Development of an industrial standard method for Total Petroleum Hydrocarbon (TPH) analysis

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1 Development of an industrial standard method for Total Petroleum Hydrocarbon (TPH) analysis Vasilios G. Samaras

2 Topics of presentation Introduction Aim of the Project Project Outline First Results and Discussion Conclusions Future Research

3 Definition of Petroleum Hydrocarbons All Aromatic Hydrocarbon compounds which contain between 10 and 40 carbon atoms are associated with the release of a petroleum product to the environment Gasoline Range Organics (GRO): C6 C10 (volatile aromatic and aliphatic hydrocarbons) Diesel Range Organics (DRO): C8 C30 (aliphatic and aromatic hydrocarbons including the 16 EPA PAHs) Extended Diesel Range Organics (EDRO): C10 C40 (contains some of the lubricating oil fraction)

4 Total Petroleum Hydrocarbon analysis Various methods Gravimetric IR (Infrared spectroscopy) UVF (Ultraviolet fluorescence) GC/FID GC/MS Limitations of the TPH analysis Lack of standardisation No comparable results between laboratories Limited scope of the existing methods Detection limits of the current methodologies don t reach the national legislation limit Table 1. Main parameters of the existing predominant analytical methods

5 Aim of the project Develop, optimize and validate a standard method for TPH analysis to be used in the environmental laboratories and industry Simple, Fast and Precise analytical method Applicable for waste, surface, ground and seawater Low detection limits ( mg/l<) Cost effective Environmental friendly Attractive for both National regulators and the industry

6 Originality of the project Many analytical methods are available for the determination of the target compounds but none applicable for all types of water (waste, surface, ground and seawater) at the low microgram per liter level (mg/l)

7 Analytical plan A typical analytical method proceeds with the following steps: Collection and preservation requirements specific to environmental matrix and analytes of interest Extraction seperates the analytes of interest from the sample matrix Cleanup may be necessary to remove interfering compounds Measurement quantifies the analytes Each step affects the final result, and a basic understanding of the steps is vital to data interpretation

8 Project Outline

9 First results and Discussion

10 Evaluation of the existing method ISO Targets compounds: hydrocarbon fractions from C10 to C40 range

11 Extraction efficiency of different organic solvents at three ph levels Fig. Mean absolute recoveries (percent, n=3) of the target compounds at different ph values of the loading solution (0.5 L) with 10 ml of extraction solvent.

12 Extraction efficiency of Dichloromethane

13 Conclusions Research to date has included a review of current methodologies and trends for the TPH analysis in water. Limitations of each existing method were identified and a new analytical plan was developed. This review was aimed at clarifying the elution efficiency of different organic solvents used for the extraction of TPH and the effect of the ph of the loading solution (acidic or neutral) on the extraction efficiency

14 Future Research The next step in this project includes the testing of different analytical parameters affecting the quality of results: Surface water Seawater Wastewater Groundwater Spiking with different concentrations of mineral oil (low, medium and high concentrations of hydrocarbons) Testing different volumes of water sample and extraction solvent Adsorbent selection (Florisil, silica gel, alumina) Matrix interference Validation

15 Thank you for your attention Vasilios Samaras Contact details T.E. Laboratories Ltd Tullow, Co. Carlow, Ireland Tel (0) Fax +353 (0)

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