O preparo da amostra é uma das etapas mais importantes em toda a análise química. O isolamento e a concentração dos componentes da amostra são cruciais e busca-se sempre que essas etapas sejam as mais simples e consumam o mínimo possível de tempo e reagentes. Nos últimos anos, um tipo de material tem se mostrado bastante útil para análises químicas a partir de fluidos biológicos, os polímeros molecularmente impressos (MIPs). Os MIPs são sintetizados por reações de polimerização, na presença de uma molécula molde (template). A molécula molde se liga aos monômeros funcionais do polímero durante a reação de polimerização e permanece ligada à superfície das cadeias poliméricas quando a reação se completa. Terminada a polimerização, realiza-se a completa lavagem das moléculas molde, assim, restam na superfície polimérica cavidades tridimensionais complementares à molécula empregada como molde. Essas cavidades permitem a ligação reversível e preferencial da molécula molde ou outras com estrutura química semelhante. A Cannabis sativa é a droga ilícita mais consumida em todo o mundo e nos últimos anos muita atenção tem se voltado a seus efeitos toxicológicos no corpo humano e a aplicações medicinais. Nesta dissertação, foi sintetizado um MIP com a molécula molde catequina para a extração e posterior análise por LC-MS/MS dos canabinóides Δ9-tetrahidrocanabinol (THC), 11-hidroxi-Δ9-tetrahidrocannabinol (THC-OH) e 11-nor-Δ9-tetrahidrocannabinol-9-ácido carboxílico (THC-COOH) em amostras de urina. O MIP produzido foi empacotado em microdispositivo e empregado no preparo das amostras de urina por microextração por sorvente empacotado (MEPS). O método desenvolvido apresentou boa linearidade (valores de r de 0,977 para o THC e 0,994 para THC-OH e THC-COOH). Os limites de detecção e de quantificação foram respectivamente de 5 ng mL-1 e 20 ng mL-1, para os compostos THC e THC-OH, na faixa linear de 25 a 250 ng mL-1. Para o composto THC-COOH os limites de detecção e quantificação alcançados foram de 1 ng mL-1 e 5 ng mL-1, respectivamente, na faixa linear de 5 a 170 ng mL-1. O método apresentou valores razoáveis de precisão entre 3,2% (THC-COOH) e 25,1% (THC) e de exatidão, que variou entre -18,4 e 17,4 (ambos para o THC). O MIP empregado no preparo da amostra mostrou-se mais seletivo e específico do que materiais normalmente empregados para a extração dos canabinoides das amostras de urina, além de a técnica de extração por MEPS apresentar baixo consumo de solventes e amostra para a extração dos analitos e posterior análise por LC-MS/MS. / The sample preparation is one of the most important steps in every chemical analysis. The isolation and concentration of the sample components are crucial and it is always sought that these steps are simple and consume the lowest amount of time and reagents. In the recent years, a type of material has proved to be very useful for chemical analyzes of biological fluids, the molecularly imprinted polymers (MIPs). MIPs are synthesized by polymerization reactions in the presence of a template molecule. The template molecule binds to the functional monomers of the polymer during the polymerization reaction and remains bonded to the surface of the polymeric chains after the reaction is complete. After the polymerization is finished, the complete washing of the template molecules is carried out, thus, three-dimensional cavities, complementary to the molecule used as a template, remain on the polymer surface. These cavities allow the reversible and preferential bonding of the template molecule or others with similar chemical structure. Cannabis sativa is the most commonly consumed illicit drug in the world and in recent years much attention has focused on its toxicological effects on human body and for medical applications. In this master dissertation, a MIP was synthesized with the catechin molecule as template, for extraction and subsequent analysis by LC-MS/MS of the cannabinoids Δ9-tetrahydrocannabinol (THC), 11-hydroxy-Δ9-tetrahydrocannabinol (THC-OH), and 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic acid (THC-COOH) in urine samples. The MIP produced was packed in a microdevice and used in the preparation of the urine samples by microextraction by packed sorbent (MEPS). The developed method showed good linearity (r values of 0.977 for THC and 0.994 for THC-OH and THC-COOH). The detection and quantification limits were respectively 5 ng mL-1 and 20 ng mL-1 for THC and THC-OH in the linear range from 25 to 250 ng mL-1. For the compound THC-COOH the limits of detection and quantification achieved were 1 ng mL-1 and 5 ng mL-1, respectively, in the linear range from 5 to 170 ng mL-1. The method presented reasonable values of precision, between 3.2% (for THC-COOH) and 25.1% (for THC) and displayed accuracy ranging from -18.4 to 17.4 (both for THC). The MIP used in the sample preparation was more selective and specific than other materials usually employed for the extraction of the cannabinoids from the urine samples. The MEPS technique also showed low consumption of solvents and sample for sample preparation, extraction of analytes and subsequent analysis by LC-MS/MS.

Η απορρύπανση των υδάτων αποτελεί αναγκαία και καθιερωμένη από δεκαετίες πρακτική. Η απορρύπανση με τη μέθοδο της ρόφησης είναι μία από την πληθώρα των τεχνικών που εφαρμόζονται. Το περισσότερο διαδεδομένο ροφητικό υλικό είναι ο ενεργός άνθρακας, του οποίου όμως το υψηλό κόστος παραγωγής, οδήγησε την επιστημονική έρευνα στην αναζήτηση εναλλακτικών, υλικών χαμηλότερου κόστους. Για το σκοπό αυτό, το επιστημονικό ενδιαφέρον έχει στραφεί σε πολλά υλικά κυρίως οργανικής προέλευσης, αλλά και σε ανόργανα υλικά, όπως τα οξείδια των μετάλλων, τα οποία αφθονούν στη φύση. Στην παρουσα εργασία έγινε μελέτη της ροφητικής ικανότητας φυσικών οξειδίων, για τη ρόφηση αρωματικών οργανικών ενώσεων και βαρέων μετάλλων. Πιο συγκεκριμένα, μελετήθηκε ο μηχανισμός της ρόφησης του φαινανθρενίου, της 2-ναφθόλης και του υδραργύρου από οξείδια αργιλίου, τιτανίου, αργιλίου/πυριτίου και σιδήρου, με σκοπό την αξιολόγηση των υλικών αυτών ως ροφητικών υλικών και τη σύγκριση των αποτελεσμάτων με αυτά της ρόφησης των αντίστοιχων ρύπων από υλικά που παρασκευάζονται από την πυρόλυση πρώτης ύλης βιολογικής προέλευσης. Για τη μελέτη της κινητικής της ρόφησης του φαινανθρενίου και της 2-ναφθόλης πραγματοποιήθηκαν πειράματα σε θερμοκρασία περιβάλλοντος, σε θαλασσινό και γλυκό συνθετικό νερό, με διαφορετικές ποσότητες ροφητικού υλικού (χωρίς χημική επεξεργασία) και για διαφορετικό χρόνο επαφής. Από τα πειράματα αυτά μετρήθηκε η κινητική της ρόφησης καθώς και το ποσοστό απομάκρυνσης των ρύπων από το διάλυμα. Από τις μετρήσεις που έγιναν, προέκυψε ότι το ποσοστό απομάκρυνσης του φαινανθρενίου από το διάλυμα αυξάνεται αυξανομένης της ποσότητας του ροφητικού υλικού. Η σταθερά της ρόφησης Kd, κυμάνθηκε σε ένα εύρος τιμών από 1 έως 10 L/Kg, τιμές 2 έως 4 τάξεις μεγέθους μικρότερες από αυτές άλλων ροφητικών υλικών βιολογικής προέλευσης, ή προϊόντων πυρόλυσης. Τη μεγαλύτερη ικανότητα ρόφησης φαινανθρενίου επέδειξε η γ-αλούμινα με ειδική επιφάνεια 270 m2/g, με μέγιστη απομάκρυνση φαινανθρενίου το 55 % της αρχικής συγκέντρωσης έπειτα από 8 ημέρες, ενώ τη μικρότερη ικανότητα ρόφησης η γ-αλούμινα με ειδική επιφάνεια 120 m2/g, με μέγιστη απομάκρυνση το 14 % της αρχικής συγκέντρωσης, έπειτα από 10 ημέρες. Η τιτάνια, με ειδική επιφάνεια 120 m2/g, είχε ως αποτέλεσμα την απομάκρυνση του 52 % της αρχικής συγκέντρωσης φαινανθρενίου, σε 8 ημέρες. Από τα πειράματα ρόφησης της 2-ναφθόλης από την γ-αλούμινα, δεν προέκυψε μετρήσιμη ρόφηση. Η ρόφηση του υδραργύρου από την γ-αλούμινα (ειδική επιφάνεια 131 m2/g), και τα οξείδια σιδήρου μελετήθηκε με πειράματα στους 25 °C, σε pH 5 και με χρόνο εξισορρόπησης τις 24 h. Από τα πειράματα προέκυψε ισόθερμη καμπύλη και έγινε προσπάθεια προσαρμογής της σε μοντέλα ρόφησης. Παρατηρήθηκε αύξηση του ποσοστού απομάκρυνσης του υδραργύρου, με αύξηση της μάζας της γ-αλούμινας. Το μέγιστο ποσοστό απομάκρυνσης, ήταν το 93 % της αρχικής συγκέντρωσης και επιτεύχθηκε με μάζα γ-αλούμινας ίση και μεγαλύτερη από 1 g. Για τιμή Ce=15 mg/L, μετρήθηκε qe=0,91 mg/g, τιμή 1 έως 2 τάξεις μεγέθους μικρότερη από αυτές άλλων ροφητικών υλικών βιολογικής προέλευσης ή προϊόντων πυρόλυσης. Τα οξείδια σιδήρου, παρότι είχαν ειδική επιφάνεια 55 m²/g, δεν παρουσίασαν μετρήσιμη ροφητική ικανότητα για κανέναν από τους ρύπους, που μελετήθηκαν στην παρούσα εργασία. Συνοψίζοντας μπορούμε να πούμε ότι τα ανόργανα υλικά που μελετήθηκαν στην παρούσα εργασία, παρόλο που παρουσιάζουν μεγάλες τιμές ειδικής επιφάνειας, δεν μπορούν να χαρακτηρισθούν ως αξιόλογα ροφητικά υλικά, τόσο για τη ρόφηση των οργανικών ρύπων φαινανθρένιο και 2-ναφθόλη, όσο και για τη ρόφηση του υδραργύρου. / Water treatment is a necessary and standard practice since decades. Adsorption technology in water treatment is one of many techniques being used. Activated carbon is the most widely applied adsorbent in water treatment, however its high production cost has led scientific research to investigate alternative low cost sorbent materials. This need has developed scientific interest towards novel materials most of them derived from biomass, but also inorganic oxides that are abundant in nature. The present study focuses on the investigation of the capacity of natural oxides to adsorb aromatic organic compounds and heavy metals. Specifically, sorption of phenanthrene, 2-naphthol and mercury onto aluminum, titanium, silicon and ferric oxides was examined, for the evaluation of these materials as sorbents, compared to pyrolized biomaterials. For the study of sorption of phenanthrene and 2-naphthol, batch experiments were conducted at room temperature, using artificial seawater and fresh water, different mass of sorbent material at different contact time. Sorption kinetics and the pollutant removal percentages were determined. The proportion of phenanthrene removal increased with the increase of the mass of the sorbent material. Sorption distribution coefficient Kd ranged between 1 and 10 L/Kg. These values are 2 to 4 orders of magnitude lower than the respective values shown for biomaterials and for pyrolysis products, respectively. Maximum sorption capacity of phenanthrene (55 % proportion removal) was shown by γ-alumina, with a specific surface area equal to 270 m2/g, after 8 days. Minimum sorption capacity (14 % proportion removal) was shown by γ-alumina, with a specific surface area equal to 120 m2/g, after 10 days. Titania, with a specific surface area equal to 120 m2/g, adsorbed a proportion of 52 % of the initial concentration of phenanthrene, after 8 days. Sorption experiments of 2-naphthol from γ-alumina, did not show a measurable sorption. Sorption of mercury from γ-alumina and ferric oxides was studied, conducting batch experiments at 25 °C, pH 5, 24 h contact time. The experiments resulted to an isotherm curve that was evaluated using different sorption isotherm models. An increase of the proportion of mercury removal, with the increase of the mass of γ-alumina was observed. Maximum proportion of mercury removal (93% of the initial concentration) was observed with the addition of γ-alumina of 1 g or more. At Ce=15 mg/L, qe=0,91 mg/g was measured. This value is 1 to 2 orders of magnitude lower, than the respective values shown for biomaterials and for pyrolysis products, respectively. Even though ferric oxides’ specific surface area was estimated at 55 m²/g, they did not show a measurable sorption capacity for any of the pollutants tested in the present study. Even though the materials examined in the present study, were of large specific surface area, their sorptive properties shown, are not competitive with the respective properties of biomaterials. Thus, they cannot be considered as promising sorbents for the removal of phenanthrene, 2-naphthol, or mercury from water.

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPES / The water pollution causes changes in physical, chemical and biological water, which interfere with their quality, preventing its use for human consumption. Most chemical contaminants in surface water are related to industrial and agricultural sources. Since, with farming the Brazil pollute existing water resources making use of pesticides and fertilizers. This study aims to develop a fast and efficient method based on extraction techniques in solid phase (SPE) and high-performance liquid chromatography with UV detection in the ultraviolet and visible with diode array (HPLC UV-Vis / DAD) for the determination of pesticides, endocrine disruptors, epoxiconazole, fenarimol, fenbuconazole, flusilazole, flutriafol, and vinclozolin in water using biocarvões produced from agro-industry waste as an alternative sorbent for SPE. Tests with the analytes allowed the adjustment of the chromatographic conditions for simultaneous analysis of five selected pesticides. The optimal condition for the extraction of analytes was performed using 0.5 g of adsorbent to 50 mL of ultrapure water and eluted with 5 mL of acetonitrile. The biochar produced from coconut waste was tested as an adsorbent for the extraction by SPE and showed good recovery results between 75% ± 9 - 119 ± 12% for the concentration levels of 0.5 to 1 ug mL-1. The parameters studied to validate the method were: linearity and sensitivity, obtaining a good sensitivity and linear response with 0.9998 coefficients in the range of 0.01 to 10 ug mL-1; precision based on the precision of measurements (Intra) and intermediate precision (interday), obtaining results of 0.1-1%, 0.6-1%, respectively; accuracy with recovery values of 60 ± 37% - 117 ± 3% to the concentration levels of from 0.025 to 0.1 mg L-1 and 75 ± 9% - 119 ± 12% for levels 0.5 to 1 ug mL- 1 related to the biochar and C18, respectively. The LD 0.01 to 0.025 in range and LQ from 0.025 to 0.5 ug mL-1. The method developed was adequate for the determination of pesticides in water samples. / A poluição aquática provoca mudanças nas características físicas, químicas e biológicas das águas, as quais interferem na sua qualidade, impossibilitando o seu uso para o consumo humano. A maioria dos contaminantes químicos presentes em águas superficiais estão relacionados às fontes industriais e agrícolas. Uma vez que, com a atividade agrícola o Brasil polui os recursos hídricos existentes fazendo uso de agrotóxicos e fertilizantes. O presente trabalho tem como objetivo desenvolver um método rápido e eficiente baseado nas técnicas de extração em fase sólida (SPE) e cromatografia líquida de alta eficiência com detector espectrofotométrico na região do ultravioleta e visível com arranjo de diodos (HPLC UV-Vis/DAD) para a determinação dos agrotóxicos, perturbadores endócrinos, epoxiconazol, fenarimol, fenbuconazol, flusilazol, flutriafol, e vinclozolina, em água, utilizando biocarvões produzidos a partir de rejeitos de agroindústria, como adsorvente alternativo para a SPE. Testes realizados com os analitos permitiram o ajuste das condições cromatográficas para análise simultânea de cinco agrotóxicos selecionados. A condição ótima de extração dos analítos consistiu em utilizar 0,5 g do adsorvente para 50 mL de água ultrapurificada e eluição com 5 mL de acetonitrila. O biocarvão produzido a partir de rejeitos de coco foi testado como adsorvente para a extração por SPE e apresentou resultados satisfatórios de recuperação entre 75 ± 9% – 119 ± 12% para os níveis de concentração 0,5 a 1 μg mL-1. Os parâmetros estudados para a validação do método foram: linearidade e sensibilidade, obtendo-se uma boa sensibilidade e resposta linear com coeficientes de 0,9998 no intervalo de 0,01 a 10 μg mL-1; precisão com base nos estudos de repetibilidade (intradia) e precisão intermediária (interdia), obtendo-se resultados de 0,1–1%, 0,6–1%, respectivamente; exatidão com valores de recuperação entre 60 ± 37% – 117 ± 3%, para os níveis de concentração 0,025 a 0,1 μg mL-1 e 75 ± 9% – 119 ± 12% para os níveis 0,5 a 1 μg mL-1, com relação ao C18 e o biocarvão, respectivamente. O LD no intervalo de 0,01–0,025 e LQ 0,025-0,5 μg mL-1. O método desenvolvido se mostrou adequado para determinação de agrotóxicos em amostras de água.

Neste trabalho, os anticorpos policlonais e monoclonais anti-fluoxetina foram produzidos em coelhos e camundongos, respectivamente, por imunização com o conjugado fluoxetina-soroalbumina bovina. Os anticorpos obtidos foram caracterizados em função da especificidade contra o fármaco por ELISA (enzyme linked immunosorbent assay) e posteriormente, purificados por afinidade em coluna fluoxetina-agarose labmade. Os anticorpos purificados foram imobilizados covalentemente na superfície vítrea das barras SBSE (extração sortiva em barra de agitação) labmade. Após a derivatização das barras com 3-aminopropiltrietoxisilano, dois métodos distintos de acoplamento dos anticorpos às barras SBSE foram avaliados: ativação com glutaraldeído e succinilação seguida de ativação via éster N-hidroxisuccinimida (NHS). A funcionalização das barras SBSE foi comprovada através da imobilização de enzima peroxidase (HRP) em lugar do anticorpo e posterior ensaio enzimático com as barras. Várias barras SBSE com diferentes áreas (1,2; 2,4; e 4,0 cm2) foram preparadas, dentre as quais, as com maior área imunosorvente apresentaram maiores taxas de recuperação do fármaco. A avaliação da morfologia da superfície da barra SBSE imunosorvente foi realizada através de Microscopia Eletrônica de Varredura (MEV). As variáveis do processo SBSE de imunoafinidade foram otimizadas para estabelecer o equilíbrio de sorção antígeno-anticorpo em um menor tempo de análise e obtenção de limite de quantificação compatível com o intervalo terapêutico do fármaco. As capacidades adsortivas das barras imunosorventes foram de 1,2 e 8 microgramas por cm2 para anticorpos policlonais e monoclonais, respectivamente. Os imunosorventes desenvolvidos apresentaram reatividade-cruzada apenas com norfluoxetina (metabólito ativo de fluoxetina). As barras imunosorventes foram reutilizadas aproximadamente 30 vezes, sem perda significativa da eficiência das extrações. Baseados nos parâmetros de validação analítica avaliados, os métodos de SBSE/LC-FD de imunoafinidade desenvolvidos são adequados para a determinação de fluoxetina em amostras de plasma de pacientes em terapia com o fármaco, para fins de monitorização terapêutica. Por conseguinte, esses métodos foram aplicados com êxito para análises de amostras de plasma de pacientes idosos em terapia com Prozac®. Neste trabalho, o método MEPS (microextração em sorvente empacotado)/LC-UV também foi desenvolvido e validado para análise simultânea de sertralina, paroxetina, citalopram, fluoxetina e mirtazapina em amostras de plasma para fins de monitorização terapêutica. As variáveis do processo MEPS foram otimizadas (pH e volume da amostra, força iônica, volume dos ciclos aspirar-dispensar e condições de dessorção) para estabelecer o equilíbrio de sorção em menor tempo de análise e obter sensibilidade analítica adequada para a determinação dos antidepressivos no intervalo terapêutico. O método MEPS/LC-UV desenvolvido permitiu integração da dessorção dos analitos e injeção da amostra no sistema cromatográfico (LC-UV) em uma única etapa, usando a microsseringa de extração MEPS. A fase extratora MEPS, M1 (C8/SCX), foi reutilizada mais de 50 vezes com perda mínima da eficiência da extração, comprovando a robustez do material sorvente. Segundo os parâmetros de validação analítica avaliados, o método MEPS/LC-UV desenvolvido é adequado para a determinação de antidepressivos em amostras de plasma para fins de monitorização terapêutica. / In this work, polyclonal and monoclonal anti-fluoxetine antibodies were developed in rabbits and mice by immunization with fluoxetine-bovine albumin conjugate, respectively. The developed antibodies were characterized on the basis of the specificity against the drug by ELISA (enzyme linked immunosorbent assay) and, subsequently they were purified by labmade fluoxetine-agarose affinity column. The purified antibodies were covalently immobilized onto the glass surface of labmade SBSE (stir bar sorptive extraction) bars. After derivatization of the bars with 3-aminopropyltriethoxysilane, two distinct methods were evaluated for the antibodies coupling to the SBSE bars: activation with glutaraldehyde and succinylation activation via ester N-hydroxysuccinimide (NHS). The functionalization of SBSE bars was confirmed by the immobilization of peroxidase (HRP) instead of the antibody and, subsequent enzymatic assay with the bars. Several SBSE bars with different areas (1.2, 2.4, and 4.0 cm2) were prepared, among of them the largest immunosorbent area showed higher recovery rates of the drug. The evaluation of surface morphology of the SBSE immunosorbent bar was performed using scanning electron microscopy (SEM). The SBSE immunoaffinity variables were optimized to establish sorption equilibrium of antigen-antibody in a short time analysis and to obtain the limit of quantification compatible with the therapeutic range of the drug. The adsorptive capacities of the immunosorbent bars were 1.2 and 8 micrograms per cm2 for polyclonal and monoclonal antibodies, respectively. The developed immunosorbents showed cross-reactivity only with norfluoxetine (active metabolite of fluoxetine). The immunosorbent bars were reused approximately 30 times without significant loss of the extraction efficiency. Based on evaluated analytical validation parameters, the developed immunoaffinity SBSE/LC-FD methods are suitable for the determination of fluoxetine in plasma samples from patients on therapy with the antidepressant for therapeutic drug monitoring. Therefore, these methods were successfully applied for the analysis of plasma samples from elderly patients undergoing therapy with Prozac®. In this work, the method MEPS (microextraction by packed sorbent)/ LC-UV was also developed and validated for the simultaneous analysis of sertraline, paroxetine, citalopram, fluoxetine and mirtazapine in plasma samples for therapeutic drug monitoring. The MEPS process variables were optimized (pH, sample volume, ionic strength, draw-eject cycles volume and desorption conditions) to establish the sorption equilibrium in a short time analysis and to obtain adequate analytical sensitivity for determination of antidepressants within therapeutic range. The developed MEPS/LC-UV method allowed integration of the analytes desorption and sample injection in the chromatographic system (LC-UV) in a single step, using a MEPS extraction microsyringe. The MEPS extraction phase, M1 (C8/SCX) was reused over 50 times with minimum loss of extraction efficiency, proving the robustness of the sorbent material. According to the evaluated analytical validation parameters, the developed MEPS/LC-UV method is suitable for the determination of antidepressants in plasma samples for therapeutic drug monitoring.

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В магистерской диссертации представлена методология пошагового синтеза композиционного сорбента на основе катионообменника и гидроксида титана (IV). Показаны результаты сорбции меди (II) и других тяжелых металлов синтезированным композиционным сорбентом. Для математического моделирования результатов сорбции были использованы изотермы Ленгмюра, Фрейндлиха и Темкина. Установлено, что модель Ленгмюра наиболее точно описывает сорбционный процесс. Определены константы модели Ленгмюра и площадь удельной поверхности композиционного сорбента. Гранулы композиционного сорбента изучены с помощью методов сканирующей электронной микроскопии (СЭМ) и энергодисперсионного микроанализа (ЭДМА). Вычислены коэффициенты распределения меди (II) в гранулах композиционного сорбента и степень сорбции меди (II) из водных растворов CuSO4 различной концентрации. / The methodology of stepwise synthesis of the composite sorbent based on cation exchanger and tin(IV) hydroxide was demonstrated. The sorption results of copper(II) and other heavy metals onto the composite sorbent are presented. Langmuir, Freundlich and Temkin adsorption isotherms were used in mathematical modeling of the sorption data. The Langmuir model most accurately describes the sorption process. The constants of the Langmuir model and the specific surface area of the composite sorbent were defined. Granules of the composite sorbent were studied by scanning electron microscopy (SEM) and energy-dispersive X-ray microanalysis (EDXMA). The distribution coefficients of copper(II) in the composite sorbent and the sorption degree from CuSO4 aqueous solutions of various concentrations were computed.

Abstract in English / Incineration is still a widely utilised method for treating healthcare risk waste in the Republic of South Africa. As much as incinerators are needed, the fact that they are still a critical source of hazardous toxic air pollutants that are not easy to manage cannot be disregarded. The Ministry of Environmental Affairs has promulgated a new regulation for General and Hazardous Waste Thermal Treatment. This exceedingly stringent air pollution legislation requires that existing incinerators be modified or redesigned to meet the new air quality standards, or face closure in the event that they fail to comply. The regulation contains strict emission requirements for concentrations of stack gases such as CO2, NO2, NOx, HCl, HF, CO, SO2, as well as TOC and PM. To be certain that emissions are within the standard, incineration facilities are instructed to reduce the acid gas emissions and to have permanent on-line monitoring equipment for stack testing of regulated pollutants. Since the promulgation of the new legislation in April 2015, none of the incinerators in South Africa has been able to achieve the new requirements. This study, based on the quantitative approach, was conducted in search of a cost-effective method of controlling acid gas emissions from incinerators without major adjustments to the plants. During the study, 60 kg of sorbacal Ca(OH)2 was injected into a lime feeder every day. A variable speed drive was used to inject Ca(OH)2 into the furnace continuously at a rate of between 2.5 kg/h and 3.5 kg/h. The temperature was maintained between 850°C and 1200°C with the use of four gas burners. Two manual blowers were utilised to ensure a continuous flow of Ca(OH)2 into the reaction chamber and filtration system. Comparative analysis was done to compare gas emission levels before and after the use of hydrated lime. Descriptive statistics were used to compute the mean, frequency and percentages, while Wilcoxon sign rank test established whether hydrated lime was significant in reducing gaseous emissions or not. Wilcoxon sign rank test showed a statistically significant difference (P<0.05) in the reduction of all gaseous emissions using hydrated lime, except particulate matter where there was a significant increase in emissions. This technology was able to achieve high removal efficiency of 97% for HCl, 86% for HF, 83% for NOx, 87% for SO2 and 74% for NO2. The optimum temperature for SO2 and NOx was 1020°C. For HCl it was between 1190°C and 1200°C, and for NO2 it was between 1120°C and 1200°C. The amount of particulate matter increased along with the concentration of the Ca(OH)2 injections. Ca(OH)2 was found to be cost effective in the controlling and capturing of gaseous emissions. It is recommended that combustion requirements, such as heat, oxygen and turbulence, be considered to reduce the amount of gases generated during the incineration of healthcare risk waste. It is also recommended that electrostatic precipitators be used instead of fabric filters to improve the efficiency of capturing the particulate matter. / Environmental Sciences / M.Sc. (Environmental Science)

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