Purity testing of organometallic catalysts by packed capillary supercritical fluid chromatography.
A packed capillary column supercritical fluid chromatography system with flame ionization detection has been used for purity testing of candidates for homogeneous catalysis such as methyl tricarbonyl pentamethylcyclopentadienyl tungsten [Cp*W(CO)3Me], methyl tricarbonyl cyclopentadienyl tungsten [CpW(CO)3Me], tetramethyl pentamethylcyclopentadienyl iridium (Cp*IrMe4), trimethyl (1,4,7-trimethyl-1,4,7-triazocyclononane) rhodium (CnRhMe3), trimethylphosphine hydride dicarbonyl cyclopentadienyl molybdenum [eta5-CpMoH(CO)2PMe3] and triphenylphosphine hydride dicarbonyl cyclopentadienyl molybdenum [eta5-CpMoH(CO)2PPh3]. A mass limit of detection of 240 pg was found for eta5-CpMoH(CO)2PMe3 when using a 60-nl injection volume and pure CO2 as mobile phase on a 5 microm Kromasil C18 column. The stability of the catalysts in solution has been examined. After 24 h more than 70% of eta5-CpMoH(CO)2PMe3 and 50% of eta5-CpMoH(CO)2PPh3 had decomposed. Due to the instability of the compounds the purity testing had to take place rapidly after sample dissolution.
Bruheim
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Department of Chemistry, University of Oslo, Norway. i.a.bruheim@kjemi.uio.no
Skuland
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Lundanes
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Greibrokk
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D002384:Catalysis; D002853:Chromatography, Liquid / Q000379:methods*; D009942:Organometallic Compounds / Q000032:analysis* / Q000302:isolation & purification; D012680:Sensitivity and Specificity
D009942:Organometallic Compounds