光散射法检测环境水样中的镉、铜、铅离子含量
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摘要
光散射分析技术源于二十世纪九十年代,历经了十多年的发展,它因其操作简单、灵敏度高、分析速度快等优点已被越来越多的化学工作者所学习和使用。当前该技术被广泛应用于化学分析检测领域,如重金属离子、生物大分子、表面活性剂及药物等分析检测。本文利用共振光散(?)(?)(Resonance Light Scattering, RLS)强度显著增强,对环境水样中的镉(Ⅱ)和铜(Ⅱ)含量进行了测定。此外,我们对F-7000荧光分光光度计进行了光路改装,使得原来的直角散射变为近180°后向光散射,同时利用该技术建立了铅(Ⅱ)检测的新方法。主要研究内容如下：
(1)在pH6.8 Britton-Robinson(BR)缓冲介质中,镉(Ⅱ)与邻菲啰啉(Phen)作用后与全氟辛烷磺酸(PFOS)形成离子缔合物,使体系的共振光散射信号显著增强。最大散射峰位于307.0 nm处,其增强散射信号强度与镉(Ⅱ)的浓度在6.0-342.5ng·mL-1范围内成线性关系,据此建立了测定镉(Ⅱ)含量的共振光散射分析方法,检出限为0.6 ng·mL-1,研究了反应产物的RLS光谱特征,适宜的反应条件和影响因素,考察了共存物质的影响。该方法用于自来水和实验室废水样中镉(Ⅱ)的测定,RSD≤4.4%。
(2)在pH 5.4 HAc-NaAc缓冲介质中,铜(Ⅱ)与桑色素(Morin)通过配位作用结合后能显著增强共振光散射(Resonance Light Scattering, RLS)信号,最大散射波长位于295.0 nm处,增强散射信号强度与铜(Ⅱ)浓度在0.08～12.0μmol/L范围内呈良好线性关系,据此建立了测定铜(Ⅱ)的散射分析方法,检测限为8.2 nmol/L。考查了体系的最佳反应条件及外来物质干扰,研究了体系紫外吸收光谱及荧光光谱,并讨论了反应机理。该方法用于自来水及嘉陵江水中铜(Ⅱ)含量测定,RSD≤4.5%。
(3)实验发现在pH值为4.56的Britton-Robinson (B-R)缓冲溶液中,环丙沙星(CIP)与刚果红(CR)及铅离子通过静电引力和疏水作用形成离子缔合物,导致近180°后向光散射(Backward Light Scattering,BLS)信号显著增强,最大散射波长位于399 nm处,增强的散射信号强度与Pb(Ⅱ)浓度在0.5～60.0μmol/L范围内呈线性关系,据此建立了测定Pb(Ⅱ)的后向散射分析方法,检测限为50nmol/L。研究了体系的近180°后向光散射光谱和吸收及荧光光谱,并讨论了体系反应机理,通过BLS实验测定了体系适宜反应条件及外来物质的干扰。所建立的BLS方法用于环境水样及合成样品中Pb(Ⅱ)的测定,其回收率在91.0-104.0%之间,RSD≤4.7%。
Light scattering has been studied and used by a growing number of chemical workers for its simple operation, high sensitivity and rapid analysis from 1990s. At present, the technique is widely used in the field of chemical analysis, such as detection of heavy metal ions, biological macromolecules, surface active agents and pharmaceuticals. In this dissertation, the resonance light scattering intensity significantly enhanced, which were used to determination the content of cadmium (II) and copper (Ⅱ) in environmental water samples. In addition, we modified the light path from right angle scattering to the nearly 180°Backward light scattering on F-7000 fluorescence spectrophotometer. A nevol nearly 180°backward light scattering technique has been established for detection of lead(Ⅱ). The main contents are as follows:
(1) In pH 6.8 Britton-Robinson(BR) buffer medium, a resonance light scattering (RLS) analytical method of cadmium (Ⅱ) was established based on the enhanced RLS signal due to the interaction of PFOS and chelate ion derived from the reaction between cadmium (Ⅱ) and phenanthorline (Phen). The enhanced RLS intensity at 307.0 nm is proportional to the content of cadmium (Ⅱ) in a range of 6.0-342.5 ng·mL-1. The limit of detection is 0.6 ng·mL-1. In this work, the optimum reaction conditions and the interference of foreign substances were investigated. This method has been successfully applied to determination of cadmium (Ⅱ) in tap water and laboratory waste water samples with RSD≤4.4%.
(2) In pH 5.4 HAc-NaAc buffer medium, copper (Ⅱ) and Morin through the combination of complexation significantly enhanced resonance light scattering signals. The enhanced RLS intensity at 295.0 nm is proportional to the content of copper (Ⅱ) in a range of 0.08～12.0μmol/L. The limit of detection is 8.2 nmol/L. In this work, the optimum reaction conditions and the interference of foreign substances of the system were investigated. The absorption and fluorescence spectra of the system as well as the reaction mechanism were also discussed. This method has been successfully applied to the determination of copper (Ⅱ) in tap water and river water. The RSD is less than 4.5%.
(3) A novel BLS method for the determination of lead (Ⅱ) has been developed base on the largely enhanced BLS signal at 399.0 nm due to the interaction of Ciprofloxacin (CIP), Congo red (CR) and lead ions by electrostatic forces and hydrophobic interactions to form ion-association complex in the pH 4.56 Britton-Robinson (BR) medium. The linear range of lead (Ⅱ) is 0.5～60.0μmol/L. The limit of detection (LOD) is 50 nmol/mL. In this work, the nearly 180°backward light scattering spectral, absorption and fluorescence have been studied, then discussed the system of reaction mechanism and using the backward light scattering investigated the appropriate reaction conditions, interference of foreign substances reaction mechanism. This method has been applied successfully for the determination of lead (Ⅱ) in environmental water samples and synthetic samples, the recovery between 91.0%～104.0%, RSD≤4.7%.
(1)在pH6.8 Britton-Robinson(BR)缓冲介质中,镉(Ⅱ)与邻菲啰啉(Phen)作用后与全氟辛烷磺酸(PFOS)形成离子缔合物,使体系的共振光散射信号显著增强。最大散射峰位于307.0 nm处,其增强散射信号强度与镉(Ⅱ)的浓度在6.0-342.5ng·mL-1范围内成线性关系,据此建立了测定镉(Ⅱ)含量的共振光散射分析方法,检出限为0.6 ng·mL-1,研究了反应产物的RLS光谱特征,适宜的反应条件和影响因素,考察了共存物质的影响。该方法用于自来水和实验室废水样中镉(Ⅱ)的测定,RSD≤4.4%。
(2)在pH 5.4 HAc-NaAc缓冲介质中,铜(Ⅱ)与桑色素(Morin)通过配位作用结合后能显著增强共振光散射(Resonance Light Scattering, RLS)信号,最大散射波长位于295.0 nm处,增强散射信号强度与铜(Ⅱ)浓度在0.08～12.0μmol/L范围内呈良好线性关系,据此建立了测定铜(Ⅱ)的散射分析方法,检测限为8.2 nmol/L。考查了体系的最佳反应条件及外来物质干扰,研究了体系紫外吸收光谱及荧光光谱,并讨论了反应机理。该方法用于自来水及嘉陵江水中铜(Ⅱ)含量测定,RSD≤4.5%。
(3)实验发现在pH值为4.56的Britton-Robinson (B-R)缓冲溶液中,环丙沙星(CIP)与刚果红(CR)及铅离子通过静电引力和疏水作用形成离子缔合物,导致近180°后向光散射(Backward Light Scattering,BLS)信号显著增强,最大散射波长位于399 nm处,增强的散射信号强度与Pb(Ⅱ)浓度在0.5～60.0μmol/L范围内呈线性关系,据此建立了测定Pb(Ⅱ)的后向散射分析方法,检测限为50nmol/L。研究了体系的近180°后向光散射光谱和吸收及荧光光谱,并讨论了体系反应机理,通过BLS实验测定了体系适宜反应条件及外来物质的干扰。所建立的BLS方法用于环境水样及合成样品中Pb(Ⅱ)的测定,其回收率在91.0-104.0%之间,RSD≤4.7%。
Light scattering has been studied and used by a growing number of chemical workers for its simple operation, high sensitivity and rapid analysis from 1990s. At present, the technique is widely used in the field of chemical analysis, such as detection of heavy metal ions, biological macromolecules, surface active agents and pharmaceuticals. In this dissertation, the resonance light scattering intensity significantly enhanced, which were used to determination the content of cadmium (II) and copper (Ⅱ) in environmental water samples. In addition, we modified the light path from right angle scattering to the nearly 180°Backward light scattering on F-7000 fluorescence spectrophotometer. A nevol nearly 180°backward light scattering technique has been established for detection of lead(Ⅱ). The main contents are as follows:
(1) In pH 6.8 Britton-Robinson(BR) buffer medium, a resonance light scattering (RLS) analytical method of cadmium (Ⅱ) was established based on the enhanced RLS signal due to the interaction of PFOS and chelate ion derived from the reaction between cadmium (Ⅱ) and phenanthorline (Phen). The enhanced RLS intensity at 307.0 nm is proportional to the content of cadmium (Ⅱ) in a range of 6.0-342.5 ng·mL-1. The limit of detection is 0.6 ng·mL-1. In this work, the optimum reaction conditions and the interference of foreign substances were investigated. This method has been successfully applied to determination of cadmium (Ⅱ) in tap water and laboratory waste water samples with RSD≤4.4%.
(2) In pH 5.4 HAc-NaAc buffer medium, copper (Ⅱ) and Morin through the combination of complexation significantly enhanced resonance light scattering signals. The enhanced RLS intensity at 295.0 nm is proportional to the content of copper (Ⅱ) in a range of 0.08～12.0μmol/L. The limit of detection is 8.2 nmol/L. In this work, the optimum reaction conditions and the interference of foreign substances of the system were investigated. The absorption and fluorescence spectra of the system as well as the reaction mechanism were also discussed. This method has been successfully applied to the determination of copper (Ⅱ) in tap water and river water. The RSD is less than 4.5%.
(3) A novel BLS method for the determination of lead (Ⅱ) has been developed base on the largely enhanced BLS signal at 399.0 nm due to the interaction of Ciprofloxacin (CIP), Congo red (CR) and lead ions by electrostatic forces and hydrophobic interactions to form ion-association complex in the pH 4.56 Britton-Robinson (BR) medium. The linear range of lead (Ⅱ) is 0.5～60.0μmol/L. The limit of detection (LOD) is 50 nmol/mL. In this work, the nearly 180°backward light scattering spectral, absorption and fluorescence have been studied, then discussed the system of reaction mechanism and using the backward light scattering investigated the appropriate reaction conditions, interference of foreign substances reaction mechanism. This method has been applied successfully for the determination of lead (Ⅱ) in environmental water samples and synthetic samples, the recovery between 91.0%～104.0%, RSD≤4.7%.
引文
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