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Voltammetric Determination of 8-Hydroxy-5-nitroquinoline on a Silver Solid Amalgam Electrode
Bartůňková, Erika ; Vyskočil, Vlastimil (advisor) ; Fischer, Jan (referee)
This Bachelor Thesis is dedicated to the study of the electrochemically active substance 8-hydroxy-5-nitroquinoline. The stability of the prepared standard solution was monitored by UV/VIS spectrometry throughout the electrochemical measurements. A polished silver solid amalgam electrode was chosen as the working electrode. First, the optimum conditions for the measurements were determined by DC voltammetry and differential pulse voltammetry. The calibration dependence was subsequentlymeasuredbybothtechniquesintheconcentrationrangefrom1·10−7 to 1·10−5 mol/L. The DC voltammetry method was also used to measure the calibration dependence in model matrices of drinking and well water in the concetration order of 10−6 mol/L. To further investigate the electrochemical processes and controlling processes in the electrochemical transformation of 8-hydroxy-5-nitroquinoline, the cyclic voltammetry technique was used and applied at different polarization rates.
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Use of a Solid Bismuth Drop Electrode in the Determination of the Drug Metronidazole
Jarošová, Johanka ; Vyskočil, Vlastimil (advisor) ; Fischer, Jan (referee)
The subject of the present Bachelor Thesis was the study of a new commercial solid bismuth drop electrode (SBiDE) and its use to find optimal conditions for the voltammetric determination of the drug metronidazole using the differential pulse voltammetry technique (DPV). The voltammetric behavior of the selected drug was studied as a function of pH of aqueous Britton-Robinson buffer (BR buffer) solution. BR buffer at pH 12 was chosen as the optimal medium for the determination of the drug metronidazole on SBiDE, in which the concentration dependence of metronidazole was measured in the range of 1×10−6 - 6×10−4 mol/L. The limit of quantification (LQ) was 1.38×10−6 mol/L and the limit of detection (LD) was 4.41×10−7 mol/L. The newly developed voltammetric method was used for the determination of metronidazole in the pharmaceutical forms Efloran infusion solution 500 mg/100 mL, Entizol 250 mg tablet, Entizol 500 mg vaginal tablet and Noridem infusion solution 500 mg/100 mL. The selected voltammetric method was compared with the analytical method by UV-VIS absorption spectrometry in the environment of aqueous BR buffer solution at pH 12 in the concentration range of metronidazole 2×10−5 - 8×10−5 mol/L.
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Voltammetric Determination of Warfarin at a Screen-Printed Carbon Electrode
Žužičová, Victória ; Vyskočil, Vlastimil (advisor) ; Dejmková, Hana (referee)
In this Bachelor Thesis, the electrochemical behaviour of the drug warfarin sodium was studied at a screen-printed carbon electrode (SPCE) using DC voltammetry (DCV) and differential pulse voltammetry (DPV). The dependence of the voltammetric behaviour of the substance on the pH of the medium was studied in Britton-Robinson buffer (BR buffer) in the pH range of 2.0−12.0. A pH of 7.0 was chosen as the optimum pH for both voltammetric techniques. A repeatability of 3.8% for DCV and 4.3% for DPV was determined for the selected pH. Calibration dependence was monitored under the selected optimal conditions in the concentration range 2∙10−6 to 1∙10−4 mol∙dm−3 . The limit of detection (LOD) was determined to be 1.05∙10−6 mol∙dm−3 for DCV and 2.59∙10−7 mol∙dm−3 for DPV. The limit of quantification (LOQ) was 3.50∙10−6 mol∙dm−3 for DCV and 8.62∙10−7 mol∙dm−3 for DPV. These newly developed methods were used for the determination of the active ingredient in the pharmaceutical formulation Warfarin Orion 5 mg. The values measured by voltammetric methods were compared with those obtained by spectrophotometric measurements. Key words Electrochemistry, Warfarin, Anticoagulants, Direct Current Voltammetry, Differential Pulse Voltammetry, Screen-Printed Carbon Electrode
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Voltammetric Determination of 2,4-Dichlorophenoxyacetic Acid and 2,4-Dichlorophenol on a Screen-Printed Carbon Electrode
Jančová, Jana ; Vyskočil, Vlastimil (advisor) ; Fischer, Jan (referee)
The aim of the presented Master Thesis was to study an electrochemical behaviour of 2,4-dichlorophenoxyacetic acid (2,4-D) and 2,4-dichlorophenol (2,4-DCP) resulting in the founding of optimum conditions for their voltammetric determination at a screen-printed carbon electrode (SPCE) using DC voltammetry (DCV) and differential pulse voltammetry (DPV). Voltammetric behaviour of both compounds was investigated in dependence on the pH of the medium (realized using Britton-Robinson buffer). The optimum pH for the voltammetric determination of 2,4-D on the SPCE was chosen to be pH 5,0 for both voltammetric techniques, and, for 2,4-DCP, it was chosen to be pH 6,0 for both voltammetric techniques. The determination of 2,4-D at a concentration of 1·10-4 μmol·L-1 showed good repeatability for both voltammetric techniques used (1.3% for DCV and 0.7% for DPV), and, for 2,4-DCP, it showed acceptable repeatability for both voltammetric techniques used (1.3% for DCV and 4.8% DPV). Under optimum conditions, the calibration dependence of 2,4-D was measured for DCV in the concentration range of 10-100 μmol·L-1 , with limit of quantification (LOQ) of 1.0 μmol·L-1 and limit of detection (LOD) 0.3 μmol·L-1 . Under optimum conditions, the calibration dependence of 2,4-D was measured for DPV in the concentration range...
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Electrochemical properties of synthetic drugs 3-fluorophenmetrazine and 4-methylpentedrone
Jiroušková, Eliška ; Schwarzová, Karolina (advisor) ; Dejmková, Hana (referee)
The aim of this Thesis was to clarify electrochemical properties of two new psychoactive substances. These substances are an alternative to classical drugs because they are not controlled by current legislation. It is important to determine the metabolites of these substances to be able to detect them in organism. Their electrochemical properties could explain the process of the first phase of biotransformation in human organism. Two synthetic stimulants were studied - 3-fluorophenmetrazine and 4-methylpentedrone, used as substitutes for cocaine or ecstasy. The purity of substances was controlled by HPLC with UV/Vis diode array detector and the stability was verified by UV/Vis spectrophotometry. Electrochemical properties were studied in phosphate buffer using cyclic voltammetry. For both substances was calculated theoretical HOMO and LUMO spatial distribution. This information was important to estimate parts of molecules, that can be reduced or oxidised. The analytical method was developed on glassy carbon electrode using differential pulse voltammetry. Substance 3-fluorophenmetrazine was determined in phosphate buffer pH 9,0 with limit of detection of 5,1 µmol l-1 . The linear range of calibration curve is from 7,0 to 107,0 µmol/l, R = 0,9988. 4-methylpentedrone was determined in phosphate...
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Voltammetric Determination of Genotoxic Nitrobiphenyls
Horáková, Eva ; Vyskočil, Vlastimil (advisor) ; Navrátil, Tomáš (referee)
The presented diploma thesis is devoted to study of determination of 4-nitrobiphenyl (4-NBP) in model river water by DC voltammetry (DCV) and differential pulse voltammetry (DPV) at m-AgSAE (diploma thesis relates to bachelor thesis, in it DCV and DPV methods for determination of 4-NBP in deionized water were developed). Limit of determination (LOD) is 2·10-7 mol·l-1 by DCV and 4·10-7 mol·l-1 by DPV. The adsorptive stripping DPV (AdSDPV) technique was tested to archive lower LOD the AdSDPV, optimal conditions were not found. Electrochemical behavior of 2-nitrobiphenyl (2-NBP) at m-AgSAE was studied. Optimal conditions for its determination by both techniques DCV and DPV were found in methanol-0,01 mol·l-1 LiOH (1:9) and in this medium peak current dependence in 1·10-7 mol·l-1 to 1·10-4 mol·l-1 2-NBP (LOD ≈ 2·10-7 mol·l-1 by DCV and 1·10-7 mol·l-1 by DPV) concentration range was measured. Developed methods were successfully tested for determination of 2-NBP in drinking and river water samples. For both mediums obtained LODs were 2·10-7 mol·l-1 by DCV and 1·10-7 mol·l-1 by DPV. AdSDPV technique was unsuccessfully tested to achieve lower LOD. Optimal conditions for simultaneous determination of 4-NBP and 2-NBP by DPV technique at m-AgSAE were found: methanol-0,25 mol·l-1 acetate buffer (pH = 6,0) 3:7....
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Voltammetric Determination of Dinitronaphthalenes Using Single Crystal Silver Amalgam Electrode
Tvrdíková, Jana ; Barek, Jiří (advisor) ; Dejmková, Hana (referee)
Voltammetric methods for determination of 1,3-dinitronaphthalene (1,3-DNN), 1,5-dinitronaphthalene (1,5-DNN) and 1,8-dinitronaphthalene (1,8-DNN) using DC voltammetry (DCV) and differential pulse voltammetry (DPV) at novel single crystal silver amalgam electrode (CAgAE) were developed in this work. Developed methods may be used for determination of 1,3-DNN within a concentration range 2 - 10 μmol.L-1 with LoQ 2 μmol.L-1 using DCV and 1 - 100 μmol.L-1 with LoQ 1 μmol.L-1 by DPV; 1,5-DNN wihin a concentration range 2 - 10 μmol.L-1 with LoQ 2 μmol.L-1 using DCV and 1 - 10 μmol.L-1 with LoQ 1 μmol.L-1 by DPV and 1,8-DNN within a concentration range 2 - 10 μmol.L-1 with LoQ 2 μmol.L-1 using DCV and 0,3 - 1 μmol.L-1 with LoQ 0,3 μmol.L-1 by DPV. An attepmt to decrease LoQ by adsorptive stripping differential pulse voltammetry was not successful. Process of electrochemical reduction of selected dinitronaphthalenes on the working electrode was also studied by cyclic voltammetry. This work verified the use of CAgAE as alternative electrode material to mercury electrodes for determination of electrochemically reducible organic compounds in aqueous-methanolic media. Small dimensions of the CAgAE are the main advantages which predetermine its use in voltammetric microvolume batch analysis and amperometric detection in...
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Voltammetric Determination of 5-Nitrobenzimidazole Using Non-Traditional Electrode Materials
Chládková, Barbora ; Vyskočil, Vlastimil (advisor) ; Zima, Jiří (referee)
5 Abstract This Diploma Thesis is targeted on the determination of 5-nitrobenzimidazole (5-NBIA) using following techniques: DC voltammetry (DCV) and differential pulse voltammetry (DPV). As working electrodes, a silver amalgam paste electrode (AgA-PE), which was constructed for this determination in the form of a new prototype, a bismuth film electrode (BiFE), at which the optimum conditions for the deposition of the bismuth film at a suitable substrate (glassy carbon electrode and gold electrode were tested for this purpose) were initially optimized, and a glassy carbon electrode (GCE) were used. The optimum conditions for the voltammetric determination of 5-NBIA at the AgA-PE (in a medium of Britton-Robinson buffer (BR-buffer) of pH 7.0 for both DCV and DPV), at the BiFE with gold substrate (BR-buffer of pH 9.0 for both DCV and DPV; the film was deposited "ex situ" in a stirred plating solution (1000 mg L-1 Bi(III) solution in 0.1 mol L-1 acetate buffer of pH 4.5) for 300 s), and at the GCE (BR-buffer of pH 5,0 for both DCV and DPV). Under these conditions, calibration dependences were measured in the concentration ranges of 0.1 - 100 µmol L-1 (pro DCV a DPV na AgA-PE) and 1 - 100 µmol L-1 (pro DCV a DPV na BiFE a GCE), and the limits of quantification (LQs) were calculated for particular methods: LQ ≈...
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Determination of Lead Using FIA Technique with Spectrophotometric and Electrochemical Detection
Hála, Petr ; Vyskočil, Vlastimil (advisor) ; Rychlovský, Petr (referee)
The aim of this thesis was the determination of lead in water samples using complexating reaction with 4-(2-pyridylazo)-resorcinol in medium of 2-amino-2- hydroxymethyl-propan-1,3-diol hydrochloride buffer (Tris·HCl). Firstly, for the determination was chosen UV/VIS molecular spectrometry in a static arrangement. Subsequently, the method was performed in flow injection arrangement. The calibration was performed under optimal experimental conditions. The limits of detection for static and flow injection arrangements were 0.097 mol dm-3 and 0.27 mol dm-3 , respectively. Secondly, the determination of lead by differential pulse voltammetry was performed. The electrochemical properties of lead complex were investigated. During these experiments it was found out that small amount of this complex was adsorbed on the surface of silver solid amalgam electrode. The calibration was performed, the limit of detection was 0.020 mol dm-3 . Keywords Lead, 4-(2-pyridylazo)-resorcinol, flow injection analysis, UV/VIS molecular spectrometry, differential pulse voltammetry, silver solid amalgam electrode.
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