The effect of different relative humidity (RH) on the response of a six-polymer coated Quartz Crystal Microbalance (QCM) sensor based electronic nose (EN) was investigated, RH 30 and 50% respectively. Increases in the sensor responses were observed for an increase in RH. A stainless steel pre-concentration tube (PCT) containing Porapak-S and a nichrome heating element was developed to minimise the effect and allow for chromatographic pre-separation. Breakthrough times of chemical compounds through the PCT were experimentally determined and used to select a mixture of water and toluene as a suitable sample for pre-separation. The PCT was capable of separating the water from the toluene and the EN was competent at evaluating the concentration of toluene in the solution.