Department of Chemistry, Renewable Natural Resources and Chemistry of Living Environment, University of Jyväskylä, P.O. Box 35, FI-40014, Jyväskylä, Finland.
Department of Chemistry, Renewable Natural Resources and Chemistry of Living Environment, University of Jyväskylä, P.O. Box 35, FI-40014, Jyväskylä, Finland.
Anal Chim Acta. 2019 Dec 27;1092:24-31. doi: 10.1016/j.aca.2019.09.075. Epub 2019 Oct 10.
The determination of ultra-trace concentrations of Hg in natural water samples via preconcentration using 3D printed metal scavenger technique followed by inductively coupled plasma mass spectrometry (ICP-MS) was developed. The determination of Hg in certified reference material ERM-CA615 (groundwater) was performed with high accuracy and precision resulting in recovery of 100 ± 3% and RSD <2.5%, respectively. Selective laser sintering (SLS) 3D printing was used to fabricate the scavengers using a mixture of polyamide-12 powder with thiol-functionalized silica. The preconcentration procedure is based on the adsorption of Hg on the scavenger and followed by elution of the preconcentrated Hg from the filter with 0.3% thiourea in 8% HCl prior to its determination by ICP-MS. A preconcentration factor of 92.8 can be achieved by filtering 495 mL of water followed with the elution step. Very low instrumental detection limit and method detection limit were obtained resulting in 0.013 and 0.037 ng L, respectively. The method was applied successfully for the determination of Hg in different lake and river water samples. The developed method is the first preconcentration method enabling simple and accurate determination of Hg in pg L concentrations in natural waters with ICP-MS.
采用 3D 打印金属清除剂技术预浓缩，随后结合电感耦合等离子体质谱法（ICP-MS），对天然水样中的痕量汞进行了测定。采用该方法对地下水标准参考物质 ERM-CA615 中的汞进行了准确、精密的测定，回收率为 100±3%，相对标准偏差（RSD）小于 2.5%。采用选择性激光烧结（SLS）3D 打印技术，利用混合聚酰胺-12 粉末和巯基功能化二氧化硅来制备清除剂。预浓缩过程基于 Hg 在清除剂上的吸附，然后用 0.3%硫脲在 8%盐酸中从滤器上洗脱预浓缩的 Hg，最后用 ICP-MS 进行测定。通过过滤 495mL 水并进行洗脱步骤，可实现 92.8 的浓缩因子。仪器检测限和方法检测限非常低，分别为 0.013 和 0.037ng/L。该方法成功地应用于不同湖泊和河水样品中 Hg 的测定。所开发的方法是第一个预浓缩方法，可与 ICP-MS 结合，简单、准确地测定天然水中 pg L 浓度的 Hg。
