β-diketonates for chromatographic analysis

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Hunt, A.C., 1984. β-diketonates for chromatographic analysis. PhD, Nottingham Trent University.

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Abstract

Three novel fluorinated, aromatic β-diketones, p-Methylbenzoyl-1,1,1-trifluoroacetone (p-Me-bta), Pentafluorobenzoyltrifluoroacetone (pfbtfa) and 1,1,1,2,2,3,3-heptafluoro-6-(pentafluorophenyl)-4,6-hexanedione (pfbhfh), based upon Benzoyl-1,1,1-trifluoroacetone (bta) have been synthesised, and the respective Group I, II, Ki, Cu, Zn, Pb, Cd and Hg chelates and complexes prepared. The solution stability, IE, UV and NMR spectroscopic, polarographic, thermal and vapour pressure properties of the chelates were systematically studied, and the conclusions derived applied to the gas and liquid chromatography of the metal chelates.

The β-diketones pfbtfa and pfbhfh and their respective metal chelates, though possessing fluoro-phenyl substitution, were shown nevertheless to behave spectroscopically, and polarographically in a manner similar to aliphatic-aliphatic terminally substituted β-diketones. Substituent effects in the β-diketonates were shown to operate equally on the oxygen atoms and the chelated metal ion. No evidence of a delocalised electron system within the chelate ring was observed. Physical parameters such as infra-red metal-oxygen bond stretch, polarographic half-wave potential and chelate methine proton resonance position, were linearly related to metal chelate solution stability constant.

The β-diketones were shown to impart insufficient thermal stability and volatility to the studied metals. Gas chromatography was only applied to the pfbtfa chelates, and proved largely unsuccessful. Liquid chromatography of the chelates confirmed the structural implications predicted from spectroscopic and polarographic studies.

Item Type:

Thesis

Creators:

Hunt, A.C.

Date:

1984

ISBN:

9781369325683

Identifiers: