Optimization of an automated FI-FT-IR procedure for the determination of o-xylene, toluene and ethyl benzene in n-hexane.

The development and optimization of an automated flow injection (FI) manifold coupled with a Fourier transform infrared (FT-IR) detector for the determination of toluene, ethyl benzene and o-xylene in an n-hexane matrix is described. FT-IR parameters optimized were resolution and number of co-added scans; FI parameters optimized were type of pump tubing, carrier flow rate and sample volume. ATR and transmission flow cells were compared for the determination of o-xylene, the ATR cell was easier to use and gave better figures of merit, except for sensitivity, for which the transmission cell was twice as good. Multivariate calibration routines were applied to the FI-FT-IR data and the PLS1 algorithm gave relative root mean standard errors of crossvalidation (RRMSECVs) < 7% for all three analytes using mean-centred data and the first derivative for o-xylene.