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For the first time, the application of polytetrafluoroethylene powder as an extractant phase collector or holder in liquid-phase microextraction has been developed. For this purpose, the analytical performances of two different ways of applying polytetrafluoroethylene powder in microextraction methods including polytetrafluoroethylene physisorption-assisted emulsification microextraction and dispersive liquid-phase microextraction via polytetrafluoroethylene extractant phase holders have been compared for analysis of aliphatic hydrocarbons in aqueous phases. Under the same conditions, the former showed better extraction efficiencies over the latter and as a result, it was applied as preconcentration and cleanup step in the analysis of aliphatic hydrocarbons in sediment samples followed by gas chromatography analysis. The linearity of the polytetrafluoroethylene physisorption-assisted emulsification microextraction method was obtained over a range of 3.7 and 2000 ng/g ( R2 > 0.993). The relative standard deviations were less than 6.5% ( n = 3). The limits of detection and quantification obtained by this method were 1.1-9.0 and 3.7-30 ng/g, respectively, indicating that satisfactory results were achieved by the procedure. [ABSTRACT FROM AUTHOR]