ASTM C1163-03
(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 can 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 required 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 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.
General Information
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Standards Content (Sample)
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Designation:C1163–03
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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope most alpha-emitting actinides. Although numerous separation
methods are used, the final sample preparation technique has
1.1 This practice covers the preparation of separated frac-
historically been by electrodeposition. However, electrodepo-
tions of actinides for alpha spectrometry as an alternate to
sition may have some drawbacks, such as time required,
electrodeposition. It is applicable to any of the actinides that
incompatibility with prior chemistry, thick deposits, and low
can be dissolved in dilute hydrochloric acid. Examples of
recoveries.These problems can be minimized using the neody-
applicable samples would be the final elution from an ion
mium fluoride method.
exchange separation or the final strip from a solvent extraction
2 4.2 The sample mounting technique described in this prac-
separation.
tice is rapid, adds an additional purification step, since only
1.2 This standard does not purport to address all of the
those elements that form insoluble fluorides are mounted, and
safety concerns, if any, associated with its use. It is the
the sample and filter media can be dissolved and remounted if
responsibility of the user of this standard to establish appro-
problems occur. The recoveries are better and resolution
priate safety and health practices and determine the applica-
approaches normal electrodeposited samples. Recoveries are
bility of regulatory limitations prior to use. For a specific
sufficiently high that for survey work, if quantitative recoveries
hazard statement, see Section 8.
are not necessary, tracers can be omitted. Drawbacks to this
2. Referenced Documents technique include use of very hazardous hydrofluoric acid and
the possibility of a non-reproducible and ill-defined counting
2.1 ASTM Standards:
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geometry from filters that are not flat. Also, although the total
D 1193 Specification for Reagent Water
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turn around time for coprecipitation may be less than for
D 3084 Practice for Alpha-Particle Spectrometry of Water
electrodeposition, coprecipitation required more time and at-
3. Summary of Test Method
tention from the analyst.
3.1 Guidance is provided for the sample mounting of
5. Interferences
separated actinides using coprecipitation with neodymium
5.1 Calculation of a result from a sample that gives poor
fluoride. The purified samples are prepared and mounted on a
resolution should not be attempted since it probably implies an
membrane filter to produce a deposit that yields alpha spectra
error in performing the separation or mounting procedure.
equal to electrodeposited samples. Samples can be prepared
more rapidly than by electrodeposition and have comparable
6. Apparatus
resolution.
6.1 Alpha Spectrometer—A system should be assembled
4. Significance and Use
that is capable of 60 to 70 keV resolution on an actual sample
prepared by this practice, have a counting efficiency of greater
4.1 The determination of actinides by alpha spectrometry is
than 20 %, and a background of less than 0.005 cpm over each
an essential function of many environmental programs. Alpha
designated energy region. Resolution is defined as the full-
spectrometry allows the identification and quantification of
width at half-maximum (FWHM) in keV, or the distance
between those points on either side of the alpha energy peak
where the count is equal to one-half the maximum count.
1
This practice is under the jurisdiction ofASTM Committee C26 on the Nuclear
Additional information can be found in Practice D 3084.
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
6.2 Filter—25-mm 0.1 µm pore, polypropylene membrane
Test.
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Current edition approved July 10, 2003. Published August 2003. Originally filter or equivalent.
approved in 1992 as C 1163 – 92. Last previous edition approved in 1998 as
6.3 Vacuum Funnel—Polysulfone twist-lock with stainless
C 1163 – 98.
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steel screen for filter mounting.
2
Hindman, F. D., “Actinide Separations for Alpha Spectrometry Using Neody-
mium Fluoride Coprecipitation,” Analytical Chemistry, 58, 1986, pp. 1236–1241.
3
Annual Book of ASTM Standards, Vol 11.01.
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Annual Book of ASTM Standards, Vol 11.02. Available from Pall Life Sciences, Ann Arbor, MI, catalog number M5PU025.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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