Baytak Sıtkı, Arslan Zikri
Department of Chemical Engineering, Faculty of Engineering, Süleyman Demirel University, Isparta 32260, Turkey.
Department of Chemistry and Biochemistry, Jackson State University, Jackson, MS 39217, USA.
Clean (Weinh). 2015 Jun 1;43(6):822-829. doi: 10.1002/clen.201400348.
This study presents a simple, robust and environmentally friendly solid phase preconcentration procedure for multielement determination by inductively coupled plasma optical emission spectrometry (ICP-OES) using diphenylcarbazone (DPC) impregnated TiO nanopowder (-TiO). DPC was successfully impregnated onto -TiO in colloidal solution. A number of elements, including Co(II), Cr(III), Cu(II), Fe(III), Mn(II) and Zn(II) were quantitatively preconcentrated from aqueous solutions between pH 8 and 8.5 at a flow rate of 2 mL min, and then eluted with 2 mL of 5% (v/v) HNO. A mini-column packed with 0.12 g DPC impregnated -TiO retained all elements quantitatively from up to 250 mL multielement solution (2.5 μg per analyte) affording an enrichment factor of 125. The limits of detection (LOD) for preconcentration of 50 mL blank solutions (n = 12) were 0.28, 0.15, 0.25, 0.22, 0.12, and 0.10 μg L for Co, Cr, Cu, Fe, Mn, and Zn, respectively. The relative standard deviation (RSD) for five replicate determinations was 0.8, 3.4, 2.6, 2.2, 1.2 and 3.3% for Co, Cr, Cu, Fe, Mn and Zn, respectively, at 5 μg L level. The method was validated with analysis of Freshwater (SRM 1643e) and Lobster hepatopancreas (TORT-2) certified reference materials, and then applied to the determination of the elements from tap water and lake water samples by ICP-OES.
本研究提出了一种简单、稳健且环境友好的固相预富集方法，用于通过电感耦合等离子体发射光谱法（ICP - OES）使用二苯卡巴腙（DPC）浸渍的TiO纳米粉末（-TiO）进行多元素测定。DPC成功地浸渍到胶体溶液中的-TiO上。包括Co(II)、Cr(III)、Cu(II)、Fe(III)、Mn(II)和Zn(II)在内的多种元素在pH 8至8.5的水溶液中以2 mL min的流速进行定量预富集，然后用2 mL 5%（v/v）的HNO洗脱。填充有0.12 g DPC浸渍的-TiO的微型柱能从高达250 mL的多元素溶液（每种分析物2.5 μg）中定量保留所有元素，富集因子为125。50 mL空白溶液（n = 12）预富集的检测限（LOD）对于Co、Cr、Cu、Fe、Mn和Zn分别为0.28、0.15、0.25、0.22、0.12和0.10 μg L。在5 μg L水平下，Co、Cr、Cu、Fe、Mn和Zn五次重复测定的相对标准偏差（RSD）分别为0.8%、3.4%、2.6%、2.2%、1.2%和3.3%。该方法通过对淡水（SRM 1643e）和龙虾肝胰腺（TORT - 2）有证标准物质的分析进行了验证，然后应用于通过ICP - OES测定自来水和湖水样品中的元素。
