本文選題：鉍膜電極　切入點(diǎn)：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(wú)毒、易制備、電極表面容易更新等優(yōu)點(diǎn),著重于制備不同類(lèi)型的非汞膜電極,通過(guò)SEM對(duì)電極表面膜進(jìn)行了表征,并通過(guò)陽(yáng)極溶出伏安法對(duì)鉛、鎘離子進(jìn)行了檢測(cè)。研究了不同條件下制備的新型非汞膜電極對(duì)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(guò)陽(yáng)極溶出伏安法,用該電極檢測(cè)了鉛離子和鎘離子,實(shí)驗(yàn)結(jié)果說(shuō)明,該電極對(duì)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(shí)間為5 s的條件下制備的鉍膜電極性能最好,檢測(cè)過(guò)程中120 s為最佳富集時(shí)間。Pb~(2+)和Cd~(2+)靈敏度最高分別可達(dá)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(cè)試過(guò)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(duì)鉍膜電極進(jìn)行了修飾改性,制備了PEDOT/Bi復(fù)合修飾電極。通過(guò)陽(yáng)極溶出伏安法,用該電極檢測(cè)了鉛離子和鎘離子,檢測(cè)結(jié)果表明,在沉積電流電壓為1.1 V,沉積時(shí)間為10 min的條件下,制備的PEDOT/Bi復(fù)合修飾電極檢測(cè)性能最好。Pb~(2+)和Cd~(2+)靈敏度分別可達(dá)1.24μA/μg·L-1,1.85μA/μg·L-1。并且對(duì)該電極進(jìn)行了重現(xiàn)性和干擾性的測(cè)定。得到鎘、鉛峰電流的相對(duì)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(shí)具有較好的穩(wěn)定性。干擾性實(shí)驗(yàn)證明了常見(jiàn)的離子對(duì)測(cè)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(guò)陽(yáng)極溶出伏安法,用該電極檢測(cè)了鉛離子和鎘離子,實(shí)驗(yàn)結(jié)果說(shuō)明,沉積電流密度為525 mA/cm2,沉積時(shí)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(dá)0.34μA/μg·L-1,0.07μA/μg·L-1。發(fā)現(xiàn)其靈敏度很低,所以對(duì)銻膜電極進(jìn)行了改進(jìn),又制備了鉍銻復(fù)合電極。檢測(cè)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(duì)重金屬離子均具有良好的響應(yīng)能力,因此可以說(shuō)明新型非汞膜電極具有較大的應(yīng)用價(jià)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(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類(lèi)號(hào)】：O657.1

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