本文選題：電化學傳感器 + 同時檢測�。� 參考：《遼寧大學》2017年碩士論文

【摘要】：環(huán)境污染物的分析與檢測對環(huán)境保護和人類健康具有十分重要的意義。電化學方法相比于其他傳統(tǒng)的檢測手段來說,具有響應速度快、高靈敏、低成本和小型化等優(yōu)點,已經(jīng)在食品安全和環(huán)境保護等方面引起了廣泛關(guān)注。本論文成功制備了ILs-CaFe_2O_4/MWCNTs、ZnFe_2O_4/SWCNTs和ILs@NiCo_2O_4-P三種新型雙金屬納米復合電極材料,構(gòu)筑新型環(huán)境污染物電化學傳感器并建立了相關(guān)檢測體系,實現(xiàn)了對農(nóng)藥多菌靈(CBZ)、噻菌靈(TBZ)和有毒金屬(Tl~+、Pb~(2+)、Cu~(2+))的分析。本論文主要開展工作如下:合成ILs-CaFe_2O_4/MWCNTs納米復合材料,建立了CBZ的電化學分析方法。該材料具有良好的分散性和導電性。運用循環(huán)伏安法(CV)探究了CBZ在修飾電極上的電化學行為,研究發(fā)現(xiàn)CBZ在ILs-CaFe_2O_4/MWCNTs/GCE上發(fā)生擴散控制的不可逆的氧化反應過程,且為兩電子兩質(zhì)子參與的電化學過程�；贗Ls-CaFe_2O_4和MWCNTs之間的協(xié)同作用,該傳感器對CBZ的氧化表現(xiàn)出優(yōu)異的電催化能力,大大提高了CBZ的電化學響應信號。研究了實驗條件對CBZ電化學行為的影響。在pH 4.0的PBS中,CBZ的線性濃度范圍是0.03~105.0μmol/L,檢出限(LOD)為9.41 nmol/L(S/N=3)。該方法成功實現(xiàn)了蘋果、西紅柿和稻田水中CBZ的檢測,加標回收率在94.7%到105.5%之間,并具有良好的穩(wěn)定性和重現(xiàn)性。通過一步水熱合成方法制備Zn Fe_2O_4/SWCNTs復合材料,構(gòu)筑了Zn Fe_2O_4/SWCNTs/GCE傳感器,應用于CBZ和TBZ的同時定量測定。該修飾電極具有高的導電性和大的電極表面積,有效提高了CBZ和TBZ與電極之間的電子轉(zhuǎn)移能力。運用循環(huán)伏安法(CV)和差分脈沖伏安法(DPV)研究了CBZ和TBZ在ZnFe_2O_4/SWCNTs/GCE上的電化學行為。研究了不同因素對CBZ和TBZ電化學信號的影響,并探究了相關(guān)的電化學反應機理。結(jié)果表明,CBZ的電化學反應為吸附控制的準可逆的氧化還原反應過程,TBZ表現(xiàn)為擴散控制的不可逆的氧化反應過程。在pH 7.0的PBS中,CBZ和TBZ均在0.5~100.0μmol/L濃度范圍內(nèi)呈線性,LOD(S/N=3)分別為0.09和0.05μmol/L。該傳感器成功應用于實際樣品中CBZ和TBZ的同時測定,且具有良好的穩(wěn)定性和抗干擾能力。成功制備三種形貌的NiCo_2O_4(NiCo_2O_4納米粒子(NiCo_2O_4-N)、NiCo_2O_4納米片(NiCo_2O_4-P)和NiCo_2O_4納米微球(NiCo_2O_4-S))作為電極修飾材料。對比實驗發(fā)現(xiàn)電化學性能依賴于電極材料的種類、形貌、比表面積等特征,因此,高表面的多孔性的NiCo_2O_4-P材料被選擇作為電極材料。本實驗中,用高導電的ILs代替?zhèn)鹘y(tǒng)的碳材料,結(jié)合高吸附性的NiCo_2O_4-P,構(gòu)建ILs@NiCo_2O_4-P/GCE,實現(xiàn)了對Tl~+,Pb~(2+)和Cu~(2+)的同時檢測。由于其具有獨特的多孔結(jié)構(gòu)、高的比表面積和良好的電子傳導性,該修飾電極表現(xiàn)出優(yōu)異的電化學活性。在pH 4.0的HAc-NaAc溶液中,運用差分脈沖溶出伏安法(DPASV)實現(xiàn)了對Tl~+,Pb~(2+)和Cu~(2+)的同時分析,T1+,Pb~(2+)和Cu~(2+)分別在0.1~100.0、0.1~100.0和0.05~100.0μg/L的濃度范圍內(nèi)表現(xiàn)出良好的線性關(guān)系,LOD(S/N=3)分別為0.046、0.034和0.029μg/L。傳感器成功應用于水樣和土壤樣品中金屬離子含量的測定,結(jié)果令人滿意,具有實際應用價值。
[Abstract]:The analysis and detection of environmental pollutants is of great significance for environmental protection and human health. Compared with other traditional methods, electrochemical methods have many advantages, such as fast response, high sensitivity, low cost and miniaturization. It has attracted wide attention in food safety and environmental protection. This paper has been successful in this paper. Three kinds of new bimetal nanocomposite electrode materials ILs-CaFe_2O_4/MWCNTs, ZnFe_2O_4/SWCNTs and ILs@NiCo_2O_4-P were prepared to construct a new electrochemical sensor for environmental pollutants and establish a related detection system. The analysis of pesticide carbendazim (CBZ), TBZ (TBZ) and toxic metals (Tl~+, Pb~ (2+) and Cu~ (2+)) was analyzed. This paper was mainly carried out in this paper. The following work is as follows: the synthesis of ILs-CaFe_2O_4/MWCNTs nanocomposites and the electrochemical analysis of CBZ have been established. The material has good dispersion and conductivity. The electrochemical behavior of CBZ on the modified electrode is investigated by cyclic voltammetry (CV), and the irreversible oxidation of CBZ on ILs-CaFe_2O_4/MWCNTs/GCE has been found. The reaction process, and the electrochemical process involved in the two electron two protons. Based on the synergy between ILs-CaFe_2O_4 and MWCNTs, the sensor shows excellent electrocatalytic ability for the oxidation of CBZ and greatly improves the electrochemical response signal of CBZ. The influence of the experimental conditions on the electrochemical behavior of CBZ is studied. In the PBS of pH 4, the linearity of CBZ The concentration range is 0.03~105.0 mu mol/L and the detection limit (LOD) is 9.41 nmol/L (S/N=3). This method successfully realized the detection of CBZ in apple, tomato and rice field water, and the recovery rate was between 94.7% and 105.5%, and it had good stability and reproducibility. The Zn Fe_2O_4/SWCNTs composite was prepared by one step water heating method, and Zn Fe_2O was constructed. The _4/SWCNTs/GCE sensor is applied to the simultaneous quantitative determination of CBZ and TBZ. The modified electrode has high conductivity and large electrode surface area, which effectively improves the electron transfer ability between CBZ and TBZ and electrodes. The electrochemical behavior of CBZ and TBZ on ZnFe_2O_4/SWCNTs/GCE is studied by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The effects of different factors on the electrochemical signals of CBZ and TBZ were studied and the mechanism of the electrochemical reaction was explored. The results showed that the electrochemical reaction of CBZ was a quasi reversible redox reaction process of adsorption control, and TBZ was an irreversible oxidation reaction over the diffusion control. In PBS of pH 7, CBZ and TBZ were in 0.5~100.0 micron mo. The l/L concentration range is linear, LOD (S/N=3) is 0.09 and 0.05 mol/L. respectively. The sensor is successfully applied to the simultaneous determination of CBZ and TBZ in actual samples, and has good stability and anti-interference ability. The three morphologies of NiCo_2O_4 (NiCo_2O_4 nanoparticles (NiCo_2O_4-N), NiCo_2O_4 nanoscale (NiCo_2O_4-P) and NiCo_2O_4 Na) are successfully prepared. Mi Weiqiu (NiCo_2O_4-S) was used as an electrode modification material. The comparison experiment found that the electrochemical performance depended on the types, morphology, surface area and other characteristics of the electrode materials. Therefore, the porous NiCo_2O_4-P material on high surface was selected as the electrode material. In this experiment, the high conductivity ILs was used instead of the traditional carbon material and the high adsorptive NiCo_ was used. 2O_4-P, constructed ILs@NiCo_2O_4-P/GCE, realized simultaneous detection of Tl~+, Pb~ (2+) and Cu~ (2+). Because of its unique porous structure, high surface area and good electronic conductivity, the modified electrode showed excellent electrochemical activity. In HAc-NaAc solution of pH 4, the differential pulse stripping volt (DPASV) was used to realize the Tl. The simultaneous analysis of ~ +, Pb~ (2+) and Cu~ (2+) shows that T1+, Pb~ (2+) and Cu~ (2+) show a good linear relationship in the concentration range of 0.1~100.0,0.1~100.0 and 0.05~100.0 micron respectively. The results are successfully applied to the determination of metal ions in water samples and soil samples, respectively. The results are satisfactory. Practical application value.
【學位授予單位】：遼寧大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：X830;O657.1

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