The measurement of very low concentrations of organic compounds in the environment has been a subject of research for many years. Recently, the sample preparation in the analysis of aqueous samples has been achieved by solid phase microextraction (SPME). This method has been shown to be fast, inexpensive, solventless, portable and automatable. SPME has several advantages over conventional liquid-liquid extraction. SPME has been shown to be a quantitative technique for volatile and semivolatile compounds from gaseous and liquid samples. The quantization by SPME is also linear over four orders of magnitude. As this method can reach a detection limit of 15 ppt (parts per trillion) for several compounds and can be easily automated, the analysis of volatile organic compounds (VOCs) in the environment, in particular, water samples, is highly advantageous by this method. This study will describe the analysis of volatile organics, BTEX, and halogenated organics in water. The lowest limit of detection, linearity, and other parameters will be discussed. The analysis of a soil sample taken near an oil storage tank for VOCs by SPME will be described. A comparison between different fibers (different types of coating materials and film thickness) using different columns will be described in this work.