Purity testing of organometallic catalysts by micro liquid chromatography-electron ionization mass spectrometry

Citation
I. Bruheim et al., Purity testing of organometallic catalysts by micro liquid chromatography-electron ionization mass spectrometry, CHROMATOGR, 50(7-8), 1999, pp. 479-484
Citations number
15
Categorie Soggetti
Chemistry & Analysis","Spectroscopy /Instrumentation/Analytical Sciences
Journal title
CHROMATOGRAPHIA
ISSN journal
00095893 → ACNP
Volume
50
Issue
7-8
Year of publication
1999
Pages
479 - 484
Database
ISI
SICI code
0009-5893(199910)50:7-8<479:PTOOCB>2.0.ZU;2-D
Abstract
A micro liquid chromatography-mass spectrometry system utilizing 100 mu m i . d. packed capillary columns has been used for purity testing of organomet allic catalysts. The total effluent, 1 mu Lmin(-1) from the column, was int roduced directly into the ion source of a bench-top quadrupole mass spectro meter and electron ionization mass spectra were acquired. In full scan mode a mass limit of detection of 10-15 ng was achieved for the organometallic compounds investigated. The catalysts dimethyl pentamethylcyclopentadienyl iridium dimethylsulphoxide (Cp*Ir(DMSO)Me-2) and di(pentamethylcyclopentadi enyl dichloro iridium) ((Cp*IrCl2)(2)) were purity tested and their electro n ionization mass spectra recorded. Impurities present down to 1 % of the m ain compound could be determined using large volume injection.