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1
Hesko, Ondrej. "Elektrochemická analýza RNA: Vývoj metódy vhodnej pre charakterizáciu produktov neenzymatickej polymerácie cyklických nukleosid monofosfátov za podmienok modelujúcich prebiotické prostredie." Master's thesis, Vysoké učení technické v Brně. Fakulta chemická, 2019. http://www.nusl.cz/ntk/nusl-401876.
Повний текст джерелаАнотація:
This thesis focuses on the optimazation of the electrochemical method, which characterizes products of untemplated nonenzymatic polymerization of 3',5' -cyclic guanosine monophosphate (cGMP) under conditions modeling prebiotic environment. An adsorptive transfer stripping techniques on carbon electrode and gel electrophoresis were used. The method was optimized on the model system of oligonucleotides located in solution of cGMP on carbon electrode, where DNA and RNA adsorb. This technique allows simple removing of interfering substances such as cGMP, which are not present in the original sample, but they do not adsorb on the surface of electrode or they adsorb weaker than oligonucleotides or polynucleotides. Analyses are based on the selective desorption of cGMP from the surface of the carbon electrode by the chemical and physical methods before the measurement of linear voltammetry itself. Detergents, such as SDS, Tween 20 and Triton x-100 with different concentrations and electrostatic repulsions of cGMP with different negative potentials on the carbon electrode were used for the selective desorption of cGMP. The selective desorption of cGMP was observed for all detergents and inserted negative potentials. Used methods were compared and the most effective detergent for selective desorption of cGMP was SDS. Desorption of oligonucleotides was minimalized by inserted positive potential on washed carbon electrode in 0,01% SDS in basic medium. This optimized method was used on electrochemical analysis of preliminary samples of untemplated nonenzymatic polymerization of 3',5' -cGMP and compared to the analysis of gel electrophoresis.
2
Hadjichari, Andrew Michael, University of Western Sydney, and School of Civic Engineering and Environment. "Determination of heavy metals on macro- and micro-electrodes by adsorptive cathodic stripping voltammetry and anodic stripping voltammetry." THESIS_XXXX_CEE_Hadjichari_A.xml, 1999. http://handle.uws.edu.au:8081/1959.7/602.
Повний текст джерелаАнотація:
This thesis describes the application of macro, micro, ultra-microelectrodes and microelectrode arrays to the measurement of trace concentrations of nickel and cobalt in sediment and natural waters by adsorptive cathodic stripping voltammetric methods. In addition the measurement of tin by adsorptive cathodic stripping voltammetry in sediment and natural waters is discussed. Also, the application of macroelectrodes and microelectrode arrays to the measurement of lead, cadmium and zinc in sediment and natural waters by anodic stripping voltammetry is considered. In all cases the determination of the six metals was optimised by investigating the influence of various significant parameters, such as in-situ mercury plating, complexing agent concentration, scan rate, pulse height, accumulation time and potential, buffer concentration and pH. The results obtained for these investigations are discussed in this thesisDoctor of Philosophy (PhD)
3
Hadjichari, Andrew Michael. "Determination of heavy metals on macro- and micro-electrodes by adsorptive cathodic stripping voltammetry and anodic stripping voltammetry /." View thesis, 1999. http://library.uws.edu.au/adt-NUWS/public/adt-NUWS20030828.122855/index.html.
Повний текст джерелаАнотація:
Thesis (Ph. D) -- University of Western Sydney, Nepean, 1999.A thesis presented for the degree of Doctor of Philosophy, Centre for Electrochemical Research and Analytical Technology, University of Western Sydney, Nepean. Includes bibliographical references.
4
Moreira, Josino Costa. "Adsorptive stripping voltammetry of derivatized biological molecules and metal complexes." Thesis, Loughborough University, 1991. https://dspace.lboro.ac.uk/2134/14142.
Повний текст джерелаАнотація:
Differential pulse stripping voltammetry preceded by a non-faradaic preconcentration step is a very powerful technique for the direct determination of metal complexes, drug compounds and proteins. Small molecules like the amino acids can play a very important role in the biochemistry of living organisms. Despite their importance, these substances (except for cystine and cysteine) are generally not strongly adsorbed on mercury and /or do not possess any electroactive group in their molecular structure making their determination by direct electroanalytical techniques difficult or even impossible. These difficulties can be overcome by reacting these compounds with derivatising reagents (1). Initially here, derivatisation techniques for the determination of amino acids were studied. Methods are presented for the determination of tyrosine and histidine after coupling with diazotised sulphanilic acid (chapter 3) and for amino acids in general, and glycine in particular, as methyl or phenylthiohydantoin derivatives (chapter 5). Nanomolar levels of histidine were determined by accumulating the amino acid in the presence of an excess of copper(II) using the reduction peak of its copper(II) complex (chapter 4) for detection. The uses of polyamino acids as electrode modifiers were also studied and a method for the determination of copper(II) based on its accumulation at a hanging mercury electrode modified by adsorption of a polyhistidine film (chapter 6) and of hexacyanoferrate(III) after preconcentration on a copper modified polylysine film electrode (chapter 7) are proposed. As an offshoot of the diazo coupling derivatization of tyrosine and histidine, a method for the determination of copper(ll) by reaction with diazo-1 H-tetrazole (DHT) and accumulation of its complex on the HMDE (chapter 8) is presented.
5
Pablo, Fleurdelis, of Western Sydney Nepean University, and Faculty of Science and Technology. "Adsorptive stripping voltammetry of trace elements on a glassy carbon mercury film electrode." THESIS_FST_XXX_Pablo_F.xml, 1994. http://handle.uws.edu.au:8081/1959.7/207.
Повний текст джерелаАнотація:
This thesis describes the development of new adsorptive cathodic stripping voltammetric methods for reliable determination of some trace metals in biological and environmental materials on a glassy carbon mercury film electrode. In particular, the development of these methods involved selection of a suitable complexing agent for the respective metal ion studied, characterization of the electrode processes, investigation of factors affecting the voltammetric response such as concentration and pH of supporting electrolyte, concentration of complexing agent, accumulation potential, accumulation time and electrode rotation rate. Also, organic and inorganic interferences, linear concentration range, and detection limits were carefully considered. Furthermore, the analytical application of the method was demonstrated for each metal in biological and/or environmental materials, after optimization of the sample decomposition procedure. Some conclusions : the results obtained by the AdCSV method for the determination of tin in juices agreed reasonably with those obtained by atomic absorption method; the use of the adsorptive voltammetric technique after dry-ashing and UV treatment of the samples was successfully demonstrated for the determination of vanadium in standard reference materials such as urban particulate matter, peach leaves, apple leaves and bovine liver; and, the use of the adsorptive stripping voltammetric technique, after decomposition of samples by dry-ashing and UV treatment, was successfully demonstrated for the determination of molybdenum in peach leaves, apple leaves and bovine liver samples.Doctor of Philosophy (PhD)
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Pablo, Fleurdelis. "Adsorptive stripping voltammetry of trace elements on a glassy carbon mercury film electrode /." View thesis, 1994. http://library.uws.edu.au/adt-NUWS/public/adt-NUWS20030826.113026/index.html.
Повний текст джерела
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Shubietah, Raqi Moh'd Hasan. "Adsorptive stripping voltammetry as a method of analysis of some pharmaceutical and other purine derivatives." Thesis, Loughborough University, 1995. https://dspace.lboro.ac.uk/2134/11215.
Повний текст джерелаАнотація:
Adsorptive stripping voltammetry (AdSV) is a recent technique (initially named by Lam, Kalvoda and Kopanica in 1983) in which there is generally a nonelectrolytic accumulation (adsorption) of the determinand followed by a cathodic reductive or anodic oxidative scan. In this work, a hanging mercury drop electrode (HMDE) was used to accumulate several purine derivatives with and without the addition of Cu(lI) in a suitable buffer (usually Britton-Robinson, pH 7.5). In the presence of copper(lI) the copper(l) purine complex was usually accumulated at about -0.1 V. Some of the compounds studied (i.e dimenhydrinate, theophylline, guanine and azathioprine) can be determined as free compounds (i.e with no Cu(lI) added) after accumulation at potentials ranging from 0 to -0.2 V versus Ag/AgCI reference electrode. The determination of these compounds was made after optimising pH, buffer constituents, accumulation potential and accumulation time. The addition of Cu(lI) to these purines makes possible accumulation at shorter accumulation times , and improves the detection limits. For example, the detection limit of azathioprine in the presence of Cu(lI) is as low as 2x10-10 M. Both differential-pulse polarography (DPP) and DP-AdCSV (differential pulse adsorptive cathodic stripping voltammetry) were used in the determination of theophylline and azathioprine in their dosage forms (tablets). The relative standard deviations for the determination of the pharmaceutical purines in their tablets were 3.0%. 4.2% and 1.3% for the measured concentrations of dimenhydrinate(1.5x10-7 M) , theophylline(2x10-7 M) by AdSV ; and azathioprine(2x10-6 M) by DPP, respectively . Other purines (eg xanthine,1,3-dimethyluric acid and some methylguanines) did not give peak currents useful for their determination. The addition of Cu(lI) was necessary to obtain satisfactory peak currents for these purines. At low copper(lI) concentrations (Le.< 10-6 M), it is suggested that the purines form Cu(l) complexes which are adsorbed at the HMDE surface: Cu(lI) + Cu(O) + 2 L ~ 2 Cu(I)-L adsorbed.
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Tekenya, Ronald. "Graphene-modified pencil graphite mercury-film electrodes for the determination of trace metals by cathodic adsorptive stripping voltammetry." University of the Western Cape, 2018. http://hdl.handle.net/11394/6552.
Повний текст джерелаАнотація:
>Magister Scientiae - MScThis project focuses on the simple, fast and highly sensitive adsorptive stripping voltammetry detection of Nickel and Cobalt complexed with DMG and Nioxime respectively at a Reduced Graphene Oxide modified pencil graphite electrode in water samples. This research as well demonstrates a novel electrochemically reduced graphene oxide (ERGO)/mercury film (MF) nanocomposite modified PGE, prepared through successive electrochemical reduction of graphene oxide (GO) sheets and in-situ plated mercury film. The GO and graphene were characterized using FT-IR, HR-SEM, HR-TEM, XRD and Raman spectroscopy. The FT-IR results supported by Xray diffraction analysis confirmed the inclusion of oxygen moieties within the graphitic structure during the chemical oxidation step. Microscopic and spectroscopic analysis was used to confirm the stackings of graphene on the pencil electrode. The ERGO-PG-MFE, in combination with a complexing agents of [dimethylglyoxime (DMG) and Nioxime] and square-wave cathodic stripping voltammetry (SW-CSV), was evaluated towards the individual determination of Ni2+ and Co2+ respectively and simultaneous determination of both metals from the combination of DMG and Nioxime mixture. A single-step electrode pre-concentration approach was employed for the in-situ Hg-film electroplating, metal-chelate complex formation and its non-electrolytic adsorption at – 0.7 V for the individual analysis of Ni2+ and Co2+. The current response due to metal-ligand(s) complex reduction were studied as a function of experimental variables; deposition/accumulation potential, deposition/accumulation time, rotation speed, frequency and amplitude and carefully optimized for the individual determination of Ni2+and Co2+ and simultaneous determination of Ni2+ and Co2+ at low concentration levels (μg L-1) in 0.1 M NH3- NH4Cl buffer solution (pH 9.4) solution. The recorded limit of detection for the individual analysis of Ni2+and Co2+ was found to be 0.120 μg L-1 and 0.220 μg L-1 respectively, at an accumulation time of 120 s for both metals. The recorded limit of detection of the simultaneous analysis of Ni2+ and Co2+ was found to be 6.1 μg L-1 and 1.8 μg L-1 respectively. The ERGO-PG-MFE further demonstrated a highly selective stripping response toward all trace metal analysis. The testing of the applicability of graphene-based sensor and method in laboratory tap water samples was evaluated. This electrode was found to be sensitive enough to detect metal ions in the tap water samples at the 0.2 μg L-1 level for individual analysis and 0.001 μg L-1 for simultaneous, well below WHO standards.
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Pokpas, Keagan William. "Microfluidic graphenised-paper electroanalytical devices (μGPED) for adsorptive cathodic stripping voltammetric detection of metal contaminants". University of the Western Cape, 2017. http://hdl.handle.net/11394/5506.
Повний текст джерелаАнотація:
Philosophiae Doctor - PhDThe need for clean, non-toxic drinking water supplies, free of pollutants and metal contamination is vital in impoverished areas and the developing world alike. With this in mind, the development of accurate, inexpensive, portable and simple devices for remote sensing applications is therefore pivotal for early detection and the prevention of illnesses. Over the last two decades, adsorptive stripping voltammetry (AdSV) has emerged as a superior detection method over common analytical techniques due to its low-cost instrumentation, unskilled labour and ability to detect a wide range of analytes.
2020-08-31
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Sanga, Nelia Abraham. "Determination of heavy metals at the electrochemically reduced graphene oxide mercury film electrode (ERGO-HgF-PGE) using adsorptive stripping voltammetry." University of Western Cape, 2020. http://hdl.handle.net/11394/7718.
Повний текст джерелаАнотація:
>Magister Scientiae - MScThis work reports the use of a pencil graphite electrode (PGE) as inexpensive and sensitive electrochemical sensing platform fabricated by using electrochemically reduced graphene oxide (ERGO) in conjunction with an in-situ plated thin mercury film. For the first time the ERGOHgF-PGE sensor is proposed for simultaneous detection of cadmium (Cd2+), copper (Cu2+), lead (Pb2+) and zinc (Zn2+) using N-Nitroso-N-phenylhydroxylamine (cupferron) as complexing agent by square-wave adsorptive cathodic stripping voltammetry (SW-AdCSV). The technique is based on the adsorption of cupferron- metal ion complexes onto the surface of the ERGO-HgFPGE at 0.1 V for 60 s carried out in 0.1 M acetate buffer solution (pH 4.6). The synthesized graphene oxide (GO) and graphene nanosheets (GNs) were characterized using different analytical techniques such as FT-IR which confirms the presence of oxygen moieties embedded in the graphitic structure and further demonstrated by UV-Vis, validating the synthesis of GO
2023
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Ranawaka, Arachchige Dinusha. "Ion transfer stripping voltammetry method using conductive polymer to low concentration detection of environmental contaminants." Thesis, Arkansas State University, 2016. http://pqdtopen.proquest.com/#viewpdf?dispub=10095768.
Повний текст джерелаАнотація:
Detecting environmental contaminants such as Selective serotonin reuptake inhibitors (SSRIs) and Cr (VI) compounds is essential since they are highly toxic contaminants of many drinking water supplies leading to adverse health effects. Selective serotonin reuptake inhibitors are common antidepressants therapeutics and fluoxetine; Prozac®, citalopram; Celexa ® and sertraline; Zoloft® were successfully detected in this study. Ion transfer stripping voltammetry (ITSV) was applied to detect those as cations at nanomolar concentrations using an inexpensive and disposable pencil lead electrode, with a lower detection limit of 30 nM. The pencil lead electrode was modified using the conducting polymer Poly (3, 4-ethylenedioxythiophene) (PEDOT-C14) and PVC (poly-vinyl chloride) membrane. The PVC/PEDOT-C14 -modified electrode demonstrated a linear current response from 100 to 1000 nM for these therapeutics. Ion transfers of Hydrogen chromate as anions were studied using a double-polymer modified glassy carbon electrode using the conducting polymer poly (3-octylthiophene) (POT), and PVC membrane. Lipophilicity of Hydrogen chromate ions were evaluated comparing to other common inorganic contaminants. Exhaustive stripping of Hydrogen chromate ions in cyclic voltammetry and their relative high lipophilicity infer that ITSV can be successfully applied to detect them in future studies.
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Leve, Zandile Dennis. "Determination of paracetamol at the electrochemically reduced graphene oxide-metal nanocomposite modified pencil graphite (ERGO-MC-PGE) electrode using adsorptive stripping differential pulse voltammetry." University of Western Cape, 2020. http://hdl.handle.net/11394/7350.
Повний текст джерелаАнотація:
>Magister Scientiae - MScThis project focuses on the development of simple, highly sensitive, accurate, and low cost electrochemical sensors based on the modification of pencil graphite electrodes by the electrochemical reduction of graphene oxide-metal salts as nanocomposites (ERGO-MC-PGE; MC = Sb or Au nanocomposite). The electrochemical sensors ERGO-Sb-PGE and ERGO-Au-PGE were used in the determination of paracetamol (PC) in pharmaceutical formulations using adsorptive stripping differential pulse voltammetry. The GO was prepared from graphite via a modified Hummers’ method and characterized by FTIR and Raman spectroscopy to confirm the presence of oxygen functional groups in the conjugated carbon-based structure whilst, changes in crystalline structure was observed after XRD analysis of graphite and GO.
2023-10-07
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Ghaffari, Nastaran. "Electrochemical deposition of Graphene Oxide- metal nano-composite on Pencil-Graphite Electrode for the high sensitivity detection of Bisphenol A by Adsorptive Stripping Differential Pulse Voltammetry." University of the Western Cape, 2018. http://hdl.handle.net/11394/6336.
Повний текст джерелаАнотація:
Magister Scientiae - MSc (Chemistry)Electrochemical platforms were developed based on pencil graphite electrodes (PGEs) modified electrochemically with reduced graphene oxide metal nanoparticles (ERGO–metalNPs) composite and used for the high-sensitivity determination of Bisphenol A (BPA) in water samples. Synergistic effects of both reduced Graphene Oxide sheets and metal nanoparticles on the performance of the pencil graphite electrode (PGE) were demonstrated in the oxidation of BPA by differential pulse voltammetry (DPV). A solution of graphene oxide (GO) 1 mg mL-1 and 15 ppm of metal stock solutions (1,000 mg L-1, atomic absorption standard solution) (Antimony or Gold) was prepared and after sonication deposited onto pencil graphite electrodes by cyclic voltammetry reduction. Different characterization techniques such as FT-IR, HR-SEM, XRD and Raman spectroscopy were used to characterize the GO and ERGO–metalNPs. Parameters that influence the electroanalytical response of the ERGO–SbNPs and ERGO–AuNPs such as, pH, deposition time, deposition potential, purging time were investigated and optimized. Well-defined, reproducible peaks with detection limits of 0.0125 μM and 0.062 μM were obtained for BPA using ERGO–SbNPs and ERGO–AuNPs respectively. The rGO-metalNPs–PGE was used for the quantification of BPA in tap water sample and proved to be suitable for the detection of BPA below USEPA prescribed drinking water standards of 0.087 μM.
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Gomes, Patricia. "Duloxetina : desenvolvimento e validação de métodos analíticos e estudos da estabilidade." reponame:Biblioteca Digital de Teses e Dissertações da UFRGS, 2009. http://hdl.handle.net/10183/132790.
Повний текст джерелаАнотація:
A duloxetina (DLX) é um duplo inibidor seletivo balanceado da recaptação de serotonina e norepinefrina empregado para o tratamento do transtorno depressivo maior e para o manejo da dor neuropática diabética periférica. O objetivo deste estudo foi desenvolver e validar métodos analíticos para determinação de DLX em cápsulas e realizar estudos da estabilidade do fármaco. A substância usada como padrão de referência nas análises foi caracterizada por espectroscopia no infravermelho, ressonância magnética nuclear (RMN), calorimetria diferencial de varredura e espectrometria de massas. As análises qualitativas foram realizadas por cromatografia em camada delgada (CCD), espectrofotometria na região do ultravioleta (UV) e cromatografia líquida de alta eficiência (CLAE) permitindo a identificação do fármaco no produto farmacêutico. A espectrofotometria UV, CLAE e voltametria de redissolução catódica (CSV) foram validadas para determinação quantitativa de DLX em cápsulas. Estes métodos propostos foram específicos, robustos, lineares, precisos e exatos para determinação de DLX em microgrânulos de revestimento entérico. Estudos preliminares da estabilidade da DLX durante o desenvolvimento do método indicativo de estabilidade por CLAE demonstraram que o fármaco foi rapidamente degradado em meio ácido, na presença de peróxido de hidrogênio e de radiação a luz UVC, enquanto que este foi mais estável em meio alcalino. A cinética de degradação descreveu as mudanças na concentração da DLX em condição ácida e sob fotodegradação. A degradação ácida da DLX, em solução de HCl 0,1 M, mostrou cinética aparente de zero ordem e a fotodegradação demonstrou uma cinética aparente de primeira ordem. O produto de degradação principal observado na hidrólise ácida (PDA-14) foi analisado e isolado por CCD preparativa. Espectros de RMN-1H, RMN-13C e COSY foram avaliados e a estrutura do PDA-14 foi confirmada como 1-naftol. Esta substância produz efeitos citotóxicos e consequentemente o produto farmacêutico é uma cápsula de gelatina contendo microgrânulos com revestimento entérico para evitar a degradação ácida da DLX no estômago.The duloxetine (DLX) is a double balanced selective serotonin and norepinephrinereuptake inhibitor employed for the treatment of major depressive disorder and for the management of diabetic peripheral neuropathic pain. The aim of this study was to develop and validate analytical methods to the determination of DLX in capsules and accomplish studies of this drug stability. The substance used as reference standard in the analysis was characterized by infrared spectroscopy, nuclear magnetic resonance (NMR), differential scanning calorimetry, and mass spectrometry. The qualitative analyses were performed by thin layer chromatography (TLC), ultraviolet spectrophotometry (UV), and high performance liquid chromatography (HPLC) allowing the identification of the drug in pharmaceutical dosage form. The UV spectrophotometry, HPLC, and cathodic stripping voltammetry (CSV) were validated for quantitative determination of the DLX in capsules. These proposed methods were specific, robust, linear, precise, and accurate to the determination of DLX in entericcoated pellets. Preliminary studies of DLX stability during the development of stability-indicating HPLC method demonstrated that the drug was rapidly degraded in acid medium, in the presence of hydrogen peroxide and light UVC radiation, while it was more stable in alkali medium. The kinetics of degradation described the concentration changes of DLX in acid condition and on photodegradation. The acid degradation of DLX in 0.1M HCl solution showed apparent zero-order kinetics and the photodegradation demonstrated apparent first-order kinetics. The main degradation product observed in acid hydrolysis (DP-14) was analyzed and isolated by TLC preparative. 1H NMR, 13C NMR and COSY spectra were evaluated and the structure of DP-14 was confirmed as 1-naphthol. This substance produces cytotoxic effects and consequently the finished pharmaceutical dosage form is a gelatin capsule containing enteric-coated pellets to avoid the acid degradation of DLX in the stomach.
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Schneider, Alexandre Batista. "Voltametria adsortiva na determinação de traços e ultra-traços de Zr(IV), V(V),Ti(IV), Mo(VI), Hf(IV), Nb(V) e Ta(V) em águas naturais." Universidade Federal de Santa Maria, 2014. http://repositorio.ufsm.br/handle/1/4257.
Повний текст джерелаАнотація:
Coordenação de Aperfeiçoamento de Pessoal de Nível SuperiorSingle sensitive sequential AdSV methods were developed and optimized for the determination of trace zirconium, vanadium, titanium and molybdenum in river, estuary and seawater, independent of the salinity and content of organic matter in the sample. The methods are based on the accumulation of Zr(IV)-and V(V)-cupferron-oxalic acid-1,3-diphenylguanidine complexes and the accumulation of Ti(IV)-and Mo(VI)-mandelic acid at the hanging mercury drop electrode (HMDE). Differential pulse, adsorption potential of -0.6, -0.2, -0.1 and -0.1 V (vs. Ag/AgCl), adsorption time of 400, 20, 120 and 1 s and scan rates of 0.01, 0.06, 0.02 and 0.02 V s-1 for Zr(IV), V(V), Ti(IV) and Mo(VI), respectively, were used as instrumental parameters. The reduction peak for the complexes of Zr(IV), V(V), Ti(IV) and Mo(VI) appeared nearly -0.95, -0.65, -0.85 and -0.4 V, respectively. The variations of the peak current as well as the peak potential of each metal complexes were plotted against the apparent ionic strengths. The proposed voltammetric methods were applied in German and Brazilian rivers and estuaries as well as in seawater from the North Sea collected at the north of Germany and the Atlantic Ocean, collected during scientific cruise between Chile and Germany, as interesting and very simple alternatives to very laborious and time-consuming pre-existent methods, based on outline pre-concentration and separation from the matrix and subject to external contamination. The limits of detection and determination were in the range of ppt-levels and the methods accuracy were evaluated by recoveries tests and by measuring V(V) and Mo(VI) in two NRCC reference materials. Estuarine mixtures experiments were also carried out with the aim to get more insight on the distribution of Ti(IV), Zr(IV), Mo(VI) and V(V) along the estuaries of the rivers Rhine, Weser and Elbe with the North Sea. In this context, natural fresh waters were mixed with seawater at different ratios.
Métodos sensíveis e sequenciais de voltametria adsortiva de redissolução foram desenvolvidos e otimizados para a determinação de traços e ultra-traços de zircônio, vanádio, titânio e molibdênio em águas de rio, estuário e mar, independentemente da salinidade e conteúdo de matéria orgânica na amostra. Os métodos são baseados na acumulação de complexos de Zr(IV) e V(V) com cupferron-ácido oxálico-1,3-difenilguanidina e de complexos de Ti(IV) e Mo(VI) com ácido mandélico no eletrodo de mercúrio de gota pendente (HMDE). Pulso diferencial, potenciais de adsorção de -0,6; -0,2; -0,1 e -0,1 V (vs Ag/AgCl), tempos de adsorção de 400, 20, 120 e 1 s e velocidades de varredura de 0,01; 0,06; 0,02 e 0,02 V s-1, para Zr(IV), V(V), Ti(IV) e Mo(VI), respectivamente, foram usados como parâmetros instrumentais. Os picos de redução para os complexos de Zr(IV), V(V), Ti(IV) e Mo(VI) surgiram próximos de -0,95; -0,65; -0,85 e -0,4 V, respectivamente. As variações de corrente de pico assim como de potencial de pico de cada complexo dos metais foram plotados contra as forças-iônicas aparentes das amostras. Os métodos voltamétricos propostos foram aplicados em águas de rio e estuário coletadas na Alemanha e no Brasil e em amostras de água do mar do Mar do Norte coletadas no norte da Alemanha e Oceano Atlântico, coletadas durante expedição científica entre o Chile e Alemanha. Estes métodos se mostraram ser alternativas simples a métodos bastante complexos e demorados, baseados em pré-concentração outline e separação da matriz, sujeitos a contaminação externa. Os limites de detecção e quantificação estavam na ordem de partes por trilhão e a exatidão dos métodos foi avaliada através de teste de recuperação de amostras adicionadas com os analitos em estudo e em 2 materiais de referência certificados. Também foram realizados experimentos de mistura estuarina com o objetivo de obter informações da distribuição de Ti(IV), Zr(IV), Mo(VI) e V(V) ao longo de estuários dos rios Reno, Weser e Elba com o Mar do Norte. Neste intuito, as águas dos rios e do mar foram misturadas em diferentes razões.
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Nobre, Eva Michelly Carvalho Santana. "PROCEDIMENTO VOLTAMÉTRICO OTIMIZADO PARA DETERMINAÇÃO DE Ni2+ EM AMOSTRAS PRÉ-TRATADAS DE BIODIESEL, USANDO ELETRODO MODIFICADO COM FILME DE MERCÚRIO." Universidade Federal do Maranhão, 2011. http://tedebc.ufma.br:8080/jspui/handle/tede/920.
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Previous issue date: 2011-07-04The presence of metals in biodiesel can be related to raw material, the process used to obtain biodiesel or its storage and can cause reactions of oxidation, corrosion and clogging engines, besides causing risks to human health and the environment. In this paper, we propose a procedure based on voltammetric experimental conditions suitable for the determination of Ni2+ ion in biodiesel (B100) through Square Wave Adsorptive Stripping Voltammetry, using the mercury film electrode prepared ex situ. First, the mercury film was prepared and then was conducted the analysis of a biodiesel pre-treated (digested) sample. The sample digestion was performed with microwave oven in a closed system in the presence of ultra-pure nitric acid and hydrogen peroxide. After this, ammonia buffer 0.01 mol L-1 pH 9.23 and NaOH 0.46 mol L-1 was added into the cell to adjust the pH of the sample to a final value of approximately 9.2. Finally, the chelator dimethylglyoxime (DMG) 0.01 mol L-1 was added, which acts as a complexing element to capture the Ni2+ ion. Next, several voltammetric experiments, in the absence and presence of increasing aliquots of biodiesel and standard solution of the metallic ion, were performed to optimize the analysis conditions. The results indicate that the Square Wave Adsorptive Stripping Voltammetry (VAdRSWV) appeared suitable for measurements of trace metal in Biodiesel (B100) in concentrations up to 10-8 mol L-1. The experiments carried out by successive addition of aliquots of a standard solution of Ni2+ ions provided a linear response of peak current with the concentration of metal ion. Each sample of biodiesel was analyzed in triplicate, with very satisfactory results from the analytical point of view, once we were dealing with trace element analysis, especially in terms of accuracy (recovery 105%) and precision (RSD 9.61%) for the Ni2+ metal ion, using a confidence limit of 98%.
A presença de metais no biodiesel pode estar relacionada com a matéria-prima, com o processo utilizado para a obtenção do biodiesel ou com sua estocagem e pode provocar reações de oxidação, corrosão e entupimento em motores, além de causar riscos à saúde humana e ao meio ambiente. Neste trabalho, é proposto um procedimento voltamétrico com base em condições experimentais adequadas para a determinação do íon Ni2+ em biodiesel (B100) por Voltametria Adsortiva de Redissolução no modo Onda Quadrada, usando o eletrodo de Filme de Mercúrio preparado no modo ex situ. Inicialmente, o filme de mercúrio foi preparado e a seguir realizaram-se as análises com amostra de biodiesel pré-tratada (digerida). A digestão da amostra foi realizada com forno de micro-ondas em sistema fechado, na presença de ácido nítrico ultra-puro e peróxido de hidrogênio. Após essa etapa, foi adicionado tampão amônia 0,01 mol L-1 pH 9,23 e NaOH 0,46 mol L-1 na célula para ajustar o pH da amostra para um valor final de aproximadamente 9,2. Por fim, foi adicionado o quelante dimetilglioxima (DMG) 0,01mol L-1 que funciona como complexante para captura do íon Ni2+. Após esta etapa, vários experimentos voltamétricos, na ausência e presença de alíquotas crescentes de biodiesel e solução padrão do íon metálico foram realizados para otimizar as condições de análise. Os resultados obtidos indicam que a Voltametria Adsortiva de Redissolução no modo Onda Quadrada (VAdRSWV) apresentou resultado satisfatório para medidas do metal traço em Biodiesel (B100), em concentrações de até 10-8 mol L-1. Os experimentos realizados pela adição sucessiva de alíquotas de uma solução padrão do íon Ni2+ proporcionaram uma resposta linear da corrente de pico com a concentração do íon metálico. Cada amostra de biodiesel foi analisada em triplicata, apresentando resultados bastante satisfatórios do ponto de vista analítico por se tratar de análise de elementos traços, principalmente, em termos de exatidão (recuperação de 105 %) e precisão (DPR de 9,61%), para o íon metálico Ni2+, utilizando um limite de confiança de 98%.
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LIN, ZHENG-HUI, and 林正輝. "Analysis of nickel as 8-hydroxyquinolate by adsorptive stripping voltammetry." Thesis, 1986. http://ndltd.ncl.edu.tw/handle/28382020061774504041.
Повний текст джерела
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Tatum, Clarissa E. "Novel Electrochemical Detections of Biologically and Environmentally Relevant Substances." 2010. http://trace.tennessee.edu/utk_graddiss/918.
Повний текст джерелаАнотація:
Development and studies of new electrochemical methods for the detection of various biologically and environmentally relevant substances are the focus of this dissertation. A dual amperometric sensor, capable of the simultaneous, real-time determination of NO and O,2, has been developed and optimized. Many tests were performed in order to reduce cross-talking between the two sensors, and an electro-deposited polymer, poly-5-amino-1-naphthol, was shown to reduce the cross-talking to insignificant levels. The use of bismuth-based electrodes in the detection of various metals has been explored. A bismuth bulk electrode has been developed, optimized, and used for the individual and simultaneous determination of Pb(II), Cd(II), and Zn(II). The fundamental electrochemistry of several bismuth-based electrodes in the system used for Cr(VI) analysis has also been explored, and many interactions among the electrode material, ligand, and analyte were observed, particularly the formation of a soluble bismuth-ligand complex. Electrochemical analysis of Cr(VI) was attempted at all of the bismuth-based electrodes, with success at the thin bismuth film electrode. A series of surface modifications were made to the glassy carbon substrate, in an attempt to remove any co-adsorbed contaminants and to understand the sensitivity of the chromium detection process. Inevitably, it was found that the contaminating source was contaminants in the nitrogen gas used for solution deaeration. Upon switching to argon, detection became highly reproducible and showed strong linearity with the Cr(VI) concentration.
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Ječmínková, Jana. "Voltametrické stanovení chloramfenikolu a ofloxacinu na borem dopované diamantové filmové elektrodě." Master's thesis, 2011. http://www.nusl.cz/ntk/nusl-296342.
Повний текст джерелаАнотація:
Voltammetric methods for the determination amphenicol antibiotic chloramphenicol (CAP) and quinolone antibiotic Ofloxacin (OFL) were developed. TTechniques differential pulse voltammetry (DPV) and DC voltammetry (DCV) for determination of both substances at boron doped diamond film electrode (BDDFE) were used. The effect of pH of Britton-Robinson buffer was tested and the stability of the signal with repeated measurements was monitored. Optimal pH 6 was used for determining of CAP by both, DPV and DCV techniques. Media of pH 4 for determining of OFL by DPV and DCV was optimal. Under these conditions linear dependences in the calibration concentration region 1.10 -6 - 1.10-4 mol.l -1 were obtained. The limit of determination for the method for CAP by DPV at 3.10 mol.l , by -6 -1 DCV at 3.10 mol.l and for -6 -1 OFL by DPV at 1.10 mol.l -6 -1 and by DCV at 4.10 mol.l -7 -1 was found. The developed methods were used for the determination of CAP in the drug samples Spersadex comp. and OFL determination in drug samples Zanocin 200. Method for solid phase extraction of OFL from samples of urine with voltammetric detection was developed with limit of determination at 7.10 mol.l . -6 -1
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Dansby-Sparks, Royce Nicholas. "New Electrochemical and Optical Detection Methods for Biological and Environmental Applications." 2010. http://trace.tennessee.edu/utk_graddiss/788.
Повний текст джерелаАнотація:
Detection of chromium and vanadium is of interest for biomedical and environmental applications. The two metals have narrow limits between being essential and toxic for humans. Ultra-sensitive techniques have been studied to measure Cr and V at low concentrations found in human blood and environmental samples. Bismuth film and mercury-alloy electrodes have been developed as alternatives to traditional Hg-based electrodes for Cr and V detection. While catalytic adsorptive stripping voltammetry (CAdSV) has been used to detect Cr and V, little is known about the process. The mechanisms of CAdSV have been probed to provide a better understanding of its exceptional sensitivity and selectivity.
Near-real time monitoring of plume gas constituents is desired as a diagnostic tool for combustion efficiency, ensuring safe testing conditions and observing releases of green house gasses. Ground testing rockets is a crucial preliminary step that ensures their performance during critical space missions. Optical sol-gel sensors for carbon dioxide have been developed for remote sensing applications. They are inexpensive and are compatible with the harsh environments encountered during rocket plume tests. The sensors are a viable approach to compliment current infrared (IR) measurements for real-time carbon dioxide detection. Additional work on kerosene and isopropyl alcohol sensing has been explored for incorporation into a multi-analyte sensing platform.
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Havlíková, Štěpánka. "Voltametrické stanovení chloramfenikolu a chlorambucilu na amalgámových elektrodách." Master's thesis, 2015. http://www.nusl.cz/ntk/nusl-331222.
Повний текст джерелаАнотація:
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...
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Maška, Jan. "Elektrochemické stanovení Fomesafenu." Master's thesis, 2013. http://www.nusl.cz/ntk/nusl-323466.
Повний текст джерелаАнотація:
The submitted work deals with the application of voltammetric determination of Fomesafen using non-traditional mercury meniscus modified silver solid amalgam electrode on model samples of Fomesafen in real aqueous matrices of drinking and river water. This method of measurement has been developed and optimized in my bachelor thesis, which the diploma thesis is related to. Fomesafen belongs to a group of herbicides used on a mass scale in the late 20th century in the USA and in many countries around the world still used even today. Among its side effects according to the EPA include, among others, potential carcinogenicity to humans and confirmed carcinogenicity to some mammals (such as rats) which led to a legislative regulation on its use in many countries around the world including the USA, the European Union and many others. Silver solid amalgam electrode has been developed with the intention to limit the use of mercury in accordance with new legislation of the European Union and the concept of green analytical chemistry. Despite the low levels of mercury mainly bound in the form of virtually harmless silver amalgam electrode retains very similar electrochemical properties with proven mercury electrodes. As part of the thesis, direct determination of a number of partial extraction of Fomesafen...
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Tvrdíková, Jana. "Voltametrické stanovení dinitronaftalenů pomocí krystalové stříbrné amalgámové elektrody." Master's thesis, 2011. http://www.nusl.cz/ntk/nusl-297233.
Повний текст джерелаАнотація:
Voltammetric methods for determination of 1,3-dinitronaphthalene (1,3-DNN), 1,5-dinitronaphthalene (1,5-DNN) and 1,8-dinitronaphthalene (1,8-DNN) using DC voltammetry (DCV) and differential pulse voltammetry (DPV) at novel single crystal silver amalgam electrode (CAgAE) were developed in this work. Developed methods may be used for determination of 1,3-DNN within a concentration range 2 - 10 μmol.L-1 with LoQ 2 μmol.L-1 using DCV and 1 - 100 μmol.L-1 with LoQ 1 μmol.L-1 by DPV; 1,5-DNN wihin a concentration range 2 - 10 μmol.L-1 with LoQ 2 μmol.L-1 using DCV and 1 - 10 μmol.L-1 with LoQ 1 μmol.L-1 by DPV and 1,8-DNN within a concentration range 2 - 10 μmol.L-1 with LoQ 2 μmol.L-1 using DCV and 0,3 - 1 μmol.L-1 with LoQ 0,3 μmol.L-1 by DPV. An attepmt to decrease LoQ by adsorptive stripping differential pulse voltammetry was not successful. Process of electrochemical reduction of selected dinitronaphthalenes on the working electrode was also studied by cyclic voltammetry. This work verified the use of CAgAE as alternative electrode material to mercury electrodes for determination of electrochemically reducible organic compounds in aqueous-methanolic media. Small dimensions of the CAgAE are the main advantages which predetermine its use in voltammetric microvolume batch analysis and amperometric detection in...
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Murcková, Klára. "Voltametrické stanovení herbicidu Aclonifenu pomocí rtuťových elektrod." Master's thesis, 2012. http://www.nusl.cz/ntk/nusl-307470.
Повний текст джерелаАнотація:
Presented Diploma Thesis is focused on electroanalytical determination of the herbicide Aclonifen, which belongs to a group of herbicides derived from diphenylether. These herbicides are used due to their effects - inhibition of protoporfyrinogen oxidase synthesis and also inhibition of biosynthesis of carotenoids. Due to its widespread use in agricultural, toxical effects on humans and because of its negative impacts particularly on aquatic ecosystems there is a need for methods capable of determining the presence of Aclonifen in the environment to monitor its ecological impacts. Optimal conditions for the determination of Aclonifen have been investigated in BR buffer - methanolic solution and in BR buffer. Electrochemical behavior of the substance has been studied using direct current voltammetry (DCV), differential pulse voltammetry (DPP) and adsorptive stripping voltammetry (AdSV) on the hanging mercury drop electrode (HMDE) and by using TAST polarography and differential pulse polarography (DPP) on the dropping mercury electrode (DME). UV/VIS spectrophotometric detection was used for comparison to electrochemical detection. Used wavelengths were 308 nm and 388 nm. For electrochemical determination of Aclonifen the above mentioned techniques were used and following results were obtained: DCV...
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Косых, А. С., та A. S. Kosykh. "Разработка и исследование электрохимических сенсоров на основе углеродных нанотрубок для инверсионной вольтамперометрии : магистерская диссертация". Master's thesis, 2016. http://hdl.handle.net/10995/43866.
Повний текст джерелаАнотація:
Цель работы состояла в определении оптимальных значений диаметра и массы углеродных нанотрубок (УНТ) в нафионсодержащей модифицирующей пленке для получения наилучших электрохимических и аналитических характеристик толстопленочных углеродсодержащих электродов (ТУЭ).
В ходе работы синтезированы многостенные УНТ со средним диаметром dср ≈ 23 нм методом каталитического пиролиза этанола и проведена кислотная очистка полученного материала от металлических частиц катализатора и других модификаций углерода. Аналогичным способом обработаны коммерческие УНТ с dср ≈ 147 и 16 нм от Sigma-Aldrich.
Успешно изготовлены 36 типов ТУЭ без УНТ и на основе УНТ в условиях варьирования массового содержания УНТ в диапазоне MУНТ = 0,3-10,0 мкг на поверхности ТУЭ. Аттестация поверхностей электродов проведена методами оптической и электронной микроскопии. Изучены электрохимические характеристики изготовленных ТУЭ методами циклической вольтамперометриии и импедансной спектроскопии. Выполнено определение ионов железа (III) в модельном растворе методом адсорбционной инверсионной вольтамперометрии. Установлены оптимальные значения среднего диаметра УНТ dср ≥ 23 нм и массы УНТ MУНТ = 5,0-10,0 мкг на поверхности ТУЭ для получения наилучших электрохимические и аналитические характеристики. Разработанные ТУЭ на основе УНТ могут применяться для определения ионов тяжелых металлов в реальных водах с концентрацией меньшей предельно-допустимых значений, установленных нормативными документами.The aim is to determine the optimal values of the diameter and weight of carbon nanotubes (CNT) in modifier film containing Nafion for the best electrochemical and analytical characteristics of the thick film of carbon-containing electrodes (TFCE). Multi-walled CNT with an average diameter dav ≈ 23 nm were synthesized by the catalytic pyrolysis of ethanol and purified from the metal catalyst particles and other modifications of carbon, using mixture of concentrated sulfuric and nitric acids. Commercial CNT with dav ≈ 147 and 16 nm from Sigma-Aldrich were treated by a similar procedure. The batch of 36 types of TFCE without CNT and based on CNT varied by weight of CNT (MCNT) on TFCE surface in the range of 0,3-10,0 μg was made. The electrode surfaces were studied by optical and electron microscopy. The electrochemical characteristics of obtained TFCE by cyclic voltammetry and electrochemical impedance spectroscopy were investigated. The detection of Fe (III) ions in a model solution was carried out by adsorptive stripping voltammetry. The optimal values of the average diameter of CNT dav ≥ 23 nm and a weight of CNT on TFCE surfaces MCNT = 5,0-10,0 μg were determined. These parameters allow us to reach the best electrochemical and analytical characteristics of modified TFCE. Developed TFCE based on CNT may be used for the detection of heavy metal ions in real water with a concentration of less maximum permissible values, established by regulations.