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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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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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Voltammetric Determination of 5-Nitroimidazole - The Structural Unit of Nitroimidazole Drugs
Šmídková, Monika ; Vyskočil, Vlastimil (advisor) ; Fischer, Jan (referee)
Presented Diploma Thesis deals with the study of electrochemical behavior of 5-nitroimidazole (5-NI), with the search for optimal conditions for its determination using techniques of DC voltammetry (DCV) and differential pulse voltammetry (DPV) at a mercury meniscus modified silver solid amalgam electrode (m-AgSAE) and at a boron-doped diamond film electrode (BDDFE), and with the comparison of reached limits of quantification (LQs). The optimal conditions found for measuring calibration dependences of 5-NI at the m-AgSAE in deionized water were as follows: Britton-Robinson buffer of pH 7.0 and 10.0 for DCV and DPV, respectively. At both thechniques, it is advisable to use an electrochemical regeneration of the electrode surface by the application of a couple of regeneration potentials Ereg,1 = 0 mV and Ereg,2 = −800 mV. The calibration dependences were measured in the concentration range from 1·10−6 to 1·10−4 mol·l−1 , with the LQs of 1.0·10−6 mol·l−1 for DCV at the m-AgSAE and 1.5·10−6 mol·l−1 for DPV at the m-AgSAE. The concentration dependences of 5-NI at the BDDFE were measured using the DCV technique in the BR buffer of pH 3.0. For the DPV technique, the optimal medium seemed to be the BR buffer of pH 2.0, however, because of the presence of an interfering peak in the supporting electrolyte,...
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Voltammetric Determination of 4-Nitrobiphenyl at a Mercury Meniscus Modified Silver Solid Amalgam Electrode
Horáková, Eva ; Barek, Jiří (advisor) ; Schwarzová, Karolina (referee)
The presented bachelor thesis is devoted to study of electrochemical behavior of 4-nitrobiphenyl (4-NBP) and to finding of optimum conditions for its' determination using direct current voltammetry (DCV) and differential pulse voltammetry (DPV) at a mercury meniscus modified silver solid amalgam electrode (m-AgSAE). The aim was to achieve the lowest possible limit of determination and to verify the applicability of the newly developed method for determination of 4-NBP in model samples of drinking water. Methanol-acetate buffer pH 4,8 (3:7) was found as an optimum medium for the determination of 4 NBP at a m-AgSAE in deionized water. During DCV it is not necessary to apply electrochemical regeneration of the working electrode, during DPV it is proper to apply following regeneration potentials: Ereg,1 = 0 mV, Ereg,2 = -1300 mV. The concentration dependence of the peak current was found to be linear for both methods for 10-5, 10-6 and 10-7 mol∙l-1 concentration ranges. The limit of determination of 4-NBP both by DCV and by DPV is 2∙10-7 mol∙l-1. The optimum medium for the determination of 4-NBP in drinking water is the mixture of the sample and acetate buffer pH 4,8 in the 9:1 ratio.. During DCV regeneration was not applied, during DPV it was applied with the following regeneration potentials: Ereg,1...
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Voltammetric Determination of Genotoxic 6-Nitrochrysene at a Mercury Meniscus Modified Silver Solid Amalgam Electrode
Šmídková, Monika ; Vyskočil, Vlastimil (advisor) ; Fischer, Jan (referee)
This Bachelor Thesis is devoted to the study of electrochemical behavior of 6-nitrochrysene (6-NCH) and to the finding of the optimum conditions for its determination using direct current voltammetry (DCV) and differential pulse voltammetry (DPV) at a mercury meniscus modified silver solid amalgam electrode (m-AgSAE). For measuring the concentration dependences of 6-NCH, the optimum medium methanol - BR buffer pH 9.0 (1:1) and the proper regeneration potentials Ereg,1 = 0 mV, Ereg,2 = -600 mV have been chosen for DCV at m-AgSAE and the medium methanol - BR buffer pH 10.0 (1:1) and the proper regeneration potentials Ereg,1 = 0 mV, Ereg,2 = -750 mV have been chosen for DPV at m-AgSAE. The concentration dependence was found to be linear only for the lowest concentration range of 10-7 mol·l-1 . In the concentration range of 10-6 mol·l-1 , the concentration dependences observed were polynomial. This result indicates a possible adsorption of 6-NCH on the surface of working electrode. Reached limits of quantification (LQ) were 1·10-7 mol·l-1 for DCV at m-AgSAE and 5·10-8 mol·l-1 for DPV at m-AgSAE. For comparison, the concentration dependence of 6-NCH was measured in methanol using UV-VIS spectrophotometry. Reached LQ ~ 1·10-7 mol·l-1 is comparable with LQs reached using DCV and DPV techniques.
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Electrochemical Investigation of Novel Redox Indicatiors for Detection of DNA Damage
Otépka, Tomáš ; Vyskočil, Vlastimil (advisor) ; Fischer, Jan (referee)
Cílem této práce bylo zkoumání nových redoxních systémů, které by bylo možné využít pro detekci poškození DNA na rtuťovým meniskem modifikované stříbrné pevné amalgámové elektrodě (m-AgSAE). Jako slibné se nabízely komplexy 1,10-fenantrolinu (phen) a iontů přechodných kovů. Konkrétně byly provedeny pokusy s komplexy kobaltaných iontů a phen, jejichž příprava byla provedena slitím roztoků obou složek v příslušném poměru. Chování komplexů v této směsi bylo porovnáno se syntetizovaným komplexním kationtem [Co(phen)3]3+ , a to jednak s využitím voltametrické techniky, jednak spektrofotometricky pomocí UV/VIS spektrofotometrie. Analýzy na m-AgSAE probíhaly s využitím techniky diferenční pulsní voltamerie (DPV) ve vodném prostředí. Jako základní elektrolyt byl zvolen 0,1 mol.dm-3 KCl, který poskytoval nejširší potenciálové okno v katodické oblasti potenciálů. Nízkomolekulární DNA z lososího spermatu byla využita v následujícím modifikační kroku pro vytvoření modifikované elektrody. Poškození DNA bylo provedeno vystavením takto připraveného biosenzoru UV-C záření o vlnové délce 254 nm. Poškozená DNA naadsorbovaná na m-AgSAE byla testována pomocí DPV v elektrochemické cele obsahující ionty Co2+ nebo komplex Co2+ a phen, obojí o koncentraci 1.10-3 mol.dm-3 . Na získaných voltamogramech byla sledována...
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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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Voltammetric Determination of 5-Nitroimidazole - The Structural Unit of Nitroimidazole Drugs
Šmídková, Monika ; Vyskočil, Vlastimil (advisor) ; Fischer, Jan (referee)
Presented Diploma Thesis deals with the study of electrochemical behavior of 5-nitroimidazole (5-NI), with the search for optimal conditions for its determination using techniques of DC voltammetry (DCV) and differential pulse voltammetry (DPV) at a mercury meniscus modified silver solid amalgam electrode (m-AgSAE) and at a boron-doped diamond film electrode (BDDFE), and with the comparison of reached limits of quantification (LQs). The optimal conditions found for measuring calibration dependences of 5-NI at the m-AgSAE in deionized water were as follows: Britton-Robinson buffer of pH 7.0 and 10.0 for DCV and DPV, respectively. At both thechniques, it is advisable to use an electrochemical regeneration of the electrode surface by the application of a couple of regeneration potentials Ereg,1 = 0 mV and Ereg,2 = −800 mV. The calibration dependences were measured in the concentration range from 1·10−6 to 1·10−4 mol·l−1 , with the LQs of 1.0·10−6 mol·l−1 for DCV at the m-AgSAE and 1.5·10−6 mol·l−1 for DPV at the m-AgSAE. The concentration dependences of 5-NI at the BDDFE were measured using the DCV technique in the BR buffer of pH 3.0. For the DPV technique, the optimal medium seemed to be the BR buffer of pH 2.0, however, because of the presence of an interfering peak in the supporting electrolyte,...
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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 Genotoxic 6-Nitrochrysene at a Mercury Meniscus Modified Silver Solid Amalgam Electrode
Šmídková, Monika ; Vyskočil, Vlastimil (advisor) ; Fischer, Jan (referee)
This Bachelor Thesis is devoted to the study of electrochemical behavior of 6-nitrochrysene (6-NCH) and to the finding of the optimum conditions for its determination using direct current voltammetry (DCV) and differential pulse voltammetry (DPV) at a mercury meniscus modified silver solid amalgam electrode (m-AgSAE). For measuring the concentration dependences of 6-NCH, the optimum medium methanol - BR buffer pH 9.0 (1:1) and the proper regeneration potentials Ereg,1 = 0 mV, Ereg,2 = -600 mV have been chosen for DCV at m-AgSAE and the medium methanol - BR buffer pH 10.0 (1:1) and the proper regeneration potentials Ereg,1 = 0 mV, Ereg,2 = -750 mV have been chosen for DPV at m-AgSAE. The concentration dependence was found to be linear only for the lowest concentration range of 10-7 mol·l-1 . In the concentration range of 10-6 mol·l-1 , the concentration dependences observed were polynomial. This result indicates a possible adsorption of 6-NCH on the surface of working electrode. Reached limits of quantification (LQ) were 1·10-7 mol·l-1 for DCV at m-AgSAE and 5·10-8 mol·l-1 for DPV at m-AgSAE. For comparison, the concentration dependence of 6-NCH was measured in methanol using UV-VIS spectrophotometry. Reached LQ ~ 1·10-7 mol·l-1 is comparable with LQs reached using DCV and DPV techniques.
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