Liquidliquid extraction is widely used as a cheap and straightforward technique for the analysis of semi-volatile organic micro-pollutants in water. Classical liquidkquid extraction (LLE) can be performed in various ways. The solvent can be added directly to the water sample in a separatory funnel or a dedicated apparatus can be used where the organic solvent is used repeatedly, e.g. continuous LLE. One of the popular solvents in liquidliquid extraction of water samples is dichloromethane. It is especially due to the relatively large consumption of this and other (chlorinated) organic solvents that classical LLE has lost much of its popularity over recent years. Moreover, prior to injection, the extract often has to be preconcentrated, even if large volume injection is applied. In all cases only a fraction of the extraction liquid will be injected and thus potential sensitivity is lost. These and other factors render classical LLE a rather unattractive technique.