Herein, a chelating sorbent that employs magnetic nanoparticles (MNPs) functionalized with 1,5-bis(di-2-pyridyl)methylene thiocarbohydrazide (DPTH-MNPs) has been used to develop a simple method for the analysis of trace amounts of metal ions present in environmental samples; the method combines on-line magnetic solid phase extraction (MSPE) with atomic spectrometry. Thus, a flow injection FI-MSPE/cold vapour generation system coupled to an inductively coupled plasma optical emission spectrometry (ICP OES) method for the determination of trace amounts of noble metals, platinum group elements (PGEs: Ir, Pd, Pt, Os, and Rh), and Au and Ag in environmental samples has been developed. A magnet-based reactor designed to contain DPTH-MNPs was placed in the injection valve of the FI manifold. Several chemical and flow variables were considered as factors in the optimization process using two central composite designs; with the optimized method, the experimental detection limits for simultaneous determination, calculated as the concentration of analyte giving signals equivalent to three times the standard deviation of the blank plus the net blank intensity (LOD, peak height), were 1.5 μg L⁻¹, 0.03 μg L⁻¹, 0.65 μg L⁻¹, 0.62 μg L⁻¹, 0.57 μg L⁻¹, 0.03 μg L⁻¹, and 100 μg L⁻¹ for Pd, Ag, Os, Au, Ir, Pt, and Rh, respectively. The method offers relatively good precision (RSD 1.8–7.2%). The accuracy of the proposed method was verified using certified reference materials (CMRs, NIST 2557 autocatalyst, TMDA 54.4 fortified lake water, and SRM 1643e trace elements in fresh water) and by determining the analyte contents in spiked aqueous samples. Sea water and tap water samples obtained from Malaga (Spain) were also analysed. The determined values were in good agreement with the certified values, and the recoveries for the spiked samples were in the range of 91.8–108.1%. Additionally, the proposed method was applied in the simultaneous determination of the abovementioned 7 elements with a sample throughput of about 17 h⁻¹, thereby reducing the time of analysis and the volumes of reagents and sample required.

中文翻译：

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磁性SPE ICP OES和原位化学气相生成法同时测定痕量的Pt，Pd，Os，Ir，Rh，Ag和Au金属

在本文中，已使用采用被1,5-双（二-2-吡啶基）亚甲基硫代碳酰肼（DPTH-MNPs）官能化的磁性纳米颗粒（MNP）的螯合吸附剂来开发分析痕量金属离子的简单方法存在于环境样品中；该方法将在线磁固相萃取（MSPE）与原子光谱法结合在一起。因此，流动注射FI-MSPE /冷蒸气发生系统与电感耦合等离子体发射光谱法（ICP OES）耦合，用于测定痕量的贵金属，铂族元素（PGEs：Ir，Pd，Pt，Os ，以及Rh），以及环境样品中的Au和Ag。设计为包含DPTH-MNP的基于磁体的反应器放置在FI歧管的注入阀中。在使用两个中央复合设计的优化过程中，一些化学和流量变量被视为因素。使用优化的方法，用于同时测定的实验检测极限为1.5μgL，计算出的分析物浓度等于空白标准偏差加空白净净强度（LOD，峰高）的三倍。^-1，0.03微克大号^-1，0.65微克大号^-1，0.62微克大号^-1，0.57微克大号^-1，0.03微克大号^-1，和100μg大号^-1分别用于Pd，Ag，Os，Au，Ir，Pt和Rh。该方法提供了相对较好的精度（RSD 1.8–7.2％）。使用认证的参考材料（CMR，NIST 2557自动催化剂，TMDA 54.4强化湖水和淡水中的SRM 1643e微量元素）并通过测定加标水样中的分析物含量，可以验证所提出方法的准确性。还分析了从马拉加（西班牙）获得的海水和自来水样品。测定值与认证值非常吻合，加标样品的回收率在91.8-108.1％的范围内。另外，将所提出的方法应用于上述7种元素的同时测定，样品通量约为17 h ^-1，从而减少了分析时间以及所需的试剂和样品量。