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Dispersive micro solid-phase extraction (DµSPE) with graphene oxide as adsorbent for sensitive elemental analysis of aqueous samples by laser induced breakdown spectroscopy (LIBS)
Talanta ( IF 6.1 ) Pub Date : 2018-08-18 , DOI: 10.1016/j.talanta.2018.08.044
F.J. Ruiz , L. Ripoll , M. Hidalgo , A. Canals

In this work, the combination of dispersive micro solid-phase extraction (DµSPE) with laser-induced breakdown spectroscopy (LIBS) was evaluated for simultaneous preconcentration and detection of Zn, Cd, Mn, Ni, Cr and Pb in aqueous samples. Two adsorbent materials were tested in the microextraction step, namely graphene oxide and activated carbon. In both cases, the microextraction process consisted in the dispersion of a small quantity of adsorbent in the sample solution containing the analytes. However, while the use of activated carbon required a previous chelation of the metals, this step was avoided with the use of graphene oxide. After extraction, the analytes retained in the adsorbents were analysed by LIBS. Several experimental factors affecting the extraction of the metals (adsorbent amount, pH and extraction time) were optimized by means of the traditional univariate approach. Under optimum microextraction conditions, the analytical features of the proposed DµSPE-LIBS methods were assessed, leading to limits of detection below 100 µg kg−1 and 50 µg kg−1 with the use of activated carbon and graphene oxide, respectively, as adsorbents in the DµSPE process. Trueness evaluation of the most sensitive procedure was carried out by spike and recovery experiments in a real sample of tap water, leading to recovery values in the range 98–110%.



中文翻译:

氧化石墨烯作为吸附剂的分散微固相萃取(DµSPE),用于通过激光诱导击穿光谱法(LIBS)进行水样品的敏感元素分析

在这项工作中,评估了分散微固相萃取(DµSPE)与激光诱导击穿光谱法(LIBS)的组合,用于同时预富集和检测水性样品中的Zn,Cd,Mn,Ni,Cr和Pb。在微萃取步骤中测试了两种吸附材料,即氧化石墨烯和活性炭。在两种情况下,微萃取过程都在于将少量吸附剂分散在含有分析物的样品溶液中。但是,尽管使用活性炭需要事先将金属螯合,但使用氧化石墨烯避免了该步骤。提取后,通过LIBS分析保留在吸附剂中的分析物。影响金属提取的几种实验因素(吸附剂的量,pH和提取时间)是通过传统的单变量方法进行优化的。在最佳微萃取条件下,对提出的DµSPE-LIBS方法的分析特性进行了评估,导致检测限低于100 µg kg-1和50 µg kg -1在DµSPE工艺中分别使用活性炭和氧化石墨烯作为吸附剂。通过在真实自来水样本中进行加标和回收实验对最敏感程序的真实性评估,得出回收率在98-110%的范围内。

更新日期:2018-08-18
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