【摘要】：杯芳烴具有較豐富的活性位點、高度選擇性空腔、以及優(yōu)秀的電子傳導(dǎo)能力,故而基于杯芳烴及衍生物制備的化學(xué)修飾電極在電化學(xué)分析檢測中扮演重要角色。本文制備了三種杯芳烴及衍生物修飾碳糊電極,研究了銅離子、汞離子、鉛離子及對苯二酚的電化學(xué)行為。主要內(nèi)容概括如下:(1)以對叔丁基杯[4]芳烴(H4L)為修飾劑通過直接混合法制備了H4L-CPE,并采用電化學(xué)法對電極性能進(jìn)行了表征。在該修飾碳糊電極上研究了Cu~(2+)的電化學(xué)行為,得出了一些重要的電化學(xué)參數(shù),并與Cu~(2+)在裸碳電極的電化學(xué)行為作了對比,結(jié)果發(fā)現(xiàn)Cu~(2+)在該修飾電極上出現(xiàn)明顯的特征吸收峰,說明該修飾電極對Cu~(2+)有明顯的電催化作用。在最優(yōu)條件下,通過循環(huán)伏安法探究了氧化峰電流值與Cu~(2+)濃度之間的線性關(guān)系,結(jié)果發(fā)現(xiàn)Cu~(2+)濃度在2.5×10-7~1.0×10-5 mol/L范圍內(nèi)呈良好線性關(guān)系,最低檢出限1.33×10-8 mol/L(按3倍信噪比計算)。利用對叔丁基杯芳[4]烴修飾的碳糊電極對Cu~(2+)的檢測有較好的穩(wěn)定性和重現(xiàn)性,為高靈敏度、高選擇性測定痕量Cu~(2+)提供了一種新的方法。(2)以硫雜杯[4]芳烴為修飾劑制備了硫雜杯[4]芳烴修飾碳糊電極,懫用循環(huán)伏安法研究該修飾電極對Pb~(2+)和對苯二酚的電化學(xué)行為。在該修飾電極上研究了Pb~(2+)和對苯二酚的電化學(xué)行為,并繪制了Pb~(2+)和對苯二酚的標(biāo)準(zhǔn)曲線。由曲線可知Pb~(2+)濃度在1.0×10-7~1.0×10-5 mol/L的區(qū)間擁有良好線性關(guān)系,最低檢出限是1.56×10-8 mol/L;對苯二酚濃度在5.0×10-8~1.0×10-5 mol/L的區(qū)間內(nèi)線性關(guān)系良好,最低檢出限為6.5×10-8 mol/L。研究了干擾物質(zhì)的影響和模擬水樣的檢測。該修飾電極制備簡單,選擇吸附能力強,成本低,靈敏度高、抗干擾能力強,可用于制備檢測Pb~(2+)和對苯二酚的電化學(xué)傳感器。(3)以硫雜杯-4-冠-6為修飾劑制備了硫雜杯-4-冠-6修飾碳糊電極。該修飾電極具有豐富的活性位點和較小的電子轉(zhuǎn)移阻力。懫用循環(huán)伏安法考察Hg~(2+)在該修飾電極上的電化學(xué)行為,研究了影響電極性能的可能因素并得到了相關(guān)電化學(xué)參數(shù),線性響應(yīng)范圍為1.0×10-8~1.0×10-5 mol/L,最低檢出限為7.62×10-9 mol/L,對模擬水樣的加標(biāo)回收,結(jié)果令人滿意。
[Abstract]:Calixarene has abundant active sites, highly selective cavity and excellent electronic conductivity. Therefore, chemically modified electrodes based on calixarene and its derivatives play an important role in electrochemical analysis. Three kinds of calixarene and their derivatives modified carbon paste electrodes were prepared. The electrochemical behaviors of copper, mercury, lead and hydroquinone were studied. The main contents are summarized as follows: (1) H4L-CPE was prepared by direct mixing method with p-tert-Ding Ji calix [4] arene (H4L) as modifier, and the electrode performance was characterized by electrochemical method. The electrochemical behavior of Cu~ (2) was studied at the modified carbon paste electrode. Some important electrochemical parameters were obtained and compared with the electrochemical behavior of Cu~ (2) at the bare carbon electrode. The results show that Cu~ (2) has obvious characteristic absorption peak on the modified electrode, which indicates that the modified electrode has obvious electrocatalytic effect on Cu~ (2). Under the optimal conditions, the linear relationship between the oxidation peak current value and the concentration of Cu~ (2) was investigated by cyclic voltammetry. The results showed that the concentration of Cu~ (2) was linear in the range of 2.5 脳 10 -7 渭 m 1.0 脳 10 -5 mol/L. The lowest detection limit is 1.33 脳 10 ~ (-8) mol/L (3 times signal-to-noise ratio). The carbon paste electrode modified with p-tert-Ding Ji calix [4] hydrocarbon has good stability and reproducibility for the detection of Cu~ (2). A new method for the determination of trace Cu~ (2) with high selectivity is provided. (2) Thiocuca [4] arene modified carbon paste electrode has been prepared by using thiachax [4] arene as modifier. The electrochemical behavior of the modified electrode for Pb~ (2) and hydroquinone was studied by cyclic voltammetry. The electrochemical behaviors of Pb~ (2) and hydroquinone were studied at the modified electrode, and the standard curves of Pb~ (2) and hydroquinone were drawn. The curve shows that the concentration of Pb~ (2) is linear in the range of 1.0 脳 10 ~ (-7) mol/L and the lowest detection limit is 1.56 脳 10 ~ (-8) mol/L;. The linear range of hydroquinone concentration is 5.0 脳 10 ~ (-8) mol/L for 1.0 脳 10 ~ (-5) mol/L, and the lowest detection limit is 6.5 脳 10 ~ (-8) mol/L.. The influence of interfering substances and the detection of simulated water samples were studied. The modified electrode has the advantages of simple preparation, strong selective adsorption ability, low cost, high sensitivity and strong anti-interference ability. It can be used to prepare electrochemical sensors for the detection of Pb~ (2) and hydroquinone. (3) Thiaza-4-crown-6 modified carbon paste electrode was prepared with thiaza-4-crown-6 as modifier. The modified electrode has abundant active sites and small electron transfer resistance. The electrochemical behavior of Hg~ (2) on the modified electrode was investigated by cyclic voltammetry. The possible factors affecting the performance of the modified electrode were studied and the related electrochemical parameters were obtained. The linear response range was 1.0 脳 10-8 mol/L,. The minimum detection limit is 7.62 脳 10 ~ (-9) mol/L, for the recovery of simulated water samples, and the results are satisfactory.
【學(xué)位授予單位】：中北大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：O657.1

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