硫化物/金纳米粒子应用于汞离子光谱分析的研究
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摘要
汞是对人类具有严重生理毒性的化学元素之一。水体中的汞可由食物链在生物有机体内蓄积,对人类健康造成极大威胁。因此,对环境样品中汞离子(Hg~(2+))的检测是评估环境质量的重要指标之一,开发具有高选择性、高灵敏度、低成本且简单易行的Hg~(2+)分析方法成为关注焦点和研究热点。
纳米材料所具备的独特性质可望满足构建功能传感器的基本要求,如功能广、灵敏度高、响应速度快、检测范围宽、选择性好、稳定性好等等。本文用简便的方法制备了几种粒子形态的纳米材料,并成功用于Hg~(2+)的光谱分析。所用方法简便、快速、灵敏度高且对汞离子有很好的选择性,应用于环境样品中汞离子测定不需要对样品进行特殊的前处理。其主要内容如下:
(1)利用DNA作为模板,采用交替透析-层层组装的方法在水溶液中合成了CdS纳米颗粒(~5 nm),同时应用于Hg~(2+)的光分析测定。利用透射电镜、紫外可见光谱、荧光光谱和共振光散射光谱进行了系统表征,所合成的目标物分散性良好,在394 nm附近表现出强烈共振散射峰和339 nm处具有特征的荧光发射峰。更有趣的是,体系光散射的增强和荧光的淬灭程度与Hg~(2+)浓度之间有良好的线性,这归结于Hg-S键的生成。经过优化条件,该传感器在0.01-100μmol/L Hg~(2+)浓度范围内成良好的线性关系,最低检测浓度可达10-9 mol/L,且对Hg~(2+)具有很好选择性。?
(2)在室温下以柠檬酸三钠为稳定剂,采用相似的方法在水相中分别合成了CuS和PbS纳米粒子,并探索了合成条件,如不同浓度Cu~(2+)或Pb~(2+)与S2-的配比和不同pH值。所制备的纳米粒子的共振光散射(RLS)光谱强度(IRLS)的变化与不同浓度的Hg~(2+)加入直接相关。结果表明,在最佳实验条件下,CuS和PbS体系的IRLS分别对c(Hg~(2+))在0.01-100μmol/L和0.001-100μmol/L区间内呈现出良好的线性变化,据此建立了水中的微量汞的测定方法。
(3)酸性介质中氯化亚锡与Hg~(2+)反应可生成金属汞(Hg),金溶胶存在时,Hg可与金纳米粒子表面作用形成纳米复合物,体系在395 nm处的最大共振散射峰强度IRLS响应与体系Hg~(2+)浓度相关。由此实现了共振光散射法测定水中的微量汞,在0.1-50μmol/L浓度范围内与光散射强度的变化成正比,其线性回归方程的相关系数为0.991,检出限可达0.068μmol/L。
Mercury is one of the most toxic elements on human beings and higher organisms. Soluble mercury can enter the human body from the food chain and accumulate in human body, resulting in great harm to human health. Therefore, mercury ions analysis of environmental samples is one of the most important indicators to assess environmental quality. The development of Hg~(2+) sensor of high selectivity, high sensitivity, low cost and simple operation has become research focus.
The unique nature of nano-materials is expected to meet the basic requirements for building a sensor, such as extensive function, high sensitivity, fast response, wide detection range, good selectivity and good stability and so on. In this paper, several forms of nano- material have been prepared by means of simple methods, and successfully applied to the spectral analysis for Hg~(2+). These methods that applied to the determination of mercury ion in environmental samples are simple, rapid, high sensitivity for mercury ions analysis, and do not require a special pre-treatment. The major contents are as follows:
(1) Based on DNA as a template, CdS nanoparticles (~5 nm) has been synthesized in aqueous solution using alternate dialysis and layer-by-layer assembly method, and is applied to spectral analysis of Hg~(2+). The resultant well-dispersed CdS nanoparticles present a strong ?uorescence peak at 339 nm and RLS bands around 394 nm, which is characterized by TEM, UV-vis, ?uorescence and resonance light scattering (RLS) spectra. Interestingly, it was found that the quenching of ?uorescence and the enhancing of RLS intensity are strongly dependent on the concentration of Hg~(2+), which is due to the forming of Hg-S bond. In optimized conditions, the sensor show a good linear relationship over the range of 0.01-100μM, with a remarkable low detection limit as low as ~ 1 nm, and show a good selectivity to mercury ions.
(2) Using citrate as a stabilizing agent at room temperature, we synthesize CuS and PbS nanoparticles in aqueous phase via a similar method. And the synthetic conditions under different pH values and the ratio of sodium sulfide and copper sulfate or lead sulfate on concentration have been studied. The intensity change of resonance light scattering (IRLS) of nano-particles as-prepared directly relates to different concentrations of Hg~(2+). We have studied the effects of RLS between CuS or PbS nanoparticles and mercury ions under the conditions of different pH values and the different ratio of sodium sulfide and copper sulfate or lead sulfate on concentration. The results show that in the optimum experimental conditions, the IRLS of CuS and PbS corresponding to c(Hg~(2+)) has a good linearity in the range of 0.01-100μM and 0.001-100μM seperately. Thus, the method of determine trace mercury in water is established.
(3) SnCl_2 can react with the Hg~(2+) to form metal mercury in acid medium, and metal mercury react with gold nanoparticles once again to form nanocomposites, which has a maximum RLS peak at 395nm. According to these phenomena, the trace mercury in the water was determined by RLS technique. Experiments showed that the change of RLS intensity (IRLS) against the nanocomposites is proportional to the concentration of Hg~(2+) in the range of 0.1-50μmol/L. The correlation coefficient of linear equations is 0.991 with the detection limit of 0.068μmol/L.
纳米材料所具备的独特性质可望满足构建功能传感器的基本要求,如功能广、灵敏度高、响应速度快、检测范围宽、选择性好、稳定性好等等。本文用简便的方法制备了几种粒子形态的纳米材料,并成功用于Hg~(2+)的光谱分析。所用方法简便、快速、灵敏度高且对汞离子有很好的选择性,应用于环境样品中汞离子测定不需要对样品进行特殊的前处理。其主要内容如下:
(1)利用DNA作为模板,采用交替透析-层层组装的方法在水溶液中合成了CdS纳米颗粒(~5 nm),同时应用于Hg~(2+)的光分析测定。利用透射电镜、紫外可见光谱、荧光光谱和共振光散射光谱进行了系统表征,所合成的目标物分散性良好,在394 nm附近表现出强烈共振散射峰和339 nm处具有特征的荧光发射峰。更有趣的是,体系光散射的增强和荧光的淬灭程度与Hg~(2+)浓度之间有良好的线性,这归结于Hg-S键的生成。经过优化条件,该传感器在0.01-100μmol/L Hg~(2+)浓度范围内成良好的线性关系,最低检测浓度可达10-9 mol/L,且对Hg~(2+)具有很好选择性。?
(2)在室温下以柠檬酸三钠为稳定剂,采用相似的方法在水相中分别合成了CuS和PbS纳米粒子,并探索了合成条件,如不同浓度Cu~(2+)或Pb~(2+)与S2-的配比和不同pH值。所制备的纳米粒子的共振光散射(RLS)光谱强度(IRLS)的变化与不同浓度的Hg~(2+)加入直接相关。结果表明,在最佳实验条件下,CuS和PbS体系的IRLS分别对c(Hg~(2+))在0.01-100μmol/L和0.001-100μmol/L区间内呈现出良好的线性变化,据此建立了水中的微量汞的测定方法。
(3)酸性介质中氯化亚锡与Hg~(2+)反应可生成金属汞(Hg),金溶胶存在时,Hg可与金纳米粒子表面作用形成纳米复合物,体系在395 nm处的最大共振散射峰强度IRLS响应与体系Hg~(2+)浓度相关。由此实现了共振光散射法测定水中的微量汞,在0.1-50μmol/L浓度范围内与光散射强度的变化成正比,其线性回归方程的相关系数为0.991,检出限可达0.068μmol/L。
Mercury is one of the most toxic elements on human beings and higher organisms. Soluble mercury can enter the human body from the food chain and accumulate in human body, resulting in great harm to human health. Therefore, mercury ions analysis of environmental samples is one of the most important indicators to assess environmental quality. The development of Hg~(2+) sensor of high selectivity, high sensitivity, low cost and simple operation has become research focus.
The unique nature of nano-materials is expected to meet the basic requirements for building a sensor, such as extensive function, high sensitivity, fast response, wide detection range, good selectivity and good stability and so on. In this paper, several forms of nano- material have been prepared by means of simple methods, and successfully applied to the spectral analysis for Hg~(2+). These methods that applied to the determination of mercury ion in environmental samples are simple, rapid, high sensitivity for mercury ions analysis, and do not require a special pre-treatment. The major contents are as follows:
(1) Based on DNA as a template, CdS nanoparticles (~5 nm) has been synthesized in aqueous solution using alternate dialysis and layer-by-layer assembly method, and is applied to spectral analysis of Hg~(2+). The resultant well-dispersed CdS nanoparticles present a strong ?uorescence peak at 339 nm and RLS bands around 394 nm, which is characterized by TEM, UV-vis, ?uorescence and resonance light scattering (RLS) spectra. Interestingly, it was found that the quenching of ?uorescence and the enhancing of RLS intensity are strongly dependent on the concentration of Hg~(2+), which is due to the forming of Hg-S bond. In optimized conditions, the sensor show a good linear relationship over the range of 0.01-100μM, with a remarkable low detection limit as low as ~ 1 nm, and show a good selectivity to mercury ions.
(2) Using citrate as a stabilizing agent at room temperature, we synthesize CuS and PbS nanoparticles in aqueous phase via a similar method. And the synthetic conditions under different pH values and the ratio of sodium sulfide and copper sulfate or lead sulfate on concentration have been studied. The intensity change of resonance light scattering (IRLS) of nano-particles as-prepared directly relates to different concentrations of Hg~(2+). We have studied the effects of RLS between CuS or PbS nanoparticles and mercury ions under the conditions of different pH values and the different ratio of sodium sulfide and copper sulfate or lead sulfate on concentration. The results show that in the optimum experimental conditions, the IRLS of CuS and PbS corresponding to c(Hg~(2+)) has a good linearity in the range of 0.01-100μM and 0.001-100μM seperately. Thus, the method of determine trace mercury in water is established.
(3) SnCl_2 can react with the Hg~(2+) to form metal mercury in acid medium, and metal mercury react with gold nanoparticles once again to form nanocomposites, which has a maximum RLS peak at 395nm. According to these phenomena, the trace mercury in the water was determined by RLS technique. Experiments showed that the change of RLS intensity (IRLS) against the nanocomposites is proportional to the concentration of Hg~(2+) in the range of 0.1-50μmol/L. The correlation coefficient of linear equations is 0.991 with the detection limit of 0.068μmol/L.
引文
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