Purity testing of air-sensitive organometallic compounds by capillary supercritical fluid chromatography

• Published in: The journal of microcolumn separations 2001, Vol.13 (4), p.156-162
• Main Authors: Bruheim, I., Fooladi, E., Lundanes, E., Greibrokk, T.
• Format: Article
• Language: English
• Subjects: air-sensitive compounds; organometallic compounds; purity testing; supercritical fluid chromatography
• ISSN: 1040-7685; 1520-667X
• DOI: 10.1002/mcs.1035

Capillary supercritical fluid chromatography with flame ionization detection has been used to test the purity of air‐sensitive organometallic compounds such as bisethenepentamethylcyclopentadienylcobalt (Cp*Co(C2H4)2), dicarbonylcyclopentadienylcobalt (CpCo(CO)2), dicarbonylpentamethylcyclopentadienylcobalt (Cp*Co(CO)2), bisethenepentamethyl cyclopentadienylrhodium (Cp*Rh(C2H4)2), bisethenecyclopentadienylrhodium (CpRh(C2H4)2), carbonyl(1,3‐dimesitylimidazol‐2‐ylidene)cyclopentadienylcobalt (CpCo(CO)(carbene)) and ethene(1,3‐dimesitylimidazol‐2‐ylidene)pentamethylcyclopentadienylrhodium (Cp*Rh(C2H4)(carbene)). A sample introduction cell was constructed for loading of 10–40 mg of the air‐sensitive compounds in 100% N2 atmosphere. The sample cell was subsequently filled with toluene or pentane and the analytes in solution were injected onto the 50 μm i.d. capillary column using a timed split injector with 60 nL loop. A nonpolar (5% phenylsiloxane/95% methyl siloxane) stationary phase was used and a mobile phase consisting of 100% CO2 with pressure programming. No signs of air‐induced decomposition of the analytes were observed and impurities down to 1% could be determined using SFC‐FID. © 2001 John Wiley & Sons, Inc. J Micro Sep 13: 156–162, 2001