Rhodium and palladium β-diketonate determination with on-line supercritical fluid extraction-high performance liquid chromatography via solid phase extraction |
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| Authors: | B. W. Wenclawiak Torsten Hees Corinna E. Z?ller Hans-Peter Kabus |
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| Affiliation: | (1) University of Siegen, Department of Analytical Chemistry, Adolf-Reichwein-Strasse 9, D-57068 Siegen, Germany, DE;(2) Merck Darmstadt, Abt. LAB CHROM 3, Frankfurter Strasse 250, D-64271 Darmstadt, Germany, DE |
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| Abstract: | An on-line system of supercritical fluid extraction (SFE) and high performance liquid chromatography (HPLC) via solid phase extraction (SPE) is described for the determination of palladium and rhodium 2,2,6,6-tetramethyl-3,5-heptanedione-(thd) as well as rhodium-acetylacetonate-(acac) and benzylacetonate-(bzac) chelates. The chelates were extracted with supercritical CO2 from sand and humic acid, concentrated on SPE cartridges and analysed with HPLC. Two cartridge materials were tested and compared to off-line trapping. The percentage of the breakthrough and cartridge retained material were measured in liquid dichloromethane. The SFE conditions could be optimized to separate metal chelates during the extraction. The supercritical fluid (SF) behaviour of different ligands on rhodium were investigated. Received: 19 July 1996/Revised: 11 December 1996/Accepted: 14 December 1996 |
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