In a forensic investigation involving oil, a comparative analysis named oil spill fingerprinting between a source and an oil spill is normally performed. It is based on detecting a certain selection of biomarkers with gas chromatography (GC) coupled to mass spectrometry (MS) which are later divided into diagnostic ratios (DRs). An international guideline formed by European Committee for Standardization (CEN) denoted CEN/TR 15522-2:2012 describes the process of conducting oil spill fingerprinting. This method is currently being inspected and adjusted for standardization into EN 15522-2:2022. One section of the upcoming standard describes sample clean-up which is important to inhibit possible matrix effect that could either enhance or reduce peak intensity in the chromatogram. There is yet no conclusive SPE (Solid Phase Extraction) protocol in the current draft version of EN 15522-2:2022. The aim with this study was to develop such a protocol. Development included comparative testing of the recommended stationary phases silica and Florisil®. Additionally, the effect of both elution solvent and elution volume were investigated. The protocol must pass validation criteria to be implemented at National Forensic Centre (NFC) and possibly be used in the final version of EN 15522-2:2022. A successful method for Heavy Fuel Oil (HFO), diesel and lubricating oil was achieved with activated Florisil® as stationary phase, eluted with 6 ml dichloromethane (DCM). If the evidence material is suspected to contain FAMEs (Fatty Acid Methyl Esters), then 2 % acetone should be added to the DCM. The final SPE column was packed with 0.5 glass wool, 4 cm Florisil® and 0.5 cm sodium sulfate. Based on successful validation result, the SPE protocol should be considered for the final version of EN 15522-2:2022 as well as for implementation at NFC.

After Deepwater Horizon oil reached the Florida coast, oil was buried in Pensacola Beach (PB) sands to ~ 70 cm depth, resulting in Total Petroleum Hydrocarbon (TPH) concentrations up to ~ 2 kg per meter of beach. This study followed the decomposition of the buried oil and the factors influencing its degradation. The abundance of bacteria in oiled sand increased by 2 orders of magnitude within one week after oil burial, while diversity decreased by ~ 50%. Half-lives of aliphatic and aromatic hydrocarbons reached 25 and 22 days, respectively. Aerobic microbial oil decomposition, promoted by tidal pumping, and human cleaning activities effectively removed oil from the beach. After one year, concentrations of GC-amenable hydrocarbons at PB were similar to those in the uncontaminated reference beach at St. George Island/FL, and microbial populations that disappeared after the oil contamination had reestablished. Yet, oxihydrocarbons can be found at PB to the present day.

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The oil from the Exxon Valdez incident is still observed in different Prince William Sound beaches over two decades. The persisting oil is slightly weathered and highly toxic to the environment. Several studies investigated the reasons for lingering oil. Different remediation techniques were tried and the results were not satisfactory. Recently, it was found that the oil is stranded in a low permeability layer. Detailed explorations showed that the exchange of the nutrients and oxygen is limited in this layer. The main objective of the present study is to explain the effect of oxygen and nutrients on the degradation phenomena in the Alaskan beaches. The general approach for this study is a combination of the field experiments and lab analysis. As it is important to eliminate any cross-layer contamination, a unique sampling method was developed. The applied method involves collecting samples from the oily layer (low permeability layer), measuring oxygen levels in the field and comparing them with the nutrient samples analyzed in the lab. The findings showed that the nutrients levels were low in the beach but the lack of effective electron acceptor is the major factor limiting the biodegradation of the oil. The seawater is responsible for delivering the oxygen and nutrients to the beach during the high tide while during low tide the landward freshwater discharges to the beach. The study of the sulfate and nitrate in the beach revealed that the levels of the alternative electron acceptors were not sufficient to support anaerobic biodegradation. Finally, for successful biodegradation of the Exxon Valdez oil, adequate levels of nutrients (nitrogen and phosphorous) and along with oxygen are required. / Civil Engineering