title: Comparison of flame ionization and inductively coupled plasma mass spectrometry for the detection of organometallics separated by capillary supercritical fluid chromatography.
abstract: Organotin compounds are separated by capillary supercritical fluid chromatography (SFC) and a comparison of the detection by flame ionization (FID) and inductively coupled plasma mass spectrometry (ICP-MS) is presented. Resolution, detection limits, linear dynamic range and reproducibility are the parameters compared between SFC-FID and SFC-ICP-MS, for the detection of tri- and tetraorganotin compounds. The resolution obtained in the SFC-FID system is not always observed in SFC-ICP-MS. Degradation in resolution is due to fluctuations in transfer line temperature. Baseline resolution for the organotins considered is achieved in both systems by using a longer column. Detection limits (DLs) are calculated as 3 sigma/S, where sigma is the standard deviation of the blank signal and S is the slope of the calibration curve. Detection limits of 10.3, 12.5, 12.0 and 9.0 pg are obtained for tetrabutyltin, tributyltin chloride, triphenyltin chloride and tetraphenyltin, respectively, using SFC-FID. An improvement in detection limits of one order of magnitude is achieved by SFC-ICP-MS for the same organotins (0.26, 0.80, 0.57 and 0.20 pg, respectively). The relative standard deviations using SFC-FID for five 50-nl injections, containing 0.5 ng Sn, ranged from 3.2 to 6.4%. Using SFC-ICP-MS, five replicate injections of 0.05 ng Sn give R.S.D.s from 1.3 to 3.4%.
authors.affiliation: Department of Chemistry, University of Cincinnati, OH 45221-0172.
authors.forename: N P
authors.initials: NP
authors.lastname: Vela
authors.forename: J A
authors.initials: JA
authors.lastname: Caruso
mesh_terms: D002197:Capillary Action; D002845:Chromatography / Q000379:methods*; D005410:Flame Ionization; D013058:Mass Spectrometry / Q000379:methods*; D008970:Molecular Weight; D009947:Organotin Compounds / Q000302:isolation & purification*; D011312:Pressure; D013696:Temperature; D014835:Volatilization
chemical_list: D009947:Organotin Compounds