Voltammetric methods for the determination of diazepam (DZ) and nordiazepam (NDZ) were developed. Techniques differential pulse voltammetry (DPV) and DC voltammetry for determination of both substances at meniscus modified silver solid amalgam electrode (m-AgSAE) were used. Effect of pHa in media of mixture of Britton-Robinson buffer and methanol (9:1) and 0,1 mol.l-1 NaOH was studied. Stability of the signal with repeated measurements in 0,1 mol.l-1 and methanol (9:1) was monitored. Optimal pHa 13,2 of 0,1 mol.l-1 NaOH was used for determination of DZ by DPV and DCV techniques. Optimal pHa 10,2 in media of mixture of Britton-Robinson buffer and methanol (9:1) was used for determination of NDZ by DPV and DCV techniques. Under these conditions were measured linear dependences in the calibration. Concentration range of DZ was measured with DCV in range of 1.10-4 - 6.10-6 mol.l-1 and DPV with DCV technique in range of 1.10-4 - 2.10-6 mol.l-1. Concentration range of NDZ was measured with DCV technique in range of 1.10-4 - 4.10-6 mol.l-1 and DPV technique in range of 1.10-4 - 2.10-6 mol.l-1. The limit of detection was calculated for DZ 6,6 .10-6 mol.l-1 with DCV and 1.10-6 mol.l-1 with DPV. The limit of detection was calculated for NDZ 5,5.10-6 mol.l-1 with DCV and 1,7.10-6 mol.l-1 with DPV. Developed method...

Voltammetric methods for the determination of diazepam (DZ) and nordiazepam (NDZ) were developed. Techniques differential pulse voltammetry (DPV) and DC voltammetry were used for determination of DZ and NDZ at meniscus modified silver solid amalgam electrode (m-AgSAE). The effect of pHa on the intensity of signal was observed in the mixture of Britton-Robinson buffer and methanol (9:1), and in the mixture of 0.1 mol.l−1 NaOH and methanol (9:1). The stability of the signal during repeated measurements in the mixture of 0.1 mol.l−1 NaOH and methanol (9:1), and in the mixture of BR buffer and methanol (9:1) was monitored. Optimal pHa 13.2 of medium of 0.1 mol.l−1 NaOH and methanol (9:1) was used for determination of DZ with DPV and DCV techniques. Optimal pHa 10.1 of medium of BR buffer and methanol (9:1) was used for determination of NDZ with DPV and DCV techniques. Under these conditions linear dependencies calibration were measured. Concentration range of DZ was measured with DCV in range of 10x10−5 - 6x10−6 mol.l−1 and with DPV technique in range of 10x10−5 - 2x10−6 mol.l−1 . Concentration range of NDZ was measured with DCV technique in range of 10x10−5 - 4x10−6 mol.l−1 and with DPV technique in range of 10x10−5 - 2x10−6 mol.l−1 . The limit of detection for DZ was calculated 6.6x10−6 mol.l−1 with DCV and...

This diploma thesis is focused on the determination of chloramphenicol by differential pulse voltammetry (DPV), DC voltammetry (DCV), cyclic voltammetry (CV) and adsorptive stripping voltammetry (AdSV) on a meniscus modified silver solid amalgame electrode (m- AgSAE). For the determination of chloramphenicol the optimum conditions were found and under these conditions concentration dependences were measured and then limits of quantification were determined. The influence of pH of BR buffer was tested. For determination of chloramphenicol by DCV pH 7 was chosen as an optimum background and pH 8 was chosen as an optimmum for DPV determination. Under these conditions linear dependences were obtained in the concentration range of 1·10-6 - 1·10-4 mol·l-1 . The limit of detection of chloramphenicol by DCV was 2.3·10-6 mol·l-1 . The limit of detection of chloramphenicol by DPV was 2.1·10-6 mol·l-1 in distilled water, 2.9·10-6 mol·l-1 in river water and 4.2·10-6 mol·l-1 in drinking water. Electrochemical behavior of chloramphenicol was studied by cyclic voltammetry in BR buffer with pH 2, 6, 8, 12 and then mechanism of reduction of chloramphenicol was propose based on available literature. Chloramphenicol was determined in drug Spersadex by DPV in BR buffer with pH 8. The optimal conditions for determining...

This Diploma Thesis is focused on investigation of the voltammetric behavior of the explosive penthrite (pentaerythritol tetranitrate) (PETN) and on searching for optimum conditions for its determination using differential pulse voltammetry (DPV) at a hanging mercury drop electrode (HMDE) (this part of the Diploma Thesis follows the topic investigated in the author's Bachelor Thesis; in this Diploma Thesis, the results of the Bachelor thesis are applied to the determination of PETN in environmental matrices) and at a mercury meniscus modified silver solid amalgam electrode (m-AgSAE) and on investigation of voltammetric behavior in real samples (deionized, drinking, and river water). For investigating the behavior of PETN in aqueous-methanolic media on the m-AgSAE, mixtures of Britton-Robinson buffers (BR-buffers) and methanol in various volume ratios were used. In non-aqueous media, methanolic solutions of tetramethylammonium bromide (TMAB), tetrabutylammonium iodide (TBAI), and tetrabutylammonium chloride (TBAC) were used as supporting electrolytes. Firstly, the influence of pH (in the range of 2 - 13) and methanol content (10 - 90 vol. %) on voltammetric responses of PETN was studied. The best response was obtained at each of those pH values at the volume ratio of BR-buffer - methanol of 1:9 or...

This Diploma Thesis is focused on study of electrochemical behavior of 2,4,6-trinitrotoluene (TNT) and 2,4,6-trinitrophenol (picric acid) on finding the optimum conditions for their determination using direct current voltammetry (DCV) and differential pulse voltammetry (DPV) at a mercury meniscus modified silver solid amalgam electrode (m-AgSAE) in the solution of Britton-Robinson (BR) and on finding of the limit of quantification (LQ) for these substances. Practical applicability of the newly developed methods was verified on direct determination of TNT and picric acid in model samples of drinking and river water. Moreover, the electrochemical behaviors of TNT and picric acid was studied using cyclic voltammetry (CV). Optimum medium for the determination of TNT at m-AgSAE was: methanol-BR buffer pH 4.0 (1:9). Upon the DCV it is proper to apply regeneration potentials Ereg,1= 0 mV and Ereg,2= -1100 mV and upon the DPV was apply regeneration potentials Ereg,1= 0 mV and Ereg,2= -600 mV were applied. The concentration dependence of the peak current was found to be linear for both techniques over the concentration range of 1·10-6 -1·10-4 mol/l with LQ of 0.54 µmol/l (for DCV) and 0.46 µmol/l (for DPV). The method developed for the determination of TNT were verified on the model samples of drinking...

The aim of presented Diploma Thesis was to study an electrochemical behavior of nitroimidazole drugs metronidazole and ornidazole and to find optimal conditions for their voltammetric determination at a mercury meniscus modified silver solid amalgam electrode using DC voltammetry (DCV) and differential pulse voltammetry (DPV). Voltammetric behavior of selected drugs was investigated in dependence on the pH of the medium used (realized using a Britton-Robinson buffer (BR buffer)) and a mechanism of the reduction of both drugs was investigated using cyclic voltammetry (CV). The optimum medium for voltammetric determination of studied nitroimidazole drugs at the m-AgSAE in a region of cathodic potentials was found to be the BR buffer of pH 8.0. Then, the concentration dependences were measured in this optimum medium in the concentration range from 2·10-7 mol/L to 1·10-4 mol/L. The limits of quantification (LQs) for both metronidazole and ornidazole were found in the concentration order of 10-7 mol/L by using DCV and DPV at the m-AgSAE. The applicability of the newly developed voltammetric methods of the determination of nitroimidazole drugs was verified on the model samples of drinking and river water, with LQ ≈ 2·10-7 mol/L for both DC voltammetry and differential pulse voltammetry at the m-AgSAE....

Presented Diploma Thesis is focused on electroanalytical determination of genotoxic 4-nitroindane, one of the nitrated polycyclic aromatic hydrocarbons (NPAHs). A hydrocarbon indane (a component of petrol) is a precursor of 4-nitroindane. NPAHs are produced all above by combustion processes in gasoline and diesel engines. It has been shown that NPAHs can be many times more mutagenic or carcinogenic than their parent PAHs, so the analysis of these dangerous pollutants becomes important for modern environmental analytical chemistry. Optimal conditions for determination of 4-nitroindane have been investigated in buffered water-methanolic solutions and electrochemical transformations of 4-nitroindane have been studied by DC voltammetry (DCV), differential pulse voltammetry (DPV) and cyclic voltammetry at a hanging mercury drop electrode (HMDE) and at a mercury meniscus modified silver solid amalgam electrode (m-AgSAE). For voltammetric determination of 4-nitroindane, the following techniques were used: DCV (limit of quantification (LQ) ~ 7. 10-8 mol. l-1 ), DPV (LQ ~ 1. 10-7 mol. l-1 ) and adsorptive stripping voltammetry (AdSV; LQ ~ 7. 10-9 mol. l-1 ) at HMDE, and DCV (LQ ~ 1. 10-7 mol. l-1 ) and DPV (LQ ~ 1. 10-7 mol l-1 ) at m-AgSAE. The applicability of the newly developed...

Presented Ph.D. Thesis is focused on the development of analytical methods applicable for determination of selected xenobiotic compounds and for monitoring DNA damage they can induce. The main attention has been paid to the development and testing of non-toxic electrode materials for preparation of miniaturized electrochemical devices and novel electrochemical DNA biosensors. 2-Aminofluoren-9-one (2-AFN) was selected as a model environmental pollutant, which belongs to the group of hazardous genotoxic substances. Its carcinogenic and mutagenic effects may represent a risk to living and working environment. 2-AFN has one oxo group, where the cathodic reduction occurs, and one amino group, where the anodic oxidation occurs. The voltammetric behavior of 2-AFN in the negative potential region was investigated at a mercury meniscus modified silver solid amalgam electrode (m-AgSAE) representing a non-toxic and more mechanically robust alternative to mercury electrodes. This working electrode was subsequently used for the development of a newly designed miniaturized electrode system (MES), which has many benefits as the possibility of simple field measurements, easy portability, and the measurement in sample volume 100 µL. Moreover, a glassy carbon electrode (GCE) was used for further investigation of...