本文選題：鉍膜電極　切入點：溶出伏安法　出處：《華北理工大學(xué)》2017年碩士論文

【摘要】：新型非汞膜電極具有無毒、易制備、電極表面容易更新等優(yōu)點,著重于制備不同類型的非汞膜電極,通過SEM對電極表面膜進行了表征,并通過陽極溶出伏安法對鉛、鎘離子進行了檢測。研究了不同條件下制備的新型非汞膜電極對重金屬離子響應(yīng)性能的影響。1)采用氫氣泡模板法制備鉍膜電極,通過陽極溶出伏安法,用該電極檢測了鉛離子和鎘離子,實驗結(jié)果說明,該電極對鉛、鎘離子具有良好的響應(yīng),沉積電流密度為525 mA/cm2,沉積時間為5 s的條件下制備的鉍膜電極性能最好,檢測過程中120 s為最佳富集時間。Pb~(2+)和Cd~(2+)靈敏度最高分別可達0.44μA/μg·L-1,0.91μA/μg·L-1。但是由于鉍膜玻碳電極在電極的測試過程中容易脫落,因而該電極的重復(fù)性和穩(wěn)定性較差。2)為了提高電極的穩(wěn)定性,用PEDOT對鉍膜電極進行了修飾改性,制備了PEDOT/Bi復(fù)合修飾電極。通過陽極溶出伏安法,用該電極檢測了鉛離子和鎘離子,檢測結(jié)果表明,在沉積電流電壓為1.1 V,沉積時間為10 min的條件下,制備的PEDOT/Bi復(fù)合修飾電極檢測性能最好。Pb~(2+)和Cd~(2+)靈敏度分別可達1.24μA/μg·L-1,1.85μA/μg·L-1。并且對該電極進行了重現(xiàn)性和干擾性的測定。得到鎘、鉛峰電流的相對標(biāo)準(zhǔn)偏差分別為2.83%,6.68%,證明該電極具有較好的重現(xiàn)性,同時具有較好的穩(wěn)定性。干擾性實驗證明了常見的離子對測定結(jié)果的干擾很小。3)采用氫氣泡模板法制備了銻膜電極,通過陽極溶出伏安法,用該電極檢測了鉛離子和鎘離子,實驗結(jié)果說明,沉積電流密度為525 mA/cm2,沉積時間為10 s的條件下制備的銻膜電極性能最好。Pb~(2+)和Cd~(2+)靈敏度分別可達0.34μA/μg·L-1,0.07μA/μg·L-1。發(fā)現(xiàn)其靈敏度很低,所以對銻膜電極進行了改進,又制備了鉍銻復(fù)合電極。檢測結(jié)果顯示,其峰值電流都比較高,線性較好,并且靈敏度也都較高,Cd~(2+)靈敏度為0.61μA/μg·L-1,Pb~(2+)的靈敏度為0.65μA/μg·L-1。以上新型非汞膜電極對重金屬離子均具有良好的響應(yīng)能力,因此可以說明新型非汞膜電極具有較大的應(yīng)用價值。
[Abstract]:The new non-mercury film electrode has the advantages of non-toxic, easy preparation and easy updating on the electrode surface. It focuses on the preparation of different types of non-mercury film electrode. The surface film of the electrode is characterized by SEM, and lead is characterized by anodic stripping voltammetry.Cadmium ion was detected.The influence of new non-mercury film electrode prepared under different conditions on heavy metal ion response was studied. 1) Bismuth film electrode was prepared by hydrogen bubble template method. Lead ion and cadmium ion were detected by anodic stripping voltammetry.The experimental results show that the electrode has a good response to lead and cadmium ions, and the deposition current density is 525 Ma / cm ~ 2, and the deposition time is 5 s. The bismuth film electrode has the best performance.In the detection process, the best enrichment time was 120s, and the highest sensitivity was 0.44 渭 A / 渭 g L ~ (-1) and 0.91 渭 A / 渭 g ~ (-1), respectively.However, because bismuth film glassy carbon electrode is easy to fall off during the test process, the repeatability and stability of the electrode is poor. 2) in order to improve the stability of the electrode, the bismuth film electrode was modified with PEDOT and the PEDOT/Bi composite modified electrode was prepared.Lead and cadmium ions were detected by anodic stripping voltammetry. The results showed that the deposition current and voltage were 1.1 V and the deposition time was 10 min.The sensitivity of the prepared PEDOT/Bi composite modified electrode is 1.24 渭 A / 渭 g L ~ (-1) and 1.85 渭 A / 渭 g ~ (-1), respectively. The sensitivity of the modified electrode is 1.24 渭 A / 渭 g L ~ (-1) and 1.85 渭 A / 渭 g ~ (-1) of Cd~(2, respectively.The reproducibility and interference of the electrode were determined.The relative standard deviations of peak current of cadmium and lead are 2.83 and 6.68 respectively, which proves that the electrode has good reproducibility and good stability.The interference experiment proved that the interference of common ions to the determination results was very small. 3) Antimony film electrode was prepared by hydrogen bubble template method. The lead ion and cadmium ion were detected by anodic stripping voltammetry. The experimental results show that the antimony film electrode can be used for the determination of lead ion and cadmium ion by anodic stripping voltammetry.When the deposition current density is 525mA / cm ~ 2 and the deposition time is 10 s, the antimony film electrode has the best performance. The sensitivity of antimony film electrode is 0.34 渭 A / 渭 g L ~ (-1) / 渭 g ~ (-1) 渭 A / 渭 g 路L ~ (-1), and the sensitivity of antimony film electrode is 0.34 渭 A / 渭 g ~ (-1) / 渭 g ~ (-1).It was found that its sensitivity was very low, so the antimony film electrode was improved and bismuth antimony composite electrode was prepared.The results show that the peak current is higher, the linearity is better, and the sensitivity is also higher. The sensitivity is 0.61 渭 A / 渭 g L ~ (-1) PbBX ~ (2)) and the sensitivity is 0.65 渭 A / 渭 g ~ (-1).The new non-mercury film electrode has good response ability to heavy metal ions, so it can be concluded that the new non-mercury film electrode has great application value.
【學(xué)位授予單位】：華北理工大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：O657.1

【參考文獻】

相關(guān)期刊論文 前10條

1 張文彬;張長財;;氫氣泡模板法制備多孔鎳用于電催化氧化乙醇[J];應(yīng)用化學(xué);2015年10期

2 夏同馳;張俠;張林森;董會超;李曉峰;;氫氣泡模板法電沉積La-Ni合金薄膜電極[J];電源技術(shù);2015年07期

3 李偉新;;鉍膜電極吸附溶出伏安法測定鉛的研究[J];廣東化工;2015年06期

4 程曉紅;劉一峰;馬紅超;董曉麗;;鉍膜修飾FTO導(dǎo)電玻璃電極檢測溶液中的鉛離子[J];大連工業(yè)大學(xué)學(xué)報;2015年01期

5 雷存喜;劉蓉;沈毓儒;趙運林;董萌;曾戴弟;;預(yù)鍍鉍膜修飾碳糊電極差分脈沖伏安法測定廢水中鉛和鎘[J];分析科學(xué)學(xué)報;2014年06期

6 唐立超;唐美華;石成成;蔡清;張東明;張之翼;王濟奎;陳國松;;Nafion復(fù)合鉍膜修飾絲網(wǎng)印刷電極測定痕量鎘離子[J];現(xiàn)代化工;2014年08期

7 吳志珊;宋偉;韓倩;楊麗莉;許丹科;鐘文英;;鉍膜絲網(wǎng)印刷電極現(xiàn)場快速測定工業(yè)廢水中Pb~(2+)、Cd~(2+)[J];環(huán)境化學(xué);2013年04期

8 應(yīng)海佳;楊慧中;李琳娜;;鉍膜電極差分脈沖溶出伏安法測定鎘[J];光譜實驗室;2013年02期

9 楊海青;彭波;王偉峰;楊梅霞;潘玉瑩;馬永鈞;;復(fù)合鉍膜電極陽極溶出法測定水樣中的痕量銦[J];分析試驗室;2010年01期

10 杜續(xù)生,佘平平,汪正浩;聚乙撐二氧噻吩的導(dǎo)電性及現(xiàn)場ESR響應(yīng)的研究[J];化學(xué)學(xué)報;2003年04期

相關(guān)博士學(xué)位論文 前1條

1 陳晨;用于重金屬離子檢測的電化學(xué)傳感器研究[D];華東理工大學(xué);2013年

相關(guān)碩士學(xué)位論文 前1條

1 尹麗君;合金層過渡鉍膜與銻膜電極的制備及其分析應(yīng)用[D];中國科學(xué)技術(shù)大學(xué);2011年

，

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