On-line detection and quantification of trace impurities in vaporisable samples by direct liquid introduction process mass spectrometry

A thermal vaporiser has been designed for analysis of liquid streams by a process mass spectrometer normally used for gas analysis. Concentrations of benzene, toluene and o-xylene at mg kg−1 levels in ethanol were determined from continuous vaporisation of the liquid. Ions with m/z values of 39, 57, 73, 77, 78, 91, 92 and 106 were selected and the optimal regression model (multiple linear regression with mean-centring) was found using an automated design of experiments approach to calibration model selection. It was discovered that the linearity of the response allowed excellent calibration to be performed using only four standards (at 0 and 110 mg kg−1 for each of the three analytes) and that there were minimal inter-analyte interferences. The detection limit of benzene, toluene and o-xylene was 0.5, 0.8 and 0.5 mg kg−1, respectively. Average differences between the actual and predicted concentrations, expressed as a percentage of the actual concentrations, for 27–82 mg kg−1 of benzene, toluene and o-xylene were 0.5–1.4%, 0.0–0.4% and 0.3–1.6%, respectively, while the average relative standard deviations were 1.3–2.6%, 1.0–2.5% and 1.1–2.3%, respectively. Detection of 3 mg kg−1 changes in the concentration of each of the analytes (at the 36 mg kg−1 level) was also demonstrated, indicating the sensitivity of the technique and the potential ability of the procedure to detect minor deviations in the specification of process streams from continuous analysis.