CN102539510A - Method for determining hydrogen peroxide by using nickel lanthanum titanate/cobalt ferrite modified glassy carbon electrode - Google Patents
Method for determining hydrogen peroxide by using nickel lanthanum titanate/cobalt ferrite modified glassy carbon electrodeDownload PDFInfo
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Abstract
Translated fromChineseDescription
Translated fromChinese技术领域technical field
本发明涉及一种利用无机钙钛矿钛酸镍镧负载铁酸钴修饰玻碳电极作为过氧化氢电化学传感器快速测定过氧化氢溶液的方法，属电化学分析检测技术领域。The invention relates to a method for rapidly measuring hydrogen peroxide solution by using an inorganic perovskite nickel-lanthanum titanate-loaded cobalt ferrite-modified glassy carbon electrode as a hydrogen peroxide electrochemical sensor, which belongs to the technical field of electrochemical analysis and detection.
背景技术Background technique
钙钛矿型复合氧化物因具有天然钙钛石(CaTi03)晶体结构而得名，常以通式ABO3表示，理想的钙钛矿型氧化物(ABO3)为立方结构。在ABO3型钙钛矿结构中，A2+和O2–共同构成近似立方密堆积，每个A2+有l2个氧配位，02–同时属于8个BO6八面体，每个02–有6个阳离子(4个A和2个B)连接，B2+有6个氧配位，占据着02–形成的全部氧八面体空隙。钙钛矿型复合氧化物ABO3是一种具有独特物理性质和化学性质的新型无机非金属材料，A位一般是稀土或碱土元素离子，B位为过渡元素离子，A位和B位皆可被半径相近的其他金属离子部分取代而保持其晶体结构基本不变，因此在理论上它是研究催化剂表面及催化性能的理想样品。由于这类化合物具有稳定的晶体结构、独特的电磁性能作为一种新型的功能材料，在环境保护和工业催化等领域具有很大的开发潜力。钙钛矿钛酸镍镧负载铁酸钴即是其中一种特定组成的无机钙钛矿材料，因此具有一般钙钛矿所具有的催化、导电等特点，将其修饰在电极表面有很好的电化学催化性能，可直接用于过氧化氢电化学传感器的制作。The perovskite-type composite oxide is named for its natural perovskite (CaTi03 ) crystal structure, usually represented by the general formula ABO3 , and the ideal perovskite-type oxide (ABO3 ) has a cubic structure. In the ABO3 -type perovskite structure, A2+ and O2– together form an approximate cubic close-packed structure, each A2+ has l2 oxygen coordination, and 02– belongs to 8 BO6 octahedra at the same time, each 02– has 6 cations (4 A and 2 B) connected, and B2+ has 6 oxygen coordinations, occupying all the oxygen octahedral voids formed by 02– . Perovskite-type composite oxide ABO3 is a new type of inorganic non-metallic material with unique physical and chemical properties. The A site is generally a rare earth or alkaline earth element ion, and the B site is a transition element ion. Both the A site and the B site are acceptable. It is partially replaced by other metal ions with similar radius and keeps its crystal structure basically unchanged, so theoretically it is an ideal sample for studying the surface and catalytic performance of catalysts. Because this kind of compound has stable crystal structure and unique electromagnetic properties, as a new type of functional material, it has great development potential in the fields of environmental protection and industrial catalysis. Perovskite nickel lanthanum titanate-supported cobalt ferrite is one of the inorganic perovskite materials with a specific composition, so it has the characteristics of catalysis and conductivity that general perovskites have, and it is very good to modify it on the surface of the electrode. The electrochemical catalytic performance can be directly used in the fabrication of hydrogen peroxide electrochemical sensors.
过氧化氢是一种强氧化剂，适用于伤口消毒及环境、食品消毒。到目前为止，测定过氧化氢的方法主要有分光光度法、滴定法和电化学方法等。电化学方法由于其分析速度快，成本低，且灵敏度高等优点已经受到普遍关注。Hydrogen peroxide is a strong oxidizing agent, suitable for wound disinfection, environment and food disinfection. So far, the methods for determining hydrogen peroxide mainly include spectrophotometry, titration and electrochemical methods. Electrochemical methods have received widespread attention due to their advantages of fast analysis speed, low cost, and high sensitivity.
发明内容Contents of the invention
本发明的目的是提供一种无机钙钛矿钛酸镍镧负载铁酸钴修饰玻碳电极的制备方法及其作为过氧化氢电化学传感器，并对过氧化氢进行检测的方法。The purpose of the present invention is to provide a preparation method of an inorganic perovskite nickel lanthanum titanate-supported cobalt ferrite modified glassy carbon electrode and a method for detecting hydrogen peroxide as an electrochemical sensor for hydrogen peroxide.
本发明一种用钛酸镍镧/铁酸钴修饰玻碳电极测定过氧化氢的方法，其特征在于具有以下的过程和步骤：The present invention uses nickel lanthanum titanate/cobalt ferrite modified glassy carbon electrode to measure hydrogen peroxide, which is characterized in that it has the following processes and steps:
a. 玻碳电极的预处理：首先将玻璃态碳电极即玻碳电极用0.05 mmAl2O3抛光粉和抛光绒布对所述玻碳电极进行抛光，抛光至镜面，然后依次用蒸馏水、稀硝酸溶液、无水乙醇及二次蒸馏水超声清洗干净，待用；a. Pretreatment of the glassy carbon electrode: first, the glassy carbon electrode, that is, the glassy carbon electrode, is polished with 0.05 mmAl2 O3 polishing powder and polishing flannelette to the mirror surface, and then distilled water, dilute nitric acid Solution, absolute ethanol and double distilled water were ultrasonically cleaned, and then used;
b. 钛酸镍镧/铁酸钴修饰玻碳电极的制备：首先用二次蒸馏水配置一定浓度的钛酸镍镧/铁酸钴悬浊液，两者之比为20：1，最适宜的浓度为0.5 ～ 2.5 mg/mL，在室温下超声振荡24小时；在处理好的玻碳电极表面上滴加上述钛酸镍镧/铁酸钴悬浊液5 mL；然后放置于红外灯下烤干，约15分钟；烤干后在室温下放置半个小时，随后用二次蒸馏水淋洗掉残余物，然后在0.1 M的氢氧化钠溶液中，在–1～1 V的电位窗口中用循环伏安法扫描至稳定，然后用二次蒸馏水淋洗干净，最终制得钛酸镍镧/铁酸钴修饰玻碳电极；b. Preparation of nickel lanthanum titanate/cobalt ferrite modified glassy carbon electrode: first prepare a certain concentration of nickel lanthanum titanate/cobalt ferrite suspension with double distilled water, the ratio of the two is 20:1, the most suitable Concentration of 0.5 ~ 2.5 mg/mL, ultrasonic oscillation at room temperature for 24 hours; drop 5 mL of the above-mentioned nickel lanthanum titanate/cobalt ferrite suspension on the surface of the treated glassy carbon electrode; then place it under an infrared lamp to bake Dry, about 15 minutes; after drying, place it at room temperature for half an hour, then rinse off the residue with twice distilled water, and then use it in a 0.1 M sodium hydroxide solution in a potential window of –1 to 1 V Cyclic voltammetry was used to scan until it was stable, and then rinsed with double distilled water to finally prepare a nickel-lanthanum titanate/cobalt ferrite-modified glassy carbon electrode;
c. 钛酸镍镧/铁酸钴修饰玻碳电极作为过氧化氢电化学传感器检测过氧化氢浓度：所述修饰玻碳电极可直接用于过氧化氢的电化学测定；其测定方法如下：将所述的钛酸镍镧/铁酸钴修饰玻碳电极作为工作电极、饱和甘汞电极作为参比电极、铂片电极作为辅助电极，组成三电极系统；测定过氧化氢时将三电极系统置于10 mL 的0.1 M NaOH溶液中，从–1 V 到1 V 的电位范围内循环伏安法扫描20段以活化电极；然后在工作电极上施加一定的阳极电位，记录下电流—时间曲线，当背景电流达到稳态后，用微量进样器向0.1 M NaOH溶液中加过氧化氢标准溶液；在不同过氧化氢溶液浓度下测得传感器对过氧化氢的电流响应值，并在浓度0.1μM～8.2mM范围内，得到电流与过氧化氢浓度的线性关系曲线，其线性相关系数r = 0.997，利用标准曲线法对过氧化氢进行分析检测。c. Nickel lanthanum titanate/cobalt ferrite modified glassy carbon electrode is used as hydrogen peroxide electrochemical sensor to detect hydrogen peroxide concentration: the modified glassy carbon electrode can be directly used for electrochemical determination of hydrogen peroxide; its determination method is as follows: The nickel lanthanum titanate/cobalt ferrite modified glassy carbon electrode is used as the working electrode, the saturated calomel electrode is used as the reference electrode, and the platinum plate electrode is used as the auxiliary electrode to form a three-electrode system; when measuring hydrogen peroxide, the three-electrode system Place in 10 mL of 0.1 M NaOH solution, scan 20 segments of cyclic voltammetry in the potential range from –1 V to 1 V to activate the electrode; then apply a certain anode potential on the working electrode, and record the current-time curve , when the background current reached a steady state, a standard solution of hydrogen peroxide was added to the 0.1 M NaOH solution with a micro-injector; the current response value of the sensor to hydrogen peroxide was measured at different concentrations of the hydrogen peroxide solution, and the concentration In the range of 0.1 μM to 8.2 mM, a linear relationship curve between the current and the concentration of hydrogen peroxide is obtained, and the linear correlation coefficientr = 0.997, and the hydrogen peroxide is analyzed and detected by the standard curve method.
本发明的优点和特点如下所述：Advantages and characteristics of the present invention are as follows:
本发明利用了钙钛矿的电催化作用，在不用酶的条件下对过氧化氢的氧化产生了电化学催化作用，不仅避免了酶存在条件下失活不稳定的缺点，而且该修饰电极大大提高了分析检测过氧化氢浓度的灵敏度。The present invention utilizes the electrocatalysis of perovskite to produce electrochemical catalysis for the oxidation of hydrogen peroxide without enzymes, which not only avoids the disadvantage of unstable inactivation under the condition of enzymes, but also greatly improves the performance of the modified electrode. The sensitivity of analyzing and detecting the concentration of hydrogen peroxide is improved.
本发明中的修饰电极是一种新型的电化学传感器，用于实际样品测定，具有快速、灵敏、准确等特点。本发明的测试方法具有良好的重现性和稳定性。本发明中的新型修饰玻碳电极的制备方法具有成本低、简单快速、易操作等优点。The modified electrode in the present invention is a new type of electrochemical sensor, which is used for the determination of actual samples and has the characteristics of fast, sensitive and accurate. The test method of the invention has good reproducibility and stability. The preparation method of the novel modified glassy carbon electrode in the present invention has the advantages of low cost, simple and fast, easy operation and the like.
附图说明Description of drawings
图1为本发明中在含有过氧化氢溶液（0.1 M）的0.1 M氢氧化钠溶液中在裸玻碳电极（b）、钛酸镍镧负载铁酸钴修饰玻碳电极（a）上的循环伏安图；Fig. 1 is in the 0.1 M sodium hydroxide solution containing hydrogen peroxide solution (0.1 M) in the present invention on bare glassy carbon electrode (b), nickel lanthanum titanate supported cobalt ferrite modified glassy carbon electrode (a) Cyclic voltammogram;
图2为本发明中在搅拌下在0.1 M氢氧化钠溶液中依次加入过氧化氢溶液（0.1 M）的裸玻碳电极（a），钛酸镍镧负载铁酸钴修饰玻碳电极(b)的电流–时间曲线；Figure 2 is a bare glassy carbon electrode (a) in which hydrogen peroxide solution (0.1 M) is added sequentially to 0.1 M sodium hydroxide solution under stirring in the present invention, and a nickel-lanthanum titanate-loaded cobalt ferrite-modified glassy carbon electrode (b ) current-time curve;
图3为最佳条件下，加入不同浓度的过氧化氢标准溶液的电流-时间曲线图。Figure 3 is the current-time curve of adding different concentrations of hydrogen peroxide standard solutions under the optimal conditions.
具体实施方式Detailed ways
现将本发明的具体实施例叙述于后。Specific embodiments of the present invention are now described in the following.
实施例：本实施例中的修饰玻碳电极的制备方法和步骤如下：Embodiment: The preparation method and steps of the modified glassy carbon electrode in this embodiment are as follows:
（1）玻碳电极的预处理：首先将玻璃态碳电极即玻碳电极用0.05 mmAl2O3抛光粉和抛光绒布对所述玻碳电极进行抛光，抛光至镜面，然后依次用蒸馏水、稀硝酸溶液、无水乙醇及二次蒸馏水超声清洗干净，待用；(1) Pretreatment of the glassy carbon electrode: firstly, the glassy carbon electrode, that is, the glassy carbon electrode, is polished with 0.05 mmAl2 O3 polishing powder and polishing flannelette to the mirror surface, and then distilled water, dilute Nitric acid solution, absolute ethanol and twice-distilled water were ultrasonically cleaned, and then used;
（2）钙钛矿钛酸镍镧负载铁酸钴修饰玻碳电极的制备：首先用二次蒸馏水配置一定浓度的钛酸镍镧负载铁酸钴悬浊液，两者之比为20：1，最适宜的浓度为0.5 ～ 2.5mg/mL，在室温下超声振荡24小时；在处理好的玻碳电极表面上滴加上述钛酸镍镧负载铁酸钴悬浊液5 mL；然后放置于红外灯下烤干，约15分钟；烤干后在室温下放置半个小时，随后用二次蒸馏水淋洗掉残余物，然后在0.1 M的氢氧化钠溶液中，在 –1 ～ 1 V的电位窗口中用循环伏安法扫描至稳定，然后用二次蒸馏水淋洗干净，最终制得钛酸镍镧负载铁酸钴修饰玻碳电极（即钛酸镍镧/铁酸钴修饰玻碳电极）。(2) Preparation of perovskite nickel-lanthanum titanate-loaded cobalt ferrite-modified glassy carbon electrode: first, prepare a certain concentration of nickel-lanthanum titanate-loaded cobalt ferrite suspension with double distilled water, and the ratio of the two is 20:1 , the most suitable concentration is 0.5 ~ 2.5mg/mL, ultrasonic vibration at room temperature for 24 hours; on the surface of the treated glassy carbon electrode, 5 mL of the above-mentioned nickel lanthanum titanate-loaded cobalt ferrite suspension was added dropwise; then placed in Dry under infrared light for about 15 minutes; after drying, place it at room temperature for half an hour, then rinse off the residue with double distilled water, and then in 0.1 M sodium hydroxide solution, at –1 ~ 1 V The potential window was scanned by cyclic voltammetry until it was stable, and then rinsed with double distilled water to finally prepare a nickel-lanthanum titanate-loaded cobalt ferrite-modified glassy carbon electrode (that is, nickel-lanthanum titanate/cobalt ferrite-modified glassy carbon electrode ).
钛酸镍镧负载铁酸钴（钛酸镍镧/铁酸钴）修饰玻碳电极对过氧化氢的电化学测定：Electrochemical determination of hydrogen peroxide on nickel-lanthanum titanate-supported cobalt ferrite (nickel-lanthanum titanate/cobalt ferrite) modified glassy carbon electrode:
测定方法如下：将所述的钛酸镍镧负载铁酸钴修饰玻碳电极作为工作电极、饱和甘汞电极作为参比电极、铂片电极作为辅助电极，组成三电极系统；测定过氧化氢时将三电极系统置于10 mL 的0.1 M NaOH溶液中，从 –1 V 到1 V 的电位范围内循环伏安法扫描20段以活化电极；然后在工作电极上施加一定的阳极电位，记录下电流—时间曲线，当背景电流达到稳态后，用微量进样器向0.1 M NaOH溶液中加过氧化氢标准溶液；在不同过氧化氢溶液浓度下测得传感器对过氧化氢的电流响应值，并在浓度0.1 μM ～8.2 mM范围内，得到电流与过氧化氢浓度的线性关系曲线，其线性相关系数r = 0.997，利用标准曲线法对过氧化氢进行分析检测。The determination method is as follows: use the nickel-lanthanum titanate-loaded cobalt ferrite-modified glassy carbon electrode as the working electrode, the saturated calomel electrode as the reference electrode, and the platinum sheet electrode as the auxiliary electrode to form a three-electrode system; Place the three-electrode system in 10 mL of 0.1 M NaOH solution, and scan 20 segments of cyclic voltammetry in the potential range from –1 V to 1 V to activate the electrodes; then apply a certain anode potential to the working electrode, and record Current-time curve, when the background current reaches a steady state, add hydrogen peroxide standard solution to 0.1 M NaOH solution with a micro-injector; measure the current response value of the sensor to hydrogen peroxide at different concentrations of hydrogen peroxide solution , and in the concentration range of 0.1 μM to 8.2 mM, a linear relationship curve between the current and the hydrogen peroxide concentration was obtained, and the linear correlation coefficientr = 0.997, and the hydrogen peroxide was analyzed and detected by the standard curve method.
作为过氧化氢传感器的修饰玻碳电极的催化作用表征：在含有过氧化氢溶液（0.1 mM）的0.1 M氢氧化钠溶液中在裸玻碳电极（b）、钛酸镍镧负载铁酸钴修饰玻碳电极（a）上的循环伏安图如图1所示。从图中可以看出，裸玻碳电极对于过氧化氢的加入电流几乎没有变化，而钛酸镍镧负载铁酸钴修饰玻碳电极在过氧化氢加入后，在原来基础上峰电流明显增强，说明修饰电极对过氧化氢有明显的催化氧化作用。同样，在搅拌下，向0.1 M的氢氧化钠中依次加入0.1 mM的过氧化氢得到如图2所示时间–电流曲线。在裸电极上电流响应很小，但是在修饰电极上电流响应增大10倍左右，所以利用此曲线也能表明钛酸镍镧负载铁酸钴有很好的催化作用。Catalytic characterization of modified glassy carbon electrodes as hydrogen peroxide sensors: bare glassy carbon electrode (b), nickel lanthanum titanate supported cobalt ferrite in 0.1 M sodium hydroxide solution containing hydrogen peroxide solution (0.1 mM) The cyclic voltammogram on the modified glassy carbon electrode (a) is shown in Fig. 1. It can be seen from the figure that the bare glassy carbon electrode has almost no change in current when hydrogen peroxide is added, while the peak current of the nickel-lanthanum titanate-loaded cobalt ferrite-modified glassy carbon electrode is significantly enhanced after the addition of hydrogen peroxide. , indicating that the modified electrode has an obvious catalytic oxidation effect on hydrogen peroxide. Similarly, under stirring, 0.1 mM hydrogen peroxide was sequentially added to 0.1 M sodium hydroxide to obtain the time-current curve shown in Figure 2. The current response on the bare electrode is very small, but the current response on the modified electrode increases by about 10 times, so this curve can also show that nickel lanthanum titanate supported cobalt ferrite has a good catalytic effect.
电化学检测过氧化氢： 在最佳测试条件下，钛酸镍镧负载铁酸钴修饰玻碳电极对过氧化氢的时间–电流响应如图3所示。由图可见，达到98%稳态电流的时间小于5s，响应时间非常短，随着过氧化氢浓度的增加，传感器对过氧化氢的电流响应逐渐增大，在0.1 mM ~ 8.2 mM范围内，电流与过氧化氢浓度成线性关系，如图3所示。线性方程为I (mA) = 0.2246C (mM) + 14.938，线性相关系数为0.997。Electrochemical detection of hydrogen peroxide: Under the optimal test conditions, the time-current response of the nickel-lanthanum titanate-supported cobalt ferrite-modified glassy carbon electrode to hydrogen peroxide is shown in Figure 3. It can be seen from the figure that the time to reach 98% of the steady-state current is less than 5s, and the response time is very short. As the concentration of hydrogen peroxide increases, the current response of the sensor to hydrogen peroxide gradually increases. In the range of 0.1 mM to 8.2 mM, The current has a linear relationship with the concentration of hydrogen peroxide, as shown in Figure 3. The linear equation is I (mA) = 0.2246C (mM) + 14.938, and the linear correlation coefficient is 0.997.
本发明方法制备的电极，重现性和稳定性良好。对于过氧化氢传感器，11次重复测定的标准偏差为2.3%。电极不用时在4℃存放一星期后，电流响应仍保持为初始电流的95%。且10倍的铟，铬等金属离子，5倍的镍，有轻微的干扰；50倍柠檬酸，10倍的镁离子几乎不干扰测定，5倍的铜离子对测定干扰较大。其最低检测限为23.5 nM。The electrode prepared by the method of the present invention has good reproducibility and stability. For the hydrogen peroxide sensor, the standard deviation of 11 replicates was 2.3%. After the electrode was stored at 4°C for one week when not in use, the current response remained at 95% of the initial current. And 10 times of indium, chromium and other metal ions, 5 times of nickel, have slight interference; 50 times of citric acid, 10 times of magnesium ions hardly interfere with the determination, and 5 times of copper ions interfere greatly with the determination. Its lowest detection limit was 23.5 nM.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103149256A (en)* | 2013-02-27 | 2013-06-12 | 上海大学 | Electrochemical Sensor Modified by SrNiFeO3 Glassy Carbon Electrode and Its Measurement Method for H2O2 |
| CN105181770A (en)* | 2015-09-09 | 2015-12-23 | 上海大学 | Preparation method of manganese dioxide/graphene/titanium dioxide-modified glassy carbon electrode for electrochemical detection of hydrogen peroxide and application of preparation method |
| CN113433187A (en)* | 2021-07-01 | 2021-09-24 | 常州大学 | LaMnO3Electrochemical sensor of chitosan non-enzymatic hydrogen peroxide and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103149256A (en)* | 2013-02-27 | 2013-06-12 | 上海大学 | Electrochemical Sensor Modified by SrNiFeO3 Glassy Carbon Electrode and Its Measurement Method for H2O2 |
| CN105181770A (en)* | 2015-09-09 | 2015-12-23 | 上海大学 | Preparation method of manganese dioxide/graphene/titanium dioxide-modified glassy carbon electrode for electrochemical detection of hydrogen peroxide and application of preparation method |
| CN113433187A (en)* | 2021-07-01 | 2021-09-24 | 常州大学 | LaMnO3Electrochemical sensor of chitosan non-enzymatic hydrogen peroxide and preparation method thereof |
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