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首页> 外文期刊>Analytical Sciences >Thermospray Flame Furnace-AAS Determination of Copper after On-line Sorbent Preconcentration Using a System Optimized by Experimental Designs
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Thermospray Flame Furnace-AAS Determination of Copper after On-line Sorbent Preconcentration Using a System Optimized by Experimental Designs

机译:实验设计优化的系统在线热富集-热喷雾火焰炉-AAS法测定铜

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The present paper describes the on-line coupling of a flow-injection system to a new technique, thermospray flame furnace-AAS (TS-FF-AAS), for the preconcentration and determination of copper in water samples. Copper was preconcentrated onto polyurethane foam (PUF) complexed with ammonium O,O-diethyldithiophosphate (DDTP), while elution was performed using 80% (v/v) ethanol. An experimental design for optimizing the copper preconcentration system was established using a full factorial (24) design without replicates for screening and a Doehlert design for optimization, studying four variables: sample pH, ammonium O,O-diethyldithiophosphate (DDTP) concentration, presence of a coil and the sampling flow rate. The results obtained from the full factorial and based on a Pareto chart indicate that only the pH and the DDTP concentration, as well as their interaction, exert influence on the system within a 95% confidence level. The proposed method provided a preconcentration factor of 65 fold, thus notably improving the detectability of TS-FF-AAS. The detection limit was 0.22 µg/dm3 and the precision, expressed as the relative standard deviation (RSD) for eight independent determinations, was 2.7 and 1.1 for copper solutions containing 5 and 30 µg/dm3, respectively. The procedure was successfully applied for copper determination in water samples.
机译:本文介绍了一种流动注射系统与热喷雾火焰炉AAS(TS-FF-AAS)的新技术的在线耦合,该技术用于水样品中铜的预浓缩和测定。将铜预浓缩到与O,O-二乙基二硫代磷酸铵(DDTP)络合的聚氨酯泡沫(PUF)上,同时使用80%(v / v)乙醇进行洗脱。建立了用于优化铜预浓缩系统的实验设计,其中使用了不进行重复筛选的全因子设计(24)设计和用于优化的Doehlert设计,研究了四个变量:样品pH,O,O-O-二乙基二硫代磷酸(DDTP)浓度,线圈和采样流量。从全因子分析并基于帕累托图获得的结果表明,只有pH和DDTP浓度及其相互作用在95%的置信度内对系统产生影响。所提出的方法提供了65倍的预富集因子,从而显着提高了TS-FF-AAS的可检测性。检出限为0.22 µg / dm3,用8个独立测定的相对标准偏差(RSD)表示的精密度,对于含5和30 µg / dm3的铜溶液,分别为2.7和1.1。该程序已成功应用于水样中铜的测定。

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