Study on Synthesis of Metallic Complex and Application in Electroanalysis Chemistry

　　Study on Synthesis of Metallic Complex and Application in Electroanalysis Chemistry
　　Many metal organic complexes and organic compounds are widely used as carrier of ion-selective electrode because of special planar coordinated, this is a new cross domain with widely developing prospect among metal organic chemistry, chemical sensor and even more other subjects. Design and synthesis of excellent ion-selectivity electrodes has been one of the important areas in the research of chemical sensors. In this paper, the research focuses on the development of new Cube neodymium magnet solvent polymeric membrane (SPM) ion selective electrodes based on the novel metallic complex as neutral carriers. They can be applied as electrochemical sensors in practice sample analysis.PartⅠof this thesis deals with design of neutral carrier for solvent polymeric membrane salicylate electrode with high selectivity1. o-N-salicylidene-aminophenol-imidazole metallic complexes of copper (Ⅱ) and nickel (Ⅱ) were synthesized. We firstly study the potentiometric response characteristics of the anion-selective solvent polymeric membrane electrode based on complex of Cu(Ⅱ) as neutral carrier, which demonstrates excellent selectivity toward the salicylate ion (Sal-) and anti-Hofmeister selectivity sequence: Sal-, ClO4-, SCN-, I-, NO2-, CI-, F-, Br-, H2PO4-. The electrode exhibits a near-Nemstian potentiometric response in the range 3.0×10-6～1.0x10-1 mol/L with a detection limit of 1.5x10-6 mol/L and a slope of -58.7mV/dec. in pH 4.0 of phosphate buffer solution at 20℃. The response mechanism is discussed in view of the AC. The electrode can be applied to the determination of salicylate in pharmaceutical preparations with satisfactory results.2. The anion response characteristics of o-N-salicylidene-aminophenol metallic complexes as carrier are described. The results show that the electrode based on o-N-salicylidene-aminophenol copper(Ⅱ) [Cu(o-NSAP)] demonstrates excellent potentiometric response towards salicylate (Sal-) and anti-Hofmeister selectivity sequence in following order: Sal-, ClO4-, SCN-, I-, Cl-, NO2-, F-, Br-, H2PO4-.
　　The electrode demonstrates a near-Nemstian potentiometric response in the range 1.0×10-5～1.0×10-1 mol/L with a detection limit of 5.8×10-6 mol/L and a slope of -59.1 mV/dec, in pH 4.0 of phosphate buffer solution at 25℃. The response mechanism of the electrode was also studied with the AC impedance technique. The electrode can be applied to the determination of salicylate in pharmaceutical preparations with satisfactory results.3. We study the potentiometric response characteristics of the anion-selective PVC membrane electrode based on [La(Ⅲ)(Phen)(Oxine)] complex as neutral carrier, which displays a preferential response to salicylate and an anti-Hofmeister selectivity sequence in following order: Sal-, ClO4-, SCN-, I-, Br-, NO2-, SO32-, Cl-, SO42-. The electrode exhibits a quasinernstian response with a linear range of 1.0×10-5～1.0×10-1mol/L, a detection http://www.chinamagnets.biz limit of 9.8×10-6 mol/L and aslope of -58.5 mV/dec, in pH 4.0 of phosphoratebuffer solution at 20℃. The response mechanism is discussed in view of the AC impedance technique. The electrode can be applied to medicine analysis.PartⅡof this thesis deals with design of neutral carrier for solvent polymeric membrane mercury (Ⅱ) electrode with high selectivity.A novel PVC (polyvinyl chloride) membrane electrode that exhibits high potentiometric response for Hg2+ based on bis(amino-triazole sulfurethers) (BATS) as an suitable neutral carrier was developed. The electrode exhibits a wide concentration range of 1.0×10-5～1.0×10-1 mol/L (the limit of detection is 8.5×10-6 mol/L) for Hg(NO3)2 with a Nemstian slope of 33.4 mV/dec, at pH 2.0. It has a fast response time of about 10 s and can be used for at least 2 months. The membrane sensor could be used in pH range of 1.3-3.3 and revealed good selectivity for Hg2+ over a wide variety of other metal ions. The response mechanism is discussed in view of the AC impedance technique. The electrode was applied to the determination of mercury in different samples and binary mixtures with satisfactory results.