ASTM C1561-10

Standard Guide for Determination of Plutonium and Neptunium in Uranium Hexafluoride by Alpha Spectrometry

SIGNIFICANCE AND USE
The method is applicable to the analysis of materials to demonstrate compliance with the specifications set forth in Specifications C787 and C996.
The method can be used to quantify Pu and Np in U-rich matrix before to recycle them.
SCOPE
1.1 This method covers the determination of plutonium and neptunium isotopes in uranium hexafluoride by alpha spectroscopy. The method can also be applicable to any matrix that may be converted to a nitric acid system.
1.2 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 requirements prior to use.

General Information

• Status: Historical
• Publication Date: 30-Sep-2010
• ICS: 71.040.50 - Physicochemical methods of analysis
• Technical Committee: C26 - Nuclear Fuel Cycle
• Drafting Committee: C26.05 - Methods of Test

Relations

• Replaces: ASTM C1561-03 - Standard Guide for Determination of Plutonium and Neptunium in Uranium Hexafluoride by Alpha Spectrometry
• Effective Date: 01-Oct-2010
• Replaced By: ASTM C1561-10(2016) - Standard Guide for Determination of Plutonium and Neptunium in Uranium Hexafluoride and U-Rich Matrix by Alpha Spectrometry
• Effective Date: 01-Jun-2016
• Referred By: ASTM C761-18 - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Uranium Hexafluoride
• Effective Date: 01-Oct-2010
• Referred By: ASTM C799-19 - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Uranyl Nitrate Solutions
• Effective Date: 01-Oct-2010

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:C1561 −10
StandardGuide for
Determination of Plutonium and Neptunium in Uranium
1
Hexafluoride and U-Rich Matrix by Alpha Spectrometry
This standard is issued under the fixed designation C1561; 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 4. Summary of Test Method
1.1 This method covers the determination of plutonium and 4.1 An aliquot of hydrolyzed uranium hexafluoride equiva-
lenttoapproximately0.5gofuraniumisconvertedtoanoxalic
neptunium isotopes in uranium hexafluoride by alpha spectros-
copy.Themethodcanalsobeapplicabletoanymatrixthatmay acid-nitric acid system and the uranium is selectively removed
be converted to a nitric acid system. via solid phase extraction. Plutonium and neptunium are
further purified by additional solid phase extractions. The
1.2 This standard does not purport to address all of the
plutonium and neptunium are then co-precipitated with neo-
safety concerns, if any, associated with its use. It is the
dymium as the fluorides and counted by alpha spectrometry.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
4.2 Tracer recoveries using this method are typically be-
bility of regulatory requirements prior to use. tween 75 and 90 % for uranium hexafluoride, for different
matrix (with impurities): ~ 10 %.The resolution of the tracer is
2. Referenced Documents typically less than 40 keV full-width at half-maximum.
2
2.1 ASTM Standards: 4.3 The minimum detectable activity will vary with tracer
recovery, sample size, instrument background, and counting
C787 Specification for Uranium Hexafluoride for Enrich-
ment efficiency.
C996 Specification for Uranium Hexafluoride Enriched to
235
Less Than 5 % U 5. Significance and Use
C1163 Practice for MountingActinides forAlpha Spectrom-
5.1 The method is applicable to the analysis of materials to
etry Using Neodymium Fluoride
demonstrate compliance with the specifications set forth in
C1475 Guide for Determination of Neptunium-237 in Soil
Specifications C787 and C996.
D1193 Specification for Reagent Water
D3084 Practice for Alpha-Particle Spectrometry of Water 5.2 ThemethodcanbeusedtoquantifyPuandNpinU-rich
D3648 Practices for the Measurement of Radioactivity matrix before to recycle them.
3. Terminology 6. Interferences
3.1 reagent blank—DI water processed the same as the
6.1 Incomplete removal of U-234 from the neptunium
samples; used in the determination of the minimum detectable
fraction could result in a false positive for the Np-237 analysis.
activity.
The method has been shown to adequately remove uranium at
enrichments up to 5 %. If the method is used for the analysis of
3.2 region-of-interest (ROI)—the channels, or region, in the
materials at greater than 5 % enrichment, a blank consisting of
alpha spectra in which the counts due to a specific radioisotope
uranium at the same enrichment as the samples should be
appear on a functioning calibrated alpha spectrometry system.
analyzed to show adequate removal of the U-234.
6.2 APu tracer is used to monitor the chemical recovery of
the Np. Spiked analyses should be performed to confirm the
1
This guide is under the jurisdiction ofASTM Committee C26 on Nuclear Fuel
Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of Test. appropriateness of this correction; fractionation of Np and Pu
Current edition approved Oct. 1, 2010. Published October 2010. Originally
during the separation could lead to incorrect test results.
approved in 2003. Last previous edition approved in 2003 as C1561-03. DOI:
10.1520/C1561-10.
2
7. Instrumentation
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
7.1 Alpha Spectrometry System—See Practices D3084 and
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. D3648 for a description of the apparatus.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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C1561−10
8. Apparatus 9.17 Nitric Acid (2M)—Add 125 mL of concentrated nitric
acid to 500 mL of water; dilute to a final volume of 1 L.
8.1 Ion Exchange Columns, able to hold a 10 mL resin bed
and 15 mL solution washes.
9.18 Oxalic Acid in 1M HCl(0.1M)—Dissolve12.6goxalic
acid dihydrate in 500 mL of 1M HCl; dilute to a final volume
8.2 Filter Paper, 0.1 µm pore size, 25-mm diameter, com-
3
of 1 L with 1M HCl.
patible with HF.
9.19 Oxalic Acid in 2M HNO
...

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:C1561–03 Designation: C1561 – 10
Standard Guide for
Determination of Plutonium and Neptunium in Uranium
1
Hexafluoride and U-Rich Matrix by Alpha Spectrometry
This standard is issued under the fixed designation C1561; 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 method covers the determination of plutonium and neptunium isotopes in uranium hexafluoride by alpha spectroscopy.
The method couldcan also be applicable to any matrix that may be converted to a nitric acid system.
1.2 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
requirements prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
C787 Specification for Uranium Hexafluoride for Enrichment
235
C996 Specification for Uranium Hexafluoride Enriched to Less Than 5 % U
C1163 Practice for Mounting Actinides for Alpha Spectrometry Using Neodymium Fluoride
C1475 Guide for Determination of Neptunium-237 in Soil
D1193 Specification for Reagent Water
D3084 Practice for Alpha-Particle Spectrometry of Water
D3648 Practices for the Measurement of Radioactivity
3. Terminology
3.1 reagent blank—DI water processed the same as the samples; used in the determination of the minimum detectable activity.
3.2 region-of-interest (ROI)—the channels, or region, in the alpha spectra in which the counts due to a specific radioisotope
appear on a functioning calibrated alpha spectrometry system.
4. Summary of Test Method
4.1 An aliquot of hydrolyzed uranium hexafluoride equivalent to approximately 0.5 g of uranium is converted to an oxalic
acid-nitric acid system and the uranium is selectively removed via solid phase extraction. Plutonium and neptunium are further
purified by additional solid phase extractions. The plutonium and neptunium are then co-precipitated with neodymium as the
fluorides and counted by alpha spectrometry.
4.2Tracer recoveries using this method are typically between 75 and 90%. The resolution of the tracer is typically less than 40
keV full-width at half-maximum.
4.2 Tracer recoveries using this method are typically between 75 and 90 % for uranium hexafluoride, for different matrix (with
impurities): ~ 10 %. The resolution of the tracer is typically less than 40 keV full-width at half-maximum.
4.3 The minimum detectable activity will vary with tracer recovery, sample size, instrument background, and counting
efficiency.
5. Significance and Use
5.1 The method is applicable to the analysis of materials to demonstrate compliance with the specifications set forth in
Specifications C787 and C996.
5.2 The method can be used to quantify Pu and Np in U-rich matrix before to recycle them.
1
This guide 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 Feb. 10, 2003. Published March 2003. DOI: 10.1520/C1561-03.
Current edition approved Oct. 1, 2010. Published October 2010. Originally approved in 2003. Last previous edition approved in 2003 as C1561-03. DOI:
10.1520/C1561-10.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM 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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
C1561 – 10
6. Interferences
6.1 Incomplete removal of U-234 from the neptunium fraction could result in a false positive for the Np-237 analysis. The
methodhasbeenshowntoadequatelyremoveuraniumatenrichmentsupto5 %.Ifthemethodisusedfortheanalysisofmaterials
at greater than 5 % enrichment, a blank consisting of uranium at the same enrichment as the samples should be analyzed to show
adequate removal of the U-234.
6.2 A Pu tracer is used to monitor the chemical recovery of the Np. Spiked analyses should be performed to confirm the
appropriateness of this correction; fractionation of Np and Pu during the separation could lead to incorrect test results.
7. Instru
...