ASTM C1267-17

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
5.1 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.  
5.2 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.  
5.3 The ruggedness of the titration method has been studied for both the volumetric (6) and the weight (7)  titration of uranium with dichromate.  
5.4 Fitness for Purpose of Safeguards and Nuclear Safety Application—Methods intended for use in safeguards and nuclear safety applications shall meet the requirements specified by Guide C1068 for use in such applications.  
5.4.1 When used in conjunction with the appropriate certified reference materials (SRM6 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).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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific safeguard and safety precaution statements, see Section 5.  
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

• Status: Historical
• Publication Date: 31-Oct-2017
• ICS: 27.120.30 - Fissile materials and nuclear fuel technology
• Technical Committee: C26 - Nuclear Fuel Cycle
• Drafting Committee: C26.05 - Methods of Test

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: C1267 − 17
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 2. Referenced Documents
3
2.1 ASTM Standards:
1.1 This test method, commonly referred to as the Modified
C696Test Methods for Chemical, Mass Spectrometric, and
Davies and Gray technique, covers the titration of uranium in
SpectrochemicalAnalysis of Nuclear-Grade Uranium Di-
product, fuel, and scrap materials after the material is dis-
oxide Powders and Pellets
solved. The test method is versatile and has been ruggedness
C799Test Methods for Chemical, Mass Spectrometric,
tested. With appropriate sample preparation, this test method
Spectrochemical,Nuclear,andRadiochemicalAnalysisof
can give precise and unbiased uranium assays over a wide
2
Nuclear-Grade Uranyl Nitrate Solutions
variety of material types (1, 2). Details of the titration
C859Terminology Relating to Nuclear Materials
procedure in the presence of plutonium with appropriate
C1068Guide for Qualification of Measurement Methods by
modifications are given in Test Method C1204.
a Laboratory Within the Nuclear Industry
1.2 Uranium levels titrated are usually 20 to 50 mg, but up
C1128Guide for Preparation of Working Reference Materi-
to 200 mg uranium can be titrated using the reagent volumes
als for Use in Analysis of Nuclear Fuel Cycle Materials
stated in this test method.
C1204Test Method for Uranium in Presence of Plutonium
1.3 The values stated in SI units are to be regarded as
by Iron(II) Reduction in Phosphoric Acid Followed by
standard. No other units of measurement are included in this
Chromium(VI) Titration
standard.
C1346Practice for Dissolution of UF from P-10 Tubes
6
C1347Practice for Preparation and Dissolution of Uranium
1.4 This standard does not purport to address all of the
Materials for Analysis
safety concerns, if any, associated with its use. It is the
4
2.2 NIST Standard:
responsibility of the user of this standard to establish appro-
SRM 136ePotassium Dichromate (Oxidimetric Standard)
priate safety, health, and environmental practices and deter-
5
2.3 NBL Standard:
mine the applicability of regulatory limitations prior to use.
CRM 112AUranium Metal Standard
For specific safeguard and safety precaution statements, see
Section 5.
3. Terminology
1.5 This international standard was developed in accor-
3.1 Except as otherwise defined herein, definitions of terms
dance with internationally recognized principles on standard-
are as given in Terminology C859.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
4. Summary of Test Method
mendations issued by the World Trade Organization Technical
4.1 Samplesarepreparedbydissolutiontechniquesdetailed
Barriers to Trade (TBT) Committee.
in Practices C1346, C1347, or Refs (2), (3), and (4). Appro-
priate uncertainties for sampling and weight determination
1 3
ThistestmethodisunderthejurisdictionofASTMCommitteeC26onNuclear For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Test. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Nov. 1, 2017. Published November 2017. Originally the ASTM website.
4
approved in 1994. Last previous edition approved in 2011 as C1267–11. DOI: Available from National Institute of Standards and Technology (NIST), 100
10.1520/C1267-17. Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http://www.nist.gov.
2 5
Theboldfacenumbersinparenthesesrefertothelistofreferencesattheendof NewBrunswickLaboratory(NBL)CertifiedReferenceMaterialsCatalog(U.S.
this standard. Department of Energy), http://science.energy.gov/nbl.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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C1267 − 17
should be applied to the overall precision and bias calculations 5.4.1 When used in conjunction with the appropriate certi-
6
for the final result. Aliquants containing 20 to 200 mg of fied reference materials (SRM or CRM), this procedure can
uranium are prepared by weight. The sample is fumed to demonstrate traceability to the national measurement base.
dryness after the appropriate acid treatment. The sample is Howev
...

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: C1267 − 11 C1267 − 17
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. 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 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
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 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. For specific safeguard and safety precaution statements, see Section 45.
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
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
C859 Terminology Relating to Nuclear Materials
C1068 Guide for Qualification of Measurement Methods by a Laboratory Within the Nuclear Industry
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
1
This test method is under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of Test.
Current edition approved June 1, 2011Nov. 1, 2017. Published June 2011November 2017. Originally approved in 1994. Last previous edition approved in 20062011 as
C1267 – 06.C1267 – 11. DOI: 10.1520/C1267-11.10.1520/C1267-17.
2
The boldface numbers in parentheses refer to the list of references at the end of this standard.
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. 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.http://science.energy.gov/nbl.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
C1267 − 17
3. Terminology
3.1 Except as otherwise defined herein, definitions of terms are as given in Terminology C859.
4. Summary of Test Method
4.1 Samples are prepared by dissolution techniques detailed in Practices C1346, C1347, or Refs (2), (3), and (4). Appropriate
uncertainties for sampling and weight determinat
...