A set-up procedure for the minimisation of signal noise of a capillary inlet mass spectrometer system, enabling direct use of data without noise ®ltering or drift correction, is described. A reliable calibration method was developed, involving standard calibration mixtures determined by the extreme vertices design. This novel method was shown to be the most accurate in comparison with a number of commonly used methods. These procedures enabled reliable on-line fermenter headspace gas analysis. With a relatively inexpensive mass spectrometer, monitoring of a fermentation and accurate estimation of oxygen uptake rate, carbon dioxide evolution rate, respiratory quotient and biomass concentration was possible.