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Micro-mechanical Sensor and Laser Photoacoustics for Diagnostics in Gases
Vlasáková, Tereza ; Nesměrák, Karel (advisor) ; Wild, Jan (referee)
The aim of the thesis is to study mechanical properties of nanomaterials (multi-layer graphene, silicon, mica) suitable to be used as novel pressure sensors in laser photoacoustic spectroscopy. Membranes (diameter ~ 4 mm, thickness ~ 100 nm) were prepared by mechanical exfoliation method and then attached to a glass window in several slightly different designs. Movement of these membranes was detected using HeNe laser beam reflected from the membrane's surface onto a position sensitive detector. Methanol was used as a model gas and the signal was collected from studied element and microphone simultaneously. Acoustic wave, induced inside a measuring cell by periodic thermal variations, causes the membranes to move. The movement of a membrane is influenced by its mechanical properties, which is possible to determine by fitting the measured data into a mathematical model. Comparison of the output data of all membranes' measurements shows, that the signal intensity is influenced by the method of attaching membrane to a glass window and by volume of free space on a side of a membrane. Metallization of the membrane's surface (~ 70 nm) decreases its springiness thus decreases the sensitivity. Several membranes reached sensitivity comparable with top class microphone.
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Electrochemical oxidation of Bile Acids on Carbon Based Electrodes. The Possible Use in Electroanalysis.
Klouda, Jan ; Nesměrák, Karel (advisor) ; Zima, Jiří (referee)
The goal of this master's thesis was to examine the possibility of oxidation of seven selected bile acids and evaluate whether such processes are suitable for analytical purposes. The secondary goal was to describe the oxidation products of bile acid electrolysis. The experiments were carried out in a non-aqueous medium of acetonitrile and in a mixed medium of acetonitrile:water using linear sweep and cyclic voltammetry. The working electrode materials employed for voltammetric experiments were: highly oriented pyrolytic graphite, -cyclodextrin modified glassy carbon and boron doped diamond. Preparative electrolysis was carried out on a platinum electrode in the non-aqueous medium of acetonitrile. Experiments have shown that neither the highly oriented pyrolytic graphite electrode nor the -cyclodextrin modified glassy carbon electrode are suitable for analytical purposes under conditions used. The results achieved on the boron doped diamond electrode, on the other hand, have not yet been described in the literature. Primary bile acids cholic and chenodeoxycholic were oxidized at approximately 0.5 V lower potential in the mixed medium of acetonitrile:water than in the papers using carbon electrodes published until now. Products of oxidation on the platinum electrode were separated by TLC and...
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Determination of Heparin by Sequential Injectin Analysis with Spectrophotometric Detection
Lišková, Růžena ; Hraníček, Jakub (advisor) ; Nesměrák, Karel (referee)
In this work the determination of heparin using Sequential Injection Analysis (SIA) technique with spectrophotometric detection was studied. The principle of this method was measuring the decrease of absorbance of phenothiazine dyes in its maximum wavelength caused by its interaction with heparin. The decrease is proportional to concentration of heparin in sample. The aim of this work was to find optimum conditions for determination of heparin by the SIA with spectrophotometric detection and to try to apply this measurement to real sample under these conditions. Three phenothiazine dyes were used: Methylene Blue, Azure A and Azure B and for each of them an optimum concentration was found. Their values were for methylene blue 4.0 ∙ 10-5 mol/dm3 and 5.0 ∙ 10-5 mol/dm3 for Azure A and Azure B. 150 µl was chosen as an optimum amount of heparin and reagent aspirated. Optimum reaction time was 0 s and flow rate during measurement 1.5 ml/min. Working concentration range was found between 0.23 and 15 mg/dm3 for methylene blue, 1.2 and 13 mg/dm3 for Azure A and 0.67 and 12 mg/dm3 for Azure B. Limit of detection varied between 0.09 - 0.35 mg/dm3 and limit of quantification between 0.30 and 1.2 mg/dm3 for different dyes. Relative standard deviation was determined as a measure of repeatability. Its values were...
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Electrochemical Oxidaction of Thioxoacetamides in Acetnonitrile Medium
Kudláček, Karel ; Nesměrák, Karel (advisor) ; Schwarzová, Karolina (referee)
Electrochemical oxidation of eight newly synthesized derivatives of 2-(fenylamino)-2-thioxoacetamidein 0,1 mol dm-3 sodium perchlorate - including effects of acid, base, and water - was studied. It was found that oxidation carried out in two subsequent steps, each of them is connected with exchanging of one electron. The oxidation is localised on sulphur atom, it is exchanged by oxygen atom in the final oxidation product. The effect of substituents on the course of electrochemical oxidation was also studied.
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The Comparison of Methods for Determination of Procaine in Medical Formulations
Baptistová, Adéla ; Nesměrák, Karel (advisor) ; Červený, Václav (referee)
The aim of this bachelor thesis was to compare four analytical methods for determination of procaine hydrochloride in medical formulations in terms of precision and measurement trueness, and its time, and financial cost. The selected methods are: titration with potassium bromate, titration with sodium nitrite, UV spectrophotometry, VIS spectrophotometry. Three injection solutions of different concentrations (0.2%, 0.5%, and 1.0% of procaine) were analysed. VIS spectrophotometry provides the most precise results, whereas determination by UV spectrophotometry is the least precise. Measurement trueness is found for UV spectrophotometry and both titrations. UV spectrophotometry is the cheapest method, while titration with sodium nitrite is the most expensive method. Titration with potassium bromate is the least time-consuming method, while VIS spectrophotometry is the most time- consuming method. Keywords: procaine, bromatometric titration, titration with sodium nitrite, UV and VIS spectrophotometry
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Cyclic Voltammetry as a Detection Technique in High Performance Liquid Chromatography
Burešová, Helena ; Nesměrák, Karel (advisor) ; Schwarzová, Karolina (referee)
The aim of the thesis was to study the possibility of employment of cyclic voltammetry as a detection technique in liquid chromatography. The phenothiazine derivatives (chlorpromazine hydrochloride, diethazine hydrochloride, and thioridazine hydrochloride) were used as model compounds. Firstly, the comparison of two potential detectors (tubular detector and bulk "wall-jet" detector) was accomplished. Only bulk "wal-jet" detector satisfied. Next, the conditions for the separation and detection of studied phenothiazines on RP-select B LiChrospher® 60 (250×4 mm) column with cyclic voltammetry as the detection techniques were optimized. The best separation is achieved in mobile phase consisted from the solution of 0.1 mol dm-3 sodium perchlorate in acetonitrile-water (80:20) mixture. The effect of flow rate of mobile phase and scan rate of polarization of the electrode on the symmetry of chromatographic peak was also followed, and optimal values of 0.5 ml min-1 for flow rate, and of 0.5 V s-1 for scan rate, were found. Under optimized conditions the calibration dependences of studied phenothiazines were measured in the range from 5×10-5 to 1×10-3 mol dm-3 for chlorpromazine, and in the range from 8×10-5 to 1×10-3 mol dm-3 for diethazine and thioridazine. The developed method was applied to...
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Analysis of degradation of substances of historical pharmaceutical preparations
Vašíčková, Pavla ; Nesměrák, Karel (advisor) ; Kozlík, Petr (referee)
The aim of this thesis is the analysis of transformations of the composition of pharmaceutical preparations from the years 1930-1997. The alkaloids and opium alkaloids are active substances of these pharmaceutical preparations. Pharmaceutical preparations were in form of tablet and injection solution. The presence of active compounds and their degradation products were detected using RP-HPLC with spectrometric detection. The MS/MS fragmentation pathways of compounds found were proposed. The high stability of some active substances was proved (codeine, ethylmorphine and theobromine) while some other compounds were completely decomposed.
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Flow injection analysis of selected glycosaminoglycans with spectrofluorimetric detection
Tichá, Renata ; Nesměrák, Karel (advisor) ; Rychlovský, Petr (referee)
The thesis is focused on a determination of heparin and chondroitin sulfate, using flow injection analysis with spectrofluorimetric detection. The determination is based on the interaction of negatively charged heparin, chondroitin sulfate resp., with a cationic dye (azure B or phenosafranine) which is manifested by the decrease in fluorescence intensity of the dye in its emission maximum. The optimal conditions for the determination in static mode were found, and calibration dependencies were measured. The conditions of FIA were optimized and following parameters were established: the volume of dispensed sample of 100 ml, the length of the reaction coil 60 cm, the flow rate 0.7 ml min-1 , the concentration of azure B 1.6×10-5 mol dm-3 , the concentration of phenosafranine 3.5×10-5 mol dm-3 . For the determination of heparin using azure B it was found: LOD = 0.023 IU ml-1 , LOQ = 0.186 IU ml-1 , and linear dynamic range 0.19-1.43 IU ml-1 . For the determination of heparin using phenosafranine it was found: LOD = 0.102 IU ml-1 , LOQ = 0.192 IU ml-1 , and linear dynamic range 0.19-1.79 IU ml-1 . For the determination of chondroitin sulfate using azure B it was found: LOD = 0.58 mg dm-3 , LOQ = 2.37 mg dm-3 , and linear dynamic range 2.37-8.32 mg dm-3 . The developed determination was applied to the...
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Possibilities of Electrochemical Analysis Using a System of Electrodes With Non-Specific Response
Ederer, Jakub ; Nesměrák, Karel (advisor) ; Ludvík, Jiří (referee)
The master thesis present the possibilities of processing of electrochemical data from a group of four electrodes with non-selective response (simple sensor array) for electrochemical analysis with potential application of the results achieved in the construction of the sensor field type "electronic tongue". This simple system was applied to the sample simulating the food product. Electrochemical data were processed through mathematical operations such as Gaussian approximation, deconvolution or using basic mathematical operations.
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Voltammetric detection of stigmasterol at boron-doped diamond electrode in mixed media
Benešová, Lenka ; Schwarzová, Karolina (advisor) ; Nesměrák, Karel (referee)
V o l t a m m e t r i c d e t e c t i o n o f s t i g m a s t e r o l a t b o r o n d o p e d d i a m o n d e l e c t r o d e i n m i x e d m e d i a L e n k a B e n e š o v á Univerzita Karlova v Praze Přírodovědecká fakulta Praha 2015 Abstract The aims of the study thesis was to suggest suitable solvent for oxidation of stigmasterol on boron doped diamond electrode. Cyclic voltammetry in mixed media of water and organic solvents was used for this purpose. First of all, the effect of organic solvent on potential window of boron doped diamond electrode was studied. Solvents used were methanole, isopropanole, N-dimethylformamide and acetonitrile; the water components was phosphate buffer (0,075 mol.l-1, pH 3,0). It was deduced from the results, that suitable solvent for detection of stigmasterol on was the acetonitrile, which provided sufficiently large potential window in anodic area. Keywords: boron doped diamond electrode, cyclic voltammetry, organic solvent, oxidation, stigmasterol
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