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Title: Alternate method of source preparation for alpha spectrometry: No electrodeposition, no hydrofluoric acid

Abstract

An alternate method of preparing actinide alpha counting sources was developed in place of electrodeposition or lanthanide fluoride micro-precipitation. The method uses lanthanide hydroxide micro-precipitation to avoid the use of hazardous hydrofluoric acid. Lastly, it provides a quicker, simpler, and safer way of preparing actinide alpha counting sources in routine, production-type laboratories that process many samples daily.

Authors:
ORCiD logo [1];  [2];  [1];  [1]
  1. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Nuclear and Radiological Protection Division
  2. Univ. of Kentucky, Lexington, KY (United States). Dept. of Chemistry
Publication Date:
Research Org.:
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
1338494
Grant/Contract Number:
AC05-00OR22725
Resource Type:
Journal Article: Accepted Manuscript
Journal Name:
Journal of Radioanalytical and Nuclear Chemistry
Additional Journal Information:
Journal Volume: 311; Journal Issue: 1; Journal ID: ISSN 0236-5731
Publisher:
Springer
Country of Publication:
United States
Language:
English
Subject:
38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEAR CHEMISTRY; alpha spectrometry; actinide source preparation; micro-precipitation; lanthanide hydroxide; electrodeposition

Citation Formats

Kurosaki, Hiromu, Mueller, Rebecca J., Lambert, Susan B., and Rao, Govind R. Alternate method of source preparation for alpha spectrometry: No electrodeposition, no hydrofluoric acid. United States: N. p., 2016. Web. doi:10.1007/s10967-016-4942-y.
Kurosaki, Hiromu, Mueller, Rebecca J., Lambert, Susan B., & Rao, Govind R. Alternate method of source preparation for alpha spectrometry: No electrodeposition, no hydrofluoric acid. United States. doi:10.1007/s10967-016-4942-y.
Kurosaki, Hiromu, Mueller, Rebecca J., Lambert, Susan B., and Rao, Govind R. 2016. "Alternate method of source preparation for alpha spectrometry: No electrodeposition, no hydrofluoric acid". United States. doi:10.1007/s10967-016-4942-y. https://www.osti.gov/servlets/purl/1338494.
@article{osti_1338494,
title = {Alternate method of source preparation for alpha spectrometry: No electrodeposition, no hydrofluoric acid},
author = {Kurosaki, Hiromu and Mueller, Rebecca J. and Lambert, Susan B. and Rao, Govind R.},
abstractNote = {An alternate method of preparing actinide alpha counting sources was developed in place of electrodeposition or lanthanide fluoride micro-precipitation. The method uses lanthanide hydroxide micro-precipitation to avoid the use of hazardous hydrofluoric acid. Lastly, it provides a quicker, simpler, and safer way of preparing actinide alpha counting sources in routine, production-type laboratories that process many samples daily.},
doi = {10.1007/s10967-016-4942-y},
journal = {Journal of Radioanalytical and Nuclear Chemistry},
number = 1,
volume = 311,
place = {United States},
year = 2016,
month = 7
}

Journal Article:
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  • This paper presents an evaluation of an alternate method for preparing environmental samples for 129I analysis by accelerator mass spectrometry (AMS) at Idaho National Laboratory. The optimal sample preparation method is characterized by ease of preparation, capability of processing very small quantities of iodide, and ease of loading into a cathode. Electrodeposition of iodide on a silver wire was evaluated using these criteria. This study indicates that the electrochemically-formed silver iodide deposits produce ion currents similar to those from precipitated silver iodide for the same sample mass. Furthermore, precipitated silver iodide samples are usually mixed with niobium or silver powdermore » prior to loading in a cathode. Using electrodeposition, the silver is already mixed with the sample and can simply be picked up with tweezers, placed in the sample die, and pressed into a cathode. The major advantage of this method is that the silver wire/electrodeposited silver iodide is much easier to load into a cathode.« less
  • Procedures are described by which all ..cap alpha..-emitting elements except radium and polonium can be mounted in a form suitable for ..cap alpha.. spectrometry without need for electrodeposition. The actinides except uranium are precipitated as hydroxides with 50 ..mu..g of cerium carrier from a strongly alkaline solution of ethylenediaminetetraacetic acid. The precipitate is mounted on a 25-mm membrane filter with 0.1-..mu..m pore for spectrometry. The resolution is almost as good as that obtained by electrodeposition on polished stainless steel, and the yield is generally greater than 95%. Uranium can be prepared similarly for ..cap alpha.. spectrometry by reducing it tomore » the quadrivalent state with titanium trichloride in dilute acid and precipitating uranous fluoride.« less
  • Alpha particle counting is based on the response of an electronic counting system to an incident alpha particle. Alpha spectrometry is used in our employee surveillance bioassay program to measure the concentration of isotopes of Am, Pu and U contained on sample source preparations. Nuclides of Am, Pu and U are separated from the sample matrix by anion exchange and are electroplated on a stainless steel disc. The plated source diameter is 12.7 mm. A tracer is added to the sample before anion exchange as a quality control procedure to provide a measure of chemical yield. Tracer alpha-particle emissions aremore » recorded in a preassigned calibrated area of the energy spectrum and chemical recovery is calculated by the ratio of tracer counts per second divided by the tracer activity in becquerels (Bq). Percent tracer recovery may also be calculated by introducing the average counting efficiency factor in the denominator. Tracer yield is then used to provide a reliable estimate of the sample's analyte counts that are recorded in other preassigned energy dependent areas of the spectrum. The tracer spectrum in the presence or absence of other nuclides also provides evidence of the performance characteristics of the alpha spectrometer, for example, chamber vacuum and electronics. Electroplated samples are counted in any one of 96 detectors. The backgrounds of these detectors are maintained at less than 3 counts per 70,000 s over a 190 keV energy window to provide a limit of detection of less than 0.37 mBq per sample at the 95% confidence level. In this paper, resolution of the photopeak is shown to be a function of the source to detector distance and a function of degraded alpha energies due to Fe or other extraneous materials on the plated surface.« less
  • The influence of hydrofluorica acid on the behavior of arsenic and antimony in hydride generation with NaBH/sub 4/ was investigated by means of the radiotracers /sup 76/As and /sup 124/Sb. Simultaneously, the corresponding extinctions were measured. Up to a concentration of 1% hydrofluoric acid present in hydrochloric acid sample solutions does not affect the hydrogenation of As(III) and Sb(III). In solutions with higher HF concentration, As(V) forms (AsF/sub 5/OH)/sup -/ ions which do not react with NaBH/sub 4/. After the (AsF/sub 4/OH)/sup -/ ions are hydrolyzed, the interference of hydrofluoric acid can be sufficiently reduced by complex formation with boricmore » acid. Antimony(V) is not hydrogenated in the presence of hydrofluoric acid, which, in addition, seriously hinders the reduction of Sb(V) to Sb(III). Improved procedures are proposed which allow the elimination of the interference of hydrofluoric acid in both the hydrogenation and the absorption measurement stages and also in the reduction of Sb(V) to Sb(III) in this medium.« less