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Cadmium And Lead Determination In Freshwater And Hemodialysis Solutions By Thermospray Flame Furnace Atomic Absorption Spectrometry Following Cloud Point Extraction

机译:浊点萃取后热喷雾火焰炉原子吸收光谱法测定淡水和血液透析溶液中的镉和铅

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摘要

Cloud point extraction was employed for the separation and preconcentration of cadmium and lead prior to the determination by thermospray flame atomic absorption spectrometry. Di-2-pyridyl ketone salicyloylhydrazone (DPKSH) was used as complexing agent and the cadmium and lead complexes were extracted from the aqueous phase by the Triton X-114 surfactant. The variables associated with the preconcentration (pH as well as DPKSH, surfactant and electrolyte concentration) were optimized by using a full factorial design with two levels, four variables and a central composite. Under the optimized conditions, a sample volume of 100 μL was introduced into a hot Ti tube at a flow rate of 0.6 mL min-1 and the integrated absorbance was measured. Calibration curves were obtained with linear ranges of 0.075-2.0 μg L-1 (Cd) and 2.5-100 μg L-1 (Pb). The detection limits of 0.04 μg L-1 (Cd) and 1.3 μg L-1 (Pb) (99.7% confidence level) were obtained. The proposed method was applied to hemodialysis solutions and water samples. The accuracy of the method was evaluated by analyzing a certified reference material (NIST CRM 1643e) and the results were in agreement with the certified values at a 95% confidence level according to t-test.
机译:在通过热喷雾火焰原子吸收光谱法测定之前,采用浊点萃取法分离和预富集镉和铅。使用二-2-吡啶基酮水杨酰hydr(DPKSH)作为络合剂,并通过Triton X-114表面活性剂从水相中提取镉和铅络合物。通过使用具有两个水平,四个变量和一个中央复合物的全因子设计,可以优化与预浓缩有关的变量(pH以及DPKSH,表面活性剂和电解质的浓度)。在优化的条件下,将100μL的样品量以0.6 mL min-1的流速引入热Ti管中,并测量积分吸光度。校正曲线的线性范围为0.075-2.0μgL-1(Cd)和2.5-100μgL-1(Pb)。获得的检出限为0.04μgL-1(Cd)和1.3μgL-1(Pb)(99.7%置信度)。该方法适用于血液透析液和水样。通过分析认证的参考物质(NIST CRM 1643e)评估了该方法的准确性,根据t检验,结果与95%置信度下的认证值相符。

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