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Cloud Point Extraction for Electroanalysis: Anodic Stripping Voltammetry of Cadmium

机译:用于电分析的浊点萃取:镉的阳极溶出伏安法

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摘要

Cloud point extraction (CPE) is a well-established technique for the pre-concentration of hydrophobic species from water without the use of organic solvents. Subsequent analysis is then typically performed via atomic absorption spectroscopy (AAS), UV-Vis spectroscopy, or high performance liquid chromatography (HPLC). However, the suitability of CPE for electroanalytical methods such as stripping voltammetry has not been reported. We demonstrate the use of CPE for electroanalysis using the determination of cadmium (Cd2+) by anodic stripping voltammetry (ASV) as a representative example. Rather than using the chelating agents which are commonly used in CPE to form a hydrophobic, extractable metal complex, we used iodide and sulfuric acid to neutralize the charge on Cd2+ to form an extractable ion pair. Triton X-114 was chosen as the surfactant for the extraction because its cloud point temperature is near room temperature (22–25° C). Bare glassy carbon (GC), bismuth-coated glassy carbon (Bi-GC), and mercury-coated glassy carbon (Hg-GC) electrodes were compared for the CPE-ASV. A detection limit for Cd2+ of 1.7 nM (0.2 ppb) was obtained with the Hg-GC electrode. Comparison of ASV analysis without CPE was also investigated and a 20x decrease (4.0 ppb) in the detection limit was observed. The suitability of this procedure for the analysis of tap and river water samples was also demonstrated. This simple, versatile, environmentally friendly and cost-effective extraction method is potentially applicable to a wide variety of transition metals and organic compounds that are amenable to detection by electroanalytical methods.
机译:浊点萃取(CPE)是一种行之有效的技术,用于在不使用有机溶剂的情况下从水中预富集疏水性物质。然后通常通过原子吸收光谱(AAS),紫外-可见光谱或高效液相色谱(HPLC)进行后续分析。但是,尚未报道CPE适用于电分析方法(如溶出伏安法)。我们通过阳极溶出伏安法(ASV)测定镉(Cd 2 + )证明了CPE在电分析中的应用。我们使用碘化物和硫酸中和Cd 2 + 上的电荷以形成可萃取的离子对,而不是使用CPE中通常使用的螯合剂形成疏水的可萃取金属络合物。选择Triton X-114作为萃取的表面活性剂,因为其浊点温度接近室温(22–25°C)。比较了CPE-ASV的裸玻碳(GC),铋涂覆的玻碳(Bi-GC)和汞涂覆的玻碳(Hg-GC)电极。用Hg-GC电极测得Cd 2 + 的检出限为1.7 nM(0.2 ppb)。还对不使用CPE的ASV分析进行了比较,观察到检出限降低了20倍(4.0 ppb)。还证明了该方法适用于分析自来水和河水样品。这种简单,通用,环保且具有成本效益的提取方法可能适用于各种可通过电分析方法检测的过渡金属和有机化合物。

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