Hughes Sarah A, Huang Rongfu, Mahaffey Ashley, Chelme-Ayala Pamela, Klamerth Nikolaus, Meshref Mohamed N A, Ibrahim Mohamed D, Brown Christine, Peru Kerry M, Headley John V, Gamal El-Din Mohamed
Shell Health - Americas, Shell Oil Company, 910 Louisiana Street, Houston, TX 77002, USA; Department of Biological Sciences, University of Alberta, Edmonton, AB, T6G 1H9, Canada; Department of Forestry and Environmental Conservation, Clemson University, Clemson, SC, 29634, USA.
Department of Civil and Environmental Engineering, University of Alberta, Edmonton, AB, T6G 1H9, Canada.
Chemosphere. 2017 Nov;187:376-384. doi: 10.1016/j.chemosphere.2017.08.123. Epub 2017 Aug 23.
There are several established methods for the determination of naphthenic acids (NAs) in waters associated with oil sands mining operations. Due to their highly complex nature, measured concentration and composition of NAs vary depending on the method used. This study compared different common sample preparation techniques, analytical instrument methods, and analytical standards to measure NAs in groundwater and process water samples collected from an active oil sands operation. In general, the high- and ultrahigh-resolution methods, namely high performance liquid chromatography time-of-flight mass spectrometry (UPLC-TOF-MS) and Orbitrap mass spectrometry (Orbitrap-MS), were within an order of magnitude of the Fourier transform infrared spectroscopy (FTIR) methods. The gas chromatography mass spectrometry (GC-MS) methods consistently had the highest NA concentrations and greatest standard error. Total NAs concentration was not statistically different between sample preparation of solid phase extraction and liquid-liquid extraction. Calibration standards influenced quantitation results. This work provided a comprehensive understanding of the inherent differences in the various techniques available to measure NAs and hence the potential differences in measured amounts of NAs in samples. Results from this study will contribute to the analytical method standardization for NA analysis in oil sands related water samples.
有几种既定方法可用于测定与油砂开采作业相关的水中的环烷酸（NAs）。由于其性质高度复杂，NAs的测量浓度和组成会因所用方法的不同而有所变化。本研究比较了不同的常见样品制备技术、分析仪器方法和分析标准，以测量从一个活跃的油砂作业中采集的地下水和工艺水样品中的NAs。一般来说，高分辨率和超高分辨率方法，即超高效液相色谱飞行时间质谱（UPLC - TOF - MS）和轨道阱质谱（Orbitrap - MS），与傅里叶变换红外光谱（FTIR）方法的测量结果在一个数量级范围内。气相色谱质谱（GC - MS）方法测得的NAs浓度始终最高，且标准误差最大。固相萃取和液液萃取的样品制备方法之间，总NAs浓度在统计学上没有差异。校准标准会影响定量结果。这项工作全面了解了用于测量NAs的各种技术的内在差异，以及因此样品中NAs测量量的潜在差异。本研究结果将有助于油砂相关水样中NA分析的分析方法标准化。
