Mutschler Anna, Stock Vivian, Ebert Lena, Björk Emma M, Leopold Kerstin, Lindén Mika
Department of Inorganic Chemistry II, Ulm University, Albert-Einstein-Allee 11, 89081 Ulm, Germany.
Department of Analytical and Bioanalytical Chemistry, Ulm University, Albert-Einstein-Allee 11, 89081 Ulm, Germany.
Nanomaterials (Basel). 2018 Dec 28;9(1):35. doi: 10.3390/nano9010035.
Trace-level detection of mercury in waters is connected with several complications including complex multistep analysis routines, applying additional, harmful reagents increasing the risk of contamination, and the need for expensive analysis equipment. Here, we present a straightforward reagent-free approach for mercury trace determination using a novel thin film sampling stick for passive sampling based on gold nanoparticles. The nanoparticles supported on a silicon wafer and further covered with a thin layer of mesoporous silica. The mesoporous silica layer is acting as a protection layer preventing gold desorption upon exposure to water. The gold nanoparticles are created by thermal treatment of a homogenous gold layer on silicon wafer prepared by vacuum evaporation. This gold-covered substrate is subsequently covered by a layer of mesoporous silica through dip-coating. Dissolved mercury ions are extracted from a water sample, e.g., river water, by incorporation into the gold matrix in a diffusion-controlled manner. Thus, the amount of mercury accumulated during sampling depends on the mercury concentration of the water sample, the accumulation time, as well as the size of the substrate. Therefore, the experimental conditions can be chosen to fit any given mercury concentration level without loss of sensitivity. Determination of the mercury amount collected on the stick is performed after thermal desorption of mercury in the gas phase using atomic fluorescence spectrometry. Furthermore, the substrates can be re-used several tens of times without any loss of performance, and the batch-to-batch variations are minimal. Therefore, the nanogold-mesoporous silica sampling substrates allow for highly sensitive, simple, and reagent-free determination of mercury trace concentrations in waters, which should also be applicable for on-site analysis. Successful validation of the method was shown by measurement of mercury concentration in the certified reference material ORMS-5, a river water.
水体中汞的痕量检测存在诸多复杂问题,包括复杂的多步分析流程、使用额外的有害试剂增加污染风险以及需要昂贵的分析设备。在此,我们展示了一种直接的无试剂方法,用于使用基于金纳米粒子的新型薄膜采样棒进行汞的痕量测定。纳米粒子负载在硅片上,并进一步覆盖有一层介孔二氧化硅薄层。介孔二氧化硅层起到保护层的作用,防止金在接触水时解吸。金纳米粒子是通过对通过真空蒸发制备的硅片上的均匀金层进行热处理而产生的。随后通过浸涂法在该金覆盖的基底上覆盖一层介孔二氧化硅。溶解的汞离子通过扩散控制的方式掺入金基质中,从而从水样(如河水)中被提取出来。因此,采样过程中积累的汞量取决于水样中的汞浓度、积累时间以及基底的尺寸。所以,可以选择实验条件以适应任何给定的汞浓度水平而不损失灵敏度。在使用原子荧光光谱法对气相中的汞进行热解吸后,测定采样棒上收集的汞量。此外,基底可以重复使用几十次而性能无任何损失,且批次间差异极小。因此,纳米金 - 介孔二氧化硅采样基底能够实现对水体中汞痕量浓度的高灵敏度、简单且无试剂的测定,这也应适用于现场分析。通过测量经认证的参考物质ORMS - 5(一种河水)中的汞浓度,表明了该方法的成功验证。