顺序注射阀上实验室电化学联用技术在痕量镉分析中的应用
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摘要
顺序注射-阀上实验室作为流动注射的第三代技术,有着全自动进样、进样体积大小可以灵活改变、仪器简单、使用方便等优点,易于实现在线检测。而电化学分析方法则有着灵敏度高、分析速度快、成本低等优点。将顺序注射-阀上实验室与电化学方法联用,在保留了各自优点的同时,使得常规电分析的繁琐过程变得简单,分析频率大大增加,同时实现了分析的全自动化,在电化学样品分析领域有着很大的应用前景。本文以顺序注射-阀上实验室为平台,采用不同的电化学技术对环境样品中的重金属镉进行了测定,主要研究内容包括以下三个部分：
设计加工了适当的阀上实验室-电化学检测流通池,将三电极整合加工到阀内,以pH为4.7的醋酸-醋酸钠缓冲溶液为支持电解质,可更新汞膜碳糊电极为工作电极,采用顺序注射-阀上实验室-微分脉冲阳极溶出伏安法实现了对重金属镉的快速测定。在最佳的实验条件下,峰电流与镉的浓度在5.0-75.0μg/L范围呈良好的线性关系,检出限为0.41μg/L,对浓度为20μg/L的试液11次重复测量的相对标准偏差为2.8%,分析频率为30/h。该方法仪器简单,样品和试剂消耗量低,操作快速。
本实验以低毒的Nafion-铋膜电极为工作电极,在自行设计的阀上实验室-电化学检测流通池内完成了对痕量镉的测定。研究了镉在0.10 mol/L的醋酸-醋酸钠缓冲溶液中溶出行为。结果表明,Nafion膜能够有效提高电子转移速率,铋膜能够有效提高镉的检出限。在最佳的实验条件下,镉的浓度在2.0-100μg/L范围内与峰电流成良好的线性关系,检出限为0.23μg/L,对浓度为50μg/L的镉溶液11次重复测量的相对标准偏差为1.72%,分析频率为45/h。通过将顺序注射-阀上实验室-阳极溶出伏安法联用,提高了检测频率,降低了常规滴汞电极由于汞的使用而带来的污染,实现了实验过程操作的全自动化。
本文首次采用顺序注射-阀上实验室系统-吸附溶出伏安法测定了工业废水中的镉,该方法快速且灵敏。样品和试剂通过柱塞泵进入检测器,镉离子在修饰电极表面富集,然后通过阳极溶出伏安法实现了对镉离子的定量。对实验中一系列的参数进行了优化,在100s的富集时间内,镉在1.0-125.0μg/L范围内与峰电流成线性关系,检出限为0.41μg/L,对25.0μg/L的镉进行重复测定,其RSD为2.70%,分析频率为27/h,运用该方法对样品进行检测,结果与ICP-OES相一致,结果令人满意。
Sequential injection lab-on-valve as the third generation flow injection technology, with automatic sample injection, volume size can be flexible to change; equipment simple, easy to use, which achieved determination procee on line. The electrochemical analysis method is with high sensitivity and analysis speed, low cost and so on merit. The sequential injection lab on valve combined with electrochemical analysis methods, retaining the advantages of each method, at the same time which making the conventional electrochemical analysis become simple, greatly increased the frequency of analysis, and achieving a fully automated analysis process. It will have great prospects in the future in the analysis field. In this paper, we used sequential injection lab on valve combined with electrochemical analysis techniques to detect the heavy metals in environmental samples; the main research includes about three parts:
Sequential rejection lab-on-valve (LOV) using renewnal mercuy film electrode was first proposed for analyzing Cd coupled with differential pulse anodic stripping voltammetry (DPASV). The electrochemical flow cell including three electrodes was designed as a part of the selection valve of the SIA (sequential injection apparatus). Under the optimal parameters, the response was linear in the concentration range from 5.0 to 75.0μg/L along with a sampling frequency of 30/h, and a detection limit of 0.41μg/L was obtained with a precision of 2.8% RSD at the level of 20μg/L. The total processing was carried out in a closed ehannel system. The established analytical procedure enhanced the repeatability and minimized sample and reagent consumption. The practical applicability was demonstrated by determination of Cd in environmental water samples.
This work exploited a sequential injection lab-on-valve (LOV) system for the determination of cadmium by anodic stripping voltammetry (ASV). A miniaturized electrochemical flow cell (EFC) was fabricated in LOV, in which a nafion coated bismuth film electrode was used as working electrode. The cadmium was electrodeposited on the electrode surface with bismuth solution, and measured with the subsequential stripping scan. Under optimal conditions, the proposed system responded linearly to cadmium concentrations in a range 2.0-100.0μg/L. The detection limit of this method was found to be 0.88μg/L. By loading a sample volume of 800μL, a sampling frequency of 25 determinations h-1 was achieved. The repeatability expressed as relative standard derivation (R.S.D.) was 3.65% for 20μg/L cadmium (n= 11). The method was applied to analysis of trace cadmium in environmental water samples and the spiked recoveries were satisfactory. By combining sequential injection lab on valve with anodic stripping voltammetry which increased testing frequency, reducing the conventional dropping mercury electrode as the use of mercury pollution caused by the experimental process. At the same time it achieves full automation.
A rapid and sensitive adsorptive stripping voltammetric assay for the determination of trace amount of cadmium was developed in a sequential injection lab-on-valve (SI-LOV) system for the first time. The sample and reagent arrangements were achieved by a syringe pump. The target metal ions were accumulated on the morin modified glassy carbon electrode surface, and the quantification step was performed by subsequent anodic stripping voltammetry. The key experimental variables relevant to the voltammetric measurement procedure were optimized. For a 100 s preconcentration time, a linear calibration curve was obtained in concentration range from 1.0 to 125.0μg/L with a sampling frequency of 27/h. The detection limit was 0.41μg/L and the relative standard deviation was 2.70% at the 25.0μg/L level (n=11). The analytical utility of the established method was applied to the determination of cadmium in real samples, and the results were validated by ICP-OES technique.
设计加工了适当的阀上实验室-电化学检测流通池,将三电极整合加工到阀内,以pH为4.7的醋酸-醋酸钠缓冲溶液为支持电解质,可更新汞膜碳糊电极为工作电极,采用顺序注射-阀上实验室-微分脉冲阳极溶出伏安法实现了对重金属镉的快速测定。在最佳的实验条件下,峰电流与镉的浓度在5.0-75.0μg/L范围呈良好的线性关系,检出限为0.41μg/L,对浓度为20μg/L的试液11次重复测量的相对标准偏差为2.8%,分析频率为30/h。该方法仪器简单,样品和试剂消耗量低,操作快速。
本实验以低毒的Nafion-铋膜电极为工作电极,在自行设计的阀上实验室-电化学检测流通池内完成了对痕量镉的测定。研究了镉在0.10 mol/L的醋酸-醋酸钠缓冲溶液中溶出行为。结果表明,Nafion膜能够有效提高电子转移速率,铋膜能够有效提高镉的检出限。在最佳的实验条件下,镉的浓度在2.0-100μg/L范围内与峰电流成良好的线性关系,检出限为0.23μg/L,对浓度为50μg/L的镉溶液11次重复测量的相对标准偏差为1.72%,分析频率为45/h。通过将顺序注射-阀上实验室-阳极溶出伏安法联用,提高了检测频率,降低了常规滴汞电极由于汞的使用而带来的污染,实现了实验过程操作的全自动化。
本文首次采用顺序注射-阀上实验室系统-吸附溶出伏安法测定了工业废水中的镉,该方法快速且灵敏。样品和试剂通过柱塞泵进入检测器,镉离子在修饰电极表面富集,然后通过阳极溶出伏安法实现了对镉离子的定量。对实验中一系列的参数进行了优化,在100s的富集时间内,镉在1.0-125.0μg/L范围内与峰电流成线性关系,检出限为0.41μg/L,对25.0μg/L的镉进行重复测定,其RSD为2.70%,分析频率为27/h,运用该方法对样品进行检测,结果与ICP-OES相一致,结果令人满意。
Sequential injection lab-on-valve as the third generation flow injection technology, with automatic sample injection, volume size can be flexible to change; equipment simple, easy to use, which achieved determination procee on line. The electrochemical analysis method is with high sensitivity and analysis speed, low cost and so on merit. The sequential injection lab on valve combined with electrochemical analysis methods, retaining the advantages of each method, at the same time which making the conventional electrochemical analysis become simple, greatly increased the frequency of analysis, and achieving a fully automated analysis process. It will have great prospects in the future in the analysis field. In this paper, we used sequential injection lab on valve combined with electrochemical analysis techniques to detect the heavy metals in environmental samples; the main research includes about three parts:
Sequential rejection lab-on-valve (LOV) using renewnal mercuy film electrode was first proposed for analyzing Cd coupled with differential pulse anodic stripping voltammetry (DPASV). The electrochemical flow cell including three electrodes was designed as a part of the selection valve of the SIA (sequential injection apparatus). Under the optimal parameters, the response was linear in the concentration range from 5.0 to 75.0μg/L along with a sampling frequency of 30/h, and a detection limit of 0.41μg/L was obtained with a precision of 2.8% RSD at the level of 20μg/L. The total processing was carried out in a closed ehannel system. The established analytical procedure enhanced the repeatability and minimized sample and reagent consumption. The practical applicability was demonstrated by determination of Cd in environmental water samples.
This work exploited a sequential injection lab-on-valve (LOV) system for the determination of cadmium by anodic stripping voltammetry (ASV). A miniaturized electrochemical flow cell (EFC) was fabricated in LOV, in which a nafion coated bismuth film electrode was used as working electrode. The cadmium was electrodeposited on the electrode surface with bismuth solution, and measured with the subsequential stripping scan. Under optimal conditions, the proposed system responded linearly to cadmium concentrations in a range 2.0-100.0μg/L. The detection limit of this method was found to be 0.88μg/L. By loading a sample volume of 800μL, a sampling frequency of 25 determinations h-1 was achieved. The repeatability expressed as relative standard derivation (R.S.D.) was 3.65% for 20μg/L cadmium (n= 11). The method was applied to analysis of trace cadmium in environmental water samples and the spiked recoveries were satisfactory. By combining sequential injection lab on valve with anodic stripping voltammetry which increased testing frequency, reducing the conventional dropping mercury electrode as the use of mercury pollution caused by the experimental process. At the same time it achieves full automation.
A rapid and sensitive adsorptive stripping voltammetric assay for the determination of trace amount of cadmium was developed in a sequential injection lab-on-valve (SI-LOV) system for the first time. The sample and reagent arrangements were achieved by a syringe pump. The target metal ions were accumulated on the morin modified glassy carbon electrode surface, and the quantification step was performed by subsequent anodic stripping voltammetry. The key experimental variables relevant to the voltammetric measurement procedure were optimized. For a 100 s preconcentration time, a linear calibration curve was obtained in concentration range from 1.0 to 125.0μg/L with a sampling frequency of 27/h. The detection limit was 0.41μg/L and the relative standard deviation was 2.70% at the 25.0μg/L level (n=11). The analytical utility of the established method was applied to the determination of cadmium in real samples, and the results were validated by ICP-OES technique.
引文
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