In the present work, a simple, rapid and economic sample pre-treatment technique, low density miniaturized homogeneous liquid-liquid extraction (LDMHLLE), was developed for determination of polycyclic aromatic hydrocarbons (PAH) and total petroleum hydrocarbons (TPH) in sediment samples. The LDMHLLE method is based on the homogeneous liquid-liquid extraction with methanol containing n-hexane as a solvent of lower density than water that after addition of water forms a distinct water immiscible phase at the top of the vial. This phase can be easily separated and injected to the gas chromatography with flame ionization detector (GC-FID) instrument for quantification. The linearity was obtained in the concentration range of 0.100-100.00 and 0.030-100.00 mg g-1 for PAH and TPH, respectively. Correlation coefficients were better than 0.99 to for PAH and TPH. The limit of detection (LOD), based on the signal-to-noise ratio (S/N), was 0.010-0.060 mg g-1 for PAH and 0.008 mg g-1 for TPH. The relative recoveries of PAH and TPH for sediment samples at spiking level of 10.0 mg g-1 were 57-92 and 91%, respectively. The method was successfully applied to corresponding standard reference material, CRM372-100 for TPH and CRM CNS391-050 for PAH.
PAH; TPH; gas chromatography-flame ionization detector; LDMHLLE; preconcentration
