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Chemiluminescence Determination of Cobalt and its Applications
Hrabalová, Veronika ; Hraníček, Jakub (advisor) ; Rychlovský, Petr (referee)
Tato bakalářská práce se zabývá optimalizací metody stanovení kobaltu (resp. kobaltnatých iontů) pomocí průtokové metody analýzy, takzvané sekvenční injekční analýzy (SIA). Jako detekční technika je použita chemiluminiscence, která je následně detekována při vhodné vlnové délce 443,68 nm citlivým spektrofotometrem. Pro analytické účely se zde využívá katalytické schopnosti kobaltnatých iontů při chemiluminiscenční reakci luminolu s peroxidem vodíku. Intenzita detekovaného chemiluminiscenčního záření je přímo úměrná koncentraci kobaltnatých iontů. V souvislosti se stanovením kobaltu bylo nutné nejprve v SIA uspořádání optimalizovat některé významné parametry. Optimální koncentrace peroxidu vodíku byla 0,5 % a průtoková rychlost 4,0 ml.min-1 . Dále byly optimalizovány průtokové rychlosti a reakční objemy luminolu a vzorku. Za optimálních podmínek byly zjištěny základní charakteristiky stanovení kobaltu. Limit detekce byl 0,29 mg.l-1 , citlivost stanovení byla 481 l.mg-1 . Dále byla studována katalytická schopnost dalších 7 prvků, resp. jejich iontů (Cu2+ , Cr3+ , Fe3+ , Zn2+ , Mn4+ , Ag+ a Ni2+ ). Tato studie byla provedena z hlediska možných interferencí při stanovení kobaltu. Z výše uvedených iontů, pouze ionty Cu2+ vykazovaly katalytický účinek, který byl ovšem nevýznamný oproti iontům Co2+ . Při...
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Determination of Titanium and Phosphorus by Atomic Absorption Spectrometry
Jeníková, Eva ; Hraníček, Jakub (advisor) ; Rychlovský, Petr (referee)
Předkládaná bakalářská práce se zabývá optimalizací metod stanovení titanu a fosforu technikou atomové absorpční spektrometrie s plamenovou atomizací ve složení acetylen-oxid dusný. Pro jednotlivá stanovení byly experimentálně nalezeny optimální hodnoty pro průtokovou rychlost acetylenu, koncentraci přídavku hliníku či vápníku, výšku paprsku nad hranou hořáku a jiné faktory pro zvýšení analytického signálu. Za těchto experimentálně zjištěných podmínek bylo provedeno stanovení a zjištění základní charakteristiky metod u obou prvků. Významnost stanovení těchto dvou prvků souvisí s tím, že materiály na bázi titanu a oxidu titaničitého povrchově modifikované sloučeninami fosforu jsou perspektivní pro řadu biomedicínských i průmyslových aplikací. Powered by TCPDF (www.tcpdf.org)
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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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The Comparison of Methods for the Determination of Riboflavin in Medical Preparations.
Houšť, Jiří ; Nesměrák, Karel (advisor) ; Rychlovský, Petr (referee)
Cílem této bakalářské práce bylo porovnat vybrané analytické metody sloužící ke stanovení riboflavinu v určených léčivých přípravcích. Mezi metody, u kterých probíhalo jejich zhodnocení z hlediska pravdivosti, preciznosti a časové náročnosti, byla zařazena spektrofotometrie v UV/VIS oblasti, spektrofluorimetrie a voltametrie. Jednotlivá stanovení probíhala na pěti různých přípravcích, které se nacházely ve čtyřech lékových formách: tablety, potahované tablety, lyofilizáty pro přípravu infuzního roztoku a sirup. Nejpravdivější výsledky poskytlo spektrofotometrické stanovení v UV/VIS oblasti, pravým opakem bylo stanovení voltametrické. Nejpreciznější metodou byla spektrofluorimetrie. Časově nejnáročnější se ukázala voltametrie, nejméně času naopak zabralo spektrofotometrické stanovení v UV/VIS oblasti. Klíčová slova: riboflavin, UV/VIS spektrofotometrie, fluorimetrie, voltametrie
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Identification of polyphenolic compounds in plant extracts
Rýdlová, Iveta ; Rychlovský, Petr (advisor) ; Hraníček, Jakub (referee)
Thesis "Identification of selected polyphenols in extracts of medicinal plants" is divided into two parts. The first part is devoted to describing a general division polyphenolic compounds, their antioxidant activity and lists of the methods which are used for the analysis of these substances. The second part deals with the identification of these selected compounds using the RP - HPLC method with UV detection-DAD, and then with the tandem mass spectrometer with a triple quadrupole. The method was optimized, in this method was used gradient elution with 10-90% acetonitrile, 0,1% formic acid and deionized water. Analysis time was 38 minutes. Elution agents ran from polar to less polar substances. First of all eluted substances which contained the hydroxyl group directly on the benzene ring as e.g. phenolic acids, further eluted aglycones with bound sugar, which provides a higher polarity of the substance (flavanones glycosides), further followed the flavonols without attached saccharide units, at the latest the flavones eluted. This optimized method has proved to be reliable with good repeatability and accuracy for separation of polyphenols. Using the UV spectrometry the stability was measured. Due to the stability the substances proved to be stable compounds where their UV spectra don't change with...
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Electrochemical Oxidation of Selected Bille Acids in Acetonitrile
Klouda, Jan ; Nesměrák, Karel (advisor) ; Rychlovský, Petr (referee)
The use of voltammetry for determining bile acids and similar compounds is described in literature, but in most cases separation precedes. The goal of this bachelor's thesis was to develop a method for direct determination and identification of seven selected bile acids. The experiments were carried out in non-aqueous medium of acetonitrile using DC voltammetry. As the working electrode a rotating disc platinum electrode and a rotating disc glassy carbon electrode were employed. Platinum electrode proved not to be suitable for this kind of use. The GCE on the other hand showed some potential, but the chemical properties of the bile acids exclude its use in terms of identification.
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Sensitivity increasing of gold determination by electrochemical volatile species generation with AAS detection
Vacek, Tomáš ; Hraníček, Jakub (advisor) ; Rychlovský, Petr (referee)
This thesis is focused on increasing the senstitivity of gold determination by electrochemical volatile species generation using two different types of electrolytic cells in continuous flow setting. Externally heated quartz tube atomizer was used as means of atomization and detection of gold with atomic absorption spectrometer. Generation parameters were optimized for electrolytic cell with an ion exchange (nafion) membrane. After selection of new cathode material (Cu) the carrier gas (Ar) flow rate was optimized, where an additional inlet of carrier gas was found to have possitive effect on increasing the sensitivity of determination of gold and efficiency of volatile specie transport to the atomizer. Experiments with Antifoam B showed possitive effect on generation, thus calibration was carried out for optimized experimetal conditions reaching detection limit of 0,53 mg.dm−3 . The efficiency of volatile specie transfer from liquid to gaseous phase was determined between 60 - 65 % by measuring the residual gold content in liquid waste by F-AAS method. Subsequently the effieciency of electrolytic generation of volatile gold specie with radioactive tracer isotopes and autoradigraphy was determined to 0,6 %. These methods confirmed adsorption of generated species on apparatus surface. Using ICP-MS as...
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Determination of vitamin B12 by flow analysis with chemiluminiscent detection
Svobodová, Kateřina ; Hraníček, Jakub (advisor) ; Rychlovský, Petr (referee)
This thesis reports determination of vitamin B12 by flow techniques of analysis. This method is based on luminol-peroxide chemiluminiscence assay for the detection of cobalt (II) ions in vitamin B12 molecules. The method includes releasing of Co2+ from the vitamin B12 using different types of its decomposition; these are mentioned in this thesis. The efficiency of the decomposition of real samples of vitamin B12 in this study reached 74.43 %. The high efficiency was achieved with 1.5 mmol.l-1 K2S2O8 and irradiation time 1 minute. In the FIA mode, the linear range obtained was between 1.0 to 500 mg.l-1 with a relative standard deviation (RSD) 2.59% (n = 10), limit of detection (LOD) 55 µg.l-1 . The minimum sample volume required and the time of analysis were 60 µl and 140.2 s. In the SIA mode, the linear range obtained was between 0.01 to 50 mg.l-1 with an RSD = 4.5% (n = 10), LOD = 25 µg.l-1 . The minimum sample volume required and the time of analysis were 250 µl and 80.1 s. Interference study showed that from wide range of interfering ions were selected only Ni2+ , Zn2+ and NO2 - , that from concentration level 50 mg.l-1 they significantly affect the determination of the Co2+ in solution. The intensity of chemiluminiscence most suppress ion Zn2+ . The solution with the concentration ratio of Co2+...
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Dissociation Constants of Perfluorocarboxylic Acids
Vlasáková, Tereza ; Nesměrák, Karel (advisor) ; Rychlovský, Petr (referee)
Bachelor's thesis is concerned on dissociation exponents of perfluoroalkanoic acids. The published values of dissociation exponents have been reviewed. The dissociation exponents of six selected perfluoroalkanoic acids (from perfluoropentanoic to perfluorodecanoic acid) were determined using neutralization potentiometric titration method. The values of determined dissociation exponents ranges from pKa = 2,17 to 2,44, and they are in agreement with known data. The decrease of value of dissociation exponent with increasing number of carbon in alkyl chain has been observed. Also, the increase of values of dissociation exponents of perfluoroalkanoic acids in comparison with theirs nonfluorinated analogs has been confirmed.
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