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Application of low-cost electrothermal vaporization capacitively coupled plasma microtorch optical emission spectrometry for simultaneous determination of Cd and Pb in environmental samples

机译:低成本电热汽化电容耦合等离子体微炬光发射光谱法同时测定环境样品中的镉和铅

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The study discusses the applicability and analytical capability of a laboratory miniaturized system including a small-sized electrothermal vaporizer with Rh filament and a low power (15 W) and low Ar consumption (150 ml min(-1)) capacitively coupled plasma microtorch interfaced with a low resolution microspectrometer for the simultaneous determination of Cd and Pb in environmental samples by optical emission spectrometry. Ten-microliter samples were dried (100 degrees C, 80 s) and vaporized (1500 degrees C, 6 s) by filament heating, then sample vapor was introduced into plasma via an Ar stream and 20 successive emission episodes were recorded with 500 ms integration time per episode. The operating parameters of the electrothermal vaporization device and plasma were optimized in order to achieve the simultaneous determination of the two elements with best analytical performance. The method was verified by analyzing CRMs of soil, and then applied to real samples digested in aqua regia. The standard addition method was used to compensate for the non-spectral matrix effects on the analytical signal. Under the optimized conditions the limits of detection were 130 +/- 35 mu g kg(-1) (13 pg) for Cd at 228.802 nm and 2100 +/- 175 mu g kg(-1) (210 pg) for Pb at 368.346 nm. Recovery was in the range 98 +/- 18% for Cd and 103 11% for Pb for 95% confidence interval, while the relative standard deviation of repeatability was 4-12% (n = 3). The investigated instrumentation has analytical potential and prototyping perspective to be used for toxic element determination in environmental samples. (C) 2015 Elsevier B.V. All rights reserved.
机译:该研究讨论了实验室小型系统的适用性和分析能力,该系统包括带有Rh灯丝和低功率(15 W)和低Ar消耗(150 ml min(-1))的电容耦合等离子体微炬的小型电热蒸发器。一种低分辨率显微光谱仪,用于通过光发射光谱法同时测定环境样品中的Cd和Pb。将十微升样品干燥(100摄氏度,80 s)并通过灯丝加热蒸发(1500摄氏度,6 s),然后通过Ar流将样品蒸汽引入等离子体,并以500 ms积分记录20次连续发射事件每集时间。优化了电热汽化装置和等离子体的操作参数,以便以最佳分析性能同时测定两个元素。该方法通过分析土壤的CRM进行了验证,然后应用于在王水中消化的真实样品。使用标准加法来补偿非光谱矩阵对分析信号的影响。在优化的条件下,对于228.802 nm处的Cd,检测限为130 +/- 35μg kg(-1)(13 pg),对于380 pb处的Pb,检测限为2100 +/- 175μg kg(-1)(210 pg) 368.346 nm。在95%的置信区间内,镉的回收率在98 +/- 18%,铅的回收率在103 11%的范围内,而重复性的相对标准偏差为4-12%(n = 3)。所研究的仪器具有分析潜力和原型设计前景,可用于测定环境样品中的有毒元素。 (C)2015 Elsevier B.V.保留所有权利。

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