ASTM C1163-14

Standard Practice for Mounting Actinides for Alpha Spectrometry Using Neodymium Fluoride

SIGNIFICANCE AND USE
5.1 The determination of actinides by alpha spectrometry is an essential function of many environmental and other programs. Alpha spectrometry allows the identification and quantification of most alpha-emitting actinides. Although numerous separation methods are used, the final sample preparation technique has historically been by electrodeposition (Practice C1284). However, electrodeposition may have some drawbacks, such as time required, incompatibility with prior chemistry, thick deposits, and low recoveries. These problems may be minimized by using the neodymium fluoride coprecipitation method whose performance is well documented (1-6).4 To a lesser extent cerium fluoride has been used (7) but is not addressed in this practice.  
5.2 The sample mounting technique described in this practice is rapid, adds an additional purification step, since only those elements that form insoluble fluorides are mounted, and the sample and filter media can be dissolved and remounted if problems occur. The recoveries are better and resolution approaches normal in electrodeposited samples. Recoveries are sufficiently high that for survey work, if quantitative recoveries are not necessary, tracers can be omitted. Drawbacks to this technique include use of very hazardous hydrofluoric acid and the possibility of a non-reproducible and ill-defined counting geometry from filters that are not flat and may not be suitable for long retention. Also, although the total turn around time for coprecipitation may be less than for electrodeposition, coprecipitation requires more time and attention from the analyst.
SCOPE
1.1 This practice covers the preparation of separated fractions of actinides for alpha spectrometry. It is applicable to any of the actinides that can be dissolved in dilute hydrochloric acid. Examples of applicable samples would be the final elution from an ion exchange separation or the final strip from a solvent extraction separation.2  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 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 a specific hazard statement, see Section 9.

General Information

• Status: Historical
• Publication Date: 31-May-2014
• ICS: 71.040.50 - Physicochemical methods of analysis
• 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: C1163 − 14
Standard Practice for
Mounting Actinides for Alpha Spectrometry Using
1
Neodymium Fluoride
This standard is issued under the fixed designation C1163; 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 fluoride. The purified samples are prepared and mounted on a
membrane filter to produce a deposit that yields alpha spectra
1.1 This practice covers the preparation of separated frac-
of sufficient quality for most analytical methodologies.
tions of actinides for alpha spectrometry. It is applicable to any
Samples can be prepared more rapidly using coprecipitation
of the actinides that can be dissolved in dilute hydrochloric
than by electrodeposition and have comparable resolution.
acid. Examples of applicable samples would be the final
elution from an ion exchange separation or the final strip from
5. Significance and Use
2
a solvent extraction separation.
5.1 The determination of actinides by alpha spectrometry is
1.2 The values stated in SI units are to be regarded as
an essential function of many environmental and other pro-
standard. No other units of measurement are included in this
grams.Alpha spectrometry allows the identification and quan-
standard.
tification of most alpha-emitting actinides.Although numerous
1.3 This standard does not purport to address all of the
separation methods are used, the final sample preparation
safety concerns, if any, associated with its use. It is the
technique has historically been by electrodeposition (Practice
responsibility of the user of this standard to establish appro-
C1284). However, electrodeposition may have some
priate safety and health practices and determine the applica-
drawbacks, such as time required, incompatibility with prior
bility of regulatory limitations prior to use. For a specific
chemistry, thick deposits, and low recoveries. These problems
hazard statement, see Section 9.
may be minimized by using the neodymium fluoride copre-
cipitation method whose performance is well documented
2. Referenced Documents
4
(1-6). To a lesser extent cerium fluoride has been used (7) but
3
2.1 ASTM Standards:
is not addressed in this practice.
C859 Terminology Relating to Nuclear Materials
5.2 The sample mounting technique described in this prac-
C1284 Practice for Electrodeposition of the Actinides for
tice is rapid, adds an additional purification step, since only
Alpha Spectrometry
those elements that form insoluble fluorides are mounted, and
D1193 Specification for Reagent Water
the sample and filter media can be dissolved and remounted if
D3084 Practice for Alpha-Particle Spectrometry of Water
problems occur. The recoveries are better and resolution
3. Terminology
approachesnormalinelectrodepositedsamples.Recoveriesare
3.1 For definitions of terms in this standard, refer to sufficientlyhighthatforsurveywork,ifquantitativerecoveries
are not necessary, tracers can be omitted. Drawbacks to this
Terminology C859.
technique include use of very hazardous hydrofluoric acid and
4. Summary of Test Method
the possibility of a non-reproducible and ill-defined counting
4.1 Guidance is provided for the sample mounting of
geometry from filters that are not flat and may not be suitable
separated actinides using coprecipitation with neodymium
for long retention.Also, although the total turn around time for
coprecipitation may be less than for electrodeposition, copre-
1
This practice is under the jurisdiction ofASTM Committee C26 on the Nuclear
cipitation requires more time and attention from the analyst.
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
Test.
6. Interferences
CurrenteditionapprovedJune1,2014.PublishedJuly2014.Originallyapproved
in 1992. Last previous edition approved in 2008 as C1163 – 08. DOI: 10.1520/
6.1 Calculation of a result from a sample that gives poor
C1163-14.
resolution should not be attempted since it probably implies an
2
Hindman, F. D., “Actinide Separations for α Spectrometry Using Neodymium
error in performing the separation or mounting procedure.
Fluoride Coprecipitation,” Analytical Chemistry, 58, 1986, pp. 1238–1241.
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
4
Standards volume information, refer to the standard’s Document Summary page on The boldface numbers in parentheses refer to a list of references at the end of
the ASTM website. this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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...

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: C1163 − 08 C1163 − 14
Standard Practice for
Mounting Actinides for Alpha Spectrometry Using
1
Neodymium Fluoride
This standard is issued under the fixed designation C1163; 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 practice covers the preparation of separated fractions of actinides for alpha spectrometry as an alternate to
electrodeposition. spectrometry. It is applicable to any of the actinides that can be dissolved in dilute hydrochloric acid. Examples
of applicable samples would be the final elution from an ion exchange separation or the final strip from a solvent extraction
2
separation.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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 a specific hazard statement, see Section 9.
2. Referenced Documents
3
2.1 ASTM Standards:
C859 Terminology Relating to Nuclear Materials
C1284 Practice for Electrodeposition of the Actinides for Alpha Spectrometry
D1193 Specification for Reagent Water
D3084 Practice for Alpha-Particle Spectrometry of Water
3. Terminology
3.1 For definitions of terms in this standard, refer to Terminology C859.
4. Summary of Test Method
4.1 Guidance is provided for the sample mounting of separated actinides using coprecipitation with neodymium fluoride. The
purified samples are prepared and mounted on a membrane filter to produce a deposit that yields alpha spectra equal to
electrodeposited samples. of sufficient quality for most analytical methodologies. Samples can be prepared more rapidly using
coprecipitation than by electrodeposition and have comparable resolution.
5. Significance and Use
5.1 The determination of actinides by alpha spectrometry is an essential function of many environmental and other programs.
Alpha spectrometry allows the identification and quantification of most alpha-emitting actinides. Although numerous separation
methods are used, the final sample preparation technique has historically been by electrodeposition. electrodeposition (Practice
C1284). However, electrodeposition may have some drawbacks, such as time required, incompatibility with prior chemistry, thick
deposits, and low recoveries. These problems may be minimized by using the neodymium fluoride method.coprecipitation method
4
whose performance is well documented (1-6). To a lesser extent cerium fluoride has been used (7) but is not addressed in this
practice.
1
This practice is under the jurisdiction of ASTM Committee C26 on the Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of Test.
Current edition approved July 15, 2008June 1, 2014. Published August 2008July 2014. Originally approved in 1992. Last previous edition approved in 20032008 as
C1163 – 03.C1163 – 08. DOI: 10.1520/C1163-08.10.1520/C1163-14.
2
Hindman, F. D., “Actinide Separations for Alphaα Spectrometry Using Neodymium Fluoride Coprecipitation,” Analytical Chemistry, 58, 1986, pp. 1236 1238–1241.
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
The boldface numbers in parentheses refer to a list of references at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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C1163 − 14
5.2 The sample mounting technique described in this practice is rapid, adds an additional purification step, since only those
elements that form insoluble fluorides are mounted, and the sample and filter media can be dissolved and remounted if problems
occur. The recoveries are better and resolution approaches normal in electrodeposited samples. Recoveries are sufficiently high that
for survey work, if quantitative recoveries are not necessary, tracers can be omitted. Drawbacks to this technique include use of
very hazardous hyd
...