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Determination Of Boron In Water Samples By Electrothermal Atomic Absorption SpectrometrySimsek, Nail Engin 01 September 2012 (has links) (PDF)
Boron (B) is a rare element on Earth crust with a natural abundance of 0.001%. However, boron content of water and soils may be significantly high in the regions with rich boron reserves. In addition, extensive use of agrochemicals in soils as well as various natural processes increases the boron concentration in water. Despite B is an essential element for all living creatures, it may pose risks at high level exposures. World Health Organization (WHO) has recommended a daily intake of 1 to 13 mg B for adults.
Turkey has almost 70% of world boron reserves principally in four regions: Kü / tahya, Emet / Balikesir, Bigadiç / Eskisehir, Kirka and Bursa, Kemalpasa. The boron content of water in these regions may go up to significant levels. Therefore, it is important to determine B in drinking water from these regions.
Electrothermal atomic absorption spectrometry (ETAAS) is a relatively sensitive technique for determination of boron. However, the technique suffers from formation of molecular boron compounds. Therefore, use of chemical modifiers and pyrolytically coated graphite tubes modified with refractory carbide forming elements (Ta, W, Zr, Pd, Ru, Os) were utilized to develop a reliable and sensitive method. Based on optimization studies, Tantalum (Ta) coated tube and co-injection of 5.0 µ / L 0.01 mol/L Ca(NO3)2, 5.0 µ / L 0.05 mol/L citric acid together with 15.0 µ / L sample solution prepared in 1000 mg/L Mg(NO3)2 have been chosen as optimum conditions. Optimum temperatures for pyrolysis and atomization temperatures were determined as 1100 and 2700 ° / C, respectively. Under these conditions, a detection limit of 0.088 mg/L and a characteristic mass of 186 pg for 15.0 µ / L sample volume were obtained. The accuracy of the method was checked by EnviroMAT-Waste Water EU-L-1 CRM and NIST 1573a Tomato Leaves SRM analyses.
Drinking water samples were collected from Balikesir, Bigadiç / and Kü / tahya, Emet and analyzed by the developed method. Samples were also analyzed by more sensitive techniques / ICP-OES and ICP-MS for a comparison study. The results are compatible with each other.
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Causes and impact of surface water pollution in Addis Ababa, Ethiopia / Orsaker och effekter av ytvattenföroreningar i Addis Abeba, EtiopienEriksson, Malin, Sigvant, Jonathan January 2019 (has links)
Surface water is globally becoming more and more a scarce resource, and in Addis Ababa the capital of Ethiopia, river water quality has been degraded due to anthropological forcing for many years. Therefore, the study objective was to investigate causes and impact of surface water pollution in Kebena and Great Akaki rivers. The technical aspect of the study focused on analysing the parameters E. coli, phosphate, nitrate and total ammonia nitrogen in 34 different sampling sites in the western part of the Great Akaki catchment. The other aspect was to evaluate authorities’ and companies’ perspective on the water quality, usage and future plans to mitigate further pollution of rivers. Another perspective was to interview households and farmers regarding their view on usage, water quality and health risks. The main finding was a high surface water contamination in both Kebena and Akaki river, throughout the city, mostly from domestic, municipality and industrial wastewater and solid waste. E. coli concentrations exceeded thresholds given by WHO. Concentrations of phosphate and total ammonia nitrogen strongly indicated eutrophication. Nitrate values were lower than expected with no perceived healthrisk. The interview study with authorities, households and farmers indicated irrigation as the main usage. Little to moderate health risks perceived by farm users and high health risks perceived by authorities for farmers were found. Therefore, addressing a stronger collaboration between authorities and the local community is important. In addition, the implementation of mitigation strategies should be strengthened and the stakeholders need to be accountable for their actions. A continued monitoring of pollutants as well as a multi-sectoral approach to solidwaste and wastewater management will help improve the river water quality. / Ytvatten blir globalt allt mer en knapp resurs och i Addis Abeba, huvudstaden i Etiopien, har flodernas vattenkvalitet under många år försämrats på grund av antropogen påverkan. Denna studie syftar till att undersöka orsaker och påverkan på ytvattenföroreningar i floderna Kebena och Akaki. Den tekniska aspekten av studien inkluderar vattenanalyser av parametrarna E.coli, fosfat, nitrat och totalt ammonium kväve som utfördes på 34 olika provtagningsplatser i västra delen av Great Akakis avrinningsområde. Den andra aspekten var att utvärdera myndigheters och företags perspektiv på vattenkvalité, flodvattnets användningsområden och framtida planer för förbättring av föroreningsgraden i floderna. Ett annat perspektiv var att intervjua hushåll och lantbrukare angående deras bild av ytvattenanvändning, om vattenkvaliteten och hälsorisker. Studiens huvudsakliga upptäckt är en genomgående hög föroreningsgrad i stadens flodvatten. Föroreningen består till största del av avlopp och avfall från hushåll, kommuner och industrier. Koncentrationerna av E.coli överskred WHO:s gränsvärden. Halterna av fosfat och totalt ammoniumkväve indikerade övergödning. Nitratvärdena visade lägre halter än förväntat och därmed ingen påvisad hälsorisk. Intervjustudien med myndigheter, hushåll och lantbrukare påvisade att ytvattnet mest används för bevattning av åkermark. Lantbrukarna uppfattade en liten till medelhög hälsorisk med denna användning, medan myndigheter ansåg att lantbrukarna utsattes för en hög risk. Därför är ett starkare samarbete mellan myndigheter och samhället viktigt. Dessutom behöver implementationen av förbättringsåtgärder förbättras och alla aktörer måste göras ansvariga för sina handlingar. En fortsatt övervakning av föroreningar och ett multi-disciplinärt arbetssätt vid avfall- och avloppshantering kommer att vara till hjälp vid förbättring av vattenkvaliteten i floden.
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Pesquisa de genes codificadores de enterotoxinas e B-lactamases em Aeromonas jandaei e Aeromas hydrophila provenientes de ambientes aquáticos / Enterotoxins and -lactamases encoding genes investigation in Aeromonas jandaei e Aeromonas hydrophila from aquatic environmentsBalsalobre, Livia Carminato 22 May 2009 (has links)
O gênero Aeromonas está amplamente distribuído em ambientes aquáticos, e estudos recentes incluem o gênero no grupo de patógenos emergentes, devido à sua freqüente associação com infecções locais e sistêmicas em humanos. Este trabalho foi realizado com o objetivo de pesquisar por meio da PCR e confirmar por meio de seqüenciamento, a ocorrência dos genes de virulência act, alt e ast, e resistência cphA, blaIMP, blaVIM, blaSPM-1, blaCTXM, blaTEM e blaSHV, verificando também o perfil de resistência a partir de antibiogramas, e a ocorrência de plasmídios nas cepas estudadas. A partir dos resultados observou-se que das 100 cepas selecionadas inicialmente, 87 pertenciam às espécies A. jandaei (46) e A. hydrophila (41). Dentre as quais pôde-se observar a ocorrência de act, alt e ast, respectivamente em 70,7 por cento (29), 97,6 por cento (40) e 26,8 por cento (11) das cepas de A. hydrophila, e em 4,4 por cento (2), 0 por cento (0) e 32,6 por cento (15) nas cepas de A. jandaei. Os genes blaIMP, blaVIM, blaSPM-1, blaCTX-M, e blaSHV não foram encontrados em nenhuma cepa. O gene cphA foi encontrado em 97,6 por cento (40) e 100 por cento (46) das cepas de A. hydrophila e A. jandaei, respectivamente e o gene blaTEM foi encontrado em 97,6 por cento (40) das cepas de A. hydrophila e em 85 por cento (39) das cepas de A. jandaei. Foi verificada a presença de plasmídio em 10/41 (24,4 por cento) das cepas de A. hydrophila e em 16/46 (34,9 por cento) das cepas de A. jandaei / The genus Aeromonas is widely distributed in aquatic environments, and recent studies include the genus in the emergent pathogens group, due to its frequent association with local and systemic human infections. This work was carried out aiming the investigation and sequencing virulence (act, alt and ast) and resistance (cphA, blaIMP, blaVIM, blaSPM-1, blaCTX-M, blaTEM e blaSHV) genes, also verifying the resistance profile of the strains using antibiograms and the occurrence of plasmids. From the 100 strains analyzed in this study, 87 belonged to A. jandaei (46) and A. hydrophila (41) species. Out of which it was observed the occurrence of act, alt and ast, respectively in 70.7 per cent (29), 97.6 per cent (40) and 26.8 per cent (11) of A. hydrophila strains, and in 4.4 per cent (2), 0 per cent (0) e 32.6 per cent (15) of A. jandaei strains. The genes blaIMP, blaVIM, blaSPM-1, blaCTX-M e blaSHV were not found. CphA gene was found in 97.6 per cent (40) and 100 per cent (46) of A. hydrophila and A. jandaei strains, respectively and blaTEM gene was found in 97.6 per cent (40) of A. hydrophila strains and in 85 per cent (39) of A. jandaei strains. Presence of plasmid was found in 10/41 (24.4 per cent) of A. hydrophila strains and in 16/46 (34,9 per cent) of A. jandaei strains
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Pesquisa de genes codificadores de enterotoxinas e B-lactamases em Aeromonas jandaei e Aeromas hydrophila provenientes de ambientes aquáticos / Enterotoxins and -lactamases encoding genes investigation in Aeromonas jandaei e Aeromonas hydrophila from aquatic environmentsLivia Carminato Balsalobre 22 May 2009 (has links)
O gênero Aeromonas está amplamente distribuído em ambientes aquáticos, e estudos recentes incluem o gênero no grupo de patógenos emergentes, devido à sua freqüente associação com infecções locais e sistêmicas em humanos. Este trabalho foi realizado com o objetivo de pesquisar por meio da PCR e confirmar por meio de seqüenciamento, a ocorrência dos genes de virulência act, alt e ast, e resistência cphA, blaIMP, blaVIM, blaSPM-1, blaCTXM, blaTEM e blaSHV, verificando também o perfil de resistência a partir de antibiogramas, e a ocorrência de plasmídios nas cepas estudadas. A partir dos resultados observou-se que das 100 cepas selecionadas inicialmente, 87 pertenciam às espécies A. jandaei (46) e A. hydrophila (41). Dentre as quais pôde-se observar a ocorrência de act, alt e ast, respectivamente em 70,7 por cento (29), 97,6 por cento (40) e 26,8 por cento (11) das cepas de A. hydrophila, e em 4,4 por cento (2), 0 por cento (0) e 32,6 por cento (15) nas cepas de A. jandaei. Os genes blaIMP, blaVIM, blaSPM-1, blaCTX-M, e blaSHV não foram encontrados em nenhuma cepa. O gene cphA foi encontrado em 97,6 por cento (40) e 100 por cento (46) das cepas de A. hydrophila e A. jandaei, respectivamente e o gene blaTEM foi encontrado em 97,6 por cento (40) das cepas de A. hydrophila e em 85 por cento (39) das cepas de A. jandaei. Foi verificada a presença de plasmídio em 10/41 (24,4 por cento) das cepas de A. hydrophila e em 16/46 (34,9 por cento) das cepas de A. jandaei / The genus Aeromonas is widely distributed in aquatic environments, and recent studies include the genus in the emergent pathogens group, due to its frequent association with local and systemic human infections. This work was carried out aiming the investigation and sequencing virulence (act, alt and ast) and resistance (cphA, blaIMP, blaVIM, blaSPM-1, blaCTX-M, blaTEM e blaSHV) genes, also verifying the resistance profile of the strains using antibiograms and the occurrence of plasmids. From the 100 strains analyzed in this study, 87 belonged to A. jandaei (46) and A. hydrophila (41) species. Out of which it was observed the occurrence of act, alt and ast, respectively in 70.7 per cent (29), 97.6 per cent (40) and 26.8 per cent (11) of A. hydrophila strains, and in 4.4 per cent (2), 0 per cent (0) e 32.6 per cent (15) of A. jandaei strains. The genes blaIMP, blaVIM, blaSPM-1, blaCTX-M e blaSHV were not found. CphA gene was found in 97.6 per cent (40) and 100 per cent (46) of A. hydrophila and A. jandaei strains, respectively and blaTEM gene was found in 97.6 per cent (40) of A. hydrophila strains and in 85 per cent (39) of A. jandaei strains. Presence of plasmid was found in 10/41 (24.4 per cent) of A. hydrophila strains and in 16/46 (34,9 per cent) of A. jandaei strains
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Enjeux de la qualité microbiologique de l'eau à l'hôpital : impact sur les colonisations et infections nosocomiales à pseudomonas aeruginosa / Issues of hospital microbiological water qualityLefebvre, Annick 02 September 2016 (has links)
La littérature fait suspecter mais n’indique pas clairement un lien entre la contamination du réseau d’eau et les infections nosocomiales à Pseudomonas aeruginosa. Les recommandations de prélèvements d’eau sont différentes selon les pays. Notre travail s’appuie sur les données des résultats des prélèvements d’eau et des prélèvements positifs à P. aeruginosa chez les patients (colonisation ou infections nosocomiales), réalisés au CHU de Dijon entre 2005 et 2013. Les contaminations des points d’eau étaient fréquentes (17%, IC95% 15,5-18,2). Des modèles mixtes n’ont pas montré de diminution d’incidence des cas de P. aeruginosa dans le nouveau bâtiment, moins souvent contaminé, pour les unités qui ont déménagé d’un bâtiment à un autre. La méthode de Kulldorff a permis de détecter peu d’agrégats temporels de cas. Des modèles GEE (Generalized Estimated Equations) ont montré une association positive entre la proportion de prélèvements d’eau positifs dans le trimestre dans le bâtiment et l’incidence des cas nosocomiaux. Cette association était retrouvée dans les analyses en sous-groupe des données de réanimation mais ne l’était plus lorsque les unités de réanimation et d’hématologie étaient exclues.Peu d’arguments en faveur d’un rôle du réseau d’eau dans la survenue de cas de P. aeruginosa sont apportés, en dehors des services de réanimation ou d’hématologie. En raison du coût associé aux prélèvements et aux mesures correctrices, il pourrait être proposé de limiter les prélèvements à ces unités à risque. Des études prospectives génotypiques devraient être conduites afin de mieux explorer l’association entre qualité microbiologique de l’eau à l’hôpital et infections nosocomiales. / Scientific literature allows suspecting but does not clearly indicate a link between water network contamination and Pseudomonas aeruginosa healthcare-associated infections. Guidelines for water samples vary across countries.Our work is based on water samples and P. aeruginosa patients’ samples (healthcare-associated colonizations or infections) in Dijon University hospital between 2005 and 2013.Water outlets contaminations were frequent (17%, CI95% 15.5-18.2). Mixed models on units that moved from a building to another did not show a lower incidence of P. aeruginosa cases in the new building than in the others, although it was less contaminated. Kulldorff’s method allowed detecting few temporal clusters of cases. GEE (Generalized Estimated Equations) models showed a positive association between the proportions of positive water samples in the building in the quarter and the incidence of healthcare-associated cases. This association was still observed in subgroup analyses of intensive care units but was no more observed in the database excluding hematology and intensive care units. Few arguments for an association between water network contamination and P. aeruginosa healthcare-associated colonizations or infections are provided, except in hematology and intensive care units. Given the costs associated with the samples and correctives measures, it could be proposed to limit the samples to these units at risk. Prospective studies with molecular typing methods should be conducted in order to better understand the association between hospital water network microbiologic quality and healthcare-associated infections.
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Šešupės tvenkinio Marijampolėje aplinkosauginės būklės pagerinimas / Improvement of the environmental condition of the Šešupė pond in MarijampolėNagrockienė, Erika 21 June 2013 (has links)
Magistro baigiamojo darbo tikslas – išanalizuoti Šešupės tvenkinio būklės situaciją ir būklės gerinimo kryptis, bei ištirti investicinių projektų galimybes vandens telkinio būklei pagerinti. Šiame darbe yra nagrinėjama Šešupės tvenkinio aplinkosauginė būklė ir tiriamos investicinių projektų galimybės Šešupės tvenkinio būklei pagerinti. Tyrimai atlikti Šešupės tvenkinyje 2012 metais gegužės ir spalio mėn. Imti mėginiai vandens tyrimams iš trijų skirtingų vietų ir išanalizuoti aplinkotyros laboratorijoje. Atliekant vandens cheminės būklės tyrimus analizuoti šie vandens būklės rodikliai: PO-P4, Skendinčios medžiagos, Permanganato indeksas, Pb, pH, O2, N-NH4, N-NO2, N-NO3, Nb, BDS7. Tyrimams panaudoti duomenys gauti prieš tvenkinio tvarkymą ir prasidėjus rekonstrukcijai. Tyrimų metu nustatyta, kad vandens cheminė būklė ženkliai nepakito. Didžiausi vandens cheminės būklės pakitimai rasti nustatant bendrą azotą, kuris parodo vandens būklės pablogėjimą. Išaiškintos priežastys, dėl kurių atsirado vandens cheminės būklės pakitimai. Taip pat buvo nagrinėjamas geriausio scenarijaus pasirinkimas alternatyvų analizės būdu. Šiame projekte geriausias sprendimas pasirenkamas atlikus daugiakriterinę alternatyvų analizę. / The aim of this master's final paper is to analyze the condition of the Šešupė pond and the directions for improvement of this condition and also to study the possibility to implement investment projects for improvement of the condition of the pond. This paper analyzes the environmental condition of the Šešupė pond and studies the possibility to implement investment projects for improvement of the condition of the Šešupė pond. Analyses were conducted in the Šešupė pond during the period from May to October 2012. Water samples for the analyses were collected at three different places of the pond and analyzed in an environmental science laboratory. The analysis of water chemical status included the following water status indicators: PO-P4, materials in suspension, permanganate index, Pb, pH, O2, N-NH4, N-NO2, N-NO3, Nb, BDS7. Data used for the analyses were obtained before reconstruction of the pond and at the beginning of reconstruction. The analysis has shown that the water chemical status has not changed significantly. The most significant changes of the water chemical status were found during the analysis of total nitrogen which is the indicator of water status deterioration. The reasons of the changes of the water chemical status were clarified. Also I have studied the selection of the best scenario through the analysis of the alternatives. The best solution in this project is selected after multi-criteria analysis of the alternatives.
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Novel Developments on the Extraction and Analysis of Polycyclic Aromatic Hydrocarbons in Environmental SamplesWilson, Walter 01 January 2014 (has links)
This dissertation focuses on the development of analytical methodology for the analysis of polycyclic aromatic hydrocarbons (PAHs) in water samples. Chemical analysis of PAHs is of great environmental and toxicological importance. Many of them are highly suspect as etiological agents in human cancer. Among the hundreds of PAHs present in the environment, the U.S. Environmental Protection Agency (EPA) lists sixteen as "Consent Decree" priority pollutants. Their routine monitoring in environmental samples is recommended to prevent human contamination risks. A primary route of human exposure to PAHs is the ingestion of contaminated water. The rather low PAH concentrations in water samples make the analysis of the sixteen priority pollutants particularly challenging. Current EPA methodology follows the classical pattern of sample extraction and chromatographic analysis. The method of choice for PAHs extraction and pre-concentration is solid-phase extraction (SPE). PAHs determination is carried out via high-performance liquid chromatography (HPLC) or gas chromatography/mass spectrometry (GC/MS). When HPLC is applied to highly complex samples, EPA recommends the use of GC/MS to verify compound identification and to check peak-purity of HPLC fractions. Although EPA methodology provides reliable data, the routine monitoring of numerous samples via fast, cost effective and environmentally friendly methods remains an analytical challenge. Typically, 1 L of water is processed through the SPE device in approximately 1 h. The rather large water volume and long sample processing time are recommended to reach detectable concentrations and quantitative removal of PAHs from water samples. Chromatographic elution times of 30 - 60 min are typical and standards must be run periodically to verify retention times. If concentrations of targeted PAHs are found to lie outside the detector's response range, the sample must be diluted (or concentrated), and the process repeated. In order to prevent environmental risks and human contamination, the routine monitoring of the sixteen EPA-PAHs is not sufficient anymore. Recent toxicological studies attribute a significant portion of the biological activity of PAH contaminated samples to the presence of high molecular weight (HMW) PAHs, i.e. PAHs with MW ≥ 300. Because the carcinogenic properties of HMW-PAHs differ significantly from isomer to isomer, it is of paramount importance to determine the most toxic isomers even if they are present at much lower concentrations than their less toxic isomers. Unfortunately, established methodology cannot always meet the challenge of specifically analyzing HMW-PAHs at the low concentration levels of environmental samples. The main problems that confront classic methodology arise from the relatively low concentration levels and the large number of structural isomers with very similar elution times and similar, possibly even virtually identical, fragmentation patterns. This dissertation summarizes significant improvements on various fronts. Its first original component deals with the unambiguous determination of four HMW-PAHs via laser-excited time-resolved Shpol'skii spectroscopy (LETRSS) without previous chromatographic separation. The second original component is the improvement of a relatively new PAH extraction method - solid-phase nanoextraction (SPNE) - which uses gold nanoparticles as extracting material for PAHs. The advantages of the improved SPNE procedure are demonstrated for the analysis of EPA-PAHs and HMW-PAHs in water samples via GC/MS and LETRSS, respectively.
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Desarrollo de métodos automáticos de análisis por inyección en flujo multijeringa(MSFIA)para la determinación del ión sulfuro en aguasFerrer Trovato, Laura 29 March 2007 (has links)
Se han desarrollado métodos basados en análisis por inyección en flujo multijeringa (MSFIA) para determinar automáticamente sulfuro en muestras ambientales y aguas residuales, con detección espectrofotométrica previa transformación química del analito (acoplamiento oxidativo del sulfuro con N-N-dimetil-p-fenilendiamina en presencia de Fe(III) para formar azul de metileno).- Sistema MSFIA con difusión gaseosa para aislar el analito de matrices complejas sin ningún pretratamiento manual de la muestra.- Sistema MSFIA con pre-concentración en fase sólida (optrodo de reflectancia difusa sobre disco de membrana) para determinar niveles traza. - Método MSFIA que combina separación y pre-concentración en línea del sulfuro, para ofrecer elevadas selectividad y sensibilidad.- Sistema MSFIA inteligente totalmente automatizado para determinar sulfuro en un amplio rango de concentraciones, capaz de auto-ajustarse sin ninguna intervención del analista.- Estudio comparativo de metodologías en flujo para determinar sulfuro en matrices acuosas. Se discuten críticamente distintas técnicas y sistemas de detección empleados. / Multisyringe flow injection analysis (MSFIA) systems for automatic determination of sulfide in environmental and wastewater samples have been developed exploiting spectrophotometric detection prior derivatization of the analyte (oxidative coupling of sulfide with N-N-dimethyl-p-phenylenediamine in presence of Fe(III) to form methylene blue).- A MSFIA system was coupled to gas-diffusion separation to achieve the isolation from complex matrices without any pre-treatment batch sample.- An optrode using disk-based solid-phase extraction in a MSFIA set-up is proposed to determine trace levels.- A hyphenated method that combines the separation and pre-concentration is presented reaching high selectivity and sensitivity. - A fully automated smart MSFIA system for sulfide monitoring in a wide concentration range is proposed choosing by itself the best approach to quantify the analyte without the analyst intervention.- A review of flow-based methodologies for sulfide determination in aqueous matrices is presented. The characteristics of automated protocols using several detection systems are discussed.
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Preconcentration strategies in capillary electrophoresis for the determination of pharmaceutical and personal care productsMaijó Ferré, Irene 17 July 2012 (has links)
L'objectiu principal d'aquestaTesi Doctoral és el desenvolupament de diferents estratègies per disminuir els límits de detecció de l’electroforesicapil•lar per a la determinació de compostos farmacèutics i els productes de cura personal. Aquestes estratègies es basen en les tècniques de preconcentració electroforètiques i cromatogràfiques, i l'ús de l’espectrometria de masses com a sistema de detecció. Com a tècniques de preconcentració electroforètiques s'han estudiat les tècniques de samplestacking i sweeping, i com a tècnica de preconcentració cromatogràficas’ha avaluat l'acoblament en línia entre l'extracció en fase sòlida i l'electroforesicapil•lar (In-line SPE-CE). Entre elsPPCPs, aquesta tesi doctoral es centra específicament en els antiinflamatoris no esteroïdals(AINE), els parabens i els filtres ultraviolats.
Un altre dels objectius d'aquestaTesi Doctoral és estudiarl’aplicabilitat de les metodologies desenvolupades per a l'anàlisi de mostres ambientals per determinar PPCP. / The main objective of this Doctoral Thesis is the development of different strategies to decrease the detection limits of capillary electrophoresis for the determination of pharmaceutical and personal care products. These strategies are based on electrophoretic and chromatographic preconcentration techniques, and the use of mass spectrometry as a detection system. The electrophoretic preconcentration techniques studied included sample stacking techniques and sweeping while the chromatographic preconcentration technique evaluated was in-line coupling between solid phase extraction and capillary electrophoresis. With respect to PPCPs, this Doctoral Thesis focuses specifically on non-steroidal anti-inflammatory drugs (NSAIDs), parabens and UV-filters.
Another objective of this Doctoral Thesis is to study the suitability of the developed methodologies for the determination of PPCPs in environmental samples.
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Desenvolvimento de método de pré-concentração empregando 1-(2-piridilazo)-2-naftol imobilizado em sílica funcionalizada C18 para determinação de metais em águas naturais por ICP OESCarvalho, Roberta Natália Carneiro da Silva 05 1900 (has links)
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(Dissertação_mestrado__(03.11_)).pdf: 1756144 bytes, checksum: 6a5c8a2f486f154eba91b5aa9780dde0 (MD5) / CNPQ / A determinação de metais em águas naturais por Espectrometria de Emissão Óptica com
Plasma Indutivamente Acoplado (ICP OES), em geral, deve envolver etapas de pré-
concentração, devido os níveis de concentração dos metais em água serem muitas vezes
abaixo dos limites de detecção da técnica. Dessa forma, o objetivo desse trabalho foi
desenvolver um método de pré-concentração em fase sólida sensível e simples para a
determinação de cobre, ferro, níquel, manganês, chumbo e zinco em amostras de água por
ICP OES. As condições experimentais para pré-concentração foram otimizadas
considerando os fatores: concentração do eluente, volume de eluente, volume da amostra,
vazão e pH. As condições otimizadas corresponderam ao uso de 5 mL de solução de HCl
0,8 mol L-1 como eluente, volume da amostra de 50 mL, vazão de 1,9 mL min-1 e pH 9,0.
Para a determinação dos metais, as amostras, após ajuste do pH, foram percoladas com o
auxílio de uma bomba peristáltica em cartucho Sep-pak C18 com 1-(2-piridilazo)-2-naftol
(PAN) imobilizado na sílica funcionalizada C18. A eluição dos analitos foi realizada com a
passagem da solução de HCl pelo cartucho para posterior determinação por ICP OES.
Nestas condições, os limites de detecção para Cu, Fe, Mn, Ni, Pb e Zn obtidos variaram
entre 0,11 e 21 µg L-1 e os limites de quantificação entre 0,36-69 µg L-1, respectivamente. Os
desvios padrão relativos (R.S.D.) para a determinação dos analitos não ultrapassaram 9 %.
O efeito de possíveis espécies interferentes sobre a recuperação dos analitos também foram
investigados. A exatidão do método foi avaliada mediante análise de material de referência
certificado (SLEW-3 Estuariene Water Reference Material for Trace Metals) e o método
proposto foi aplicado para análise de amostras de água subterrânea, água potável e água
de rio coletadas nos municípios de Cachoeira e São Félix, Bahia, Brasil. As amostras foram
analisadas por Espectrometria de Massas com Plasma Indutivamente Acoplado (ICP-MS)
como método comparativo, não sendo observadas diferenças significativas entre estes resultados e os resultados obtidos pelo método proposto. / The determination of metals in natural waters by Inductively Coupled Plasma Optical
Emission Spectrometry (ICP OES), in general, involves pre-concentration steps, due the
concentration levels of metals in water are often below the limits of detection of this
technique. In this way, the objective of this work was to develop a pre-concentration solid
phase method for sensitive and simple determination of copper, iron, nickel, manganese,
lead and zinc in water samples by ICP OES. The experimental conditions for pre-
concentration were optimized considering the following factors: the concentration of the
eluent, eluent volume, sample volume, flow-rate and pH. The optimized conditions
corresponded to the use of 5 mL of HCl solution 0.8 mol L-1 as an eluent sample volume 50
ml, flow-rate 1.9 mL min-1 and pH 9.0. For the determination of metals by the procedure, the
samples after pH adjustment were percolated with the aid of a peristaltic pump on Sep-Pak
C18 cartridge with 1-(2-pyridylazo)-2-naphthol (PAN). The analyte elution was carried out
with the passage of the HCl solution in the cartridge for subsequent determination by ICP
OES. In these conditions, the detection limit for Cu, Fe, Mn, Ni, Pb and Zn varied between
0.11 to 21 μg L-1 and the limits of quantification from 0.36 to 69 μg L-1, respectively. The
relative standard deviation (RSD) for the analytes of this study did not exceed 9%. The effect
of possible interfering species on the recovery of the analytes was also investigated. The
accuracy of the method was evaluated by analysis of certified reference material (SLEW-3
Estuariene Water Reference Material for Trace Metals) and the proposed method was
applied to samples of ground water, drinking water and river water collected in Cachoeira
and São Félix cities, Bahia, Brazil. The samples were analyzed by Inductively Coupled
Plasma Mass Spectrometry (ICP-MS) as a comparative method do not being found
significant differences among these results and the results obtained by the proposed method.
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