ASTM C1163-14(2023)

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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For a specific hazard statement, see Section 9.  
1.4 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: Published
• Publication Date: 31-Dec-2022
• ICS: 71.040.50 - Physicochemical methods of analysis
• Technical Committee: C26 - Nuclear Fuel Cycle
• Drafting Committee: C26.05 - Methods of Test

Standards Content (Sample)

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.
Designation: C1163 − 14 (Reapproved 2023)
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 3. Terminology
1.1 This practice covers the preparation of separated frac- 3.1 For definitions of terms in this standard, refer to
tions of actinides for alpha spectrometry. It is applicable to any Terminology C859.
of the actinides that can be dissolved in dilute hydrochloric
4. Summary of Test Method
acid. Examples of applicable samples would be the final
elution from an ion exchange separation or the final strip from
4.1 Guidance is provided for the sample mounting of
2
a solvent extraction separation. separated actinides using coprecipitation with neodymium
fluoride. The purified samples are prepared and mounted on a
1.2 The values stated in SI units are to be regarded as
membrane filter to produce a deposit that yields alpha spectra
standard. No other units of measurement are included in this
of sufficient quality for most analytical methodologies.
standard.
Samples can be prepared more rapidly using coprecipitation
1.3 This standard does not purport to address all of the
than by electrodeposition and have comparable resolution.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
5. Significance and Use
priate safety, health, and environmental practices and deter-
5.1 The determination of actinides by alpha spectrometry is
mine the applicability of regulatory limitations prior to use.
an essential function of many environmental and other pro-
For a specific hazard statement, see Section 9.
grams.Alpha spectrometry allows the identification and quan-
1.4 This international standard was developed in accor-
tification of most alpha-emitting actinides.Although numerous
dance with internationally recognized principles on standard-
separation methods are used, the final sample preparation
ization established in the Decision on Principles for the
technique has historically been by electrodeposition (Practice
Development of International Standards, Guides and Recom-
C1284). However, electrodeposition may have some
mendations issued by the World Trade Organization Technical
drawbacks, such as time required, incompatibility with prior
Barriers to Trade (TBT) Committee.
chemistry, thick deposits, and low recoveries. These problems
may be minimized by using the neodymium fluoride copre-
2. Referenced Documents
cipitation method whose performance is well documented
3
4
2.1 ASTM Standards:
(1-6). To a lesser extent cerium fluoride has been used (7) but
C859 Terminology Relating to Nuclear Materials
is not addressed in this practice.
C1284 Practice for Electrodeposition of the Actinides for
5.2 The sample mounting technique described in this prac-
Alpha Spectrometry
tice is rapid, adds an additional purification step, since only
D1193 Specification for Reagent Water
those elements that form insoluble fluorides are mounted, and
D3084 Practice for Alpha-Particle Spectrometry of Water
the sample and filter media can be dissolved and remounted if
problems occur. The recoveries are better and resolution
approachesnormalinelectrodepositedsamples.Recoveriesare
1
This practice is under the jurisdiction ofASTM Committee C26 on the Nuclear
sufficientlyhighthatforsurveywork,ifquantitativerecoveries
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
are not necessary, tracers can be omitted. Drawbacks to this
Test.
Current edition approved Jan. 1, 2023. Published January 2023. Originally
technique include use of very hazardous hydrofluoric acid and
approved in 1992. Last previous edition approved in 2014 as C1163 – 14. DOI:
the possibility of a non-reproducible and ill-defined counting
10.1520/C1163-14R23.
2 geometry from filters that are not flat and may not be suitable
Hindman, F. D., “Actinide Separations for α Spectrometry Using Neodymium
Fluoride Coprecipitation,” Analytical Chemistry, 58, 1986, pp. 1238–1241. for long retention.Also, although the total turn around time for
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 re
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