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

Relations

• Refers: ASTM C859-24 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Jan-2024
• Refers: ASTM C1284-18 - Standard Practice for Electrodeposition of the Actinides for Alpha Spectrometry
• Effective Date: 01-Jun-2018
• Refers: ASTM C859-14a - Standard Terminology Relating to Nuclear Materials
• Effective Date: 15-Jun-2014
• Refers: ASTM C859-14 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 15-Jan-2014
• Refers: ASTM C859-13a - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Jun-2013
• Refers: ASTM C859-13 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-May-2013
• Refers: ASTM D3084-05(2012) - Standard Practice for Alpha-Particle Spectrometry of Water
• Effective Date: 01-Jun-2012
• Refers: ASTM C859-10b - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Nov-2010
• Refers: ASTM C859-10a - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Aug-2010
• Refers: ASTM C1284-10 - Standard Practice for Electrodeposition of the Actinides for Alpha Spectrometry
• Effective Date: 01-Jun-2010
• Refers: ASTM C859-10 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Feb-2010
• Refers: ASTM C859-09 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 15-Feb-2009
• Refers: ASTM C859-08 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 15-Sep-2008
• Refers: ASTM D1193-06 - Standard Specification for Reagent Water
• Effective Date: 01-Mar-2006
• Refers: ASTM C1284-00(2005) - Standard Practice for Electrodeposition of the Actinides for Alpha Spectrometry
• Effective Date: 01-Jun-2005

Overview

ASTM C1163-14(2023) – Standard Practice for Mounting Actinides for Alpha Spectrometry Using Neodymium Fluoride – establishes a reliable method for preparing actinide samples for alpha spectrometric analysis via neodymium fluoride coprecipitation. This practice is essential in numerous environmental and nuclear programs where the identification and quantification of alpha-emitting actinides are required. The coprecipitation technique enhances sample purity, speeds up preparation, and often increases recovery rates, while supporting accurate and high-resolution spectrometric measurements.

Key Topics

• Actinide Sample Preparation: Outlines procedures for mounting separated actinide fractions using neodymium fluoride coprecipitation instead of traditional electrodeposition. The method applies to actinides dissolvable in dilute hydrochloric acid.
• Alpha Spectrometry: Ensures deposits of sufficient quality for quantitative and qualitative analysis of alpha-emitting actinides, allowing precise measurement with high energy resolution.
• Rapid Mounting Technique: Offers a faster alternative to electrodeposition, with additional purification steps as only elements forming insoluble fluorides are co-precipitated.
• Enhanced Recovery and Resolution: Provides better recovery rates and comparable spectral resolution to electrodeposited samples; recoveries are often sufficient for survey applications even without tracers.
• Safety Considerations: Highlights use of hazardous chemicals such as hydrofluoric acid, mandating adherence to strict laboratory safety protocols due to severe health risks.

Applications

• Environmental Monitoring: Used extensively in environmental radioactivity testing programs to analyze actinide contamination in soil, water, and other media.
• Nuclear Safeguards and Research: Essential in nuclear fuel cycle management for precise actinide quantification, contributing to safeguards and proliferation resistance verification.
• Quality Assurance in Laboratory Practice: Beneficial for laboratories seeking faster throughput and reliable results when handling actinide separations, especially when prior chemistry precludes electrodeposition.
• Remounting Capability: If preparation issues arise (e.g., non-flat filters, sample loss) the sample and mount can be dissolved and re-prepared, increasing method robustness and reducing sample wastage.

Related Standards

• ASTM C1284: Standard Practice for Electrodeposition of the Actinides for Alpha Spectrometry – the traditional method referenced as an alternative.
• ASTM D3084: Practice for Alpha-Particle Spectrometry of Water – provides guidance on energy resolution and spectrometric methods.
• ASTM D1193: Specification for Reagent Water – defines water purity requirements for sample preparation.
• ASTM C859: Terminology Relating to Nuclear Materials – provides definitions relevant to actinide analysis and handling.

Practical Value

The adoption of ASTM C1163-14(2023) offers laboratories:

• Streamlined workflows for actinide alpha spectrometry with improved sample throughput.
• Flexibility in sample handling, including the ability to remount problematic samples.
• Enhanced purification during preparation, minimizing cross-contamination from interfering elements.
• High-quality alpha spectra with strong recovery, making it well-suited for both routine survey work and detailed quantitative analyses.

This standard supports consistency, repeatability, and international interoperability for anyone involved in actinide analysis by alpha spectrometry using neodymium fluoride mounting. For best outcomes, laboratories must implement robust safety practices, given the chemicals involved.

Keywords: actinides, alpha spectrometry, neodymium fluoride, sample preparation, alpha-emitting isotopes, environmental monitoring, nuclear analysis, ASTM C1163

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
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
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
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
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
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 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
C1163 − 14 (2023)
coprecipitation may be less than for electrodeposition, copre- 8.4 Neodymium Chloride Stock Solution (10 mg Nd/mL)—
cipitation requires more time and attention from the analyst. Heat 25 mL of 12M hydrochloric acid and 1.17 g of neo-
dymium oxide on a hotplate until the neodymium oxide is in
6. Interferences
solution. Cool the solution and dilute to 100 mL with water.
6.1 Calculation of a result from a sample that gives poor
8.5 Neodymium Chloride Carrier Solution (0.5 mg Nd/
resolution should not be attempted since it probably implies an
mL)—Dilute 5 mL of the 10 mg Nd/mL neodymium chloride
error in performing the separation or mounting procedure.
stock solution to 100 mL with water.
8.6 Carbon Suspension—Fume ten 47 mm cellulose filters
7. Apparatus
for about 10 min in 10 mL of 18M sulfuric acid. Cool the
7.1 Alpha Spectrometer—A system should be assembled
suspension and dilute to 500 mL with water. The carbon
that is capable of 60 keV to 70 keV resolution on an actual
suspension is used as a visual aid in identifying the presence of
sample prepared by this practice, have a counting efficiency of
the precipitate.
greater than 20 %, and a background of less than 0.005 cpm
8.7 Substrate Solution—Dilute 1 mL of the 10 mg Nd/mL
over each designated energy region. Resolution is defined as
neodymium chloride and 20 mL of 12M hydrochloric acid to
the full-width at half-maximum (FWHM) in keV, or the
400 mL with water. Add, with swirling, 10 mL of 29M
distancebetweenthosepointsoneithersideofthealphaenergy
hydrofluoric acid and 8 mL of the carbon suspension. Dilute
peak where the count is equal to one-half the maximum count.
the suspension to 500 mL with water. Each day before use,
Additional information can be found in Practice D3084.
place the substrate suspension in a sonic bath for 15 min.
7.2 Filter—25 mm 0.1 µm pore, polypropylene membrane
8.8 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
filter or equivalent that will provide suitable alpha spectrom-
chloric acid (12M HCl).
etry resolution.
8.9 3M Hydrochloric Acid—Add 250 mL concentrated hy-
7.3 Vacuum Funnel—Polysulfone twist-lock with stainless
drochloric acid to water and dilute to 1 L with water.
steel screen for filter mounting.
8.10 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid
7.4 Ultrasonic Bath.
(18M H SO ).
2 4
7.5 Plastic Centrifuge Tube, 50 mL.
8.11 Hydrofluoric Acid (48 %)—Concentrated hydrofluoric
7.6 Stainless Steel Disk, 2.54 cm diameter.
acid (29M HF). Warning—Severe burns can result from
7.7 Infrared Heat Lamp.
exposure of skin to concentrated hydrofluoric acid.
7.8 Tape, double-sided.
8.12 Neodymium Oxide (Nd O ).
2 3
8.13 80 % Ethanol.
8. Reagents
8.14 20 % Titanium Trichloride—Available as a 20 % solu-
8.1 Purity of Reagents—Reagent-grade chemicals must be
tion of titanium trichloride from commercial suppliers.
used in all procedures. Unless otherwise indicated, all reagents
should conform to the specifications of the Committee on
8.15 Sodium Sulfate Solution—Dissolve 52 g of anhydrous
Analytical Reagents of theAmerican Chemical Society, if such
sodium sulfate in 500 mL of 18M sulfuric acid.
specifications are available. Other grades may be used, if it is
8.16 Safranine-
...