Zhang Mengliang, Kruse Natalie A, Bowman Jennifer R, Jackson Glen P
Center for Intelligent Chemical Instrumentation, Clippinger Laboratories, Department of Chemistry and Biochemistry, Ohio University, Athens, Ohio, USA.
Voinovich School of Leadership and Public Affairs, Ohio University, Athens, Ohio, USA.
Appl Spectrosc. 2016 May;70(5):785-93. doi: 10.1177/0003702816638268.
An expedited field analysis method was developed for the determination of polychlorinated biphenyls (PCBs) in soil matrices using a portable gas chromatography-mass spectrometry (GC-MS) instrument. Soil samples of approximately 0.5 g were measured with a portable scale and PCBs were extracted by headspace solid-phase microextraction (SPME) with a 100 µm polydimethylsiloxane (PDMS) fiber. Two milliliters of 0.2 M potassium permanganate and 0.5 mL of 6 M sulfuric acid solution were added to the soil matrices to facilitate the extraction of PCBs. The extraction was performed for 30 min at 100 ℃ in a portable heating block that was powered by a portable generator. The portable GC-MS instrument took less than 6 min per analysis and ran off an internal battery and helium cylinder. Six commercial PCB mixtures, Aroclor 1016, 1221, 1232, 1242, 1248, 1254, and 1260, could be classified based on the GC chromatograms and mass spectra. The detection limit of this method for Aroclor 1260 in soil matrices is approximately 10 ppm, which is sufficient for guiding remediation efforts in contaminated sites. This method was applicable to the on-site analysis of PCBs with a total analysis time of 37 min per sample. However, the total analysis time could be improved to less than 7 min per sample by conducting the rate-limiting extraction step for different samples in parallel.
开发了一种快速现场分析方法,用于使用便携式气相色谱 - 质谱(GC - MS)仪器测定土壤基质中的多氯联苯(PCBs)。用便携式天平称取约0.5 g土壤样品,采用100 µm聚二甲基硅氧烷(PDMS)纤维通过顶空固相微萃取(SPME)提取PCBs。向土壤基质中加入2 mL 0.2 M高锰酸钾和0.5 mL 6 M硫酸溶液,以促进PCBs的提取。在由便携式发电机供电的便携式加热块中于100℃下进行30分钟的提取。便携式GC - MS仪器每次分析耗时不到6分钟,由内置电池和氦气瓶供电。根据GC色谱图和质谱图可对六种商业PCB混合物,即Aroclor 1016、1221、1232、1242、1248、1254和1260进行分类。该方法对土壤基质中Aroclor 1260的检测限约为10 ppm,足以指导污染场地的修复工作。此方法适用于PCBs的现场分析,每个样品的总分析时间为37分钟。然而,通过并行进行不同样品的限速提取步骤,每个样品的总分析时间可缩短至不到7分钟。