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分散液液微萃取-原子荧光光度法测定大米中的汞
引用本文:陆建平,覃梦琳,布静龙,邓扬辉,童张法.分散液液微萃取-原子荧光光度法测定大米中的汞[J].光谱学与光谱分析,2017,37(11):3606-3609.
作者姓名:陆建平  覃梦琳  布静龙  邓扬辉  童张法
作者单位:广西石化资源加工及过程强化技术重点实验室,广西大学化学化工学院,广西 南宁 530004
基金项目:广西大学大学生实验技能和科技创新能力训练基金项目,广西石化资源加工及过程强化技术重点实验室主任课题基金项目,国家自然科学基金项目
摘    要:硝酸-高氯酸(4∶1,V/V)混合酸消解样品。双硫腙为络合剂,乙醇为分散剂,四氯化碳为萃取剂,建立了分散液液微萃取-原子荧光光度法测定大米中的汞的方法。优化了原子荧光光度计工作参数和分散液液微萃取的最佳络合酸度、络合剂用量、萃取剂种类及用量等条件。实验表明,在最佳条件下,方法的线性范围为0.005~25 μg·L-1,相关系数为0.996 6,检出限为0.003 μg·L-1,相对标准偏差为3.84%,加标回收率为90%~120%。该方法灵敏度高,分析速度快,准确性高,能有效检测大米中的痕量汞。

关 键 词:大米  原子荧光光谱法  分散液液微萃取  双硫腙    
收稿时间:2015-06-16

Determination of Mercury in Rice with Dispersive Liquid-Liquid Microextraction and Atomic Fluorescence Spectrometry
LU Jian-ping,QIN Meng-lin,BU Jing-long,DENG Yang-hui,TONG Zhang-fa.Determination of Mercury in Rice with Dispersive Liquid-Liquid Microextraction and Atomic Fluorescence Spectrometry[J].Spectroscopy and Spectral Analysis,2017,37(11):3606-3609.
Authors:LU Jian-ping  QIN Meng-lin  BU Jing-long  DENG Yang-hui  TONG Zhang-fa
Institution:Guangxi Key Laboratory of Petrochemical Resource Processing and Process Intensification Technology, College of Chemistry and Chemical Engineering, Guangxi University, Nanning 530004, China
Abstract:Rice samples were digested by a mixture of nitric and perchloric acids (4 : 1,V/V ).Dithizone was used to chelate mercury ion in the sample solution,and the mercury complex was dispersed in ethanol before being extracted into carbon tetra-chloride.Thus,a method of determining mercury in rice by dispersion liquid micro extraction-atomic fluorescence spectrometry was established.The operating parameters of the instrument and optimal experimental conditions of dispersive liquid-liquid mi-croextraction were optimized,including the best complex acidity,the amount of complexing agent,extraction solvent type,the amount of dispersant dosage,and the extraction time.Experiments showed that under optimal conditions,the linear range was 0.005~25 μg·L-1 and the correlation coefficient was 0.9966 with the detection limit of 0.003 μg·L-1 ,the relative standard deviation (RSD)of 3.84%,and the recovery 95%~105% .The method is proven to be a sensitive,rapid,and accurate,way which can detect effectively trace amounts of mercury in rice.
Keywords:Rice  Atomic fluorescence spectrometry  Liquid-liquid microextraction  Dithizone  Mercury
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