Petroleum Hydrocarbon contents in tropical soilshas been increasingly recognized as an important soil degradation factor in crude oil producing areas. Hydrocarbon can impact and contaminate the soil apart from playing nutrient inhibition role in the soil. The application of an effective and sensitive analytical method to determine soil contaminants is a crucial step in monitoring and remediation processes. In the present work, we optimized the analysis of Volatile Organic Compounds (VOC) commonly present in fuel: Quantitation of fluorobenzene and monoaromatic hydrocarbons such as Benzene, Toluene, Ethylbenzene and Xylene (BTEX). At impacted locations of Well-Head (WH), Group Gathering Facility (GGF), Group Processing Facility (GPF) and non-impacted sites served as the control. Headspace (HS) and Headspace-Solid Phase Microextraction (HS-SPME) were optimized in water samples, and validated for contaminated soils, using spiked soils. Contaminants were identified and quantified by Gas Chromatography coupled to Mass Spectrometry (GC/MS). Average BTEX (2.50mgkg -1 ) and TPH (4.0mgkg -1 ) were significantly higher in GGF and the concentration was below detection limit in GPF. Examination of regression lines of BTEX and TPH to internal standard on concentration using a least-squares fit demonstrated a linear relationship with correlation coefficients was consistently greater than 0.999 at the impacted sites.