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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.
11

Aplicação de catalisador químico heterogêneo na transesterificação de miscelas etanólicas de óleo de soja / Application of a heterogeneous catalyst in the transesterification of ethanolic soybean oil miscellae

Larissa Braga Bueno Borges 03 October 2014 (has links)
A produção de biodiesel em larga escala deve impulsionar a pesquisa e desenvolvimento de tecnologias mais limpas e de menor custo relacionadas à obtenção e controle de qualidade desse combustível. A extração de óleo de soja com o solvente etanol resulta na produção de uma miscela rica em óleo, semi-refinada, que pode ser diretamente esterificável para produzir ésteres etílicos, sem a necessidade de evaporação do solvente. A transesterificação de miscelas por catálise heterogênea pode adicionar os benefícios do reaproveitamento do catalisador. O objetivo deste trabalho foi promover a otimização da transesterificação de miscelas etanólicas ricas em óleo de soja sob catálise heterogênea do fosfato de potássio tribásico (K3PO4), analisar o rendimento obtido com reutilizações do catalisador recuperado e promover sua regeneração. Foi realizada a adequação de uma técnica para quantificação do teor de ésteres, envolvendo separação por cromatografia em camada delgada associada à análise de coloração por espectrofotometria. Amostras de biodiesel de teor de ésteres conhecido foram oxidadas pela ação do dicromato de potássio em ácido sulfúrico, quantificando-se a mudança de cor do reagente de laranja para verde. O dicromato ácido foi capaz de oxidar completamente a fração isolada de ésteres, determinando os teores corretamente, à variação máxima de 2,05%, estabelecendo uma relação fixa de 0,08?g de dicromato consumido para cada ?g de biodiesel. A transesterificação com K3PO4 foi otimizada, alcançando rendimentos de 96,4% nas condições de RM 1:12, catalisador 5% e agitação 400rpm em 100 minutos de reação. O K3PO4 é um catalisador prático, pois sua utilização não requer etapas de preparação, no entanto apresentou indícios de solubilização no meio reacional. Os rendimentos obtidos com catalisador reutilizado foram baixos para todos os tratamentos de lavagem, sendo a lavagem moderada o escolhido devido a menor variabilidade de massa recuperada após as reutilizações. O catalisador regenerado resultou em rendimentos de 58,72%, equivalente a 84% do obtido com catalisador novo. O K3PO4 teve sua atividade prejudicada pelos fenômenos de saponificação e emulsificação, exigindo que mudanças sejam realizadas para que sua reutilização seja viável. A utilização de catalisadores heterogêneos e miscelas etanólicas lipídicas tem o potencial para redução dos custos de produção devido a obtenção de óleo vegetal sem a necessidade de refino e ao reaproveitamento de catalisador. / Large scale biodiesel production motivates research and development of cleaner low cost technologies related to the manufacture and quality control of this fuel. The extraction of soybean oil with the solvent ethanol results in the production of a rich in oil semi-refined miscella that can be directly esterified to produce ethyl esters, without the need of solvent evaporation. The transesterification of micellae by heterogeneous catalysis can add the benefits of reusing the catalyst. The aim of this work was to promote optimization of the transesterification of ethanolic soybean oil miscellae under heterogeneous catalysis of tripotassium phosphate (K3PO4), analyze the yield of reaction with reused catalyst and promote its regeneration. A technique for quantification of the ester content involving separation with thin layer chromatography and color analysis by spectrophotometry was also performed. Biodiesel samples of known ester content were oxidized by the potassium dichromate in sulfuric acid, and the change in color of the reagent from orange to green was quantified. The acid dichromate was able to completely oxidize the isolated fraction esters, correctly determining their content with a maximum variation of 2.05%, and revealing a fixed relation of 0,08?g of dichromate consumed per ?g of biodiesel. The transesterification with K3PO4 was optimized, reaching yields of 96.4% under the conditions of 1:12 molar ratio, 5% catalyst and 400rpm stirring in 100 minutes of reaction. The use of K3PO4 does not require preparation steps, but showed evidence of solubility in the reaction medium. Yields obtained with reused catalyst were low for all treatments, being the moderate washing (LM) chosen due to lower variability of mass recovered after reuses. The regenerated catalyst resulted in yields of 58.72%, equivalent to 84% of that obtained with fresh catalyst. The K3PO4 had its activity impaired by saponification and emulsification phenomena, requiring changes to make its reuse feasible. The use of heterogeneous catalysts with ethanolic rich in oil miscellae has the potential to reduce production costs due to the production of vegetable oil without the need of refining and the reuse of solid catalyst.
12

Efeitos do meio de cultivo sobre a sobrevivência, reprodução e sensibilidade de Ceriodaphnia dubia / Effects of culture water on survival, reproduction and sensitivity of Ceriodaphnia dubia

Mendes, Sandra Valéria Buratini 08 April 2002 (has links)
A espécie Ceriodaphnia dubia tem sido amplamente utilizada em testes de toxicidade crônica. Como a água constitui um fator essencial à sua manutenção, procurou-se avaliar a influência de três tipos de meio no cultivo e na resposta toxicológica deste microcrustáceo a três substâncias de referência. Foram acompanhadas, durante 13 a 18 gerações, a sobrevivência e a reprodução dos organismos em água natural (Reservatório de Ribeirão do Piraí, município de Salto, São Paulo, Brasil) e em dois meios reconstituídos (um simples - água mole reconstituída acrescida de selênio - e um complexo, denominado MS), avaliando-se, a cada 4 ou 5 gerações, as condições e a sensibilidade de cada cultura em testes com cloreto de sódio, dicromato de potássio e fenol. Os resultados evidenciaram um desempenho similar nos meios reconstituídos (em que padrões mínimos para sobrevivência e fecundidade nem sempre foram atendidos) e diferenciado do obtido em água natural - a mais eficiente para manutenção das culturas, onde tais padrões foram, geralmente, superados. Constatou-se a similaridade entre organismos provenientes da água natural e do meio OMS. Observou-se, também que a variabilidade dos resultados do teste ecotoxicológico difere conforme a água de diluição e a substância química utilizada, permitindo reconhecer o NaCI como substância de referência mais apropriada à avaliação da precisão deste método de ensaio, cujo coeficiente de variação máximo aceitável poderia ser estabelecido em 35%. / The species Ceriodaphnia dubia has been widely used in chronic toxicity tests. As water represents as essential factor to its maintenance, as evaluation was made of the influence of three different media in the culture and toxicological response of this microcrustacean to three reference toxicants. Survival and reproduction of this organism, reared in natural water (from Ribeirão do Piraí Reservoir), São Paulo State, Brazil) and in two reconstituted media (a simple one - reconstituted soft water, supplemented with selenium - and a complex one, called MS), were accompanied during 13 to 18 generations; at each 4 or 5 generations such cultures were evaluated in relation to health and sensitivity in toxicity tests with sodium chloride, potassium dichromate and phenol. The results indicated a similar performance in the reconstituted media (where the minimum patterns for survival and fecundity were not always reached) and differentiated from that obtained in natural water - the most suitable culture medium, where such patterns were, usually, exceeded. It was found a comparable sensitivity between natural water and MS cultures. It was also verified that the variability of the results among ecotoxicological test differs according to dilution water and chemical substance, allowing to recognize NaCl as the most suitable reference toxicant to measure the precision of this test method, whose maximum coefficient of variation could be established in 35%.
13

Validation of mercury free methods for analysis of Chemical Oxygen Demand in municipial wastewater / Validering av kvicksilverfria analysmetoder för bestämning av kemiskt syreförbrukande ämnen (COD) i kommunalt avloppsvatten

Jonsson, Sandra January 2015 (has links)
Water is used every day in society and to be able to recycle this water we depend upon efficient wastewater treatment. It is vital to test the wastewater based on different parameters. One parameter is the Chemical Oxygen Demand (COD), which defines the amount of organic substances that can be chemically oxidized within the water. The Swedish standardized analytical method for COD (SS-028142), COD(Cr) is dependent on mercury, a substance which was banned according to Swedish regulations in year 2009 but is still used due to time limited dispensations. This report is a part of a pre-procurement innovative project initiated by the Swedish Water and Wastewater Association (SWWA) in order to bring forward and evaluate mercury free analytical methods for COD for municipal wastewater. The aim was to validate three analytical methods for COD: Chloride Determination, Chloride Elimination and PeCOD and compare the analytical results to the standardized COD(Cr). Three laboratories, Käppala (Stockholm), Gryaab (Gothenburg) and Komlab (Örnsköldsvik) were included in the validation process by providing analytical data. The validation was conducted using the data as input for the statistical methods regression, correlation and analysis of variance to investigate the performance of the individual methods. As a complement to the statistical results, comments regarding the methods brought up by the laboratory staff were compiled in order to reflect on the usability and robustness of the methods.  The results indicated that the method Chloride Determination was the method most similar to the COD(Cr) method, when investigating obtained COD concentrations, required analytical time and implementation steps needed to obtain a final COD value. This result was evident by high coefficient of determination values for influent wastewater samples. The PeCOD method, which was submitted in two versions, one manual and one automatic was only able to analyze soluble COD. It was found that the PeCOD methods obtained lower COD concentrations compared to the standardized method when analyzing filtered samples. Due to highly variable correlation coefficients between the PeCOD and COD(Cr) for various types of samples indicated that no uniform linear relation between the methods was present. Analysis with the Chloride Elimination method was halted early in the validation process, but was found to receive approximately 50 percent lower COD values than the reference method  COD(Cr). Finally it can be said that the input data for conducting the statistical test were limited and further analysis should be recommended in order to validate the results with a higher certainty. / Varje dag produceras avloppsvatten i samhället och för att kunna återanvända detta vatten krävs en tillförlitlig reningsprocess. För att rena avloppsvatten effektivt är det betydelsefullt att kontinuerligt testa avloppsvattnet utifrån ett antal viktiga parametrar. En av dessa är kemisk syreförbrukning, COD, som definieras av den mängd syre som förbrukas genom fullständig kemisk oxidation av organiskt material. Den svenska standardiserade analysmetoden för COD (SS-028142) , COD(Cr) är beroende av kvicksilver för att erhålla ett korrekt analysresultat utan påverkan av kloridjoner. Kvicksilver är enligt Svensk lag förbjudet sedan år 2009, men analysmetoden är dock vanligt använd på svenska avloppsreningsverk tack vare årliga dispenser. Detta examensarbete är en del av en förkommersiell innovationsupphandling som initierats av Svenskt Vatten med mål att undersöka och validera kvicksilverfria analysmetoder för COD tillgängliga på den internationella marknaden. Projektets syfte var att utföra en validering av tre analysmetoder: Klorid Determination, Klorid Elimination och PeCOD och jämföra dess resultat med referens metoden COD(Cr). Tre olika laboratorier, Käppala (Stockholm), Gryaab (Göteborg) och Komlab (Örnsköldsvik) medverkade i projektet. Valideringen genomfördes med de statistiska metoderna regression, korrelation och variansanalys, utifrån insamlade mätdata i syfte att undersöka de givna metodernas prestanda. Som ett komplement till det statistiska testerna sammanställdes synpunkter som framkommit under analysarbetet av laboratoriepersonal, för bedömning av metodernas användarvänlighet och robusthet.  Utifrån valideringen var det tydligt att metoden Klorid Determination hade störst likhet med COD(Cr) metoden utifrån givna analysresultat, analystid samt utförda analyssteg. Detta resultat styrktes av höga värden för determinationskoefficients för inkommande avloppsvatten mellan innovatios metoden och referense metoden COD(Cr). Analysmetoden PeCOD bestod av två olika versioner, skildrade den lösliga COD innehållet i provet istället för den total COD koncentrationen som hos COD(Cr). Oavsett vilken version av PeCOD som används erhålls ett lägre COD resultat jämfört med referens metoden COD(Cr) då filtrerade prover analyserades. De framtagna varierande korrelations koefficienter mellan PeCOD och COD(Cr) indikerade att ingen enhetlig korrelation gick att finna mellan metoderna hos de olika laboratorierna. Analysmetoden COD Elimination pausades tidigt i processen men de tidiga testerna visade på halverade COD koncentrationer jämfört med referens metoden.  Slutligen kan det nämnas att mätdata som användes som indata till de beskrivna statistiska testerna var begränsade och att vidare analyser rekommenderas för att kunna bevisa givna resultat med ökad sannolikhet.
14

Estudo de inibidores de corros?o em concreto armado, visando a melhoria na sua durabilidade

Silva, Djalma Ribeiro da 01 March 2007 (has links)
Made available in DSpace on 2014-12-17T14:07:22Z (GMT). No. of bitstreams: 1 DjalmaRS.pdf: 1628891 bytes, checksum: d4993a3fdaeab8a1baca119c6780c3ac (MD5) Previous issue date: 2007-03-01 / Petr?leo Brasileiro SA - PETROBRAS / This thesis has as objective presents a methodology to evaluate the behavior of the corrosion inhibitors sodium nitrite, sodium dichromate and sodium molybdate, as well as your mixture, the corrosion process for the built-in steel in the reinforced concrete, through different techniques electrochemical, as well as the mechanical properties of that concrete non conventional. The addition of the inhibitors was studied in the concrete in the proportions from 0.5 to 3.5 % regarding the cement mass, isolated or in the mixture, with concrete mixture proportions of 1.0:1.5:2.5 (cement, fine aggregate and coarse aggregate), superplasticizers 2.0 % and 0.40 water/cement ratio. In the modified concrete resistance rehearsals they were accomplished to the compression, consistence and the absorption of water, while to analyze the built-in steel in the concrete the rehearsals of polarization curves they were made. They were also execute, rehearsals of corrosion potential and polarization resistance with intention of diagnose the beginning of the corrosion of the armors inserted in body-of-proof submitted to an accelerated exhibition in immersion cycle and drying to the air. It was concluded, that among the studied inhibitors sodium nitrite , in the proportion of 2.0 % in relation to the mass of the cement, presented the best capacity of protection of the steel through all the studied techniques and that the methodology and the monitoring techniques used in this work, they were shown appropriate to evaluate the behavior and the efficiency of the inhibitors / Esta tese tem como objetivo apresentar uma metodologia para avaliar o comportamento dos inibidores de corros?o nitrito de s?dio, molibdato de s?dio, dicromato de s?dio, bem como a suas misturas, no processo de corros?o para o a?o embutido no concreto armado, atrav?s de diferentes t?cnicas eletroqu?micas, bem como as propriedades mec?nicas desse concreto n?o convencional. Estudou-se a adi??o dos inibidores no concreto nas propor??es de 0,5 a 3,5 % em rela??o ? massa do cimento, isolados e em mistura, num tra?o 1,0:1,5:2,5 (cimento, areia e brita), superplastificante 2,0 % e rela??o ?gua/cimento 0,40. No concreto modificado foram realizados ensaios de resist?ncia ? compress?o, consist?ncia e a absor??o de ?gua, enquanto que para analisar o a?o embutido no concreto foram efetuados ensaios de curvas de polariza??o. Foram executados tamb?m ensaios de potencial de corros?o e resist?ncia de polariza??o com intuito de diagnosticar o in?cio da corros?o das armaduras inseridas em corpos-de-prova submetidos a uma exposi??o acelerada em ciclo de imers?o e secagem ao ar. Concluiu-se que, dentre os inibidores estudados, o nitrito de s?dio, na propor??o de 2,0 % em rela??o ? massa do cimento, apresentou a melhor capacidade de prote??o do a?o atrav?s de todas as t?cnicas estudadas e que a metodologia e as t?cnicas de monitoramento utilizadas neste trabalho mostraram-se adequadas para avaliar o comportamento e a efici?ncia dos inibidores
15

Toxikologisk tillväxtstudie av sötvattenalgen Raphidocelis subcapitata : En jämförelse mellan flödescytometer NovoCyte och automatisk cellräknare TC20 / Study of toxic growth inhibition with unicellular fresh water green algae Raphidocelis subcapitata : Comparison between flow cytometer NovoCyte and automatic cell counter TC20

Andersson, Eva January 2018 (has links)
Biologiska toxicitetstester utförs genom att exponera en testorganism för olika koncentrationer av kemikalier under en bestämd period. Det finns akuta toxicitetstester och kroniska. Resultat från akuta studier presenteras som EC50-värde (Effect Concentration, affecting 50 % of the population). Tester som används som underlag för riskbedömningar ska utföras på kvalitetsmässigt acceptabelt sätt som grundas på International Organization for Standardization (ISO) och Good Labaratory Practice (GLP). Syftet med studien var att studera toxisk inverkan av kaliumdikromat på encellig sötvattenalg, R. subcapitata, genom att räkna cellantal med två olika instrument: flödescytometer och automatisk cellräknare. Vidare att jämföra testernas EC50 medelvärde mot ISO 8692 angivet värde i precisions syfte och att utvärdera de båda räknemetoderna gällande precision och analystid. Kaliumdikromat användes för tillväxtinhibering vid toxicitetstest. EC50-resultaten visade ingen statistiskt signifikant skillnad mellan de båda instrumenten (p=0,47). Den akuta toxicitetsanalysens precision kunde bekräftas som giltig då båda mätmetoders EC50 medelvärden vid jämförelse med ISO 8692 värde befanns inom bestämda 95% konfidensintervallet. Vid jämförelse av studiens två mätningsmetoder, observerades större spridning kring medelvärdet i cellräknarens resultat, där tre EC50 värden hamnade utanför 95% CI. Däremot visade resultatet från flödescytometern mindre spridning och högre noggrannhet jämfört med cellräknarens. Studien visade att flödescytometer skulle kunna användas i framtida toxikologiska tester med encelliga alger, men det krävs flera upprepade försök för att bekräfta fördelar med analysen i flödescytometern. / Biological toxicity tests are performed by exposing a test organism to different concentrations of chemicals over a certain period of time. Results from acute studies are presented as EC50 (Effect Concentration, affecting 50% of the population). Tests used as a basis for risk assessments shall be performed in a quality acceptable way based on the International Organization for Standardization (ISO) and Good Laboratory Practice (GLP). The aim of this study was to study the toxic effect of potassium dichromate on unicellular green algae R. subcapitata, by counting cells with two different apparatus: flow cytometer and automatic cell counter. Additionally, to compare the EC50 mean values against the ISO 8692 value for control of test precision and to compare accuracy and analytical time of two methods. Potassium dichromate was used for growth inhibition in toxicity tests. The EC50 results showed no statistically significant difference between the two instruments (p = 0.47). The accuracy of acute toxicity analysis was confirmed as valid as both EC50 average measurement values compared to ISO 8692 value were found within the 95% confidence interval. When comparing the two methods of the study, greater spread was observed around the mean value in the cell count's results, where three EC50 values were outside 95% CI. The result of the flow cytometer had less spread and higher accuracy compared to the cell count. The study showed that flow cytometers could be used in future toxicological tests with algae, but several repeated tests are required to confirm the benefits of analysis with the flow cytometer.
16

Efeitos do meio de cultivo sobre a sobrevivência, reprodução e sensibilidade de Ceriodaphnia dubia / Effects of culture water on survival, reproduction and sensitivity of Ceriodaphnia dubia

Sandra Valéria Buratini Mendes 08 April 2002 (has links)
A espécie Ceriodaphnia dubia tem sido amplamente utilizada em testes de toxicidade crônica. Como a água constitui um fator essencial à sua manutenção, procurou-se avaliar a influência de três tipos de meio no cultivo e na resposta toxicológica deste microcrustáceo a três substâncias de referência. Foram acompanhadas, durante 13 a 18 gerações, a sobrevivência e a reprodução dos organismos em água natural (Reservatório de Ribeirão do Piraí, município de Salto, São Paulo, Brasil) e em dois meios reconstituídos (um simples - água mole reconstituída acrescida de selênio - e um complexo, denominado MS), avaliando-se, a cada 4 ou 5 gerações, as condições e a sensibilidade de cada cultura em testes com cloreto de sódio, dicromato de potássio e fenol. Os resultados evidenciaram um desempenho similar nos meios reconstituídos (em que padrões mínimos para sobrevivência e fecundidade nem sempre foram atendidos) e diferenciado do obtido em água natural - a mais eficiente para manutenção das culturas, onde tais padrões foram, geralmente, superados. Constatou-se a similaridade entre organismos provenientes da água natural e do meio OMS. Observou-se, também que a variabilidade dos resultados do teste ecotoxicológico difere conforme a água de diluição e a substância química utilizada, permitindo reconhecer o NaCI como substância de referência mais apropriada à avaliação da precisão deste método de ensaio, cujo coeficiente de variação máximo aceitável poderia ser estabelecido em 35%. / The species Ceriodaphnia dubia has been widely used in chronic toxicity tests. As water represents as essential factor to its maintenance, as evaluation was made of the influence of three different media in the culture and toxicological response of this microcrustacean to three reference toxicants. Survival and reproduction of this organism, reared in natural water (from Ribeirão do Piraí Reservoir), São Paulo State, Brazil) and in two reconstituted media (a simple one - reconstituted soft water, supplemented with selenium - and a complex one, called MS), were accompanied during 13 to 18 generations; at each 4 or 5 generations such cultures were evaluated in relation to health and sensitivity in toxicity tests with sodium chloride, potassium dichromate and phenol. The results indicated a similar performance in the reconstituted media (where the minimum patterns for survival and fecundity were not always reached) and differentiated from that obtained in natural water - the most suitable culture medium, where such patterns were, usually, exceeded. It was found a comparable sensitivity between natural water and MS cultures. It was also verified that the variability of the results among ecotoxicological test differs according to dilution water and chemical substance, allowing to recognize NaCl as the most suitable reference toxicant to measure the precision of this test method, whose maximum coefficient of variation could be established in 35%.
17

Avaliação da disponibilidade de nitrogênio para milho em sucessão a gramíneas e leguminosas de cobertura /

Godoi, Leonardo Mella de. January 2010 (has links)
Resumo: Para conhecer o potencial de plantas de cobertura no fornecimento de nitrogênio para o milho, em sistema de plantio direto, foi avaliado o N potencialmente mineralizável (N0) do solo por meio de ensaio de incubação aeróbia de longa duração e o N disponível por meio dos extratores químicos KCl a quente, Dakota do Sul modificado e tampão fosfato borato a pH 11,2. Foram utilizadas amostras de solo de experimento a campo, instalado em área de Latossolo Vermelho argiloso e conduzido em delineamento em blocos casualizados, com cinco tratamentos: testemunha com vegetação espontânea, sorgo, milheto, mucuna-preta e feijão-de-porco, e cinco repetições. A coleta de solo nas parcelas foi feita após a dessecação das plantas de cobertura e antes do cultivo de milho, nos anos agrícolas de 2007/2008 e 2008/2009. O solo coletado, representativo da profundidade de 0 a 10 cm, foi utilizado no ensaio de incubação aeróbia, em experimento em vasos, com milho, e para as análises químicas. A eficiência dos extratores foi avaliada por meio de testes de correlação, empregando como variáveis de referência o N0 e o N mineralizado acumulado por 30 semanas, obtidos no ensaio de incubação aeróbia, e a produção de matéria seca e o N acumulado na parte aérea do milho, obtidos no experimento em vasos. As plantas de cobertura não diferem entre si quanto ao potencial de fornecimento de N para o milho. O método do KCl a quente é capaz de predizer a mineralização de N, porém os métodos químicos avaliados para predizer o N disponível não são eficientes / Abstract: Aiming to determine the potential of cover crops to supply nitrogen for corn in no-tillage system, it was evaluated the soil potentially mineralizable N (N0) by long-term aerobic incubation and available N by chemical extractants (hot KCl, modified South Dakota and pH 11.2 phosphate-borate buffer). Soil samples were collected from a field experiment, installed in an Udox and carried out in a randomized block design with five treatments (control with spontaneous vegetation, Sorghum bicolor, Pennicetum glaucum, Mucuna aterrima and Canavalia ensiformis) and five replications. Plots soil sampling was made after the cover crops desiccation and before growing the corn in the agricultural seasons of 2007/2008 and 2008/2009. Soil samples collected from 0 to10 cm depth were used for long-term aerobic incubation, pots experiment with corn, and for soil chemical analysis. Extractants efficiency was evaluated by correlation tests, using as reference the N0 and the mineralized accumulated N over 30 weeks obtained from long-term aerobic incubation, dry matter production and N accumulated in maize shoots, obtained from pots experiment. Cover crops do not differ in their potential to supply nitrogen for corn. Hot KCl is able to predict the N mineralization but the chemical methods evaluated to predict the available nitrogen are not efficients / Orientador: Manoel Evaristo Ferreira / Coorientador: Mara Cristina Pessôa da Cruz / Banca: André César Vitti / Banca: José Frederico Centurion / Mestre
18

Jämförelse av olika redox-titreringsmetoders valideringsparametrar / Comparison of different redox titration methods validation parameters

Segerlund Henriksson, Ella January 2024 (has links)
A fundamental analysis performed at LKAB is the determination of the iron (II) content of the company’s iron ore products. Currently, a redox titration method using potassium dichromate as the titrator is used to determine this content. However, LKAB is considering replacing its current method due to the titrator’s harmful effects on the health and the environment. The purpose of this study is to compare different redox titration methodsvalidation parameters, to find the most suitable method for the determination of the iron (II) content. The titrators in focus for this study is potassium dichromate, cerium (IV) sulphate and potassium permanganate. Several experiments were performed to compare the three titration methods. The validation parameters determined for each method were precision, accuracy, linearity, LOD, LOQ and robustness. The titration error was also calculated. The results showed that the redox titration with potassium dichromate as the titrator had the highest accuracy at 98.95 %, while the redox titration with cerium (IV) sulphate as the titrator had the best precision at 0.099 % (for samples with a similar matrix as LKAB’s iron ore products). Based on the acquired results, it was concluded that LKAB’s current method is the most suitable for the determination of the iron (II) content in LKAB’s iron ore products. The redox titration method using cerium (IV) sulphate as a titrator is a good competitor, butdue to the method’s slightly inferior accuracy and vague end point, it fails to outcompeteLKAB’s current method. / En grundläggande analys som utförs på LKAB är fastställandet av järn (II)-halten i företagets järnmalmsprodukter. För närvarande används en redox-titreringsmetod med kaliumdikromat som titrator för bestämmelsen av denna halt. LKAB överväger dock att byta ut sin nuvarande metod på grund av titratorns hälso- och miljöfarliga effekter. Syftet med denna studie är att jämföra olika redox-titreringsmetoders valideringsparametrar, för att hitta den mest lämpligaste metoden för fastställandet av järn (II)-halten. De titratorer som studeras är kaliumdikromat, cerium (IV) sulfat och kaliumpermanganat. Flertalet experiment utfördes, för att kunna jämföra de tre titreringsmetoderna med varandra. De valideringsparametrar som bestämdes för vardera metoden var precision, noggrannhet, linjäritet, LOD, LOQ och robusthet. Titrerfelet beräknades också. Resultaten visade att redox-titrering med kalimdikromat som titrator hade högst noggrannhet på 98,95 %, medan redox-titrering med cerium (IV) sulfat som titrator hade bäst precision på 0,099 % (för prover med liknande matris som LKAB:s järnmalmsprodukter). Utifrån de resultat som erhölls så drogs slutsatsen att LKAB:s nuvarande metod är den mest lämpligaste för fastställandet av järn (II)-halten i företagets järnmalmsprodukter. Redox-titreringsmetoden med cerium (IV) sulfat som titrator är en bra konkurrent, men på grund av metodens något sämre noggrannhet och otydligare slutpunkt så misslyckas den med att konkurrera ut LKAB:s nuvarande metod.

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