鉑-二氧化錳與鉑-聚二苯胺修飾玻璃碳電極測定對苯二酚、鄰苯二酚以及亞硝酸鹽

Determination of hydroquinone, catechol and nitrite at Pt-MnO2 and Pt-polydiphenylamine modified glassy carbon electrodes

盧普良(Pu-Liang Ru)

指導教授 ： 陳生明

國立臺北科技大學/工程學院/化學工程研究所/碩士(2012年)

https://doi.org/10.6841/NTUT.2012.00149

摘要

本研究主要分為兩部分來討論，第一部份我們使用電化學方法製備了鉑-二氧化錳玻璃碳電極，使用循環伏安法和微分脈衝伏安法分析鉑-二氧化錳薄膜修飾電極的電催化特性應用於對苯二酚和鄰苯二酚的並存偵測，利用掃描式電子顯微鏡的特性觀察薄膜的表面形態，這薄膜的表面形態顯示良好的電催化特性並有助於對苯二酚和鄰苯二酚的氧化還原反應，利用循環伏安法分析薄膜偵測對苯二酚和鄰苯二酚的混合溶液顯示出良好的氧化還原波峯，利用微分脈衝伏安法分析鉑-二氧化錳修飾玻璃碳電極偵測對苯二酚和鄰苯二酚的混合溶液，出現明顯的還原波峯，鉑-二氧化錳修飾電極當中的鉑有助於電極表面的電子轉移，可以增加2倍的電流，不同濃度的對苯二酚和鄰苯二酚的偵測結果以線性迴歸表示，偵測的濃度範圍分別為15.7至427 μM 和 19.6至427 μM。
第二部份是利用鉑奈米微粒的特性應用在電催化和感測器上，為了提供一個穩定的載體以穩定鉑沉積和避免污損，本研究藉由電化學方法合成鉑-聚二苯胺複合薄膜沉積在玻璃碳電極上，而利用掃描式電子顯微鏡和電化學阻抗頻譜研究鉑-聚二苯胺複合薄膜特性。使用掃描式電子顯微鏡進行研究，顯示出鉑奈米微粒在聚二苯胺表面有良好的附著性，藉由循環伏安法和計時安培法可研究鉑-聚二苯胺複合薄膜修飾電極的電催化特性，應用在亞硝酸根離子的氧化。循環伏安圖顯示出使用鉑-聚二苯胺複合薄膜修飾電極偵測亞硝酸根離子產生的氧化波峰電壓在0.85 V，在測試過程中的氧化波峰電壓偏移了0.33 V，由此可顯示出鉑-聚二苯胺複合薄膜良好的電催化活性，接續使用計時安培法進行鉑-聚二苯胺複合薄膜測定亞硝酸鹽的定量分析，結果顯示出偵測亞硝酸鹽的濃度範圍可從1 μM至10.6 mM，有良好的線性範圍及不到1秒的應答時間，此鉑-聚二苯胺的複合材料可應用於電化學分析和感測器。

關鍵字

過錳酸鉀 ； 氯鉑酸鉀 ； 對苯二酚 ； 鄰苯二酚 ； 二苯胺 ； 亞硝酸納 ； 鄰苯二甲酸氫鉀 ； 聚二苯胺 ； 鉑 ； 奈米微粒 ； 亞硝酸鹽氧化 ； 計時安培法

並列摘要

Part I： In this study, we report the fabrication of Pt and MnO2 onto a glassy carbon electrode with by electrochemical method. The electrocatalytic property of MnO2-Pt film modified electrode for the simultaneous determination of hydroquinone (HQ) and catechol (CC) was studied by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The surface morphology of the films was characterized by scanning electron microscopy (SEM). The film showed good electrocatalytic activity towards the redox reaction of HQ and CC. CV of the film in a mixture of HQ and CC showed well defined redox peaks. DPV of the HQ and CC at MnO2-Pt modified GCE showed well separated cathodic peaks for HQ and CC. The Pt in the MnO2-Pt film helps the facile electron transfer from MnO2 to the GCE surface, thereby, increasing the current by two folds. The linear range of detection of HQ and CC were 15.7 to 427 μM and 19.6 to 427 μM respectively.
PartⅡ：Platinum nanoparticles found very wide application in electrocatalysis and sensor applications. However, Pt must be deposited in a stable matrix to increase stability and avoid fouling. In this work polydiphenylamine-Pt (Pt-PDPA) composite has been synthesized by electrochemical method on glassy carbon electrode. Pt- PDPA has been characterized by scanning electrochemical microscopy (SEM) and electrochemical impedance spectroscopy (EIS). The SEM studies showed well dispersed Pt nanoparticles on PDPA surface. The electrocatalytic activity of Pt-PDPA film modified electrode towards the oxidation of NO2– was studied by cyclic voltammetry and amperometry. Cyclic voltammograms showed that NO2– undergoes irreversible oxidation at 0.85 V at Pt-PDPA modified electrode which 0.33V less than that of bare GCE. This shows the efficient electrocatalytic activity of the composite film. The electroanalytical application of the composite film was done by amperometric technique. The film shows a response time of less than 1 s and a wide linear range of detection from 1 μM to 10.6 mM. Pt-PDPA is a promising material for electrochemical and biosensor applications.

並列關鍵字

Potassium manganate ； Potassium chloroplatinate ； Hydroquinone ； Catechol ； Diphenylamine ； Sodium Nitrite ； Potassium Hydrogen Phthalate ； Polydiphenylamine ； Platinum ； nanoparticle ； nitrite oxidation ； amperometry.

參考文獻

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