Institute of Chemical Technologies and Analytics, Division of Instrumental Analytical Chemistry, Vienna University of Technology, Getreidemarkt 9/164, 1060 Vienna, Austria.
Talanta. 2013 Jan 15;103:145-52. doi: 10.1016/j.talanta.2012.10.023. Epub 2012 Oct 12.
A novel sample pre-treatment method for multi trace element enrichment from environmental waters prior to optical emission spectrometry analysis with inductively coupled plasma (ICP-OES) is proposed, based on dispersed particle extraction (DPE). This method is based on the use of silica nanoparticles functionalized with strong cation exchange ligands. After separation from the investigated sample solution, the nanoparticles used for the extraction are directly introduced in the ICP for measurement of the adsorbed target analytes. A prerequisite for the successful application of the developed slurry approach is the use of sorbent particles with a mean size of 500 nm instead of commercially available μm sized beads. The proposed method offers the known advantages of common bead-injection (BI) techniques, and further circumvents the elution step required in conventional solid phase extraction procedures. With the use of 14.4 mL sample and addition of ammonium acetate buffer and particle slurry limits of detection (LODs) from 0.03 μg L(-1) for Be to 0.48 μg L(-1) for Fe, with relative standard deviations ranging from 1.7% for Fe and 5.5% for Cr and an average enrichment factor of 10.4 could be achieved. By implementing this method the possibility to access sorbent materials with irreversible bonding mechanisms for sample pre-treatment is established, thus improvements in the selectivity of sample pre-treatment procedures can be achieved. The presented procedure was tested for accuracy with NIST standard reference material 1643e (fresh water) and was applied to drinking water samples from the vicinity of Vienna.
一种新的样品预处理方法,用于环境水样中的多微量元素富集,然后进行电感耦合等离子体(ICP-OES)发射光谱分析,该方法基于分散颗粒萃取(DPE)。该方法基于使用带有强阳离子交换配体的硅胶纳米颗粒。从被测样品溶液中分离后,用于萃取的纳米颗粒直接引入 ICP 中,以测量吸附的目标分析物。成功应用所开发的浆料方法的前提是使用平均粒径为 500nm 的吸附剂颗粒,而不是商业上可用的μm 大小的珠子。所提出的方法具有常见的珠注入(BI)技术的已知优点,并进一步避免了传统固相萃取程序中所需的洗脱步骤。使用 14.4mL 样品,并加入乙酸铵缓冲液和颗粒浆料,检测限(LOD)从 0.03μg/L(Be)到 0.48μg/L(Fe),相对标准偏差(RSD)范围从 1.7%(Fe)到 5.5%(Cr),平均富集因子为 10.4。通过实施该方法,可以实现对具有不可逆键合机制的用于样品预处理的吸附材料的访问,从而可以提高样品预处理程序的选择性。该方法通过对 NIST 标准参考物质 1643e(淡水)进行准确性测试,并应用于维也纳附近的饮用水样品。