CN101377473B - Rapid quantitative electroanalysis method - Google Patents
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Abstract
本发明建立了一种快速分析物质浓度的定量电化学分析方法。对不同的物质选用相应的电极系统，采用循环伏安法确定待测物质的还原(或氧化)峰的电位区间，并以此为依据，确定三次电位阶跃法的电位阶跃区间。在三次电位阶跃法中记录电流-时间数据，以其中第二个电位阶跃区间对应的电流峰对时间积分，得到电量值，其与待测物质浓度呈线性关系，是定量的依据。本方法分析速度很快，操作简单。The invention establishes a quantitative electrochemical analysis method for rapid analysis of substance concentration. Select the corresponding electrode system for different substances, use cyclic voltammetry to determine the potential interval of the reduction (or oxidation) peak of the substance to be measured, and use this as a basis to determine the potential step interval of the triple potential step method. In the three potential step method, the current-time data is recorded, and the current peak corresponding to the second potential step interval is integrated with time to obtain the electric quantity value, which has a linear relationship with the concentration of the substance to be measured, and is the basis for quantification. This method has a fast analysis speed and is easy to operate.
Description
发明领域field of invention
本发明涉及一种快速的电化学定量分析方法，特别是涉及一种通过快速改变电位并以此过程中的电子转移量来确定被测物浓度的方法。The invention relates to a fast electrochemical quantitative analysis method, in particular to a method for determining the concentration of the analyte by changing the potential rapidly and using the electron transfer amount in the process.
背景技术 Background technique
电化学分析法是利用物质的电学及电化学性质来进行分析的方法。它通常是使待分析的试样溶液构成一化学电池，然后根据所组成电池的某些物理量与其化学量之间的内在联系来进行测定，可以分为电流分析法、电位分析法、电量分析法和伏安分析法等。目前，电化学分析广泛应用的方法是循环伏安法。该法控制电极电势以不同的速率，随时间以三角波形一次或多次反复扫描，电势范围是使电极上能交替发生不同和还原和氧化反应，并记录电流—电势曲线，可以通过曲线上氧化还原峰电流来进行定量分析。使用循环伏安法，由于循环路径和扫描速度的限制，对于提高分析速度帮助不大。Electrochemical analysis is a method of analysis using the electrical and electrochemical properties of substances. It usually makes the sample solution to be analyzed to form a chemical battery, and then measures it according to the internal relationship between some physical quantities of the battery and its chemical quantities, which can be divided into amperometric analysis, potential analysis, and power analysis. and voltammetric analysis. At present, the widely used method of electrochemical analysis is cyclic voltammetry. This method controls the electrode potential at different rates and repeatedly scans with a triangular waveform one or more times over time. The potential range is such that different and reduction and oxidation reactions can alternately occur on the electrode, and the current-potential curve is recorded, which can be oxidized on the curve. Recover the peak current for quantitative analysis. Using cyclic voltammetry, due to the limitations of the cycle path and scan speed, does not help much to improve the analysis speed.
电量分析法是进行电量测定的分析方法的总称，也称库仑法，是一种通过测定消耗于溶液中待测物质所需的电量来定量地测定这一物质含量的方法。通过计量一段时间内通过电解池电路中流过的电荷来对体系进行分析的方法称为计时库仑法，也称计时电量法，常被用来研究电极表面吸附现象，并定量地测定电活性物质或表面活性物质在电极表面吸附量的电化学分析法。而这种方法的选择性不佳，不宜用作复杂溶液中的定量分析。Coulometric analysis is the general term for the analytical methods for the determination of electric quantity, also known as the coulometric method, which is a method for quantitatively determining the content of the substance to be measured by measuring the amount of electricity required to consume the substance to be measured in the solution. The method of analyzing the system by measuring the charge flowing through the electrolytic cell circuit for a period of time is called the chronocoulomb method, also known as the chronoelectric method, which is often used to study the adsorption phenomenon on the electrode surface and quantitatively determine the electroactive substances or Electrochemical analysis of the amount of surface active substances adsorbed on the electrode surface. However, this method has poor selectivity and is not suitable for quantitative analysis in complex solutions.
电位阶跃法是以电位阶跃信号作为控制信号同时测出相应的电流值，可以绘制出电流—时间曲线。这种方法常用于极化曲线的绘制。The potential step method uses the potential step signal as the control signal to measure the corresponding current value at the same time, and the current-time curve can be drawn. This method is often used to draw polarization curves.
目前的污染物分析法主要是滴定分析法、重量分析法、紫外/可见/红外分光光度法、气相或液相色谱法、气相或液相质谱联用法、原子荧光/原子吸收/原子发射光谱法等。这些常规方法普遍存在分析速度慢，很难实现在线监控等缺点。而目前的快速电化学分析方法多集中在生化分析方面(如中国专利CN1975403、CN1325490)，而环保方面一般局限于水中COD的电化学分析(如中国专利CN1645127)和气体传感器方面(如中国专利CN2754096)等。这些方法针对性较强，而通用性不足，可以检测的物质比较有限。The current pollutant analysis methods are mainly titration analysis, gravimetric analysis, ultraviolet/visible/infrared spectrophotometry, gas or liquid chromatography, gas or liquid mass spectrometry, atomic fluorescence/atomic absorption/atomic emission spectrometry wait. These conventional methods generally have the disadvantages of slow analysis speed and difficulty in online monitoring. And present fast electrochemical analysis method mostly concentrates on the biochemical analysis aspect (as Chinese patent CN1975403, CN1325490), and the electrochemical analysis (as Chinese patent CN1645127) and gas sensor aspect (as Chinese patent CN2754096) of COD in environmental protection aspect are generally limited to )wait. These methods are highly targeted, but lack of versatility, and the substances that can be detected are relatively limited.
发明内容 Contents of the invention
本发明的目的是为了解决现行的水中污染物的分析方法检测速度较慢的问题，开发一种高速检测水中污染物的电化学方法，即使用窄电位连续阶跃法提高电位阶跃计时库仑法的检测选择性，同时保持快速分析特征的方法。The purpose of the present invention is to solve the problem that the detection speed of the current analysis method of pollutants in water is relatively slow, and to develop a high-speed electrochemical method for detecting pollutants in water, that is, to use the narrow potential continuous step method to improve the potential step chronocoulomb method detection selectivity while maintaining a fast method for characterizing.
本发明提供的快速电化学分析方法的原理如下：The principle of the fast electrochemical analysis method provided by the invention is as follows:
电解槽使用三电极系统，其工作电极应对被测物具有高选择性，参比电极为饱和甘汞电极(SCE)，辅助电极为铂片电极，辅助电极面积应大于等于工作电极。The electrolytic cell uses a three-electrode system. The working electrode should have high selectivity for the measured substance. The reference electrode is a saturated calomel electrode (SCE), and the auxiliary electrode is a platinum electrode. The area of the auxiliary electrode should be greater than or equal to the working electrode.
当电极上施加的电位达到或超过待测物质的还原(或氧化)电位时，待测物质可以从电极得到(或失去)电子，在电极表面上发生氧化还原反应。由于样品中待测物浓度不同，在电极表面上富集的量也不相同，因此在施加一定的电压时，发生电化学反应的物质的量不同，这就导致通路内电子转移量不同。通过检测此过程中转移的电量，发现其与样品中待测物浓度呈线性相关，此为本方法的定量依据。When the potential applied on the electrode reaches or exceeds the reduction (or oxidation) potential of the substance to be tested, the substance to be tested can get (or lose) electrons from the electrode, and a redox reaction occurs on the surface of the electrode. Due to the different concentration of the analyte in the sample, the amount of enrichment on the electrode surface is also different. Therefore, when a certain voltage is applied, the amount of the substance undergoing electrochemical reaction is different, which leads to the difference in the amount of electron transfer in the channel. By detecting the amount of electricity transferred during this process, it is found that it is linearly related to the concentration of the analyte in the sample, which is the quantitative basis of this method.
本方法的特点是通过循环伏安法确定待测物质的还原(或氧化)峰的电位区间，此峰电位区间尽可能窄，称为窄电位，以此电位区间为依据进行窄电位连续阶跃测试，因而只有待测物质可以被还原(或氧化)。这就是本方法排除干扰物、提高选择性的依据。The characteristic of this method is to determine the potential range of the reduction (or oxidation) peak of the substance to be tested by cyclic voltammetry. test, thus only the substance to be tested can be reduced (or oxidized). This is the basis for this method to eliminate interfering substances and improve selectivity.
本发明提供的快速定量电分析方法，其步骤如下：The rapid quantitative electroanalysis method provided by the invention has the following steps:
1)分析方法中的电池系统使用三电极系统，在电解槽中加入待测水样，带鲁金毛细管的电解槽中进行循环伏安扫描，在循环伏安曲线上按照待测物质的还原(或氧化)峰位置确定窄电位阶跃范围(V1，V2)。1) The battery system in the analysis method uses a three-electrode system. Add the water sample to be tested in the electrolytic cell, and perform cyclic voltammetry scanning in the electrolytic cell with a Lujin capillary. or oxidation) peak position to determine the narrow potential step range (V 1 , V 2 ).
2)分析方法中电位控制方法为改进的三次电位阶跃法，记录电流—时间数据(图1)。第一次电位阶跃范围为0→V1，电位到达V1后保持1～5秒，此过程中，凡是还原(氧化)电位高于(低于)V1的电活性物质会发生还原(氧化)反应，从而除去电极附近的干扰物；第二次电位阶跃范围为V1→V2，电位到达V1后保持1～5秒，此过程中，待测物质发生电化学还原(或氧化)反应，记录电子转移量即电量作为定量依据；第三次电位阶跃范围为V2→0，阶跃后稳定1～5秒，使得电极表面的基团恢复为初始状态，便于下次检测。此方法总时间不超过15秒，速度很快。2) In the analysis method, the potential control method is the improved three-potential step method, and the current-time data are recorded (Fig. 1). The first potential step range is 0→V 1 , and the potential is maintained for 1 to 5 seconds after reaching V 1 . During this process, any electroactive substance with a reduction (oxidation) potential higher (lower) than V 1 will be reduced ( Oxidation) reaction, so as to remove the interfering substances near the electrode; the second potential step range is V 1 →V 2 , and the potential is kept for 1 to 5 seconds after reaching V 1. During this process, the substance to be tested undergoes electrochemical reduction (or Oxidation) reaction, record the amount of electron transfer, that is, the amount of electricity as a quantitative basis; the third potential step range is V 2 → 0, and it stabilizes for 1 to 5 seconds after the step, so that the groups on the electrode surface return to the initial state, which is convenient for the next detection. The total time of this method does not exceed 15 seconds, which is very fast.
3)分析方法中的样品测定方法为：配制待测物质的标准浓度溶液系列，采用2)中所述方法分别测定并记录电流—时间数据。根据电流—时间数据，在第二次电位阶跃时间范围内，以电流对时间积分，得到电量值。以标准浓度溶液系列的电量值—待测物质浓度为坐标系采用最小二乘法拟合的直线，即为标准曲线；按照2)所述方法测定未知样品的电流—时间数据，计算电量值并根据标准曲线求得未知样品浓度。3) The sample determination method in the analysis method is: prepare a standard concentration solution series of the substance to be tested, and use the method described in 2) to measure and record the current-time data respectively. According to the current-time data, within the time range of the second potential step, the electric quantity value is obtained by integrating the current with respect to time. The electric value of the standard concentration solution series-the concentration of the substance to be tested is the straight line fitted by the least squares method in the coordinate system, which is the standard curve; measure the current-time data of the unknown sample according to the method described in 2), calculate the electric charge value and according to The standard curve was used to obtain the concentration of unknown samples.
与现有技术相比，本发明所述的优点在于：Compared with prior art, the described advantage of the present invention is:
与气相色谱/气质连用法相比，本方法不需要大型仪器，成本低；样品无需萃取分离，前处理简单；样品不用色谱分离，分析速度快。与分光光度法相比，本方法无需显色剂，操作简单；与原子吸收/发射光谱法相比，本方法设备简单，操作方便，线性范围较宽，可检测高浓度样品。Compared with gas chromatography/gas chromatography, this method does not require large-scale instruments, and the cost is low; the sample does not need extraction and separation, and the pretreatment is simple; the sample does not need chromatographic separation, and the analysis speed is fast. Compared with the spectrophotometric method, the method does not need a chromogenic agent, and the operation is simple; compared with the atomic absorption/emission spectrometry, the method has simple equipment, convenient operation, wide linear range, and can detect high-concentration samples.
附图说明 Description of drawings
图1三次电位阶跃法采集的电流—时间数据Figure 1 The current-time data collected by the triple potential step method
具体实施方式 Detailed ways
实施实例1：Implementation example 1:
使用硝基还原酶修饰电极为工作电极，铂片电极为辅助电极，饱和甘汞电极为参比，取窄电位区间(-0.60V，-0.80V)，从0V开始负向电位阶跃，第一次阶跃时间3秒，第二次阶跃时间3秒，第三次阶跃时间2秒。待测溶液pH 7.5，还原峰定量，溶液不用除氧，此方法可以用于检测水中硝基苯，避免通气除氧造成的误差，而氧气还原再第一次阶跃时已经完成，不会造成干扰。Use the nitroreductase modified electrode as the working electrode, the platinum sheet electrode as the auxiliary electrode, and the saturated calomel electrode as the reference, take a narrow potential interval (-0.60V, -0.80V), and start from 0V to the negative potential step, the first The first step time is 3 seconds, the second step time is 3 seconds, and the third step time is 2 seconds. The pH of the solution to be tested is 7.5, the reduction peak is quantitative, and the solution does not need to be deoxygenated. This method can be used to detect nitrobenzene in water to avoid errors caused by aeration and deoxygenation. However, the oxygen reduction has been completed at the first step and will not cause interference.
实施实例2：Implementation example 2:
使用玻碳电极为工作电极，铂片电极为辅助电极，饱和甘汞电极为参比，取窄电位区间(0.51V，0.60V)，从0V开始正向电位阶跃，第一次阶跃时间2秒，第二次阶跃时间2秒，第三次阶跃时间2秒。待测溶液pH 5.6，氧化峰定量，此方法可以用于检测阿魏酸浓度。Use a glassy carbon electrode as the working electrode, a platinum sheet electrode as the auxiliary electrode, and a saturated calomel electrode as the reference. Take a narrow potential range (0.51V, 0.60V), start a positive potential step from 0V, and the first step time 2 seconds, the second step time is 2 seconds, and the third step time is 2 seconds. The pH of the solution to be tested is 5.6, and the oxidation peak is quantified. This method can be used to detect the concentration of ferulic acid.
实施实例3：Implementation example 3:
使用玻碳电极为工作电极，在2.0V预先极化2分钟后再在-1.0V极化1分钟，然后浸入硝酸铅溶液，在搅拌条件下活化10分钟后使用，铂丝电极为辅助电极，银/氯化银电极为参比，取窄电位区间(-0.40V，-0.55V)，从0V开始负向电位阶跃，第一次阶跃时间2秒，第二次阶跃时间3秒，第三次阶跃时间2秒。待测溶液pH 5.0，还原峰定量，此方法可以用于检测水溶液中铅离子(Pb2+)的浓度。Use a glassy carbon electrode as the working electrode, pre-polarize at 2.0V for 2 minutes, then polarize at -1.0V for 1 minute, then immerse in the lead nitrate solution, activate it for 10 minutes under stirring conditions, and use it. The platinum wire electrode is the auxiliary electrode. The silver/silver chloride electrode is used as a reference, and a narrow potential interval (-0.40V, -0.55V) is taken, and the negative potential step is started from 0V, the first step time is 2 seconds, and the second step time is 3 seconds , the third step time is 2 seconds. The pH of the solution to be tested is 5.0, and the reduction peak is quantified. This method can be used to detect the concentration of lead ions (Pb 2+ ) in aqueous solution.
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| CN101782545A (en) * | 2010-03-09 | 2010-07-21 | 中国科学院过程工程研究所 | Method for purifying ionic liquid concentration |
| CN104062339B (en) * | 2014-07-09 | 2016-08-31 | 华南师范大学 | [Ru (tatp) 3] 2+ modified electrode and the method being used for detecting glucose in blood, uric acid and ascorbic acid thereof |
| CN110186981A (en) * | 2019-04-19 | 2019-08-30 | 九江德福科技股份有限公司 | A kind of Quantitative Monitoring method of chloride ion |
| CN113219025B (en) * | 2021-05-07 | 2023-07-25 | 安徽大学 | Method for quantitatively detecting potassium bromate |
| CN113418824B (en) * | 2021-05-07 | 2023-02-10 | 华东理工大学 | Method for testing gas adsorption capacity |
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| US5562815A (en) * | 1994-02-09 | 1996-10-08 | Pacesetter Ab | Apparatus and method for the electrochemical determination of the oxygen concentration of a liquid medium |
| CN1278063A (en) * | 1999-05-28 | 2000-12-27 | 株式会社明电舍 | Electrochemical analysis using electrode coated with conductive diamond, and electrochemical analysis system therewith |
| EP1236995A1 (en) * | 1995-11-16 | 2002-09-04 | USF Filtration and Separations Group Inc. | Repetitive potential step method for amperometric detection |
| CN1715899A (en) * | 2004-07-02 | 2006-01-04 | 中国科学院福建物质结构研究所 | Preparation method of a novel residual chlorine detection electrode |
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| US5562815A (en) * | 1994-02-09 | 1996-10-08 | Pacesetter Ab | Apparatus and method for the electrochemical determination of the oxygen concentration of a liquid medium |
| EP1236995A1 (en) * | 1995-11-16 | 2002-09-04 | USF Filtration and Separations Group Inc. | Repetitive potential step method for amperometric detection |
| CN1278063A (en) * | 1999-05-28 | 2000-12-27 | 株式会社明电舍 | Electrochemical analysis using electrode coated with conductive diamond, and electrochemical analysis system therewith |
| CN1715899A (en) * | 2004-07-02 | 2006-01-04 | 中国科学院福建物质结构研究所 | Preparation method of a novel residual chlorine detection electrode |
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