用对磺基苯亚甲基硫代若丹宁为显色剂固相萃取光度法测定环境样品中痕量汞
Solid Phase Extraction-Photometric Determination of Trace Amount of Mercury in Environmental Samples with p-Sulfobenzylidene Thiorhodanine
摘 要
合成了新试剂对磺基苯亚甲基硫代若丹宁(SBDTR),并用红外光谱、核磁共振氢谱和元素分析鉴定其结构.试验表明:在pH 3.5的HOAc-NaOAc缓冲介质中,吐温-80存在下,SBDTR与汞反应生成2∶1稳定络合物,该络合物可被Waters Sep-Pak C18固相萃取小柱固相萃取,用乙醇洗脱后在乙醇介质中,在此络合物的吸收峰550 nm波长处测定其吸光度.体系的摩尔吸光率为8.42×104L·mol-1·cm-1.汞的质量浓度在0.1~4.0 mg·L-1范围内符合比耳定律,应用于河水及食品试样中汞的测定,所得结果与原子吸收光谱法的测定结果相符.
对磺基苯亚甲基若丹宁
汞
光度法
环境样品
Solid phase extraction
Photometry
p-Sulfobenzylidenethio-rhodanine
Mercury(Ⅱ)
Environmental samples
Abstract
A new chromogenic reagent,namely p-sulfobenzylidene thiorhodanine (abbreviated as SBDTR) was synthesized and its molecular structure verified by elemental analysis,IR spectrometry and 1HNMR. It was found that in an acetate buffer medium of pH 3.5 and in the presence of Tween-80,a stable complex was formed between SBDTR and Hg(Ⅱ) in the mole ratio of 2 to 1. The complex formed was extracted on the Waters Sep-Pak C18 solid-phase extraction (SPE) mini-column and eluted with a definite amount of ethanol. The eluate was collected in a microabsorption cell and its absorbance measured at its absorption maxima 550 nm. Beer′s law was held in the range of 0.1-4.0 mg of Hg(Ⅱ) per liter of solution. Molar absorptivity of the reaction system was found to be 8.42×104L·mol-1·cm-1. Several samples of river water and foodstuff were analyzed by the proposed method,giving results in comformity with the results obtained by AAS.
中图分类号 O657.31
所属栏目 试验与研究
基金项目
收稿日期 2007/3/6
修改稿日期
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备注司超(1985-),男,云南昆明人,研究方向为应用化学及分析化学.
引用该论文: SI Chao,LI Hai-tao,TAI Xi,YIN Jia-yuan,HU Qiu-fen. Solid Phase Extraction-Photometric Determination of Trace Amount of Mercury in Environmental Samples with p-Sulfobenzylidene Thiorhodanine[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2008, 44(1): 8～11
司超,李海涛,台希,尹家元,胡秋芬. 用对磺基苯亚甲基硫代若丹宁为显色剂固相萃取光度法测定环境样品中痕量汞[J]. 理化检验－化学分册, 2008, 44(1): 8～11
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参考文献
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【3】王亮,陶溶溶,杨光宇,等.新试剂5-(3-甲基-2-吡啶)亚甲基若丹宁光度法测定汞的研究[J].干旱环境监测,1998,12(4):197-198．
【4】汪朝存,哈成勇.4,4′-对偶氮苯重氮氨基偶氮苯与汞(Ⅱ)的显色反应及其应用[J].化学通报,2000,63(4):44-46．
【5】胡秋芬,杨光宇,尹家元.对磺酸基苯亚甲基若丹宁固相萃取光度法测定水中的汞[J].分析试验室,2002,21(4):93-95．
【6】周艳梅,李丽清,王贵方,等.汞-2-(3,5-二氯-2-吡啶偶氮)-5-二甲氨基苯酚-OP显色体系的应用[J].冶金分析,2000,20(1):38-40 ．
【7】张海霞,邓华,刘满仓,等.用于固相萃取的聚乙二醇交联辛烷基、苯基、氨基和氰基固定相[J].分析化学,2001,28(9):1172-1180．
【8】谷学新,邹红,朱若华.分析化学中的分离技术[J].分析试验室,2001,20(3):96-108．
【9】胡秋芬,杨光宇,汤丹俞,等.2-(2-喹啉偶氮)-5-二乙氨基苯甲酸固相萃取光度法测定环境水样中的镍[J].分析化学,2002,30(6):563-565．
【10】Yang G Y,Dong X C,Hu Q F,et al. Solid phase extratration and spectrophotometric determination of cobalt with QADMAB[J]. Anal Lett,2002,35:1735-1745．
【11】杨亚玲,胡秋芬,杨光宇,等.2-(2-吡啶偶氮)-5-二甲氨基酚固相萃取光度法测定饮用水中铜[J].光谱实验室,2002,19(4):544-546．
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