La0.6Ca0.4Mn0.8Ni0.2O3-, La0.6Ca0.4Mn0.8Fe0.2O3- und La0.75Ca0.25Mn0.5Fe0.5O3-Volumenmaterialien wurden im potentiometrischen Messaufbau bereits erfolgreich auf ihre NO-Sensitivität getestet. Keramischen Nanomaterialien werden generell eine Reihe neuer oder verbesserter Eigenschaften (verbessertes Sinterverhalten, erhöhte NOx-Sensitivität, höhere Leitfähigkeit) zugesprochen. La0.6Ca0.4Mn0.8Ni0.2O3, La0.6Ca0.4Mn0.8Fe0.2O3 und La0.75Ca0.25Mn0.5Fe0.5O3 wurden mittels PVA/Sucrose-Methode, Aktivkohlemethode und Fällungssynthese als Nanomaterialien sowie mit Festkörperreaktion als Volumenmaterialien dargestellt und mit typischen Charakterisierungsmethoden untersucht. Die Materialien wurden in verschiedenen Schichtdicken auf YSZ-Substrate aufgetragen und potentiometrisch sowie impedanzspektroskopisch auf ihre NO-Sensitivität und die Querempfindlichkeit gegenüber NO2 und Propylen geprüft. Potentiometrische Messungen im NO-Gasstrom ergeben eine Abhängigkeit der NO-Sensitivität von der Partikelgröße, der Schichtdicke und der Beschichtungsmethode. Impedanzspektroskopische Messungen an beidseitig beschichteten YSZ-Substraten zeigen ebenfalls eine Abhängigkeit des Zellwiderstands von der NO-Konzentration und der Partikelgröße. Die Nanomaterialien zeigen bei unterschiedlichen Sauerstoffpartialdrücken im untersuchten Temperaturbereich (300°C bis 850°C) höhere Leitfähigkeiten als die Volumenmaterialien gleicher Zusammensetzung. Dieses Verhalten wird mit dem höheren Sauerstoffaustausch der Nanomaterialien in Verbindung gebracht, der zur Erzeugung zusätzlicher Defekte in der Kristallstruktur führt. Die Nanostruktur und somit eine entsprechend hohe Leitfähigkeit bleiben bei hohen Sintertemperaturen (T > 1000°C), die der Herstellung gasdichter Presslinge dienen, erhalten. XANES- und Photoelektronenspektroskopie wurden verwendet, um die Punktdefekte zu definieren.

Объектом исследования являются некоторые классы индивидуальных антиоксидантов: SH- содержащие, полифенолы и имеющие в своей структуре фурановый цикл, а также водные экстракты лекарственных трав, которые содержат описанные классы соединений, восполняющих в организме дефицит соединений, борющихся со свободнорадикальным окислением. Цель работы - изучение влияния матричного эффекта на определение антиоксидантной емкости индивидуальных антиоксидантов и экстрактов трав. Изучение литературных данных выявило, что среди прочих достаточно простым и информативным является потенциометрический метод определения антиоксидантной емкости. В рамках работы были применены и сравнены два способа реализации данного метода: с использованием одной формы K3[Fe(CN)6] и системы K3[Fe(CN)6]/ K4[Fe(CN)6], определено значение АОЕ объектов исследования с учетом и без учета матрицы, изучено влияние концентрации антиоксиданта на результаты эксперимента. По результатам измерений и расчетов было сделано заключение, что на результаты потенциометрического определения антиоксидантной емкости оказывает влияние матрица в той или иной степени в зависимости от объекта, отклоняя угол электродной функции. Данный эффект увеличивается с возрастанием концентрации исследуемого объекта. Результаты, полученные двумя способами несколько разнятся ввиду специфики каждого из них. Помимо этого, были выявлены соединения-лидеры по оказанию антиоксидантного действия среди проанализированных экстрактов трав. / The object of the study is some classes of individual antioxidants: SH-containing, polyphenols and having a furan cycle in their structure, and water extracts of medicinal herbs that contain the described classes of compounds that replenish the deficiency of compounds in the body that fight free radical oxidation. The aim of the work is to study the influence of the matrix effect on the determination of the antioxidant capacity of individual antioxidants and herbal extracts. The study of literature data revealed that, among others, a potentiometric method for determining the antioxidant capacity is quite simple and informative. two ways of implementing this method were applied and compared: using one form of K3[Fe(CN)6] and the system K3[Fe(CN)6]/ K4[Fe(CN)6], the value of the antioxidant capacity of the research objects was determined taking into account and without taking into account the matrix, the effect of the antioxidant concentration on the experimental results was studied. Based on the results of measurements and calculations, it was concluded that the matrix of the object influences the results of potentiometric determination of antioxidant capacity, deviating the angle of the electrode function. This effect increases with increasing concentration of the investigated object. The results obtained by the two methods are somewhat different due to the specifics of each of them. In addition, the leading compounds were identified in providing antioxidant action among the analyzed herbal extracts.

No description available.

A despeito dos avanços instrumentais, as titulações continuam sendo largamente aplicadas em laboratórios de química analítica. Seu amplo uso está relacionado com a boa exatidão em aplicações bem estabelecidas e freqüente indicação como método de referência (p. ex., farmacopéias), equipamentos simples, comuns e de custo reduzido, consumo moderado de tempo e de reagentes. Entre as técnicas de titulação, destacam-se as potenciométricas (TP), empregadas universalmente para a quantificação de um ou mais componentes ácidos ou básicos em soluções aquosas ou não aquosas, possibilitando ainda determinar as constantes de dissociação de ácidos e de protonação de bases. Na análise de dados de TP são, via de regra, empregados os métodos clássicos (derivadas), porém, para sistemas compreendendo componentes multiprotonáveis, as inflexões das curvas de titulação deixam ser nítidas, especialmente em baixas concentrações. Nestas condições desfavoráveis, ainda assim podem-se obter resultados satisfatórios recorrendo a métodos de linearização das curvas ou analisando os dados por regressão não linear (RNL), facilmente implementáveis em computadores, hoje disseminados nos laboratórios. Outra técnica clássica para acompanhamento de titulações é a condutimétrica (TC), menos utilizada que a TP nos dias atuais, salvo para ácidos ou bases muito fracas, servindo para prover dados complementares em estudos de formação de complexos ou na caracterização de amostras ambientais. Tipicamente os pontos estequiométricos coincidem com a intersecção de segmentos de reta. Para amostras muito diluídas, com sistemas multipróticos ou com elevada concentração de eletrólitos em relação às espécies tituladas, a interpretação gráfica fica dificultada e a precisão decai. Pesquisas recentes mostraram que é possível aproveitar informações obtidas por TP para alimentar modelos de regressão não linear de TC e, assim, obter informações mais completas das amostras estudadas. No presente trabalho, avançou-se nesta linha criando programas computacionais para a análise simultânea de dados obtidos por TC e TP, empregando o método de RNL e minimizando os desvios (ou o quadrado dos desvios) dos dois conjuntos completos de dados para prover caracterização mais completa das amostras e melhoria na precisão dos resultados. Um programa de simulação de dados de TC e TP das mais diversas combinações e concentrações de sistemas ácido-base, com recursos para acrescentar erros aleatórios às variáveis simuladas, foi também desenvolvido. Permitiu verificar a validade e potencialidade do método da TPC-RNL e aperfeiçoar o programa de análise simultânea de dados. O programa de TPC-RNL foi aplicado inicialmente à re-avaliação de dados de titulações de água de chuva anteriormente coletadas e analisadas por outro colaborador do grupo. Como exemplo de aplicação original a amostras reais difíceis tanto para a TC como a TP isoladamente, determinou-se, por TPC, baixas concentrações de ácidos orgânicos de baixo peso molecular em amostras obtidas do produto de oxidação acelerada do biodiesel. Os resultados se mostraram compatíveis com os obtidos por outro pesquisador que recorreu à eletroforese capilar, sendo que o pH, a condutividade e a força iônica das amostras também foi reproduzida pelo programa Peak Master alimentado com as concentrações ajustadas por RNL / Despite all the advances in instrumental techniques, titrations are still widely applied in analytical chemistry laboratories. Its widespread use is associated with good accuracy, well established applications, simple, readily available and low cost equipment, moderate consumption of time and reagents and frequent indication as a reference method (eg., Pharmacopoeias). Potentiometric titrations (PT) outstands among other techniques, being universally used for the quantification of one or more basic or acidic components in aqueous or non aqueous samples and enabling further determination of the dissociation constants of acids and bases. Data analysis of PT with the glass electrode is typically done by finding the inflections of the curves with help of simple derivatives. However, PT curves of systems with multiprotonable components, specially at very low concentrations, fail to show sharp inflections. Under such unfavorable conditions, satisfactory results can still be obtained by using curve linearization methods or nonlinear regression (NLR) methods, now at the reach of every laboratory computer. Another classic technique for following titrations is conductivity (CT), less used routinely than PT nowadays except for very weak acids or bases, but still valuable as a complementary technique in equilibrium studies of complex formation or for the characterization of environmental samples. The stoichiometric points of simple CTs are found at the intersection of line segments. For very dilute samples or for multiprotic systems or with high concentrations of electrolytes compared to the species to be titrated, the graphical interpretation becomes difficult and the accuracy declines. Recent research has shown that it is possible to harness information obtained by PT to render non-linear regression models of CT solvable, thus extracting more complete information of the samples. This dissertation is devoted to the development and evaluation of software for the simultaneous analysis of data from CT and PT gathered together in the laboratory or by simulation, using the method of NLR with minimization of the weighted deviations (or their squares) of the two full data sets to provide more complete characterization of the samples and to improve the precision of the results. A simulation program for generating CT and PT curves for freely combined acid-base systems over a wide concentration range, with features to add random errors to the simulated variables was also developed. The simulator was used to evaluate the validity and potentiality of the PCTNLR method and improve the software of simultaneous data analysis. The program of PCT-NLR was applied firstly to the re-evaluation of data from titrations of rainwater collected and analyzed previously by another contributor to the group. As an original application example to real samples that are difficult for CT or PT separately, low concentrations of organic acids of low molecular weight were determined by PCT-NLR in samples from accelerated biodiesel oxidation tests. The results were consistent with those obtained by another researcher who used the capillary electrophoresis. The pH, ionic strength and conductivity of the samples were also reproduced by the program Peak Master using concentrations adjusted by NLR

The goal of this study was to characterize the binding sites on the surface of wheat roots, Triticum turgidum, involved in the adsorption of protons and metals, and quantify the thermodynamic constants needed for a surface complexation model to predict metal binding. The adsorption of protons, Cd(II), Cu(II), and Ni(II) to the root surface as a function of pH and ionic strength in single metal exposure scenarios was quantitatively described using potentiometric titrations, batch metal adsorption experiments, and the least squares fitting program FITEQL. Model predictions from single metal exposures were compared to measured metal adsorption concentrations when roots were exposed to binary and ternary combinations of the metals. Proton dissociation was a function of three discrete monoprotic acid sites on the root surface with log proton dissociation constants of -4.50, -6.23, and -7.37 respectively, upon which varied ionic strength had no effect. The total proton binding capacities for the three sites were 2.58 x 10-4, 1.29 x 10-4, and 2.58 x 10-4 M, respectively. Metal complexation was best described by a two-site model having conditional stability constant log values of 3.04 and 3.30 for Cd(II), 3.21 and 3.25 for Cu(II), and 2.83 and 2.84 for Ni(II) at ionic strength 0.01M. At ionic strength 0.1 M the conditional stability constants log values were 2.37 and 3.36 for Cd(II), 3.11 and 2.56 for Cu(II), and 2.18 and 3.00 for Ni(II). When roots were exposed to binary or ternary mixtures of the metals, the two monoprotic acid single metal model did not provide ideal fits to the data indicating that adsorption in a metal mixture scenario cannot be considered additive and is dependent on the combination of metals present in the exposure environment. The experimentally determined proton dissociation constants and metal stability constants could be used in commercial geochemical speciation programs such as Visual MINTEQ to predict metal adsorption to plants. / Natural Sciences and Engineering Research Council of Canada, The Mining Association of Canada, Ontario Power Generation, Environment Canada.

A despeito dos avanços instrumentais, as titulações continuam sendo largamente aplicadas em laboratórios de química analítica. Seu amplo uso está relacionado com a boa exatidão em aplicações bem estabelecidas e freqüente indicação como método de referência (p. ex., farmacopéias), equipamentos simples, comuns e de custo reduzido, consumo moderado de tempo e de reagentes. Entre as técnicas de titulação, destacam-se as potenciométricas (TP), empregadas universalmente para a quantificação de um ou mais componentes ácidos ou básicos em soluções aquosas ou não aquosas, possibilitando ainda determinar as constantes de dissociação de ácidos e de protonação de bases. Na análise de dados de TP são, via de regra, empregados os métodos clássicos (derivadas), porém, para sistemas compreendendo componentes multiprotonáveis, as inflexões das curvas de titulação deixam ser nítidas, especialmente em baixas concentrações. Nestas condições desfavoráveis, ainda assim podem-se obter resultados satisfatórios recorrendo a métodos de linearização das curvas ou analisando os dados por regressão não linear (RNL), facilmente implementáveis em computadores, hoje disseminados nos laboratórios. Outra técnica clássica para acompanhamento de titulações é a condutimétrica (TC), menos utilizada que a TP nos dias atuais, salvo para ácidos ou bases muito fracas, servindo para prover dados complementares em estudos de formação de complexos ou na caracterização de amostras ambientais. Tipicamente os pontos estequiométricos coincidem com a intersecção de segmentos de reta. Para amostras muito diluídas, com sistemas multipróticos ou com elevada concentração de eletrólitos em relação às espécies tituladas, a interpretação gráfica fica dificultada e a precisão decai. Pesquisas recentes mostraram que é possível aproveitar informações obtidas por TP para alimentar modelos de regressão não linear de TC e, assim, obter informações mais completas das amostras estudadas. No presente trabalho, avançou-se nesta linha criando programas computacionais para a análise simultânea de dados obtidos por TC e TP, empregando o método de RNL e minimizando os desvios (ou o quadrado dos desvios) dos dois conjuntos completos de dados para prover caracterização mais completa das amostras e melhoria na precisão dos resultados. Um programa de simulação de dados de TC e TP das mais diversas combinações e concentrações de sistemas ácido-base, com recursos para acrescentar erros aleatórios às variáveis simuladas, foi também desenvolvido. Permitiu verificar a validade e potencialidade do método da TPC-RNL e aperfeiçoar o programa de análise simultânea de dados. O programa de TPC-RNL foi aplicado inicialmente à re-avaliação de dados de titulações de água de chuva anteriormente coletadas e analisadas por outro colaborador do grupo. Como exemplo de aplicação original a amostras reais difíceis tanto para a TC como a TP isoladamente, determinou-se, por TPC, baixas concentrações de ácidos orgânicos de baixo peso molecular em amostras obtidas do produto de oxidação acelerada do biodiesel. Os resultados se mostraram compatíveis com os obtidos por outro pesquisador que recorreu à eletroforese capilar, sendo que o pH, a condutividade e a força iônica das amostras também foi reproduzida pelo programa Peak Master alimentado com as concentrações ajustadas por RNL / Despite all the advances in instrumental techniques, titrations are still widely applied in analytical chemistry laboratories. Its widespread use is associated with good accuracy, well established applications, simple, readily available and low cost equipment, moderate consumption of time and reagents and frequent indication as a reference method (eg., Pharmacopoeias). Potentiometric titrations (PT) outstands among other techniques, being universally used for the quantification of one or more basic or acidic components in aqueous or non aqueous samples and enabling further determination of the dissociation constants of acids and bases. Data analysis of PT with the glass electrode is typically done by finding the inflections of the curves with help of simple derivatives. However, PT curves of systems with multiprotonable components, specially at very low concentrations, fail to show sharp inflections. Under such unfavorable conditions, satisfactory results can still be obtained by using curve linearization methods or nonlinear regression (NLR) methods, now at the reach of every laboratory computer. Another classic technique for following titrations is conductivity (CT), less used routinely than PT nowadays except for very weak acids or bases, but still valuable as a complementary technique in equilibrium studies of complex formation or for the characterization of environmental samples. The stoichiometric points of simple CTs are found at the intersection of line segments. For very dilute samples or for multiprotic systems or with high concentrations of electrolytes compared to the species to be titrated, the graphical interpretation becomes difficult and the accuracy declines. Recent research has shown that it is possible to harness information obtained by PT to render non-linear regression models of CT solvable, thus extracting more complete information of the samples. This dissertation is devoted to the development and evaluation of software for the simultaneous analysis of data from CT and PT gathered together in the laboratory or by simulation, using the method of NLR with minimization of the weighted deviations (or their squares) of the two full data sets to provide more complete characterization of the samples and to improve the precision of the results. A simulation program for generating CT and PT curves for freely combined acid-base systems over a wide concentration range, with features to add random errors to the simulated variables was also developed. The simulator was used to evaluate the validity and potentiality of the PCTNLR method and improve the software of simultaneous data analysis. The program of PCT-NLR was applied firstly to the re-evaluation of data from titrations of rainwater collected and analyzed previously by another contributor to the group. As an original application example to real samples that are difficult for CT or PT separately, low concentrations of organic acids of low molecular weight were determined by PCT-NLR in samples from accelerated biodiesel oxidation tests. The results were consistent with those obtained by another researcher who used the capillary electrophoresis. The pH, ionic strength and conductivity of the samples were also reproduced by the program Peak Master using concentrations adjusted by NLR

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No. of bitstreams: 1 marcosrodriguesfacchinicerqueira.pdf: 4104766 bytes, checksum: a30bb0a2c3edae3f0d744732482aa070 (MD5) Previous issue date: 2012-03-02 / CAPES - Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / CNPq - Conselho Nacional de Desenvolvimento Científico e Tecnológico / FAPEMIG - Fundação de Amparo à Pesquisa do Estado de Minas Gerais / Muitas pessoas sofrem da falta crônica de água potável para necessidades pessoais e, nesse contexto, a água de chuva surge como uma possível fonte alternativa. Em cima disso, foi proposto um método simples e efetivo para a determinação de cobre(II), cádmio(II), zinco(II) e chumbo(II) em 64 amostras de água de chuva de Juiz de Fora/MG/Brasil utilizando a técnica de redissolução potenciométrica. Um potenciostato μ-AUTOLAB foi utilizado para a aquisição dos dados e a célula eletroquímica consistia de um eletrodo de trabalho de carbono vítreo modificado com filme de mercúrio, um eletrodo de Ag/AgCl(sat) como eletrodo de referência e um de eletrodo de platina como eletrodo auxiliar. Foi realizada uma avaliação do pH do meio variando de 0-3 para uma determinação simultânea de Cd, Pb e Cu e de 0-6 para a determinação de Zn. Um Planejamento Estrela 22 foi realizado para a otimização das condições eletroquímicas das determinações. Para as determinações de Cd, Pb e Cu foram estudados níveis entre -1,06 e -0,64 V para o potencial de deposição (Ed), com tempo de deposição (td) entre 239 s e 662 s. Para a determinação de Zn os níveis estudados para o Ed foram entre -1,70 V e -1,10 V, com td entre 239 s e 662 s. A condição ótima encontrada para o pH do meio foi de pH = 4 para a determinação de Zn e um pH = 0 para a determinação de Cd, Pb e Cu. De acordo com as superfícies de resposta obtidas, foi estipulado para a determinação de Zn um Ed = -1,40 V e um td = 300 s e para a determinação de Cd, Pb e Cu um Ed = -1,00 V e um td = 300 s. Foram construídas curvas analíticas para verificar a linearidade do método. Os limites de detecção e quantificação foram de 1,26 e 3,83 μg L-1 para Zn, 0,38 e 1,26 μg L-1 para Cd, 0,41 e 1,36 μg L-1 para Pb e 0,96 e 3,20 μg L-1 para Cu, respectivamente. O método mostrou valores de recuperação entre 86 e 113%. As amostras de água de chuva também foram analisadas por espectroscopia de absorção atômica em forno de grafite (GFAAS), como método de referência, demonstrando uma boa correlação entre os resultados. Foram encontrados valores entre 3,93 e 13,8 μg L-1 de Zn, 3,11 e 7,51 μg L-1 de Cu, enquanto que nenhuma concentração significativa foi observada para Pb e Cd. Conforme os valores estipulados na Portaria nº 2914, de 12 de dezembro de 2011, do Ministério da Saúde, a água de chuva da região de Juiz de Fora pode ser considerada como potável com relação os parâmetros avaliados. / Many people suffer from a chronicle lack of potable water for their personal needs and, in this context, the rainwater arises as a possible alternative source. Upon this, an effective and simple method to determine copper(II), cadmium(II), zinc(II) and lead(II) in 64 rainwater samples from Juiz de Fora/MG/Brazil, using potentiometric stripping analysis (PSA), is proposed. A μ-AUTOLAB potentiostat was used for data acquisition and the electrochemical cell consisted of a working glassy carbon electrode modified with a thin mercury film, an Ag/AgCl(sat) as reference electrode and a platinum as auxiliary electrode. The pH of the medium was evaluated in the range of 0-3 for the simultaneous determination of Cd, Pb and Cu, and in the range of 0-6 for Zn. A 22 Star Design was run to optimize the analytical conditions. For Cd, Pb and Cu determination the studied levels for deposition potential (Ed) were between -1.06 V and -0.64 V, with deposition time (td) between 239 s and 662 s. For Zn determination the studied levels for Ed were between -1.70 V and -1.10 V, with td between 239 s and 662 s. The optimum medium pH conditions found were of pH = 4 for Zn determination and pH = 0 for Cd, Pb and Cu determination. According to the obtained response surfaces it was stipulated for Zn determination a Ed = -1.40 V and a td = 300 s and for Cu, Pb and Cd determination a Ed = -1.00 V and a td = 300 s. Analytical curves were constructed to verify the method linearity. The detection and quantification limits were of 1.26 and 3.83 μg L-1 for Zn, 0.378 and 1.26 μg L-1 for Cd, 0.407 and 1.36 μg L-1 for Pb and 0.960 and 3.20 μg L-1 for Cu, respectively. The method showed recovery values between 86 and 113%. The rainwater samples were also analyzed by graphite furnace atomic absorption spectrometry (GFAAS), as reference method, showing a good correlation between the results. Values between 3.93 and 13.8 μg L-1 of Zn, 3.11 and 7.51 μg L-1 of Cu were found, while no significant concentrations of Pb and Cd were found. According to the stipulated values on Portaria nº 2914, of december 12 of 2011, from Ministério da Saúde, the Juiz de Fora region rainwater can be considered potable, with respect to the evaluated parameters.

Объектами исследования служили фармацевтическая субстанция «Аргамид» и готовая лекарственная форма 1% крем «Аргамид» на основе серебряной соли сульфадимидина (Приоритетная справка на выдачу патента № 2015153574 от 14.12.2015). Данная соль и лекарственные средства на ее основе были разработаны на базе кафедры фармации УГМУ с целью обеспечения российского фармацевтического рынка эффективными антибактериальными и ранозаживляющими лекарственными препаратами отечественного производства согласно стратегии развития фармацевтической промышленности «ФАРМА-2020». Цель работы: разработка и валидация методик количественного определения серебра в исследуемых лекарственных средствах. Анализ литературных данных показал, что оптимальным методом определения серебра является метод осадительного титрования с потенциометрической индикацией конечной точки титрования. При этом, учитывая содержание серебра в анализируемых лекарственных средствах, для его определения в субстанции был выбран метод роданометрического, а в готовой лекарственной форме – йодометрического титрования. Для анализируемых лекарственных средств были подобраны оптимальные условия пробоподготовки: масса навески, концентрация растворителя; время и температура обработки пробы. В качестве индикаторного вместо дорогостоящего импортного серебряного дискового электрода использовали отечественный толстопленочный серебросодержащий электрод. Положительные результаты валидационной оценки разработанных методик, проведенной согласно требованиям Государственной Фармакопеи РФ XIII изд., позволяют считать их приемлемыми и рекомендовать для включения в проекты фармакопейных статей на исследуемые лекарственные средства. Контроль содержания серебра по разработанным методикам не требует дорогостоящего оборудования, привлечения высококвалифицированного персонала, отличается относительно коротким временем анализа, а, следовательно, может применяться испытательными лабораториями предприятия в процессе производства и центрами контроля качества во время обращения на фармацевтическом рынке исследуемых лекарственных средств. / The objects of study were pharmaceutical substance "Argamid" and finished dosage form of 1% cream "Argamid" based on silver salt sulfadimidine (Priority reference patent number 2015153574 from 14.12.2015). This salt and drugs based on it have been developed at the Department of Pharmacy UGMU to ensure that the Russian pharmaceutical market effective antibacterial and wound healing medicines domestic production according to the strategy of development of the pharmaceutical industry "Pharma 2020". Objective: Development and validation of methods of quantitative determination of silver in the investigational medicinal product. Analysis of published data shows that the best method of determining silver is the method of precipitation titration with potentiometric indication end point. However, given the content of silver in the analyzed medicaments for identification substance rodanometricheskogo method was selected, and in the final dosage form - iodometric titration. optimal conditions for sample preparation were selected to be analyzed drugs: sample weight, the concentration of solvent; Sample processing time and temperature. As an indicator instead of expensive imported silver disk electrode used domestic thick-film silver-electrode. Positive results validation assessment developed techniques conducted in accordance with the requirements of the RF State Pharmacopoeia XIII ed., Allow us to consider them acceptable and recommended for inclusion in the draft articles on the pharmacopoeia investigational medicinal products. Control of the silver content by developed techniques does not require expensive equipment, highly skilled personnel, has a relatively short analysis time, and, therefore, can be applied testing laboratories of the enterprise in the production process and quality control center during handling in the pharmaceutical market of investigational medicinal products.

The monitoring of pharmaceuticals, heavy metal, pH and free chlorine concentration in drinking water is important for public health and the environment. However, conventional laboratory-based analytical methods are labor-intensive, expensive, and time consuming. This thesis focuses on developing an integrated, highly sensitive, easy-to-use, and low-cost pharmaceuticals, heavy metal, pH and free chlorine sensing system for drinking water quality monitoring. A low-temperature, solution-processed modification of multi-walled carbon nanotubes (MWCNT) with β-cyclodextrin (βCD) on glassy carbon electrode is developed for detecting low levels of acetaminophen. The adsorption properties of βCD are combined with the high surface area of carbon nanotubes towards enhanced electrochemical sensing of acetaminophen with a limit of detection of 11 nM and linear range from 0.05-300 μM. Also, a systematic investigation is carried out using four types of modified MWCNT-βCD. A novel, one-step approach called Steglich esterification modified MWCNT-βCD results in large effective surface area, and fast electron transfer towards sensitive detection of acetaminophen and 17β-estradiol (E2, primary female sex hormone) in the range of 0.005–20 and 0.01–15 μM, with low detection limits of 3.3 and 2.5 nM, respectively. The similar MWCNT-βCD modified electrodes can also detect heavy metal ion (lead, Pb2+) with a limit of detection of <10 ppb. Low frequency noise behavior of these sensors are studied. A spin-coated Pd/PdO based pH sensor, and amine-modified carbon electrode-based free chlorine sensor are fabricated on a common substrate together with the pharmaceuticals and heavy metal sensors. A Wheatstone-bridge temperature sensor is fabricated based on silicon and PEDOT:PSS on another substrate. All the sensors are connected to an Arduino microcontroller based data acquisition system with a smartphone application interface. The integrated sensing system is easy-to-use, low-cost, and can provide accurate monitoring data with real drinking water samples. / Dissertation / Doctor of Philosophy (PhD) / Low-cost, easy-to-use, and sensitive monitoring system for pharmaceuticals, heavy metal, pH and free chlorine in drinking water is crucial for public health safety. In this thesis, we develop solution-based synthesis of multi-walled carbon nanotubes modified by β-cyclodextrin for electrochemical sensing of pharmaceuticals and heavy metal. The modification approaches are compared and characterized to analyze their electrochemical behavior and sensing performances. The developed sensors are highly sensitive toward the detection of acetaminophen (a widely used pain-killer) and estrogen hormone in drinking water. We also develop a modified spin-coating technique to deposit palladium/palladium oxide films for potentiometric pH sensor, a calibration-free free chlorine sensor based on modified carbon electrode, and a resistive temperature sensor. The developed pH, free chlorine and temperature sensors are highly sensitive, and stable with fast response time. All the sensors are integrated and interfaced with a custom-made and smartphone-controlled electronic readout system for accurate and on-site drinking water quality monitoring at low cost.

From the Proceedings of the 1973 Meetings of the Arizona Section - American Water Resources Assn. and the Hydrology Section - Arizona Academy of Science - May 4-5, 1973, Tucson, Arizona / Groundwater modeling is used to theoretically relate mining pumpage of the Navajo Sandstone to declines in the potentiometric surface at Navajo and Hopi Indian community, domestic, and stock usage locations. The shallow wells on top of Black Mesa are shown to be part of a perched water table condition which is dependent upon the hydraulic conductivity of an aquatard known as the Mancos Shale. The isolation of the aquatard allows the shallow wells to be treated as a problem separate from that of the artesian and recharge areas. Computer modeling of the groundwater system is concerned only with those Indian wells which directly tap the Navajo Sandstone in either artesian or free water table areas. The computer simulation developed is a modified version of the basic artesian aquifer routine used by the Illinois State Water Survey. Computer results correspond with the low percentage of storage withdrawal calculated for the artesian area under Black Mesa.