Water samples in the vicinity of Muncie were analyzed for trace elements such as cadmium, chromium, lead, titanium, iron, zinc, barium, calcium, potassium, manganese, sodium, strontium and magnesium. The analysis was made by a lower rotating graphite electrode partly submerged in the water being analyzed. The light emitted by the spark was analyzed using a Littrow Spectrograph. Water samples were taken from five stations along the White River in the Muncie area. The intensities of the spectral lines of trace elements and of standardized solutions were compared for quantitative analysis. Trace metals detected and concentrations in (ppm) found were as follows: Ba 0.04, Ca 72.6,. K 0.05, Mg 23.7, Mn 0.05, Na 27.1, Sr 0.70, Cr 0.02. The elements Ca, Mg, Na and K were expected to be found in high concentration and Ba, Sr, Mn and Cr were expected to be found in low concentration.In a previous study conducted at Ball State, neutron activation analysis was used in this area with positive results for eleven elements. The purpose of the present study was to extend this research by attempting to detect elements by spark-emission spectroscopy concentrating on elements that were difficult to detect by neutron activation analysis.Ball State UniversityMuncie, IN 47306

No description available.

Dissertation submitted in partial compliance with the requirements of the Masters Degree in Technology: Chemistry, in the Faculty of Applied Sciences at the Durban University of Technology, 2008. / In this work, a holistic approach to validate analytical methods was assessed by virtue of Monte Carlo simulations. This approach involves a statement of the methodsâ s scope (i.e. analytes, matrices and concentration levels) and requisites (internal or external); selection of the methodâ s (fit-for-purpose) features; pre-validation and validation of the intermediate accuracy and its assessment by means of Monte Carlo simulations. Validation of the other methodâ s features and a validity statement in terms of a â fit-for-purposeâ decision making, harmonized validation-control-uncertainty statistics and short-term routine work with the aim of proposing virtually â ready-to-useâ methods. The protocol could be transferred to other methods. The main aim is to harmonize the work to be done by research teams and routine laboratories assuming that different aims, strategies and practical viewpoints exist. As a result, the recommended protocol should be seen as a starting point. It is necessary to propose definitive (harmonized) protocols that must be established by international normalisation/accreditation entities. The Quality Assurance (Method verification and Internal Quality Control, IQC) limits, as well as sample uncertainty were estimated consistently with the validated accuracy statistics i.e. E U (E) and RSDi + U (RSDi). Two case studies were used to assess Monte Carlo simulation as a tool for method validation in analytical laboratories, the first involves an indirect polarographic method for determining nitrate in waste water and the second involves a direct determination of heavy metals in sea water by differential pulse anodic stripping voltammetry, as an example of the application of the protocol. In this sense the uncertainty obtained could be used for decision making purposes as it is very tempting to use uncertainty as a commercial argument and in this work it has been shown that the smaller the uncertainty, the better the measurement of the instrument or the laboratoryâ s reputation.

Tap water collected according to standard methods was examined for microbial presence. Epifluorescent diagnoses using redox probe 5-cyano-2,3ditolyl tetrazolium chloride (CTC), 4',6-diamidino-2-phenylindole (DAPI), and acridine orange (AO) were employed for direct evidence of microorganisms. Evidence of total (DAPI or AO), respiring (CTC) bacteria, and heterotrophic plate count (HPC) was determined on multiple occasions during the summer, fall, and winter 1996-1997. Pseudomonas aeruginosa, Acinetobacter sp., Bacillus licheniformis, and Methylobacterium rhodinum were isolated and identified by the API and Biolog system using GN and GP procedures. On the basis of comparisons presented in this study between the CTC method and the standard HPC procedure, it appeared that the number of CTC-reducing bacteria in the tap water samples was typically higher than that determined by HPC, indicating that many respiring bacteria detected by the CTC reduction technique fail to produce visible colonieson the agar media used. In the seasonal data obtained by the CTC method, no difference was shown among respiring bacterial counts obtained from June through January. In the examination of P. aeruginosa viability in presence of chlorine, the number of CTC-positive bacteria exceeded the number of CFU by more than 2 logs after exposure to chlorine, suggesting that reliance on HPC overestimate the efficacy of disinfection treatment. In inactivation assays using the Biolog MT plate, no sensitivity to chlorine or chloramine disinfectants was noted even at high concentration levels (5 mg/liter). Following initial drop, bacterial activities increased as contact time increased. Thus, it appears that the MT microplate provides too low a cell concentration, too great a contact time, and/or too low a concentration of tetrazolium dye within the well for successful analysis of disinfectant capability to selected bacterial strains isolated from distribution water. / Department of Biology

Made available in DSpace on 2015-04-11T13:53:53Z (GMT). No. of bitstreams: 1 rita.pdf: 2875613 bytes, checksum: 5e32b07a7fbd4413969184f90ce62026 (MD5) Previous issue date: 2009-11-03 / O abastecimento de água potável a uma população tem ação direta na saúde pública e na qualidade de vida por atuar diretamente na eliminação dos riscos vinculados ao consumo de água contaminada por microorganismos prejudiciais a saúde. Apesar do saneamento básico ser, segundo a OMS, um grande provedor na diminuição dos índices de morbidade e mortalidade infantil no mundo, o acesso da população ao serviço não é uma realidade presente para uma boa parcela da população urbana nas grandes cidades brasileiras. A problemática relativa a este assunto na cidade de Manaus serviu como fomento para uma análise na qualidade da água consumida em escolas. O estudo tem como objetivo avaliar as condições sanitárias da água de consumo humano e a situação higiênico-sanitária dos sistema de abastecimento de água e esgoto sanitário das edificações escolares. A pesquisa teve como fonte de dados os laudos microbiológicos e físico-químicos da água, assim como os relatórios de inspeção técnicas de cada escola gerados pelas ações de vigilância em saúde ambiental do projeto VISA na ESCOLA da Secretaria Municipal de Saúde. O estudo foi realizado nas escolas públicas municipais situadas na zona leste de Manaus. Os parâmetros selecionados nas ações de vigilância constituíram um Indicador Sintético Escolar (ISE) formado por 24 parâmetros (2 microbiológicos, 6 físico-químicos e 16 higiênico-sanitários). O ISE classificou as 103 escolas em 03 classes: adequada (18), regular (39) e inadequada (46), conforme as condições sanitárias da água e a situação higiênico-sanitária das instalações hidrosanitárias encontrada nas ações de fiscalização. A classe inadequada do ISE englobou as escolas com presença de coliformes totais e coliformes termotolerantes na água de consumo demonstrado que existe uma população sob risco de contrair doenças pelo consumo de água fora dos padrões da Portaria 518/2004 MS. A classificação do ISE foi espacializado em mapa temático por meio da técnica de geoprocessamento. O uso do ISE composto de dados mistos (quantitativos e qualitativos) na avaliação das condições sanitárias da água de consumo mostrou-se como uma ferramenta de auxilio apropriada para a vigilância em saúde ambiental utilizar nas ações de controle das condições sanitárias da água consumida nos estabelecimentos de ensino da rede pública municipal de Manaus

Esta tese descreve o desenvolvimento de metodologias eletroanalíticas, em especial a voltametria de onda quadrada com o eletrodo de gota pendente de Hg, para determinação de atrazina em águas de rios do Estados de São Paulo e em amostras de solo. A exatidão das metodologias foi avaliada por comparação com HPLC e estudos de recuperação. Inicialmente desenvolveu-se o método em modo estático, no qual a maior sensibilidade foi obtida em pH 2 e freqüência de 400 Hz, com limites de detecção e determinação de 2 e 10 microgramas L-1, respectivamente. O estudo do comportamento eletroquímico revelou que a atrazina comporta-se reversivelmente em altas freqüências de onda quadrada. Dentre os metabólitos da atrazina, a desetilatrazina e desiosopropilatrazina, também são eletroativas nas condições estudadas, sendo possíveis interferentes, ao contrário da hidroxiatrazina e didealquilatrazina. Sistemas em fluxo contínuo e de injeção seqüencial foram desenvolvidos para determinação de atrazina em extrato de solo e águas naturais, bem como em estudos de adsorção. Em águas, os limites de detecção e determinação obtidos por injeção seqüencial foram de 4,5 e 15 microgramas L-1. Estudos de adsorção revelaram que atrazina liga-se mais fortemente a solos em meios ácidos. As metodologias em fluxo permitiram um significativo aumento da velocidade analítica e economia de reagentes, automatizando as determinações. / This thesis describes the development of electroanalytical methodologies, especially the square wave voltammetry with the hanging mercury drop electrode, for determination of the herbicide atrazine in river waters of the São Paulo state and soil samples. The accuracy of the methodologies was evaluated by comparison with HPLC and recovery studies. Initially, a stationary method was developed, in which the highest sensitivity was attained at pH 2 and at frequency of 400 Hz, with detection and quantification limits of 2 and 10 micrograms L-1, respectively. The electrochemical behavior of atrazine was reversible at the higher square wave frequencies. Among the atrazine metabolites, deethylatrazine and deisopropylatrazine are also electroactive under the studied conditions, being possible interferences, contrary to hydroxyatrazine and didealkylatrazine. Continuous flow and sequential injection systems were developed for determination of atrazine in soil extracts and natural waters, as well as in adsorption studies. In waters, the detection and quantification limits attained by sequential injection were 4.5 and 15 micrograms L-1. Adsorption studies showed that atrazine binds more strongly to soil in acidic media. The flow analysis methodologies lead to significant increase in the sampling throughput and reagent saving, automating the determinations.

A oferta de água vem se tornando cada vez mais diminuta à medida que a população, a indústria e a agricultura se expandem. A contaminação dos mananciais gerada pelo descarte de efluentes domésticos e industriais leva a eutrofização, processo pela qual grande aporte de nutrientes, particularmente fosfatos, leva ao crescimento excessivo de algas. As cianobactérias são microrganismos procariontes, que vivem nos ambientes mais adversos. A floração dessas algas quando presente em mananciais destinados ao consumo humano gera sérios problemas à saúde humana, pois algumas dessas algas podem gerar toxinas, conhecidas como hepatotoxinas, neurotoxinas e dermatotoxinas, de acordo com sua ação farmacológica. Dentre as hepatotoxinas encontramos a microcistina, um heptapeptídeo cíclico que pode levar à morte em horas ou dias. O objetivo desse estudo foi viabilizar a técnica HPLC, já proposta por outros autores, para quantificar microcistinas-LR em reservatórios de água, em escala empresarial para ser implementada em laboratórios de análise de águas. Para o desenvolvimento da técnica, foram utilizadas amostras de uma lagoa com floração de Microcystis. Para determinar a eficiência da técnica cromatográfica, foram realizados estudos com outro método, através do kit ELISA. Nessa etapa do trabalho, verificou-se que a técnica HPLC é mais sensível e viável para a quantificação das microcistinas. Nos experimentos realizados com a cromatografia líquida, observou-se que a coluna C-18 LiChrosorb (25 cm) 7 Sm utilizada no método, e o solvente metanol apresentaram grande influência nos resultados. À medida que os experimentos foram executados, verificou-se o decréscimo da sensibilidade da coluna. Os resultados foram satisfatórios apenas após a limpeza realizada na coluna, onde os padrões apresentaram uma curva de correlação igual a 0,92. Este fato leva a concluir que as colunas precisam ser renovadas para análises mais sensíveis, como no caso das microcistinas. As amostras extraídas com metanol apresentaram resultados relevantes, isto é, quanto maior a concentração de metanol utilizado na extração, maior a concentração de microcistina-LR obtida nos resultados, concluindo o metanol ser o solvente apropriado para a extração. Por fim, conclui-se que o método desenvolvido é viável, apresentando algumas dificuldades para sua implantação em escala empresarial. / The water supply has been decreasing more and more as the population, industry and agriculture expand. The contamination of the water sources generated by the domestic and industrial effluents discharges leads to the eutrophization, process where the large presence of nutrients, particularly phosphates, causes excessive increase of algae. The cyanobacteria are procaryote microorganisms which live in the most diverse environments. The florescence of the algae when present in sources directed to human consumption generates serious problems to the human health, for some of them may produce toxins known as hepatotoxins, neurotoxins and dermotoxins, according to their pharmacological action. Among the hepatotoxins, the microcystin, a cyclic heptapeptide that can lead to death in hours or days, is found. The objective of this study was to make feasible the use of the HPLC technique, already proposed by other authors, to quantify microcystins-LR in water reservoirs, in enterprise scale to be implemented in water analysis laboratories. In order to develop the technique, samples of water from a pond with Microcystis florescence were utilized. To evaluate the efficiency of the chromatographic technique, studies were performed with another method, through the ELISA kit. In this phase of the work, it was verified that the HPLC technique is the most sensible and viable for the quantification of the microcystins. It was observed, in the experiments performed with the liquid chromatography, that the column C-18 LiChrosorb (25 cm) 7 Sm utilized in the method and the methanol solvent presented great influence in the results. As the experiments were realized, the decrease of the sensibility of the column was verified. The results were satisfactory only after the column being cleaned, when the patterns presented a curve of correlation equal to 0.92. This fact leads to the conclusion that the columns need to be renewed for more sensible analysis, like in the case of the microcystins. The samples extracted with methanol presented relevant results, that is, the greater the concentration of the methanol utilized, the higher the concentration of microcystin-LR obtained in the results, leading to the conclusion that methanol was the solvent adequate to the extraction. Finally, it was concluded that the method developed is feasible, presenting some difficulties concerning its implantation in enterprise scale.

Ph.D. / This study explored the possible application of a relatively new electrode called exfoliated graphite electrode (EG electrode) in the electroanalysis of organic and inorganic water pollutants. This study also explored the applicability of this electrode in the removal of heavy metal pollutants in water. The EG material was successfully prepared by intercalating bisulphate ions into graphite flakes (>300 μm) followed by thermal shock at 800°C to obtain an exfoliated graphite. After compressing the EG at high pressure, the obtained circular sheets were used to fabricate electrodes. The electrochemical profiles of EG electrode and glassy carbon electrodes (GCE) were recorded and compared using cyclic voltammetryand square wave voltammetry in the presence of various supporting electrolytes and [Fe(CN)6]3-/4-, [Ru(NH3)6]2+/3+, ferrocene redox probes. In the supporting electrolytes (KCl, H2SO4, NaOH, tetrabutylammoniumtetraflouroborate, phosphate buffers), the potential windows of EG were found, in some cases, to be about 300 mV larger than that of GCE. The diffusion coefficients (cm2s-1) of the redox probes were calculated to be 3.638 x 10-6, 1.213 x 10-6 and 4.411 x 10-6 for [Fe(CN)6]3-/4-, [Ru(NH3)6]2+/3+ and ferrocene, respectively. These values are comparable to those obtained from GCE. Furthermore, EG was modified with various nanomaterials such as poly (propylene imine) dendrimer (PPI), gold nanoparticles, silver nanoparticles, dendrimer–gold nanoparticles composite, cobalt oxide and bismuth. The morphologies of the modified electrodes were studied using scanning electron microscopy and their electrochemical reactivities in the three redox probes were investigated. The current and the reversibility of redox probes were enhanced in the presence of modifiers in different degrees with dendrimer and gold nanoparticles having a favourable edge. The electrochemical determination of o-nitrophenol by square wave voltammetry using a nanocomposite of generation 2 poly(propyleneimine) dendrimer and gold nanoparticles modified GCEand EG electrode were compared. A characteristic reduction peak between -600 mV and -700 mV for o-nitrophenol was observed with enhanced current on both GCE and EG modified electrodes.

The theses compares analytical methods according to current norms used in the Czech Republic to the methods based on the principle according to US EPA. A new device the automatic photometer Aquakem 250 makes use of the US EPA methods. Prior to its laboratory use in the Institute of Public Health in the town of Ostrava the photometer had to be validated. For the comparsion of the analytical methods ion chromatographic, isotachophoresis, spectrophotometric,titrimetric methods were used. The validation process, which was documented (in validation protocols), was time consuming and technically challenging. It was confirmed that the new Aquakem 250 analyzer provides result that are verified by methods which are in accordance with norms applicable in the Czech Republic. After a successful completion of validation and obtained accreditation the new automatic analyzer was put into regular operation in the chemically laboratory.

This thesis describes some new methods for analysis oforganic trace components from air and water by gaschromatography. The work is particularly focused on thedevelopment of new technologies for analyte enrichment, usingsorbent-based concepts. Short lengths of open tubular columnswere examined for their potential use as denuders.Polydimethylsiloxane-based stationary phases as well as anadsorbent-based column were evaluated in an equilibrium mode oftrapping. For the analytes selected, detection levels in theppb range were obtained (Paper I). A new, fully automated set-up for analysis of organic tracecomponents in aqueous samples has been developed (Paper II).The work combines specific advantages of the solid phase microextraction (SPME) technology and stir bar sorptive extractionconcept. Ultra trace components, down to 0.1 ppt could bedetected. Finally a simple method for preparation a new type ofultra thick film open tubular trap is described (Paper III).The traps are characterized by an irregular coating, and it wasdemonstrated that the performance characteristics of thesetraps were practically as good as of traps with a smooth,regular coating. The technology can be utilized in many areas,e.g. environmental monitoring, process analysis and otherfields dealing with analysis of trace organic volatiles ingaseous samples. <b>Keywords:</b>Organic trace components, volatiles, denuders,sorbent trapping, thick film trapping, open tubular traps,SPME, automation, water analysis, gas analysis, environmentalanalysis. / NR 20140805