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Analytical and spectroscopic study of indium extraction with 1,10-Bis(1-phenyl-3-methyl-5-hydroxy-4-pyrazolyl)-1,10-decanedione and its mixtures with Tri-n-octylphosphine oxide

Analytische und spektroskopische Untersuchung der Extraktion von Indium mittels 1,10-Bis(1-phenyl-3-methyl-5-hydroxy-4-pyrazolyl)-1,10-decandion und dessen Mischungen mit Tri-n-octylphosphinoxid

  • Anorganische Und Physikalische Chemie
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Summary

Complex organic phases are obtained by extraction of indium from 1M perchlorate media with chloroform solutions of 1,10-bis(1-phenyl-3-methyl-5-hydroxy-4-pyrazolyl)-1,10-decanedione, “HL-8-LH”. PMR and analytical data show that, at lowpH and for low extractant concentrations, four extracted species are present: In(L-8-L) (L-8-LH), In2(L-8-L)3, In(L-8-LH)3 and In2(L-8-L)2 (L-8-LH)2. The corresponding extraction constants have been estimated, resp. 0.0<logK 12<1.0; 1.2<logK 23<2.2; 1.0<logK 13<2.2 and 0<logK 24<3. At highestpH's, polymeric species are formed.

The extractible complex In2(L-8-L)3 has been synthesized. It contains two “(L-8-L)In” moieties whereL-8-L 2− acts as a bis-chelatant folded on the indium atom, linked by aL-8-L 2− bridge. This complex slowly rearranges in chloroform solutions to form polymeric species.

A weak synergy is observed by adding tri-n-octylphosphine oxide, “TOPO”, to the extraction solvent. The organic extraction phase mainly contains In2(L-8-L)3 (TOPO)2. The corresponding extraction constant is logK 232=6.6±0.2.31P-NMR shows that this complex is not formed byTOPO addition in the organic phase, contrary to the usual description of the synergistic effect.

Zusammenfassung

Die Extraktion von Indium aus Perchlorat-Lösungen mittels 1,10-Bis(1-phenyl-3-methyl-5-hydroxy-4-pyrazolyl)-1,10-decandion, „HL-8-LH“, in Chloroform führt zu komplexen organischen Phasen. Protonen-Kernresonanz und analytische Daten zeigen, daß bei niedrigempH und schwachen Konzentrationen an Extraktionsmittel vier extrahierte Verbindungen vorhanden sind: In(L-8-L) (L-8-LH), In2(L-8-L)3, und In2(L-8-L)2 (L-8-LH)2. Die entsprechenden Extraktionskonstanten wurden auf 0.0<logK 12<1.0; 1.2<logK 23<2.2; 1.0<logK 13<2.2 und 0<logK 24<3 geschätzt. Bei höherempH bilden sich polymere Verbindungen.

Der extrahierbare Komplex In2(L-8-L)3 wurde unabhängig synthetisiert. Er enthält zwei „(L-8-L)In“-Gruppen, in denenL-8-L 2− als ein Bis-Chelat-Ligand um das Indium-Atom gefaltet ist, und die durch eineL-8-L 2−-Brücke verbunden sind. Dieser Komplex wandelt sich in Chloroform-Lösungen langsam in polymere Verbindungen um.

Bei Zusatz von Tri-n-octylphosphinoxid („TOPO“) zum Extraktionsmittel wird ein schwacher Synergismus beobachtet, wobei die organische Phase hauptsächlich In2(L-8-L)3 (TOPO)2 enthält. Die entsprechende Extraktionskonstante war logK 232=6.6±0.2.

Die31P-Kernresonanz zeigt, daß dieser Komplex nicht durchTOPO-Addition in der organischen Phase gebildet wird, im Gegensatz zu den üblichen Annahmen über Prozesse mit synergistischem Effekt.

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Authors and Affiliations

  1. Laboratoire de Chimie Minérale et Analytique (CNRS, URA 405), Ecole Européenne des Hautes Etudes des Industries Chimiques, BP 296, F-67008, Strasbourg, France

    A. Tayeb, G. J. Goetz-Grandmont & J. P. Brunette

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  1. A. Tayeb
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  2. G. J. Goetz-Grandmont
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  3. J. P. Brunette
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Tayeb, A., Goetz-Grandmont, G.J. & Brunette, J.P. Analytical and spectroscopic study of indium extraction with 1,10-Bis(1-phenyl-3-methyl-5-hydroxy-4-pyrazolyl)-1,10-decanedione and its mixtures with Tri-n-octylphosphine oxide. Monatsh Chem 122, 453–466 (1991). https://doi.org/10.1007/BF00809797

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  • DOI: https://doi.org/10.1007/BF00809797

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