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

✍ Scribed by I. Bruheim; E. Fooladi; E. Lundanes; T. Greibrokk

• Publisher: John Wiley and Sons
• Year: 2001
• Tongue: English
• Weight: 133 KB
• Volume: 13
• Category: Article
• ISSN: 1040-7685
• DOI: 10.1002/mcs.1035

✦ Synopsis

Capillary supercritical fluid chromatography with flame ionization detection has been used to test the purity of air-sensitive organometallic compounds Ž Ž . . such as bisethenepentamethylcyclopentadienylcobalt Cp*Co C H , dicarbonyl-2 4 2 Ž Ž . . cyclopentadienylcobalt CpCo CO , dicarbonylpentamethylcyclopentadienyl-2 Ž Ž . . cobalt Cp*Co CO , bisethenepentamethyl cyclopentadienylrhodium 2 Ž Ž . . Ž Ž . . Cp*Rh C H , bisethenecyclopentadienylrhodium CpRh C H , carbonyl-2 4 2 2 4 2 Ž . Ž Ž .Ž .. 1,3-dimesitylimidazol-2-ylidene cyclopentadienylcobalt CpCo CO carbene and Ž . ethene 1,3-dimesitylimidazol-2-ylidene pentamethylcyclopentadienylrhodium Ž Ž .Ž .. Cp*Rh C H carbene . A sample introduction cell was constructed for loading 2 4

of 10᎐40 mg of the air-sensitive compounds in 100% N atmosphere. The sample 2 cell was subsequently filled with toluene or pentane and the analytes in solution were injected onto the 50 m i.d. capillary column using a timed split injector with Ž . 60 nL loop. A nonpolar 5% phenylsiloxaner95% methyl siloxane stationary phase was used and a mobile phase consisting of 100% CO with pressure programming.

2

No signs of air-induced decomposition of the analytes were observed and impurities down to 1% could be determined using SFC-FID.