Vera M Scharek, Jens Pfeifer, Jochen Vogl, Heike Traub, Björn Meermann
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引用次数: 0
Abstract
We report a quantification approach for directly determining total tin and tin-based pollutants/species in sediments via electrothermal vaporization/inductively coupled plasma-mass spectrometry (ETV/ICP-MS) utilizing an on-line isotope dilution mass spectrometry (IDMS) approach. The method was developed and validated using an estuarine sediment reference material (BCR-277R), yielding a recovery of 106%. A relative standard deviation (RSD) of 14%, comparable to published data using a similar method, was obtained. A limit of quantification (LOQ) was estimated at 0.008 mg Sn kg-1 and sufficient for quantifying the total tin mass fraction of surface sediments along the tidal River Elbe course. Hereby, a decrease towards the river mouth, presumably due to dilution effects by less polluted marine sediment, was observed. Besides total tin, monitoring of organotin compounds (OTCs)/species is of interest in sediments due to their toxic effects on aquatic life. The method's capability was extended by separating an OTC fraction in a sediment certified reference material (CRM) through the ETV temperature program. While spiking experiments with OTC standards confirmed the assignment, only a small fraction of the total certified OTC amount (3%), likely due to matrix effects, was recovered. However, applying the method to real-world samples, OTCs were detectable along the River Elbe course. By this, we demonstrated the potential of our method as a complementary fast-screening approach to species-specific analysis procedures.
我们报道了一种利用在线同位素稀释质谱(IDMS)方法,通过电热汽化/电感耦合等离子体质谱(ETV/ICP-MS)直接测定沉积物中总锡和锡基污染物/物质的定量方法。采用河口沉积物标准物质(BCR-277R)开发并验证了该方法,回收率为106%。相对标准偏差(RSD)为14%,与使用类似方法发表的数据相当。定量限(LOQ)估计为0.008 mg Sn kg-1,足以定量易北河潮汐河道表层沉积物的总锡质量分数。因此,观测到向河口方向的减少,可能是由于污染较少的海洋沉积物的稀释作用。除了总锡外,沉积物中有机锡化合物(OTCs)/物种的监测也很有意义,因为它们对水生生物有毒性作用。通过ETV温度程序分离沉淀物认证标准物质(CRM)中的OTC组分,扩展了该方法的功能。虽然使用OTC标准进行的刺钉实验确认了分配,但可能由于基质效应,仅回收了总认证OTC量的一小部分(3%)。然而,将该方法应用于现实世界的样本,可在易北河沿岸检测到otc。通过这一点,我们证明了我们的方法作为一种补充快速筛选方法的潜力,以特定物种的分析程序。
期刊介绍:
Analytical and Bioanalytical Chemistry’s mission is the rapid publication of excellent and high-impact research articles on fundamental and applied topics of analytical and bioanalytical measurement science. Its scope is broad, and ranges from novel measurement platforms and their characterization to multidisciplinary approaches that effectively address important scientific problems. The Editors encourage submissions presenting innovative analytical research in concept, instrumentation, methods, and/or applications, including: mass spectrometry, spectroscopy, and electroanalysis; advanced separations; analytical strategies in “-omics” and imaging, bioanalysis, and sampling; miniaturized devices, medical diagnostics, sensors; analytical characterization of nano- and biomaterials; chemometrics and advanced data analysis.