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用于测定水样中汞(II)的膜光极

Membrane optode for mercury(II) determination in aqueous samples.

作者信息

Kalyan Y, Pandey A K, Bhagat P R, Acharya R, Natarajan V, Naidu G R K, Reddy A V R

机构信息

Department of Environmental Sciences, S.V. University, Tirupati 517502, India.

出版信息

J Hazard Mater. 2009 Jul 15;166(1):377-82. doi: 10.1016/j.jhazmat.2008.11.027. Epub 2008 Nov 18.

Abstract

A color changeable optode for Hg(II) was prepared by the immobilization of a dye 4-(2-pyridylazo)resorcinol (PAR) and a liquid ion-exchanger trioctylmethylammonium chloride (Aliquat-336) in the tri-(2-ethylhexyl) phosphate plasticized cellulose triacetate matrix. Hg(II) and CH(3)Hg(+) from aqueous samples could be quantitatively preconcentrated in this transparent optode producing a distinct color change (lambda(max)=520 nm) within 5 min equilibration time in bicarbonate aqueous medium or 30 min in natural water. Whereas optode sample without Aliquat-336 did not change its color corresponding to Hg-PAR complex on equilibrium with the same aqueous solution containing Hg(II) ions. The uptake of Hg(II) was found to be pH dependent with a maximum (>90%) at a pH 7.5. The uptake of ions like Cu(II), Fe(II), Zn(II) and Pb(II) was negligible in the optode where as the uptake of Cd(II) and Zn(II) ions was 10-15% at pH 7.5. The optode developed in the present work was studied for its analytical application for Hg(II) in the aqueous samples by spectrophotometry, radiotracer ((203)Hg), Energy Dispersive X-ray Fluorescence (EDXRF) analyses and Instrumental Neutron Activation Analysis (INAA). The minimum amount of Hg(II) required to produce detectable response by spectrophotometry, INAA and EDXRF were found to be 5.5, 1 and 12 microg, respectively. This optode showed a linear increase in the absorbance at lambda(max)=520 nm over a concentration range of 0.22-1.32 microg/mL of Hg(II) ions in aqueous solution for 5 min. The preconcentration of Hg(II) from large volume of aqueous solution was used to extend the lower limit of concentration range that can be quantified by the spectrophotometry of optode. It was observed that preconcentration of 11 microg Hg(II) in 100mL (0.11 microg/mL) in aqueous samples gives a distinct color change and absorbance above 3 sigma of the blank absorbance. The optode developed in the present work was found to be reusable.

摘要

通过将染料4-(2-吡啶偶氮)间苯二酚(PAR)和液体离子交换剂三辛基甲基氯化铵(Aliquat-336)固定在磷酸三(2-乙基己基)酯增塑的三醋酸纤维素基质中,制备了一种用于Hg(II)的颜色可变光极。水样中的Hg(II)和CH(3)Hg(+)可在这种透明光极中进行定量预浓缩,在碳酸氢盐水溶液介质中5分钟平衡时间内或天然水中30分钟内产生明显的颜色变化(λmax = 520 nm)。而没有Aliquat-336的光极样品在与含有Hg(II)离子的相同水溶液平衡时,不会因Hg-PAR络合物而改变颜色。发现Hg(II)的摄取量与pH有关,在pH 7.5时摄取量最大(>90%)。在该光极中,Cu(II)、Fe(II)、Zn(II)和Pb(II)等离子的摄取量可忽略不计,而Cd(II)和Zn(II)离子在pH 7.5时的摄取量为10 - 15%。通过分光光度法、放射性示踪剂((203)Hg)、能量色散X射线荧光(EDXRF)分析和仪器中子活化分析(INAA),研究了本工作中开发的光极对水样中Hg(II)的分析应用。发现通过分光光度法、INAA和EDXRF产生可检测响应所需的Hg(II)的最小量分别为5.5、1和12μg。该光极在水溶液中Hg(II)离子浓度范围为0.22 - 1.32μg/mL时,在λmax = 520 nm处的吸光度在5分钟内呈线性增加。从大量水溶液中预浓缩Hg(II)用于扩展可通过光极分光光度法定量的浓度范围的下限。观察到在100mL水样中预浓缩11μg Hg(II)(0.11μg/mL)会产生明显的颜色变化,吸光度高于空白吸光度的3σ。发现本工作中开发的光极可重复使用。

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