新型非汞膜电极的制备及用于重金属离子检测

发布时间：2018-04-10 01:27

本文选题：铋膜电极　切入点：溶出伏安法　出处：《华北理工大学》2017年硕士论文

【摘要】：新型非汞膜电极具有无毒、易制备、电极表面容易更新等优点,着重于制备不同类型的非汞膜电极,通过SEM对电极表面膜进行了表征,并通过阳极溶出伏安法对铅、镉离子进行了检测。研究了不同条件下制备的新型非汞膜电极对重金属离子响应性能的影响。1)采用氢气泡模板法制备铋膜电极,通过阳极溶出伏安法,用该电极检测了铅离子和镉离子,实验结果说明,该电极对铅、镉离子具有良好的响应,沉积电流密度为525 mA/cm2,沉积时间为5 s的条件下制备的铋膜电极性能最好,检测过程中120 s为最佳富集时间。Pb~(2+)和Cd~(2+)灵敏度最高分别可达0.44μA/μg·L-1,0.91μA/μg·L-1。但是由于铋膜玻碳电极在电极的测试过程中容易脱落,因而该电极的重复性和稳定性较差。2)为了提高电极的稳定性,用PEDOT对铋膜电极进行了修饰改性,制备了PEDOT/Bi复合修饰电极。通过阳极溶出伏安法,用该电极检测了铅离子和镉离子,检测结果表明,在沉积电流电压为1.1 V,沉积时间为10 min的条件下,制备的PEDOT/Bi复合修饰电极检测性能最好。Pb~(2+)和Cd~(2+)灵敏度分别可达1.24μA/μg·L-1,1.85μA/μg·L-1。并且对该电极进行了重现性和干扰性的测定。得到镉、铅峰电流的相对标准偏差分别为2.83%,6.68%,证明该电极具有较好的重现性,同时具有较好的稳定性。干扰性实验证明了常见的离子对测定结果的干扰很小。3)采用氢气泡模板法制备了锑膜电极,通过阳极溶出伏安法,用该电极检测了铅离子和镉离子,实验结果说明,沉积电流密度为525 mA/cm2,沉积时间为10 s的条件下制备的锑膜电极性能最好。Pb~(2+)和Cd~(2+)灵敏度分别可达0.34μA/μg·L-1,0.07μA/μg·L-1。发现其灵敏度很低,所以对锑膜电极进行了改进,又制备了铋锑复合电极。检测结果显示,其峰值电流都比较高,线性较好,并且灵敏度也都较高,Cd~(2+)灵敏度为0.61μA/μg·L-1,Pb~(2+)的灵敏度为0.65μA/μg·L-1。以上新型非汞膜电极对重金属离子均具有良好的响应能力,因此可以说明新型非汞膜电极具有较大的应用价值。
[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.
【学位授予单位】：华北理工大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O657.1

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