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Title: Extraction chromatographic separations of tantalum and tungsten from hafnium and complex matrix constituents

Abstract

Ta, Hf, and W analyses from complex matrices (including environmental samples) require high purification of these analytes from each other and major/trace matrix constituents, but, current state-of-the-art Ta/Hf/W separations rely on traditional anion exchange approaches that suffer from relatively similar distribution coefficient (Kd) values for these analytes. Our work reports assessment of three commercially available extraction chromatographic resins (TEVA, TRU, and UTEVA) for Ta/Hf/W separations. Batch contact studies show differences in Ta/W,Hf Kd values of up to 10 6, representing an improvement of a factor of 100 and 300 in Ta/Hf and Ta/W Kd values (respectively) over AG1x4 resin. Furthermore, variations in the Kd values as a function of HCl concentration for TRU resin show that this resin is well suited for Ta/Hf/W separations, with Ta/Hf, Ta/W, and W/Hf Kd value improvements of 10, 200, and 30 (respectively) over AG1x4 resin. Finally, analyses of digested soil samples (NIST 2710a) using TRU resin and tandem TEVA-TRU columns demonstrate the ability to achieve extremely high purification (>99%) of Ta and W from each other and Hf, as well as enabling very high purification of Ta and W from the major and trace elemental constituents present in soils, using a single chromatographic step.

Authors:
 [1];  [1];  [1];  [2]
  1. Idaho National Lab. (INL), Idaho Falls, ID (United States)
  2. Pacific Northwest National Lab. (PNNL), Richland, WA (United States)
Publication Date:
Research Org.:
Idaho National Lab. (INL), Idaho Falls, ID (United States)
Sponsoring Org.:
USDOE Office of Nuclear Energy (NE)
OSTI Identifier:
1357615
Report Number(s):
INL/JOU-16-38216
Journal ID: ISSN 0021-9673; PII: S0021967317300547
Grant/Contract Number:
AC07-05ID14517; IAA HDTRA1618618
Resource Type:
Journal Article: Accepted Manuscript
Journal Name:
Journal of Chromatography
Additional Journal Information:
Journal Volume: 1484; Journal Issue: C; Journal ID: ISSN 0021-9673
Publisher:
Elsevier
Country of Publication:
United States
Language:
English
Subject:
07 ISOTOPE AND RADIATION SOURCES; 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; Anion Exchange; Separation; Tantalum; TEVA; TRU; Tungsten

Citation Formats

Snow, Mathew S., Finck, Martha R., Carney, Kevin P., and Morrison, Samuel S.. Extraction chromatographic separations of tantalum and tungsten from hafnium and complex matrix constituents. United States: N. p., 2017. Web. doi:10.1016/j.chroma.2017.01.019.
Snow, Mathew S., Finck, Martha R., Carney, Kevin P., & Morrison, Samuel S.. Extraction chromatographic separations of tantalum and tungsten from hafnium and complex matrix constituents. United States. doi:10.1016/j.chroma.2017.01.019.
Snow, Mathew S., Finck, Martha R., Carney, Kevin P., and Morrison, Samuel S.. Sun . "Extraction chromatographic separations of tantalum and tungsten from hafnium and complex matrix constituents". United States. doi:10.1016/j.chroma.2017.01.019. https://www.osti.gov/servlets/purl/1357615.
@article{osti_1357615,
title = {Extraction chromatographic separations of tantalum and tungsten from hafnium and complex matrix constituents},
author = {Snow, Mathew S. and Finck, Martha R. and Carney, Kevin P. and Morrison, Samuel S.},
abstractNote = {Ta, Hf, and W analyses from complex matrices (including environmental samples) require high purification of these analytes from each other and major/trace matrix constituents, but, current state-of-the-art Ta/Hf/W separations rely on traditional anion exchange approaches that suffer from relatively similar distribution coefficient (Kd) values for these analytes. Our work reports assessment of three commercially available extraction chromatographic resins (TEVA, TRU, and UTEVA) for Ta/Hf/W separations. Batch contact studies show differences in Ta/W,Hf Kd values of up to 106, representing an improvement of a factor of 100 and 300 in Ta/Hf and Ta/W Kd values (respectively) over AG1x4 resin. Furthermore, variations in the Kd values as a function of HCl concentration for TRU resin show that this resin is well suited for Ta/Hf/W separations, with Ta/Hf, Ta/W, and W/Hf Kd value improvements of 10, 200, and 30 (respectively) over AG1x4 resin. Finally, analyses of digested soil samples (NIST 2710a) using TRU resin and tandem TEVA-TRU columns demonstrate the ability to achieve extremely high purification (>99%) of Ta and W from each other and Hf, as well as enabling very high purification of Ta and W from the major and trace elemental constituents present in soils, using a single chromatographic step.},
doi = {10.1016/j.chroma.2017.01.019},
journal = {Journal of Chromatography},
number = C,
volume = 1484,
place = {United States},
year = {Sun Jan 08 00:00:00 EST 2017},
month = {Sun Jan 08 00:00:00 EST 2017}
}

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  • Ta, Hf, and W analyses from complex matrices (including environmental samples) require high purification of these analytes from each other and major/trace matrix constituents, however, current state-of-the-art Ta/Hf/W separations rely on traditional anion exchange approaches that suffer from relatively similar distribution coefficient (Kd) values for these analytes. This work reports assessment of three commercially available extraction chromatographic resins (TEVA, TRU, and UTEVA) for Ta/Hf/W separations. Batch contact studies show differences in Ta/W,Hf Kd values of up to 106, representing an improvement of a factor of 100 and 300 in Ta/Hf and Ta/W Kd values (respectively) over AG1x4 resin. Variations inmore » the Kd values as a function of HCl concentration for TRU resin show that this resin is well suited for Ta/Hf/W separations, with Ta/Hf, Ta/W, and W/Hf Kd value improvements of 10, 200, and 30 (respectively) over AG1x4 resin. Finally, analyses of digested soil samples (NIST 2710a) using TRU resin and tandem TEVA-TRU columns demonstrate the ability to achieve extremely high purification (>99%) of Ta and W from each other and Hf, as well as enabling very high purification of Ta and W from the major and trace elemental constituents present in soils, using a single chromatographic step.« less
  • A method for the determination of Zr, Mo, Hf, and W in niobium and tantalum is described. This method is based on the removal of the matrix elements by extraction with diantipyrylmethane in dichlorethane from HF medium followed by the collection of the elements to be determined on an anion exchange paper suitable for X-ray fluorescence measurement. The recovery studies were carried out with the radiotracer technique. The recoveries for the individual elements with regard to the whole procedure are between 83.1 +/- 2.3% (Mo) and 93.9 +/- 1.4% (Hf). Limits of detection for all four elements ranged from 0.2more » to 0.25 ..mu..g/g. This method was applied to the analysis of samples of different purity grade and the results are compared with those obtained by activation analysis.« less
  • A cladding layer of the refractory metal is formed on the base metal. Either simultaneously or subsequently a transfer of a refractory metal-hardening element from the mass of the base metal to the cladding layer of the refractory metal is effected. A fused salt bath is used, composed essentially of a halide of the refractory element and a diluent halide salt. The base metal incorporating the inter metalic compoundforming element (carbon, nitrogen boron or silicon) is immersed in the bath as the cathode of an electrolytic cell. After deposition of a layer of the refractcry metal on the cathode, themore » cathode is heated sufficiently to effect thermal diffusion of the intermetallic compoundforming element from the base metal into the refractory layer.« less
  • An extraction procedure has been developed for successive isolation of tungsten (/sup 178/W and /sup 181/W) and tantalum (/sup 179/Ta and /sup 182/Ta) isotopes without supports from ..cap alpha..particle-irradiated hafnium targets. The target, irradiated on a cyclotron, is dissolved in hydrofluoric acid. Tantalum isotopes are extracted with tributyl phosphate (TBP) from 1-5 M HF and are then reextracted with a 1:1 ammonia solution, and hydrofluoric acid is removed by heating. Tungsten isotopes are extracted with a chloroform solution or N-benzoyl-N-phenylhydroxylamine (BPHA) from 11-12 M H/sub 2/SO/sub 4/ or ..cap alpha..-benzoin oxime from 4.5-5.5 M H/sub 2/SO/sub 4/ and are thenmore » reextracted with a l:l ammonia solution. The yield of tungsten isotopes is not less than 95%, and the content of radioactive impurities of other isotopes is not more than 0.1%.« less