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Determination of Lead using Sequential Injection Analysis with Spectrophotometric Detection
Mušutová, Martina ; Hraníček, Jakub (advisor) ; Rychlovský, Petr (referee)
The main objective of the thesis was the determination of lead concentration in model aqueous solutions of 4-(2-Pyridylazo)-resorcinol complexating reaction with lead cation in 2-Amino-2-hydroxymethyl-propane-1,3-diol hydrochloride buffer (TRIS buffer). The UV/VIS molecular spectrometry in static arrangement was chosen with subsequent application of sequential injection analysis in flow arrangement. Calibration curve was measured and both methods were assessed. Detection threshold was 0,026 mg dm-3 in case of static arrangement and 0,70 mg dm-3 in case of flow arrangement. The interference analysis was performed, with metallic ions (Cu2+ , Zn2+ , Sn4+ ) being the most significant interferents, which also create a chromatic complex with 4-(2-Pyridylazo)-resorcinol. The interference effects were weak and almost not present for barium and potassium. Thesis concludes with determination of lead concentration in model specimen using flow arrangement. The determination by calibration curve was insufficient due to interfering ions and thus it had to be determined by standard addition method. Keywords Lead, 4-(2-pyridylazo)-resorcinol, TRIS buffer, flow sequential injection analysis, UV/VIS molecular spectrometry, interference effects
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Determination of Procaine by Flow Injection and Sequential Injection Analysis with Spectrophotometric Determination
Tomanová, Marie ; Hraníček, Jakub (advisor) ; Rychlovský, Petr (referee)
This diploma thesis is focused to the determination of procaine using flow injection and sequential injection analysis coupled with spectrophotometric detection. This determination is based on the reaction of procaine with a colouring agent, 1,2-naphthoquinone-4-sulfonic acid. An orange coloured product is formed, which is determined spectrophotometrically at the wavelength 484 nm. The high of the absorption signal of the product is directly proportional to the concentration of procaine. The aim of this work was to optimize the parameters of both methods of flow analysis so that the limit concentration of procaine can be as low as possible and at the same time, high sensibility is achieved. The next step was to apply these methods on the determination of procaine in real samples. It was found that in flow injection analysis, the absorbance of procaine hydrochloride obeys Beer's law for concentrations from 2.5 to 120 µg/ml. The linear regression equation of calibration graph was y = 0.0059x - 0.0051, with a linear regression correlation coefficient 0.9993. Limit of detection was 0.72 µg/ml. Effects of standing time (stopped-flow), flow rate, concentration of colouring agent, pH and the volume of the sample loop have been examined and optimized. It was also found that in sequential injection...
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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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Determination of Lead by Hydride Generation Atomic Absorption Spectrometry
Vošmiková, Anna ; Hraníček, Jakub (advisor) ; Rychlovský, Petr (referee)
EN This diploma thesis presents the results of determination of lead amount in aqueous samples using chemical a electrochemical hydride generation methods. Both chemical and electrochemical generation methods are widely used for elemental analysis of the hydride forming elements in trace and ultra-trace levels. First of all the electrochemical generation method was used with HCl (1,0 mol dm-3 ) as anolyte. Determined analyte with the relevant concentration was added into the HCl solution (equal concentration). During the optimization experiments the electrochemical generation method was performed in different setups and constructions (eg. membrane, and non-membrane cells, different electrode materials). Also different acids (HNO3, H2SO4) of different concentrations were tested. Unfortunately achieved results were not satisfied and reproducible. Therefore, chemical generation method was used to provide relevant results. Determination of lead was performed in both and continuous flow and flow injection mode. A crucial step for chemical hydride generation insisted in usage of hexacyanoferrate (III) (17 % m/v solution for FIA and 2 % m/v solution for continuous flow) in solution of HCl on the relevant concentration. It was found that, K3[Fe(CN)6] significantly increases the efficiency of the chemical...
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Extraction method for losartan determination in pharmaceutical compounds by sequential injection analysis with UV/VIS and fluorimetric detection
Zimmermannová, Jana ; Rychlovský, Petr (advisor) ; Hraníček, Jakub (referee)
The diploma thesis deals with the extraction method for determination of losartan using sequential injection analysis with spectrophotometric and spectrofluorimetric detection. The principle of determination is based on losartan ion-pair formation with the orange II and calmagite dyes in an acid buffer, which is then extracted into a chloroform phase. For the purposes of the analytical determination of losartan, an increase in absorbance and fluorescence emission of the ion-pair extracted into the chloroform in its absorption maximum is detected. Losartan potassium was used as the standard substance. First, the conditions for determination in a static arrangement with UV/VIS detection were verified and the basic optimization parameters of determination were measured and the basic characteristics of the determination were identified in the first part of the thesis. An SIA extraction apparatus was prepared and the control programme for the entire analytical process was created in the other part of the thesis. Then the experimental parameters of the determination were optimized and the basic characteristics for both spectrophotometric and spectrofluorimetric detection were measured. The reliability of the losartan determination using the selected methods was verified by analysing real pharmaceutical...
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Multielement analysis of flue gas residues from secondary lead smelting
Šebek, Ondřej ; Mihaljevič, Martin (advisor) ; Rychlovský, Petr (referee) ; Hruška, Jakub (referee)
Multielement analysis of flue gas residues from secondary lead smelting was tested using seven decomposition methods on four different flue gas residues and certified reference materials (CRM) CPB-2 (Pb concentrate, CCRMP). The studied samples contained both silicates and also high contents of phases with Pb, primarily Pb chlorides and sulphates. Solutions prepared by various decomposition methods were analysed using ICP OES (Al, As, Ba, Be, Bi, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Mo, Na, Ni, P, Pb, Sb, Se, Si, Sn, Sr, Ti, Tl, V, Zn). Greater yields were found for most of the elements by combined decomposition (with fusion) and decomposition by sintering. Nonetheless, both methods exhibited major losses of volatile elements (As, Bi, Sb, Tl). Thus, one of these methods must always be combined with a method of decomposition in a closed system. The work also demonstrates that, for investigation of untraditional waste geological materials (e.g. flue residues from high- temperature industrial processes), it will be necessary in the future to produce new certified reference materials with anomalous chemical and mineralogical compositions, which are not currently available on the market. Laboratory extraction tests were performed on two different types of flue residues - kinetic (30 days) with ratio L/S...
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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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