COMPARISON OF FLAME IONIZATION AND INDUCTIVELY-COUPLED PLASMA-MASS SPECTROMETRY FOR THE DETECTION OF ORGANOMETALLICS SEPARATED BY CAPILLARY SUPERCRITICAL-FLUID CHROMATOGRAPHY

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 3sigma/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%.