荧光光谱法测定二氧化硫脲
Fluorospectrophotometric Determination of Thiourea Dioxide
摘 要
在碱性加热的条件下,二氧化硫脲将没有荧光效应的硝基苯还原为具有较强荧光效应的苯胺,且苯胺的荧光强度与二氧化硫脲的浓度成线性关系.据此,提出了荧光光谱法测定二氧化硫脲的方法.优化的试验条件如下:① 反应溶液的酸度为pH 9.6;② 1.000 g·L-1硝基苯溶液的用量为2 mL;③ 反应温度为70 ℃;④ 加热时间为15 min.二氧化硫脲的质量浓度在0.06~1.2 mg·L-1范围内与其荧光强度呈线性关系,方法的检出限(3s/k)为3.1 μg·L-1.以合成水样为基体进行加标回收试验,所得回收率在93.3%~107%之间.
二氧化硫脲
苯胺
Fluorospectrophotometry
Thiourea dioxide
Aniline
Abstract
In the presence of heat and alkaline condition,thiourea dioxide is reduced into nitrobenzene without fluorescent effect and into aniline with strong fluorescent effect. Based on this fact,a fluorospectrophotometric method for the determination of thiourea dioxide was proposed. The optimized conditions found are as follows:① acidity of reaction solution:pH 9.6;② amount of 1.000 g·L-1 nitrobenzene solution:2 mL;③ temperature of reaction:70 ℃;④ time of heating:15 min. Linear relationship between values of fluorescence intensity and mass concentration of thiourea dioxide was kept in the range of 0.06-1.2 mg·L-1,with detection limit (3s/k) of 3.1 μg·L-1. On the base of synthetic sample of water,test for recovery was made by standard addition method;values of recovery found were in the range of 93.3%-107%.
中图分类号 O657.3
所属栏目 试验与研究
基金项目 广东省高校产学研基地重大项目(PT2011QH);省科技计划(2012A030600006)
收稿日期 2014/2/9
修改稿日期
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作者单位点击查看
联系人作者余倩(yuqgdut@126.com)
备注余倩(1964-),女,湖南常德人,教授,博士,研究方向为应用化学.
引用该论文: YU Qian,BI Ming-fang,SHEN Li-si,YU Lin,TAN Xu-kun. Fluorospectrophotometric Determination of Thiourea Dioxide[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(2): 142～145
余倩,毕明芳,沈丽斯,余林,谭旭坤. 荧光光谱法测定二氧化硫脲[J]. 理化检验－化学分册, 2015, 51(2): 142～145
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【5】黄晖,李丽,马乔,等.表面活性剂增敏荧光光度法测定牛奶中的三聚氰胺[J].分析化学,2010,38(2):249-252.
【6】任乃林,郭祥群.荧光光度法测定鱼肉中的氧氟沙星残留[J].食品科学,2007,28(8):386-389.
【7】方艳芬,黄应平,罗光富,等.荧光光度法测定雨水中的H2O2含量[J].光谱学与光谱分析,2008,28(4):917-921.
【8】GARCIA M D G,GALLEGOS A B,VALVERDE R S,et al. Determination of (fluoro) quinolones in environmental water using online preconcentration with column switching linked to large sample volumes and fluorescence detection[J]. Journal of Separation Science,2012,35(7):823-831.
【9】孙振艳,赵中一,郭小慧,等.荧光分析法测定维生素C[J].化学分析计量,2006,15(4):18-20.
【10】王艳.荧光分析法测定桑叶中总黄酮含量的研究[J].中国酿造,2008(6):90-91.
【11】CHEN Zhi-jun,WANG Li-min,ZOU Gang,et al. Highly selective fluorescence turn-on chemosensor based on naphthalimide derivatives for detection of copper(Ⅱ) ions[J]. Spectrochimica Acta Part A:Molecular and Biomolecular Spectroscopy,2013,105:57-61.
【12】GUI Ri-jun,AN Xue-qin,HUANG Wen-xue. An improved method for ratiometric fluorescence detection of pH and Cd2+ using fluorescein isothiocyanate-quantum dots conjugates[J]. Analytica Chimica Acta,2013,767:134-140.
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