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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
471

Avaliação de metodologia de coleta e analíse de solventes/misturas de solventes no ar em ambiente de trabalho: metanol em mistura MEG (Metanol 33% Etanol 60% e Gasolina 7%) / Evaluation of methodology of sampling and analysis of solvents in the air in the workplace. Methanol in a MEG mixture (Methanol 33%, Ethanol 60%, and Gasoline 7%

Cardoso, Luiza Maria Nunes 08 June 1995 (has links)
Este trabalho teve como objetivo principal propor procedimentos de avaliação de metodologia de coleta e análise de solventes no ar em ambiente de trabalho. Utilizou-se o metanol em mistura MEG (Metanol 33%, Etanol 60% e Gasolina 7%) como exemplo. Na época, a mistura MEG estava sendo indicada para substituir o etanol combustível, devido a sua falta no mercado. Foi montada uma atmosfera controlada dinâmica por injeção, para gerar concentrações conhecidas de vapor metanol em mistura MEG. Essa atmosfera permaneceu estável ao redor de 7,5 horas. O limite de detecção método analítico do CG-DIC, utilizado para o acompanhamento das concentrações geradas, foi de 18mg/m3 para um volume amostrado de 2mL coletado por uma válvula de coleta. Estando a atmosfera controlada apta para os testes de validação, foram realizados estudos de volume de \"breakthrough\" para coleta de metanol em tubos de sílica gel, com a finalidade de se conhecer o volume a ser amostrado em campo. Esses estudos foram realizados levando em conta as possíveis interferências de etanol, gasolina e elevada umidade relativatotal . O tempo de coleta de amostra para a mistura com umidade relativa recomendado para uma vazão de 200mL/min foi de 15 minutos. O método analítico utilizado, para a determinação de metanol coletado em tubos de sílica gel e analisado por CG-DIC. foi uma adaptação de métodos encontrados na literatura do NIOSH, para as condições da mistura. Após encontrar a melhor seletividade para o menor tempo de retenção do metanol em mistura MEG, foi determinado o limite de detecção de 9,7x 10-3µg. A precisão do método analítico encontrada foi de 2,1% e a exatidão esteve entre 89% e 97%. Estabelecida a metodologia analítica, as melhores condições de atmosfera controlada e o volume de coleta de amostra, foram realizados estudos que integram a coleta e análise ou seja, precisão e exatidão de coleta e análise e estabilidade de armazenamento. Para estudos de precisão e exatidão de coleta e análise, foram geradas concentrações de metanol em mistura MEG, com umidade ao redor de 0,5, 1 e 2 vezes o limite de tolerância brasileiro(156ppm); dessorção em água e análise por CGDIC. O coeficiente de variação total calculado para o método de coleta e análise de metanol em mistura MEG foi de 7,3% (precisão) e wazzu exatidão esteve entre 90% e 101%. As concentrações de metanol foram estáveis, em tubos adsorventes armazenados em geladeira, durante o período de estudo de 14 dias. Porém, foi constatada uma migração de metanol através da camada analítica para a camada controle de forma gradativa com o passar do tempo. As soluções, a partir da dessorção dos tubos armazenadas em geladeira, foram estáveis durante o período de estudo de 45 dias. Além desses experimentos foram também realizados estudos de capacidade de adsorção da sílica gel para metanol levando em conta os interferentes, e verificado se eram capazes de dessorver totalmente o metanol, após um certo período de coleta. Constatou-se que após 30 minutos de coleta, os interferentes (etanol, umidade e gasolina) entravam em equilíbrio com o adsorvente e o metanol. / The main objective of this work is to propose procedures for the evaluation of the methodology of the sampling and analysis of solvents in the air in the workplace. Methanol in a MEG mixture (Methanol 33%, Ethanol 60%, and Gasoline 7%) was used as an example. At that time the MEG mixture was being proposed to substitute ethanol fuel due to its shortages on the Brazilian market. An atmosphere, dynamically controlled by injection, was produced to generate the known concentrations of methanol vapour in MEG mixtures. This atmosphere remained stable for about 450 minutes. The detection Iimit, using the GC-FID analytical method to monitor the concentrations produced, was 18mg/m3 for a sample volume of 2mL sampled from a sampling valve. The controlled atmosphere being suitable for the validation tests, studies of the breakthrough volume for the sampling of methanol in silica gel tubes were carried out, with the aim of discovering the total volume to be sampled in the field. These studies were carried out taking into account the possible interference of ethanol, gasoline and the high relative humidity. The sampling time for the mixture with the recommended relative humidity with a flow rate of 200mL/min was fifteen minutes. The analytical method used for the determination of methanol sampled in silica gel tubes and analyzed by GC-FID, was based on the methods found in the NIOSH and OSHA literature, adapted to the mixture conditions. After finding the best selectivity for the lowest retention time for the methanol in the MEG mixture, the detection Iimit of 9.7 x 10-3µg was determined. The precision of the analytical method was 2.1% and the accuracy was between 89% and 97%. Having established the analytical methodology. the best conditions for the controlled atmosphere and the sampling volume, studies were carried out which integrated the sampling and the analysis, that is, the precision and the accuracy of the sampling and the analysis and the storage stability. To study the precision and the accuracy of the sampling and analysis, concentrations 1 or 2 times that of the Brazilian tolerance Iimit of methanol (156 ppm) in MEG mixture, with humidity around 0.5, were generated, using dessorption in water and analysis by GC-FID. The total coefficient of variation calculated for the method of sampling and analysis of methanol in MEG mixture was 7.3% (precision) and the accuracy was between 90% and 101% . The concentrations of methanol were stable, in adsorption tubes stored in the refrigerator, throughout the study period of fifteen days. However, a gradual migration of methanol through the analytical layer to the control layer with the passage of time was noted. The solutions from the dessorption of the tubes, stored in the refrigerator, were stable throughout the study period of 45 days. Besides these experiments, studies of the adsorption capacity of silica gel for methanol, taking into account the interferents, were also carried out, and it was verified whether these were capable of the total dessorption of the methanol, after a certain sampling period. It was noted that after thirty minutes of sampling, the interferents came into equilibrium with the adsorbent and the methanol.
472

Tratabilidade de águas residuárias contendo poluentes perigosos: estudo de caso. / Treatability of hazardous industrial wastewater: case study.

Morita, Dione Mari 29 September 1993 (has links)
O trabalho foi desenvolvido com o objetivo de caracterizar e estudar formas de tratamento de águas residuárias de indústrias de refino de óleo lubrificante e de recuperação de solventes. A fase preliminar teve por objetivo avaliar a biodegradabilidade do despejo combinado dessas duas indústrias. A segunda foi realizada em instalação piloto composta, basicamente, de uma unidade de arraste com ar/tanque de equalização, tanques de correção de pH e de aeração com tempos de detenção distintos, seguidos de tanques de sedimentação. Foram executados testes para avaliar a remoção de material solúvel em n-hexano do despejo da indústria de refino de óleo lubrificante e do efluente final. A unidade de arraste com ar difuso operando com subpressão de 15 mmhg a saída dos gases, vazão específica de ar de 20 ml/l min. E tempo de detenção de 5 dias foi eficiente na remoção de acetona, piridina, benzeno, tolueno, hexano, metil etil cetona e provavelmente solventes clorados. Não apresentou remoção significativa de álcoois, que foram eficientemente degradados no sistema biológico subsequente. Obteve-se remoções superiores a 90%, em termos de dbo e dqo, no processo biológico com tempos de detenção de 20 e 30 dias, e em torno de 80% para os demais. Os sistemas biológicos responderam bem as cargas transientes de solventes, exceto para o tolueno e o álcool isopropílico. / Traditionally, raw materials from solvent recovery and from reclaimed lubricating oil industries are considered hazardous solid waste. Consequently, the best control technology is incineration. This work was developed in order to characterize and to study ways of treating wastewaters from lubricating oil refinery and solvent recovery industries. The experimental part was divided in two phases. The preliminar step aimed to evaluate the biodegradability of combined wastewater from both industries. The second phase was basically carried out in a pilot plant composed by an air stripping unit/equalization tank, pH correction tanks and bioreactors with different retention times, followed by sedimentation tanks. Other than these assays, tests were performed to evaluate the removal of soluble material in n-hexane of the wastewater of the lubricating oil refinery industry and of the supernatant of the sedimentation tank after the bioreactor of 20 days retention.The buble aeration unit operating with a 15 mmHg suppresion to the gas exit, with a specific air flow of 20 mL/L.min. and with a retention time of 5 days was efficient to remove acetone, pyridine, benzene, toluene, hexane, methyl ethyl ketone and probably chlorinated solvents. There was no significative removal of alcohols, that were efficiently degraded in the subsequent biological system. BOD and COD removal efficiencies were better than 90% in the biological process with retention times of 20 and 30 days, and about 80% for the rest. The responses of biological systems to the transient inputs of solvents were well, except for toluene and isopropilic alcohol. Several physico-chemical processes for soluble material in n-hexane removal were studied. The only one to present effluent concentration under the legal limit was the addition of the sodium xylene-sulphonate base demulsifier to the supernatant of the sedimentation tank the bioreactor of 20 days retention.
473

Electrospray for pulmonary drug delivery

Lajhar, Fathi January 2018 (has links)
Drug administration through the pulmonary route is an ancient technique that evolved from inhaling the smoke of certain leaves as a medicine. The optimum droplet diameter for the pulmonary system deposition has been identified to be in the range from 2 to 3.5 μm, with potential deposition rates of up to 80% of this size range. Currently, the most used aerosol generator methods are the pressurized metered dose inhalers. However, they generally exhibit low deposition efficiency with less than 20 % of the spray reaching the target area of the lungs as most of the drug deposited in the upper airways. This is for the most part due to the droplet size polydispersity that is inherent in these systems. The droplets of the biggest diameter will deposit in the upper airways, and then the deposited medicine will be swallowed and absorbed in the gastrointestinal tract. This can produce adverse medical side effects. Electrospray (ES) or electrohydrodynamic atomization (EHDA) is a promising atomization process due to its ability to produce a spray with monodisperse droplet size. The current study will investigate the feasibility of using electrospray in a pulmonary drug delivery system. Assessments, selection and characterization of suitable biocompatible solvents that can be used as a lung obstruction relief drug were carried out. Tests to identify the electrospray setup necessary to produce droplet sizes in the appropriate range for deposition in the lungs were carried out. The study found that both stable and pulsating cone jet modes can produce the required droplet size and the pulsating mode can produce at least four times higher flow than stable cone jet mode. A low-cost image analysis technique developed for this work gave satisfactory results that could be compared to droplet size scaling laws from the literature. However, it proved to be relatively time consuming and further automation of this technique would make it more suitable for large-scale studies. The image analysis results show a correlation between the cone length, cone angle and the applied voltage. The droplet scaling laws discrepancies such as the solution flow rate exponent and the constant that is used by some scaling laws may be attributed to the droplet evaporation time which is quite short for the water/ ethanol solutions. The emitter diameter and the conductivity effect on the I(Q) power law and the sensitivity of the onset voltage (Vonset) to the liquid flow rate (Q), were demonstrated for solutions of triethylene-glycol (TEG), and for an ethanol-water mixture solution.
474

Ionic liquids as crystallisation media for inorganic materials

Ahmed, Ejaz, Breternitz, Joachim, Groh, Matthias Friedrich, Ruck, Michael 09 April 2014 (has links) (PDF)
Ionic liquids (ILs) have made a great impact on materials science and are being explored for potential applications in several disciplines. In this article, we briefly highlight the current state-of-the-art techniques employing ILs as new crystallisation media, working as neutral solvent, template or charge compensating species. The use of an IL as environmental friendly solvent offers many advantages over traditional crystallisation methods. The change from molecular to ionic reaction media leads to new types of materials being accessible. Room temperature ILs have been found to be excellent solvent systems for the crystallisation of a wide range of substances and morphologies ranging from nanoscopic crystals to micro- and even to macroscopic crystals. Moreover, high temperature routes, such as crystallisation from melts or gas phase deposition, have been replaced by convenient room or low temperature syntheses, employing ILs as reaction media. / Dieser Beitrag ist mit Zustimmung des Rechteinhabers aufgrund einer (DFG-geförderten) Allianz- bzw. Nationallizenz frei zugänglich.
475

Bildungsbedingungen und rationale Synthesestrategien

Hausdorf, Steffen 18 November 2011 (has links) (PDF)
MOF-5 ist der Archetyp einer neuartigen Klasse hochporöser Materialien, den Metal Organic Frameworks, die unter anderem zur Anwendung als effektive Gasspeicher geeignet sind. Im Rahmen dieser Arbeit werden die seiner Bildung zugrunde liegenden Reaktionen untersucht. Aus den Erkenntnissen dieser Untersuchungen wurden zwei neue Syntheseverfahren entwickelt. Eines der Verfahren beruht auf der Phasenumwandlung von Zinkterephthalaten und ermöglichte die Laborsynthese von MOF-5 in 100 g-Mengen. Ein zweites Verfahren bedient sich des Strukturaufbaus mit Hilfe vorgefertigter anorganischer Cluster, wodurch erstmals die Synthese von MOF-5-Homologen anderer Metalle als Zink gelang.
476

Environmental risk factors for Parkinson's disease

Gartner, Coral Elizabeth January 2006 (has links)
Parkinson's disease (PD) is a progressive, degenerative, neurological disease. The progressive disability associated with PD results in substantial burdens for those with the condition, their families and society in terms of increased health resource use, earnings loss of affected individuals and family caregivers, poorer quality of life, caregiver burden, disrupted family relationships, decreased social and leisure activities, and deteriorating emotional well-being. Currently, no cure is available and the efficacy of available treatments, such as medication and surgical interventions, decreases with longer duration of the disease. Whilst the cause of PD is unknown, genetic and environmental factors are believed to contribute to its aetiology. Descriptive and analytical epidemiological studies have been conducted in a number of countries in an effort to elucidate the cause, or causes, of PD. Rural residency, farming, well water consumption, pesticide exposure, metals and solvents have been implicated as potential risk factors for PD in some previous epidemiological studies. However, there is substantial disagreement between the results of existing studies. Therefore, the role of environmental exposures in the aetiology of PD remains unclear. The main component of this thesis consists of a case-control study that assessed the contribution of environmental exposures to the risk of developing PD. An existing, previously unanalysed, dataset from a local case-control study was analysed to inform the design of the new case-control study. The analysis results suggested that regular exposure to pesticides and head injury were important risk factors for PD. However, due to the substantial limitations of this existing study, further confirmation of these results was desirable with a more robustly designed epidemiological study. A new exposure measurement instrument (a structured interviewer-delivered questionnaire) was developed for the new case-control study to obtain data on demographic, lifestyle, environmental and medical factors. Prior to its use in the case-control study, the questionnaire was assessed for test-retest repeatability in a series of 32 PD cases and 29 healthy sex-, age- and residential suburb-matched electoral roll controls. High repeatability was demonstrated for lifestyle exposures, such as smoking and coffee/tea consumption (kappas 0.70-1.00). The majority of environmental exposures, including use of pesticides, solvents and exposure to metal dusts and fumes, also showed high repeatability (kappas &gt0.78). A consecutive series of 163 PD case participants was recruited from a neurology clinic in Brisbane. One hundred and fifty-one (151) control participants were randomly selected from the Australian Commonwealth Electoral Roll and individually matched to the PD cases on age (± 2 years), sex and current residential suburb. Participants ranged in age from 40-89 years (mean age 67 years). Exposure data were collected in face-to-face interviews. Odds ratios and 95% confidence intervals were calculated using conditional logistic regression for matched sets in SAS version 9.1. Consistent with previous studies, ever having been a regular smoker or coffee drinker was inversely associated with PD with dose-response relationships evident for packyears smoked and number of cups of coffee drunk per day. Passive smoking from ever having lived with a smoker or worked in a smoky workplace was also inversely related to PD. Ever having been a regular tea drinker was associated with decreased odds of PD. Hobby gardening was inversely associated with PD. However, use of fungicides in the home garden or occupationally was associated with increased odds of PD. Exposure to welding fumes, cleaning solvents, or thinners occupationally was associated with increased odds of PD. Ever having resided in a rural or remote area was inversely associated with PD. Ever having resided on a farm was only associated with moderately increased odds of PD. Whilst the current study's results suggest that environmental exposures on their own are only modest contributors to overall PD risk, the possibility that interaction with genetic factors may additively or synergistically increase risk should be considered. The results of this research support the theory that PD has a multifactorial aetiology and that environmental exposures are some of a number of factors to contribute to PD risk. There was also evidence of interaction between some factors (eg smoking and welding) to moderate PD risk.
477

Parental exposures and occurrence of adverse pregnancy outcomes and childhood atopic diseases /

Magnusson, Linda L., January 2006 (has links)
Diss. (sammanfattning) Stockholm : Karol. inst., 2006. / Härtill 5 uppsatser.
478

Estudo da cristaliza??o de parafinas em sistemas solventes/tensoativos/?gua

Gomes, Erika Adriana de Santana 30 December 2009 (has links)
Made available in DSpace on 2014-12-17T15:01:49Z (GMT). No. of bitstreams: 1 ErikaASG_TESE_partes_autorizadas.pdf: 3587859 bytes, checksum: 8731a4ebad1b8f6f11b36c879b4a1a76 (MD5) Previous issue date: 2009-12-30 / The WAT is the temperature at the beginning of the appearance of wax crystals. At this temperature the first wax crystals are formed by the cooling systems paraffin / solvents. Paraffins are composed of a mixture of saturated hydrocarbons of high molecular weight. The removal of petroleum from wells and the production lines means a surcharge on produced oil, thus solubilize these deposits formed due to modifications of thermodynamics has been a constant challenge for companies of oil exploration. This study combines the paraffin solubilization by microemulsion systems, the determination of WAT systems paraffin / solvent and performance of surfactant in reducing the crystallization. We used the methods: rheological and the photoelectric signal, validating the latter which was developed to optimize the data obtained due to sensitivity of the equipment used. Methods developed for description of wax precipitation are often in poor agreement with the experimental data, they tend to underestimate the amount of wax at temperatures below the turbidity point. The Won method and the Ideal solution method were applied to the WAT data obtained in solvent systems, best represented by the second interaction of Won method using the solvents naphtha, hexane and LCO. It was observed that the results obtained by WAT photoelectric signal when compared with the viscosity occur in advance, demonstrating the greatest sensitivity of the method developed. The ionic surfactant reduced the viscosity of the solvent systems as it acted modifying the crystalline structure and, consequently, the pour point. The curves show that the WAT experimental data is, in general, closer to the modeling performed by the method of Won than to the one performed by the ideal solution method, because this method underestimates the curve predicting the onset of paraffin hydrocarbons crystallization temperature. This occurs because the actual temperature measured was the crystallization temperature and the method proposes the fusion temperature measurement. / A TIAC ? a temperatura de in?cio do aparecimento dos cristais de parafina. Nesta temperatura os primeiros cristais de parafina s?o formados, pelo resfriamento de sistemas parafina/solventes. As parafinas s?o compostas de uma mistura de hidrocarbonetos saturados de alto peso molecular. A remo??o de parafinas dos po?os e das linhas de produ??o significa um custo adicional ao petr?leo produzido, portanto solubilizar estes dep?sitos formados decorrentes das modifica??es termodin?micas tem sido um desafio constante das empresas exploradoras de petr?leo. Este estudo alia a solubiliza??o paraf?nica por sistemas microemulsionados, ? determina??o da TIAC dos sistemas parafina/solvente e a atua??o do tensoativo na redu??o da cristaliza??o. Utilizaram-se os m?todos: reol?gico e o do sinal fotoel?trico, validando este ?ltimo o qual foi desenvolvido visando aperfei?oar os dados obtidos devido a sensibilidade do equipamento utilizado. M?todos desenvolvidos para descri??o da precipita??o da cera est?o freq?entemente em pobre concord?ncia com os dados experimentais; eles tendem a subestimar a quantidade de cera ?s temperaturas abaixo do ponto de turbidez. Foram aplicados os m?todos de Won e o da solu??o ideal aos dados de TIAC da parafina obtidos em sistemas com solventes, sendo melhor representado pela segunda intera??o do m?todo de Won com os solventes: nafta, hexano e LCO. Foi observado que os resultados de TIAC obtidos pelo sinal fotoel?trico quando comparados com a viscosidade, ocorrem antecipadamente, demonstrando a maior sensibilidade do m?todo desenvolvido. O tensoativo i?nico reduziu a viscosidade dos sistemas paraf?nicos, pois ele atuou modificando a estrutura cristalina, conseq?entemente o ponto de fluidez. As curvas que representam os dados experimentais da TIAC est?o, de maneira geral, mais pr?ximas da modelagem realizada pelo m?todo de Won do que da solu??o ideal, pois este m?todo subestima a curva de predi??o do in?cio da temperatura de cristaliza??o da parafina com os hidrocarbonetos. Isto ocorre porque a temperatura real medida foi a de cristaliza??o, e a proposta pelos m?todos ? a de fus?o
479

Tratabilidade de águas residuárias contendo poluentes perigosos: estudo de caso. / Treatability of hazardous industrial wastewater: case study.

Dione Mari Morita 29 September 1993 (has links)
O trabalho foi desenvolvido com o objetivo de caracterizar e estudar formas de tratamento de águas residuárias de indústrias de refino de óleo lubrificante e de recuperação de solventes. A fase preliminar teve por objetivo avaliar a biodegradabilidade do despejo combinado dessas duas indústrias. A segunda foi realizada em instalação piloto composta, basicamente, de uma unidade de arraste com ar/tanque de equalização, tanques de correção de pH e de aeração com tempos de detenção distintos, seguidos de tanques de sedimentação. Foram executados testes para avaliar a remoção de material solúvel em n-hexano do despejo da indústria de refino de óleo lubrificante e do efluente final. A unidade de arraste com ar difuso operando com subpressão de 15 mmhg a saída dos gases, vazão específica de ar de 20 ml/l min. E tempo de detenção de 5 dias foi eficiente na remoção de acetona, piridina, benzeno, tolueno, hexano, metil etil cetona e provavelmente solventes clorados. Não apresentou remoção significativa de álcoois, que foram eficientemente degradados no sistema biológico subsequente. Obteve-se remoções superiores a 90%, em termos de dbo e dqo, no processo biológico com tempos de detenção de 20 e 30 dias, e em torno de 80% para os demais. Os sistemas biológicos responderam bem as cargas transientes de solventes, exceto para o tolueno e o álcool isopropílico. / Traditionally, raw materials from solvent recovery and from reclaimed lubricating oil industries are considered hazardous solid waste. Consequently, the best control technology is incineration. This work was developed in order to characterize and to study ways of treating wastewaters from lubricating oil refinery and solvent recovery industries. The experimental part was divided in two phases. The preliminar step aimed to evaluate the biodegradability of combined wastewater from both industries. The second phase was basically carried out in a pilot plant composed by an air stripping unit/equalization tank, pH correction tanks and bioreactors with different retention times, followed by sedimentation tanks. Other than these assays, tests were performed to evaluate the removal of soluble material in n-hexane of the wastewater of the lubricating oil refinery industry and of the supernatant of the sedimentation tank after the bioreactor of 20 days retention.The buble aeration unit operating with a 15 mmHg suppresion to the gas exit, with a specific air flow of 20 mL/L.min. and with a retention time of 5 days was efficient to remove acetone, pyridine, benzene, toluene, hexane, methyl ethyl ketone and probably chlorinated solvents. There was no significative removal of alcohols, that were efficiently degraded in the subsequent biological system. BOD and COD removal efficiencies were better than 90% in the biological process with retention times of 20 and 30 days, and about 80% for the rest. The responses of biological systems to the transient inputs of solvents were well, except for toluene and isopropilic alcohol. Several physico-chemical processes for soluble material in n-hexane removal were studied. The only one to present effluent concentration under the legal limit was the addition of the sodium xylene-sulphonate base demulsifier to the supernatant of the sedimentation tank the bioreactor of 20 days retention.
480

Avaliação de metodologia de coleta e analíse de solventes/misturas de solventes no ar em ambiente de trabalho: metanol em mistura MEG (Metanol 33% Etanol 60% e Gasolina 7%) / Evaluation of methodology of sampling and analysis of solvents in the air in the workplace. Methanol in a MEG mixture (Methanol 33%, Ethanol 60%, and Gasoline 7%

Luiza Maria Nunes Cardoso 08 June 1995 (has links)
Este trabalho teve como objetivo principal propor procedimentos de avaliação de metodologia de coleta e análise de solventes no ar em ambiente de trabalho. Utilizou-se o metanol em mistura MEG (Metanol 33%, Etanol 60% e Gasolina 7%) como exemplo. Na época, a mistura MEG estava sendo indicada para substituir o etanol combustível, devido a sua falta no mercado. Foi montada uma atmosfera controlada dinâmica por injeção, para gerar concentrações conhecidas de vapor metanol em mistura MEG. Essa atmosfera permaneceu estável ao redor de 7,5 horas. O limite de detecção método analítico do CG-DIC, utilizado para o acompanhamento das concentrações geradas, foi de 18mg/m3 para um volume amostrado de 2mL coletado por uma válvula de coleta. Estando a atmosfera controlada apta para os testes de validação, foram realizados estudos de volume de \"breakthrough\" para coleta de metanol em tubos de sílica gel, com a finalidade de se conhecer o volume a ser amostrado em campo. Esses estudos foram realizados levando em conta as possíveis interferências de etanol, gasolina e elevada umidade relativatotal . O tempo de coleta de amostra para a mistura com umidade relativa recomendado para uma vazão de 200mL/min foi de 15 minutos. O método analítico utilizado, para a determinação de metanol coletado em tubos de sílica gel e analisado por CG-DIC. foi uma adaptação de métodos encontrados na literatura do NIOSH, para as condições da mistura. Após encontrar a melhor seletividade para o menor tempo de retenção do metanol em mistura MEG, foi determinado o limite de detecção de 9,7x 10-3µg. A precisão do método analítico encontrada foi de 2,1% e a exatidão esteve entre 89% e 97%. Estabelecida a metodologia analítica, as melhores condições de atmosfera controlada e o volume de coleta de amostra, foram realizados estudos que integram a coleta e análise ou seja, precisão e exatidão de coleta e análise e estabilidade de armazenamento. Para estudos de precisão e exatidão de coleta e análise, foram geradas concentrações de metanol em mistura MEG, com umidade ao redor de 0,5, 1 e 2 vezes o limite de tolerância brasileiro(156ppm); dessorção em água e análise por CGDIC. O coeficiente de variação total calculado para o método de coleta e análise de metanol em mistura MEG foi de 7,3% (precisão) e wazzu exatidão esteve entre 90% e 101%. As concentrações de metanol foram estáveis, em tubos adsorventes armazenados em geladeira, durante o período de estudo de 14 dias. Porém, foi constatada uma migração de metanol através da camada analítica para a camada controle de forma gradativa com o passar do tempo. As soluções, a partir da dessorção dos tubos armazenadas em geladeira, foram estáveis durante o período de estudo de 45 dias. Além desses experimentos foram também realizados estudos de capacidade de adsorção da sílica gel para metanol levando em conta os interferentes, e verificado se eram capazes de dessorver totalmente o metanol, após um certo período de coleta. Constatou-se que após 30 minutos de coleta, os interferentes (etanol, umidade e gasolina) entravam em equilíbrio com o adsorvente e o metanol. / The main objective of this work is to propose procedures for the evaluation of the methodology of the sampling and analysis of solvents in the air in the workplace. Methanol in a MEG mixture (Methanol 33%, Ethanol 60%, and Gasoline 7%) was used as an example. At that time the MEG mixture was being proposed to substitute ethanol fuel due to its shortages on the Brazilian market. An atmosphere, dynamically controlled by injection, was produced to generate the known concentrations of methanol vapour in MEG mixtures. This atmosphere remained stable for about 450 minutes. The detection Iimit, using the GC-FID analytical method to monitor the concentrations produced, was 18mg/m3 for a sample volume of 2mL sampled from a sampling valve. The controlled atmosphere being suitable for the validation tests, studies of the breakthrough volume for the sampling of methanol in silica gel tubes were carried out, with the aim of discovering the total volume to be sampled in the field. These studies were carried out taking into account the possible interference of ethanol, gasoline and the high relative humidity. The sampling time for the mixture with the recommended relative humidity with a flow rate of 200mL/min was fifteen minutes. The analytical method used for the determination of methanol sampled in silica gel tubes and analyzed by GC-FID, was based on the methods found in the NIOSH and OSHA literature, adapted to the mixture conditions. After finding the best selectivity for the lowest retention time for the methanol in the MEG mixture, the detection Iimit of 9.7 x 10-3µg was determined. The precision of the analytical method was 2.1% and the accuracy was between 89% and 97%. Having established the analytical methodology. the best conditions for the controlled atmosphere and the sampling volume, studies were carried out which integrated the sampling and the analysis, that is, the precision and the accuracy of the sampling and the analysis and the storage stability. To study the precision and the accuracy of the sampling and analysis, concentrations 1 or 2 times that of the Brazilian tolerance Iimit of methanol (156 ppm) in MEG mixture, with humidity around 0.5, were generated, using dessorption in water and analysis by GC-FID. The total coefficient of variation calculated for the method of sampling and analysis of methanol in MEG mixture was 7.3% (precision) and the accuracy was between 90% and 101% . The concentrations of methanol were stable, in adsorption tubes stored in the refrigerator, throughout the study period of fifteen days. However, a gradual migration of methanol through the analytical layer to the control layer with the passage of time was noted. The solutions from the dessorption of the tubes, stored in the refrigerator, were stable throughout the study period of 45 days. Besides these experiments, studies of the adsorption capacity of silica gel for methanol, taking into account the interferents, were also carried out, and it was verified whether these were capable of the total dessorption of the methanol, after a certain sampling period. It was noted that after thirty minutes of sampling, the interferents came into equilibrium with the adsorbent and the methanol.

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