Research Department, Chemistry Division, United States Navy - Naval Air Systems Command (NAVAIR). Naval Air Warfare Center, Weapons Division (NAWCWD), 1900 N. Knox Road, China Lake, California, 93555, United States.
Research Department, Chemistry Division, United States Navy - Naval Air Systems Command (NAVAIR). Naval Air Warfare Center, Weapons Division (NAWCWD), 1900 N. Knox Road, China Lake, California, 93555, United States.
Chemosphere. 2021 Jun;272:129708. doi: 10.1016/j.chemosphere.2021.129708. Epub 2021 Jan 27.
A rapid method to empirically determine the presence of trace per- and polyfluoroalkyl substances (PFAS) in solid media, such as soils, sands, and sediments, without any sample preparation, through ambient ionization mass spectrometry (MS), is described. 3D-printed cone spray ionization (3D-PCSI) is an ambient ionization technique that employs a 3D-printed conductive plastic cone to perform both sampling and ionization. The 3D-PCSI sources are fabricated in the shape of a hollowed square pyramid to hold bulk matrices, and consist of rigid walls to aid in the uniformity and consistency of sampling and ionization. Solid samples are placed within the hollowed pyramid and a solvent is added to perform an in-situ extraction, followed by spray-based ionization when a voltage is applied. The low cost of 3D-printing, its reproducibility at scale, and lack of sample preparation, enables 3D-PCSI-MS to rapidly and efficiently screen for trace PFAS, in-situ, in bulk samples. Demonstrated here is the detection of trace PFAS that were doped into six different soil and sediment matrices, by 3D-PCSI-MS, to validate the universality of the method, irrespective of matrix composition. All PFAS were identified by their indicative MS spectra and ranged in detection limits from 100 ppt to 10 ppb depending on the compound and soil classification. Legacy aqueous film forming foams (AFFF) were analyzed in soil by 3D-PCSI-MS, as were soil samples collected around an AFFF testing facility. The sampling rate for 3D-PCSI-MS was less than 2 min per sample, demonstrating the applicability to high-throughput mapping of a contaminated area.
描述了一种无需任何样品制备，通过环境电离质谱（MS）在固体介质（如土壤、沙子和沉积物）中快速检测痕量全氟和多氟烷基物质（PFAS）的方法。3D 打印锥形喷雾电离（3D-PCSI）是一种环境电离技术，它使用 3D 打印的导电塑料锥形来进行采样和电离。3D-PCSI 源被制成中空的方锥形，以容纳大块基质，并由刚性壁来帮助采样和电离的均匀性和一致性。将固体样品置于中空的金字塔内，并加入溶剂进行原位提取，然后施加电压进行喷雾电离。3D 打印的低成本、大规模的可重复性以及无需样品制备，使得 3D-PCSI-MS 能够快速高效地原位筛选痕量 PFAS，适用于各种大块样品。这里展示了通过 3D-PCSI-MS 检测掺杂在六种不同土壤和沉积物基质中的痕量 PFAS，验证了该方法的通用性，不受基质组成的影响。所有的 PFAS 都是通过其指示性 MS 谱来识别的，其检测限范围从 100 ppt 到 10 ppb 不等，具体取决于化合物和土壤分类。3D-PCSI-MS 分析了土壤中的legacy 水性成膜泡沫（AFFF），以及在 AFFF 测试设施周围采集的土壤样本。3D-PCSI-MS 的采样速度小于 2 分钟/个样品，证明了其在污染区域高通量测绘中的适用性。
