分散液液微萃取-能量色散X射线荧光光谱法测定环境水样中的痕量铜
Determination of trace copper in environmental water samples by dispersive liquid-liquid microextraction and energy dispersive X-ray fluorescence spectroscopy
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摘要: 本文采用分散液液微萃取（DLLME）技术来分离富集环境水样中痕量铜，结合薄样技术，利用能量色散-X射线荧光光谱仪（ED-XRF）对其进行检测.实验以二乙基二硫代氨基甲酸钠（DDTC）为螯合剂，对萃取剂、分散剂的种类及体积、螯合剂的用量、pH值、萃取时间等影响实验萃取效率的因素进行了优化，得出在50μL四氯化碳，0.4 mL甲醇，pH=8，DDTC质量分数为0.03%，萃取时间3 min的条件下进行实验，萃取效率最佳.实验采用内标法进行定量，检出限为0.08μg·L-1，对两种实际样品进行6次平行检测，相对标准偏差（RSD）分别为3.1%和3.3%，加标回收率为97%-105%.因此本方法适用于环境水样中铜含量的检测.Abstract: A novel method based on dispersive liquid-liquid microextraction (DLLME) and energy-dispersive X-ray fluorescence spectroscopy (ED-XRF) with thin sample technology for the preconcentration and determination of Cu(Ⅱ) in environmental water samples was developed. In the present study, sodium diethyldithiocarbamate (DDTC) was used as the chelating agent. A series of influence factors relevant to the microextraction efficiency including the type and volume of extractant and disperser solvent, the concentration of chelating reagents, pH and extraction time were optimized. The best condition was obtained as follows:50 μL carbon tetrachloride, 0.4 mL methanol, pH=8, DDTC mass fraction of 0.03% and extraction time of 3 min. The quantitative analysis was evaluated by the internal standard method under the optimal conditions, the recoveries were in the range of 97%-105% along with the detection limit of 0.08 μg·L-1. The repeatability of the developed method was also evaluated by six parallel tests for two actual samples with the relative standard deviation (RSD) of 3.1% and 3.3%, respectively. The developed method can be applied in the determination of trace copper in environmental water samples.
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