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Microtitrimetry by differential electrolytic potentiometry using metallic electrodes and nanomaterials modified metallic electrodes

Posted on:2013-05-23Degree:Ph.DType:Dissertation
University:King Fahd University of Petroleum and Minerals (Saudi Arabia)Candidate:Amro, Abdulaziz NabilFull Text:PDF
GTID:1451390008488150Subject:Chemistry
Abstract/Summary:
For the first time silver wire electrodes have been coated with carbon nanotubes using floating catalyst chemical vapor deposition (CVD) method. The production of CNTs has been conducted in a horizontal tubular reactor. Acetylene gas was used as a carbon source. Ferrocene has been used as a catalyst precursor for the growth of CNT. Different parameters have been optimized to get a high yield of CNTs and ensure their growth on the silver electrodes using univariate method. The parameters studied include the hydrogen flow rate, acetylene flow rate, temperature of the furnace, time of the reaction and the location of the electrodes in the reactor tube. The optimum conditions for those parameters were: for hydrogen and acetylene, the flow rates were 25 mL /min and 75 mL / min respectively. The furnace temperature was found to be 700 °C and the reaction time was 15 minutes. Regarding the location of the silver wires it should be located in the first 10 cm of the front side of the tube. Scanning electron microscopy (SEM) and transition electron microscopy (TEM) have been used to characterize carbon on silver electrodes. According to the experimental results, TEM figures show that CNT produced on Silver wire is multiwall carbon nanotubes MWCNT.;Silver electrodes either pure or coated with CNT were used as indicating systems in micro titration using both dc differential electrolytic potentiometry (DEP) and mark-space bias DEP techniques. All types of titrimetric reactions were investigated using different types of electrodes like Pt and gold for oxidation reduction titrations, antimony electrodes for acid base titrations, silver electrodes for precipitation titrations in addition to Ag-CNT electrodes. End points at volumes of 1 µL were determined. Different parameters were optimized like the current density, the percentage bias, the volume of the sample and the concentrations of the reactants. Microtitrimetry has been applied on several types of analytes; Ferrous, Ascorbic acid, chloride, Cyanide, Sodium Bicarbonate and Ketoconazole in aqueous and non- aqueous medium. The performance of Ag-CNT electrodes was found to be much better than the normal silver electrodes. The differential titration curves obtained were symmetrical with significant heights. For silver electrodes coated with CNT the first derivative of the potential was found to give better curves than the normal differential curves, hence the end point location was successfully achieved. A micro liter injector that can deliver volumes at a micro liter level was designed and fabricated. Microtitrimetry which requires volumes of reagents at the micro liter level can offer a solution to the large consumption of reagents in all classical titrimetric processes. Hence, large savings in reagents as well as less waste will reach the environment.
Keywords/Search Tags:Electrodes, Using, Silver, Micro, Differential, CNT, Carbon
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