普鲁士兰修饰碳黑微电极同时微分伏安法测定多巴胺和抗坏血酸

将含有1.0%普鲁士蓝的碳黑与固体石蜡按2.5∶1(质量比)混合后装入φ0.2mm的石英毛细管中,在其上端插入一铂丝并抛光后即制成普鲁士蓝修饰碳黑微电极.对多巴胺(DA)及抗坏血酸(VC)在此电极上的电化学行为及应用此电极测定两组分的最佳条件进行了研究,在定量测定中采用二次微分线性扫描伏安法.在最佳条件下,DA与VC的峰电流(i″p)分别与各自的浓度保持如下线性关系DA为4.0×10-6～8.0×10-4mol·L-1,VC为6.0×10-5～1.0×10-3mol·L-1;检出限(3σ)依次为2.0×10-6mol·L-1及1.0×10-5mol·L-1.应用此方法分析了3种含DA及VC的混合溶液,测得结果的相对标准偏差(n=8)依次小于2.0%及3.0%,回收率范围依次为96.5%～101.0%及95.0%～102.5%.     

同时测定血清中4种电解质的流动注射微电极串联电化学自动分析系统

基于流动注射-微电极串联的动态电化学技术,建立了能快速、自动、同时测定血清中K(+),Na(+),Cl(-)和Ca(2+)的分析方法和系统,并成功用于血清样品的测定.为稳定4种电极的基线电位、加快电极响应速度,优化了载流的组分:23mmol/L Na2B4O7-H3BO3(pH 7.40),0.25mmol/L K(+...     

微电极结构Ag/ZnO/NiO三层复合膜的制备及光催化性能的研究

通过溶胶-凝胶结合光还原沉积法在普通玻璃片上制备了Ag-ZnO-NiO系复合薄膜。使用SEM,PL,XRD,UV-Vis等手段对薄膜的表面形貌,物相组成及光学性质作了考察和研究。XRD和UV-Vis分析表明复合薄膜中包含NiO和ZnO的双层异质结构;FESEM结果表明Ag和ZnO分别在其各自的衬底上生长但没有形成完全覆盖,PL光谱表明三层膜的发光强度小于双层膜和单层膜。使用甲基橙为模型底物测试了薄膜在紫外线下的光催化氧化能力,结果表明,三层复合薄膜Ag/ZnO/NiO的活性相比氧化锌单层薄膜和双层薄膜有不同程度的提高。这是由于上层薄膜不能完全包裹下层膜,导致在表面形成了许多微电极结构,这些微电极结构能够使光生电子空穴对得到有效分离。     

用丝网印刷技术制备薄膜微电极的方法研究

对丝网印刷术在微电极制备方面的应用作了系统和详尽的描述,对绷网、制阳图底板、涂布感光胶、晒网、显影、坚膜、印刷等印制各步骤中所需注意事项和技巧作了总结。考察了标记方式、曝光时间、显影时间等的影响,并在优化条件下制成了微电极。用1mmol／L铁氰化钾在微电极上进行循环伏安扫描实验。结果表明,所制得的微电极条具有良好的电化学性能。用此方法可大批量制得廉价的适用于电化学研究和应用的微电极条。     

Localized dissolution electrochemistry at surface irregularities of pipeline steel

The localized electrochemical dissolution behavior at surface irregularities, including scratch, mechanically induced hole and corrosion pit, on pipeline steel was investigated in both near-neutral pH and high pH solutions by scanning vibrating micro-electrode and localized electrochemical impedance spectroscopy measurements. In near-neutral pH solution, the localized dissolution behavior at surface irregularities is dependent of their geometrical depth, which is critical to development of a local electrochemical condition to support the further localized dissolution. Therefore, surface irregularities exceeding a certain depth provide potential sites to initiate stress corrosion cracks in near-neutral pH solution. The strong passivating capability of high pH solution would result in the formation of oxide film over the whole electrode surface to “equalize” the electrochemical activity at irregularities to the intact area. Therefore, the irregularities would not result in localized dissolution electrochemistry. Consequently, localized corrosion and crack initiation are not anticipated to initiate from the geometrical irregularities in high pH solution. However, corrosion pits generating due to passive film breakdown could support the high local dissolution kinetics in high pH solution, providing potential sites for crack initiation. The effects of hydrogen-charging on anodic dissolution at regularities depend on the defect geometry and the solution pH.     

示差脉冲阳极溶出伏安法测定莲子芯中微量铅

采用自制丝网印刷微电极,结合阳极溶出法对微波消解后的莲子芯中的微量铅进行了测定.考察了微波消解条件、缓冲溶液pH值、富集电位、富集时间、脉冲强度、脉冲周期等对检测的影响.试验结果表明:在pH 3.6的乙酸-乙酸钠缓冲溶液中,-1.1 V富集10 s后,电流与铅的质量浓度在1～1 000μg·L-1范围内呈线性关系,相关系数为0.996.测定结果的相对标准偏差(n=5)小于5%,加标回收率为101.9%.     

利用毛细管效应的反射式显微红外光谱电化学池的设计与表征

报道一种新型的适用于水和非水溶剂的反射式现场显微红外光谱电化学池。该池利用毛细管效应来克服显微池中溶剂挥发和除氧的困难，保证电解薄层能长时间保持浸润和良好的工作状态。安装了５０μｍ直径的铂微盘工作电极，分别在水溶液和二氯甲烷溶液中，用Ｆｅ（ＣＮ）６＾４－／３－和二茂铁体系进行了表征。     

Preparation and characterization of carbon paste micro-electrode based on carbon nanoparticles

The present paper demonstrates the preparation and characterization of micro-electrodes based on carbon paste which is composed of carbon nano-particles with an average diameter of 30 nm and binding oil. The carbon paste electrode material is encased in pulled glass capillaries ranging in diameter from several tens down to less than ten micro-meters (r = 4.5 μm). Manipulation of the carbon paste micro-electrode (CPME) was accomplished via newly developed piston-driven system which construction and related problems are presented. Several parameters influencing the CPME performance including carbon paste composition and its electrochemical activation/preconditioning were investigated. Basic electrochemical behavior and properties were examined using typical redox system, i.e. potassium hexacyanoferrate. Applicability of the proposed carbon paste micro-electrode is illustrated by measuring some potentially interesting organic and inorganic analytes such as dopamine, ascorbic acid and selected heavy metals.