanadium(IV) solution, the uranium(IV) is titrated with chromium(VI) to a potentiometric end point.
3.3 The chromium(VI) titrant may be delivered manual
...
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