ASTM C1163-08
(Practice)Standard Practice for Mounting Actinides for Alpha Spectrometry Using Neodymium Fluoride
Standard Practice for Mounting Actinides for Alpha Spectrometry Using Neodymium Fluoride
SIGNIFICANCE AND USE
The determination of actinides by alpha spectrometry is an essential function of many environmental 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. However, electrodeposition may have some drawbacks, such as time required, incompatibility with prior chemistry, thick deposits, and low recoveries. These problems may be minimized using the neodymium fluoride method.
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 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. 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 as an alternate to electrodeposition. 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.
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.
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Designation: C1163 − 08
StandardPractice 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-
equal to electrodeposited samples. Samples can be prepared
tions of actinides for alpha spectrometry as an alternate to
more rapidly than by electrodeposition and have comparable
electrodeposition. It is applicable to any of the actinides that
resolution.
can be dissolved in dilute hydrochloric acid. Examples of
applicable samples would be the final elution from an ion
5. Significance and Use
exchange separation or the final strip from a solvent extraction
2
5.1 The determination of actinides by alpha spectrometry is
separation.
an essential function of many environmental programs. Alpha
1.2 The values stated in SI units are to be regarded as
spectrometry allows the identification and quantification of
standard. No other units of measurement are included in this
most alpha-emitting actinides. Although numerous separation
standard.
methods are used, the final sample preparation technique has
1.3 This standard does not purport to address all of the
historically been by electrodeposition. However, electrodepo-
safety concerns, if any, associated with its use. It is the
sition may have some drawbacks, such as time required,
responsibility of the user of this standard to establish appro-
incompatibility with prior chemistry, thick deposits, and low
priate safety and health practices and determine the applica-
recoveries. These problems may be minimized using the
bility of regulatory limitations prior to use. For a specific
neodymium fluoride method.
hazard statement, see Section 9.
5.2 The sample mounting technique described in this prac-
tice is rapid, adds an additional purification step, since only
2. Referenced Documents
those elements that form insoluble fluorides are mounted, and
3
2.1 ASTM Standards:
the sample and filter media can be dissolved and remounted if
C859 Terminology Relating to Nuclear Materials
problems occur. The recoveries are better and resolution
D1193 Specification for Reagent Water
approaches normal electrodeposited samples. Recoveries are
D3084 Practice for Alpha-Particle Spectrometry of Water
sufficiently high that for survey work, if quantitative recoveries
are not necessary, tracers can be omitted. Drawbacks to this
3. Terminology
technique include use of very hazardous hydrofluoric acid and
3.1 For definitions of terms in this standard, refer to
the possibility of a non-reproducible and ill-defined counting
Terminology C859.
geometry from filters that are not flat. Also, although the total
turn around time for coprecipitation may be less than for
4. Summary of Test Method
electrodeposition, coprecipitation requires more time and at-
4.1 Guidance is provided for the sample mounting of
tention from the analyst.
separated actinides using coprecipitation with neodymium
6. Interferences
1
This practice is under the jurisdiction ofASTM CommitteeC26 on the Nuclear
6.1 Calculation of a result from a sample that gives poor
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
resolution should not be attempted since it probably implies an
Test.
Current edition approved July 15, 2008. Published August 2008. Originally
error in performing the separation or mounting procedure.
approved in 1992. Last previous edition approved in 2003 as C1163 – 03. DOI:
10.1520/C1163-08.
7. Apparatus
2
Hindman, F. D., “Actinide Separations for Alpha Spectrometry Using Neo-
dymium Fluoride Coprecipitation,” Analytical Chemistry, 58, 1986, pp. 1236–1241.
7.1 Alpha Spectrometer—A system should be assembled
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
that is capable of 60 to 70 keV resolution on an actual sample
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
prepared by this practice, have a counting efficiency of greater
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. than 20 %, and a background of less than 0.005 cpm over each
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
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C1163 − 08
designated energy region. Resolution is defined as the full- 8.9 3N Hydrochlor
...
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:C1163–03 Designation:C1163–08
Standard Practice for
Mounting Actinides for Alpha Spectrometry Using
1
Neodymium Fluoride
This standard is issued under the fixed designation C 1163; 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. It is applicable to any of the actinides that can be dissolved in dilute hydrochloric acid. Examples of applicable
2
samples would be the final elution from an ion exchange separation or the final strip from a solvent extraction separation.
1.2
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 8. 9.
2. Referenced Documents
3
2.1 ASTM Standards:
C 859 Terminology Relating to Nuclear Materials
D 1193 Specification for Reagent Water
D 3084 Practice for Alpha-Particle Spectrometry of Water
3. Summary of Test Method
3.1Guidance 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. Samples can be prepared more rapidly than by electrodeposition and have comparable resolution.
Terminology
3.1 For definitions of terms in this standard, refer to Terminology C 859.
4. Significance and Use
4.1The determination of actinides by alpha spectrometry is an essential function of many environmental 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. However, electrodeposition may have
some drawbacks, such as time required, incompatibility with prior chemistry, thick deposits, and low recoveries. These problems
can be minimized using the neodymium fluoride method.
4.2The 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 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
notflat.Also,althoughthetotalturnaroundtimeforcoprecipitationmaybelessthanforelectrodeposition,coprecipitationrequired
more time and attention from the analyst. 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. Samples can be prepared more rapidly than by electrodeposition and have comparable resolution.
1
This practice is under the jurisdiction ofASTM Committee C26 on the Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of Test.
Current edition approved July 10, 2003. Published August 2003. Originally approved in 1992 as C1163–92. Last previous edition approved in 1998 as C1163–98.
Current edition approved July 15, 2008. Published August 2008. Originally approved in 1992. Last previous edition approved in 2003 as C 1163 – 03.
2
Hindman, F. D., “Actinide Separations for Alpha Spectrometry Using Neodymium Fluoride Coprecipitation,” Analytical Chemistry, 58, 1986, pp. 1236–1241.
3
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
, Vol 11.01.volume
...
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