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On-Line Solid Phase Extraction – HPLC – Orbitrap Mass Spectrometry for Screening and Quantifying Targeted and Non-Targeted Analytes in Oil Sands Process-Affected Water and Natural Waters in the Athabasca Oil Sands Region Open Access


Author or creator
Pereira, A.S.
Martin, J.W.
Additional contributors
Process Affected Water (OSPW)
Analytical Methods
Naphthenic Acid
Tar Sands
Oil Sands
Type of item
Canada, Alberta, Fort McMurray
In response to mounting evidence of local environmental contamination around the Alberta oil sands industry, the Alberta Environmental Monitoring Panel announced a new world class environmental monitoring program for the Alberta oil sands region in early 2011, and a new monitoring system is now being delivered jointly by the Government of Canada and the Government of Alberta. This new program involves much more frequent sampling of water at many locations around oil sands activity. However, a particular challenge remains that there are currently no proven or validated analytical methods for characterizing the highly complex mixture of organic compounds in bitumen-impacted waters which meet requirements for qualitative and quantitative accuracy, sensitivity, precision, and high throughput. To address this need, an on-line solid phase extraction (SPE) technique was developed for oil sands process-affected water (OSPW), and for natural surface and groundwater samples in the Athabasca oil sands region. The on-line SPE method was connected directly to a high pressure liquid chromatography – Orbitrap mass spectrometry (SPE-HPLC-Orbitrap MS) instrumental system, allowing comprehensive profiling of thousands of dissolved organic compounds, and quantitative analysis of naphthenic acids (NAs), with only 5 mL of a natural water sample. The new method improves upon existing methods by reducing sample volume requirements, eliminating sample preparation time, reducing the possibility of contamination, and increasing the accuracy and precision without sacrificing chromatographic performance, method sensitivity, or method quantitative quality. The new method is anticipated to be useful for high-throughput environmental water monitoring for purposes of current or future environmental compliance by industry, or for forensic source elucidation by monitoring programs and researchers. The method requires a small investment in equipment to setup, but can pay for itself in terms of cost (e.g., solvents and disposable SPEs), and time savings (cost of technician’s time in manual solid phase extraction or other extraction step), not to mention the more precise and higher quality data that are resultant. Considering the capital cost of any HPLC-ultra-high resolution mass spectrometer system (e.g., minimum $600k), it is the opinion of the authors that the minor additional cost of on-line solid phase extraction can be well justified for Provincial and/or Federal water monitoring around oil sands development.
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