3 resultados para end-column amperometric detection

em AMS Tesi di Laurea - Alm@DL - Università di Bologna


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In this thesis we have identified two electrochemical procedures for preparing two compounds of copper hexacyanoferrate (CuHCF) films with different compositions and structures. The deposition were carried out using a “two steps” method consisting in electrochemical oxidation of previously deposited metallic copper on carbon substrates (glassy carbon and graphite foil electrodes) in K3[Fe(CN)6] solution. Both films, CuHCF-methodA and CuHCF-methodB, were characterized by cyclic voltammetry (GC) and their study using XANES spectroscopy revealed evidence of different structures. Additionally, insertion and extraction of different cations (Na+, K+, Mg2+, Al3+ and Cs+) were performed and the results indicate that CuHCF-methodA has slightly better performances and operational stability than CuHCF-methodB. Data from galvanostatic charge-discharge tests confirme the latter observation. An application for amperometric detection of H2O2 and SEM micrographs are also reported for both films (method A and B). Comparing these results with a previous work of our research group, seems that the deposition of two different compounds using methodA and methodB is due to the different stoichiometry of ions Cu2+ e [Fe(CN)6]3– created near electrode surface during the dissolution step.

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The aminothiols are critical cellular components that play numerous and important roles in metabolism as key extracellular reducing agents, critical substrates for proteins synthesis and detoxificants of free radicals and peroxides. Because altered thiols levels in body fluids are linked to specific pathological conditions, their measurement is thus considered very important. One method to determine these compounds is the capillary electrophoresis, a technique that involves the separation of charged molecules on the basis of their movement under the influence of an applied electric field. The instrument used in this work is equipped with an amperometric detector recording the current of the thiols oxidized at the end of the capillary at a BDD electrode. The aim of this work is to find a valid method for the separations of the aminothiols analyzed, in terms of capillary coating and experimental conditions. In order to find an alternative and less expensive electrode than BDD and to increase sensitivity for the detection of the thiols, a modified electrode consisting in a carbon paste electrode containing Cobalt-phthalocyanine has been studied. In this electrode Cobalt-phthalocyanine works as electrocatalyst to enhance the oxidation reaction, meanwhile the graphite acts as conductive mean. This kind of electrode shows great sensibility and low detection limits for the thiols that have a free thiolic group, but it is not sensible to disulfides. The analysis of human plasma point out that the best method found for the capillary electrophoresis is not useful for the detection of aminothiols in a healthy person, because the very low concentrations in which they are present.

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This thesis is aimed to assess similarities and mismatches between the outputs from two independent methods for the cloud cover quantification and classification based on quite different physical basis. One of them is the SAFNWC software package designed to process radiance data acquired by the SEVIRI sensor in the VIS/IR. The other is the MWCC algorithm, which uses the brightness temperatures acquired by the AMSU-B and MHS sensors in their channels centered in the MW water vapour absorption band. At a first stage their cloud detection capability has been tested, by comparing the Cloud Masks they produced. These showed a good agreement between two methods, although some critical situations stand out. The MWCC, in effect, fails to reveal clouds which according to SAFNWC are fractional, cirrus, very low and high opaque clouds. In the second stage of the inter-comparison the pixels classified as cloudy according to both softwares have been. The overall observed tendency of the MWCC method, is an overestimation of the lower cloud classes. Viceversa, the more the cloud top height grows up, the more the MWCC not reveal a certain cloud portion, rather detected by means of the SAFNWC tool. This is what also emerges from a series of tests carried out by using the cloud top height information in order to evaluate the height ranges in which each MWCC category is defined. Therefore, although the involved methods intend to provide the same kind of information, in reality they return quite different details on the same atmospheric column. The SAFNWC retrieval being very sensitive to the top temperature of a cloud, brings the actual level reached by this. The MWCC, by exploiting the capability of the microwaves, is able to give an information about the levels that are located more deeply within the atmospheric column.