This research was designed to investigate the effect of cations on activated sludge characteristics and also to determine their influence on digestion performance. For this purpose, cations in solution and in floc were evaluated along with various activated sludge characteristics and the collected waste activated sludge underwent both anaerobic and aerobic digestion. It was found that large amounts of biopolymer (protein + polysaccharide) remained in the effluent of WWTP that received high influent sodium but had low iron and aluminum in floc. However, sludges from plants with high sodium and high iron and aluminum dewatered well and produced high quality effluents, suggesting that iron and aluminum have significant positive effects on floc properties. Following anaerobic digestion, a significant increase in solution protein occurred and correlations between solution protein, ammonium production, percentile volatile solids reduction and iron in floc were obtained. These data indicate that iron-linked protein is released to solution when iron is reduced and its degradation is responsible for volatile solids reduction in anaerobic digestion. In aerobic digestion, polysaccharide in solution increased along with calcium, magnesium and inorganic nitrogen. This implies that divalent cation-bound biopolymer might be the primary organic fraction that is degraded under aerobic digestion. Combined (anaerobic/aerobic) digestion was performed and produced further volatile solids destruction with discrete cation and biopolymer response during each phase of digestion. These results support the theory that two types of organic matter with different cation bindings are present in floc and each type is degraded under different digestion processes. / Master of Science

De nos jours, les cultures mixtes sont considérées comme une sérieuse alternative aux cultures pures pour les procédés de biotechnologie. En effet, les cultures mixtes peuvent fonctionner en réacteur continu, dans des conditions non-stériles et traiter une grande variété de substrats organiques. La principale restriction de l'utilisation de ces bioprocédés en cultures mixtes réside dans leur instabilité liée à la présence de voies métaboliques non désirées résultant d'interactions microbiennes complexes. Notamment, le rôle des bactéries de faible abondance reste à être élucidé. Ce travail a donc consisté, dans un premier temps à déterminer le rôle des bactéries minoritaires dans la production d'hydrogène par voie fermentaire en utilisant un chémostat alimenté en continu avec un milieu à base de glucose. Sept inocula ont été cultivés dans les mêmes conditions opératoires. De façon remarquable, Clostridium pasteurianum a été retrouvé comme espèce dominante de l'écosystème six fois sur sept. Seules la nature et la diversité des espèces minoritaires variaient d'un écosystème à l'autre. Ainsi, il a été montré que la structure des communautés microbiennes a une influence significative sur la production de bio-hydrogène. Au sein de ces communautés, les bactéries en proportion minoritaires jouent un rôle clé en orientant le métabolisme globale de l'écosystème. La deuxième étape de ce travail a consisté à utiliser certaines de ces espèces minoritaires comme Ingénieurs Ecologiques des Ecosystèmes microbiens (IEEM). Pour cela, la structure d'une communauté microbienne productrice d'hydrogène a été modifiée artificiellement en introduisant des souches bactériennes exogènes aux fonctions redondantes et/ou complémentaires des souches indigènes. Les résultats en réacteur batch ont montré que les performances de production d'hydrogène pouvaient être améliorées jusqu'à un facteur 3,5 par l'ajout de certaines souches. Dans l'ensemble, les résultats obtenus ne peuvent être expliqués par de simples interactions trophiques et suggèrent la présence de mécanismes d'interactions de coopération entre microorganismes. De plus, sous des conditions opératoires plus favorables (inoculum, milieu), l'insertion de certaines espèces minoritaires a permis plutôt de stabiliser le métabolisme de l'écosystème microbien sans pour autant en affecter favorablement la production d'hydrogène. Dans tous les cas, les interactions compétitives n'ont pas été favorables à la production d'hydrogène. Enfin, des essais en réacteur continu ont montré que le mode d'implantation des souches peut être un facteur primordial pour l'utilisation d'IEEM. En conclusion, ce travail a montré la potentialité d'utiliser des bactéries exogènes, en proportions minoritaires, comme facteurs biotiques pour stabiliser et/ou orienter les métabolismes microbiens vers des fonctions d'intérêt au sein des cultures mixtes microbiennes. / Nowadays mixed cultures are considered as a serious alternative to pure cultures in biotechnological processes. Mixed cultures can be operated continuously, under unsterile conditions and from various organic substrates. One of the most constraints remains the chronic instability of the mixed culture processes due to the presence of unwanted metabolic pathways resulting from complex microbial interactions. More particularly the role of bacteria in low abundance remains to be elucidated. Therefore this work consisted initially to determine the contribution of sub-dominant bacteria to fermentative hydrogen production using a chemostat continuously fed with a glucose-based medium. Seven inocula were grown under the same operating conditions. Interestingly, Clostridium pasteurianum was found as dominant in six assays on seven at steady state. Only the minority bacterial population differed with regards to their identity and diversity. Acting as true keystone species, these minority bacteria impacted substantially the metabolic network of the overall ecosystem despite their low abundance. In a second step, this work consisted in using some of these minority species as Ecological Engineers of Microbial Ecosystem (EEME). In order to study this aspect, the structure of a hydrogen-producing microbial community has been artificially modified by adding exogenous bacterial strains with redundant functions and/or complementary native strains. Results in batch reactors have shown that the hydrogen production performances could be improved to a 3.5 factor by the addition of certain strains. Results obtained can not be explained by simple trophic interactions and suggest the presence of interaction mechanism of cooperation among microorganisms. Moreover, under more favourable operating conditions (inoculum, culture medium), the addition of certain species in low abundance could stabilize the metabolism of microbial ecosystem without necessarily favourably affect the hydrogen production. In all cases, competitive interactions were not favourable for hydrogen production. Trials were then realised in continuous reactors. These trials have shown that the method used to implant strains in reactors could be a key factor for using the EEME.As a conclusion, this study has shown the potential to use exogenous bacteria, in minority proportions, as biotic factors to stabilised and/or guides microbial metabolisms to functions of interest within microbial mixed cultures.

Dans le futur, différentes sources d'énergies renouvelables comme les énergies de seconde génération produites à partir de déchets lignocellulosiques seront nécessaires pour palier à l'épuisement des énergies fossiles. Parmi ces énergies de seconde génération, le biohydrogène, le méthane et l'hythane produits à partir de procédés fermentaires anaérobies représentent des alternatives prometteuses. Cependant la production de biohydrogène et de méthane à partir de résidus lignocellulosiques est limitée par leurs structures récalcitrantes et une étape de prétraitement en amont des procédés fermentaires est souvent nécessaire. Ce travail a pour but d'étudier l'impact des facteurs biochimiques et structurels des résidus lignocellulosiques sur les performances de production d'hydrogène et de méthane, pour pouvoir par la suite développer des stratégies de prétaitements adaptées. Tout d'abord, sur un panel de vingt substrats lignocellulosiques, les potentiels hydrogène et méthane ont été corrélés aux paramètres biochimiques et structurels. Les résultats ont mis en évidence que le potentiel hydrogène est uniquement corrélé positivement à la teneur en sucres solubles. La production de méthane quant à elle est négativement corrélée à la teneur en lignine et, à un moindre degré, à la cristallinité de la cellulose, mais positivement à la teneur en sucres solubles, holocelluloses amorphes et protéines. Par la suite, des stratégies de prétraitements ont été établies pour améliorer la production d'hydrogène et de méthane. Le couplage prétaitements alcalins/enzymatique ainsi que les prétraitements à l'acide dilué, efficaces pour solubiliser les holocelluloses en sucres solubles ont été appliqués en amont de la production d'hydrogène. En combinant le pretraitement alcalin avec une hydrolyse enzymatique, le potentiel hydrogène des tiges de tournesol fut multiplié par quinze. En revanche, suite aux prétraitements acides, la production d'hydrogène fut inhibée à cause de la libération de sous-produits (furfural, 5-HMF et composés phénoliques) engendrant un changement d'espèces bactériennes vers des espèces non productrices d'hydrogène. Pour la production de méthane, cinq prétraitements thermo-chimiques (NaOH, H2O2, Ca(OH)2, HCl and FeCl3) efficaces pour délignifier ou solubiliser les holocelluloses ont été étudiés. Parmi ces prétraitements, la meilleure condition fut 55°C à une concentration de 4% NaOH pendant 24 h, résulant en une augmentation du potentiel méthane variant de 29 à 44 % en fonction des tiges de tournesol. Cette condition fut par la suite validée en réacteurs anaérobies continusavec une augmentation de 26.5% de la production de méthane. Un procédé à deux étages couplant la production d'hydrogène en batch suivi de la production de méthane en continu fut aussi étudié. Néanmoins, aucune différence significative en termes d'énergie produite ne fut observée entre les procédés à deux étages (H2/CH4) et à un étage (CH4). / In the future, various forms of renewable energy, such as second generation biofuels from lignocellulosic residues, will be required to replace fossil fuels. Among these, biohydrogen and methane produced through fermentative processes appear as interesting candidates. However, biohydrogen and/or methane production of lignocellulosic residues is often limited by the recalcitrant structure and a pretreatment step prior to fermentative processes is often required. Up to date, informations on lignocellulosic characteristics limiting both hydrogen and methane production are limited.Therefore, this work aims to investigate the effect of compositional and structural features of lignocellulosic residues on biohydrogen and methane performances for further developping appropriate pretreatments strategies. Firstly, a panel of twenty lignocellulosic residues was used to correlate both hydrogen and methane potentials with the compositional and structural characteristics. The results showed that hydrogen potential positively correlated with soluble carbohydrates only. Secondly, methane potential correlated negatively with lignin content and, in a lesser extent, with crystalline cellulose, but positively with the soluble carbohydrates, amorphous holocelluloses and protein contents. Pretreatments strategies were further developed to enhance both hydrogen and methane production of sunflower stalks. Dilute-acid and combined alkaline-enzymatic pretreatments, which were found efficient in solubilizing holocelluloses into soluble carbohydrates, were applied prior to biohydrogen potential tests. By combined alkaline-enzymatic pretreatment, hydrogen potential was fifteen times more than that of untreated samples. On the contrary, hydrogen production was inhibited after dilute-acid pretreatments due to the release of byproducts (furfural, 5-HMF and phenolic compounds) that led to microbial communities shift toward no hydrogen producing bacteria. Similarly, methane production, five thermo-chemical pretreatments (NaOH, H2O2, Ca(OH)2, HCl and FeCl3) found efficient in delignification or solubilization of holocelluloses, were considered. Among these pretreatments, the best conditions were 55°C with 4% NaOH for 24 h and led to an increase of 29-44 % in methane potential of sunflower stalks. This pretreatment condition was validated in one stage anaerobic mesophilic continuous digester for methane production and was found efficient to enhance from 26.5% the total energy produced compared to one stage-CH4 alone. Two-stage H2 (batch) / CH4 (continuous) process was also investigated. Nevertheless, in term of energy produced, no significant differences were observed between one-stage CH4 and two-stage H2 /CH4.

Cette thèse porte sur la modélisation des réacteurs membranaires anaérobies. Dans une première partie, nous proposons une analyse mathématique générique d'un modèle de digestion anaérobie en deux étapes appelé AM2. La principale limitation du développement des réacteurs membranaires étant le risque de colmatage, nous proposons, dans une seconde partie, d'étendre le modèle AM2 en incorporant une nouvelle variable d'état modélisant la dynamique des Produits Microbiens Solubles (SMP) dont le rôle dans le colmatage des membranes a été démontré. Une étude mathématique exhaustive de ce nouveau modèle appelé AM2b est réalisée pour comprendre et comparer les comportements qualitatifs des deux modèles. Dépendant des conditions de fonctionnement et des valeurs des paramètres biologiques utilisées, nous montrons que ce nouveau modèle peut se comporter comme le modèle initial AM2, ou, au contraire, présenter un comportement qualitatif très différent. L'étape suivante sera d'utiliser ce modèle pour la synthèse de régulateurs. Toutefois, le manque de capteurs en-ligne nous a amené, dans une troisième partie, à procéder à la synthèse d'un certain nombre d'observateurs d'état classiques. Au regard des caractéristiques spécifiques des bioprocédés, cette dernière partie se termine par la proposition de nouvelles pistes pour l'estimation d'état et de paramètres par des méthodes stochastiques, notamment les filtres particulaires dont nous présentons brièvement le principe. / This thesis focuses on the modeling of anaerobic membrane reactors. In the first part, we propose a generic mathematical analysis of a two-step model of the anaerobic digestion called AM2. The main limitation in the development of membrane reactors being the risk of clogging, we propose in a second part, to extend the AM2 model by incorporating a new state variable modeling the dynamics of the so-called Soluble Microbial Products (SMP) whose role in the clogging of the membranes has been demonstrated. A complete mathematical study of this new model called AM2b is realized to understand and compare the behavior of both models. Depending on operating conditions and on the model parameters values, we show that this new model can behave as the initial model AM2, or, conversely, have a completely different qualitative behavior. The next step is to use this model for the synthesis of controllers. However, the lack of online sensors led us to a third part where we carry out the synthesis of several state observers. In view of the specific characteristics of bioprocesses, this last part ends by proposing new ways to estimate both state and parameters using stochastic methods, including particulate filters which the concepts are briefly reviewed.

La digestion anaérobie est un processus de transformation de la matière organique en biogaz riche en méthane. Les déchets solides sont le plus souvent traités par une technologie par voie sèche qui est caractérisée par des teneurs en matières sèches supérieures à 20%. Du fait de la faible teneur en eau, la digestion sèche présente de nombreuses inconnus scientifiques, tant au niveau microbiologique et physico-chimique. Le but de cette thèse est de comprendre l'influence des parametres opératoires spécifiques à la digestion anaérobie par voie sèche sur les performances et le comportement des communautés microbiennes de ce processus. Les résultats obtenus montrent que l'augmentation de la teneur en matières sèches au-delà de 30% et la diminution de la surface spécifique d'échange ont un effet négatif sur le processus de digestion anaérobie. En effet lorsque la teneur en matière sèche est supérieure à 30%, le transfert des gaz dissous du milieu réactionnel vers le ciel gazeux peut limiter la méthanisation. L'analyse des populations microbiennes montre la présence de bio-indicateurs bactériens liés au non fonctionnement de la digestion anaérobie. Ces bio-indicateurs sont des clostridium et sont présents quel que soit l'inoculum utilisé. L'étude des populations méthanogènes montre une sensibilité de ces microorganismes à leur environnement : des shifts de populations méthanogènes ont été observés en fonction de la concentration en matières sèches. Ce travail a permis d'accroître les connaissances dans le domaine de la digestion anaérobie sèche, ces connaissances pouvant contribuer à améliorer les performances des procédés. / Anaerobic digestion is the transformation of organic matter into biogas rich in methane. Solid waste is treated by dry anaerobic digestion process with a total solid content higher than 20%. The high solids content make the process difficult to control. The aim of this work is to study the influence of operating parameters specific to dry anaerobic digestion on performances and behavior of microbial communities. The results show that increasing the solids content higher than 30% and decreasing the specific surface area of change have a negative effect on the anaerobic digestion process. Indeed, when the solids content exceeds 30%, the transfer of dissolved gas from the reaction mixture to the headspace can limit anaerobic digestion. The analysis of microbial populations demonstrates the presence of bacterial bio-indicators related to no-functioning anaerobic digestion. These bio-indicators correspond to the clostridium genus and are present regardless of the inoculum source. The study of methanogenic Archaea shows a sensitivity of these microorganisms. Shifts in the methanogenic populations related to the concentration of total solids were observed. This work has improved the fundamental knowledge of dry anaerobic digestion which can help improve the performance of this process.

The controlled anaerobic digestion of organic waste in a biogas facility aggregates advantages of waste treatment, energy recovery and nutrient recycling and is a promising technology to deal with contemporary issues of waste management and energy recovery. Small-scale biogas production units can be simply designed and successfully operated even in settings where means for advanced technology equipment are low and institutional capacities limited. In the country of Lebanon, landfilling and open dumping of solid waste is common practice and anaerobic treatment of waste is applied only sporadically and hence, not well-established. The aim of this study was to assess the feasibility of small-scale biogas production using organic waste, explore options for its application and propose a business model on how feedstock sourcing, facility operation and end product utilization could be realized in the research area. Research area was Ghazir village, a community within the urbanized coastal area in Lebanon. Methods were of both quantitative and qualitative nature.A techno-economic assessment served to quantify biogas and liquid digestate production rates, based on available resources of organic waste in the research area. Costs associated with installation, operation and maintenance of the proposed facility have been projected based on present examples of similar facilities in the country. Interviews with local stakeholders and a questionnaire survey among residents in the area of research allowed to identify suitable end use options for the produced biogas and served to explore communal acceptance of local biogas production. Results show that the produced biogas can be used for thermal feedstock treatment to supply local farmers with a fertilizer alternative, i.e. the liquid digestate. Organic waste that is subject to the anaerobic treatment in a digester can be provided by multiple point sources, i.e. households and a local food market in the form of source-sorted kitchen waste and unsold fruits and vegetables, respectively. Due to the current unfamiliarity with anaerobic treatment of organic waste in the research area, tests on the effects on crop yields are advised to take place before implementation of the proposed business model, as its communal benefits hinge on the suitability of the liquid digestate as a fertilizer. Economic calculations show low investment costs for the proposed facility as well as acceptable annual revenues in case the liquid digestate proves to be of interest for commercial acquisition by local farmers. The used methods and strategies in this feasibility assessment, i.e. waste quantification, yield and cost calculations, stakeholder interviews and questionnaire survey allow for replication of the taken investigation to eventually initiate small-scale biogas production using organic waste in other settings with similar conditions.

Cette étude porte sur l’influence de différents traitements sur les caractéristiques et l’évolution de la matière organique de boues de stations d’épuration (Step). Les échantillons étudiés proviennent de 3 stations municipales de la Vienne. Le premier volet développé au cours de l’étude a pour but la mise au point d’une méthode d’analyse qualitative et quantitative des constituants des boues de Step. Les résultats obtenus démontrent le potentiel de la thermochimiolyse-GCMS à caractériser, sans extraction préalable, la matière organique d’un échantillon brut. Le deuxième volet de cette thèse s’est intéressé à l’influence de différents traitements (séchages, accélérateur d’électrons et méthanisation) sur l’évolution de la matière organique. Ainsi, le séchage thermique provoque une fragilisation de la matière organique, le séchage solaire une complexification et les lits plantés de roseaux n’ont pas d’influence significative à court terme. L’application du procédé d’oxydation avancé sur une boue flottée a provoqué une acidification et des changements structuraux de la matière organique. Ainsi une faible dose (1,25 kGy) a conduit à une complexification de la matière organique alors qu’une plus forte dose (50 kGy) semble la fragiliser. La modification de la matière organique à l’issue du procédé de méthanisation concerne uniquement la fraction lipidique et notamment des acides gras. / This study investigated the influence of different treatments on the characteristics and evolution of organic matter of municipal wastewater sludge. For this, three municipal wastewater treatment plants of Vienne department were sampled.The first phase developed during the study focused on the improvement of a method for qualitative and quantitative analysis of the sewage sludge’s constituents. The presented results demonstrate the strong potential of the thermochemolysis-GCMS to characterize, without extraction, the organic matter of a raw sample.The second part of this Ph.D has focused on the influence of various treatments (drying, electron beam and methanation) on the evolution of organic matter. Thus, the thermal drying causes weakening of the organic matter while the solar drying induces its complexification and reed beds induce no significant change. The application of an advanced oxidation process on a floated sludge caused acidification and structural changes of the organic matter. A low dose (1.25 kGy) led to more complex organic matter, while a higher dose (50 kGy) seems to weaken it. The changes in organic matter induced by anaerobic digestion mainly concerned the lipid fraction, in particular fatty acids.

Duas questões da sociedade do século XXI podem ser destacadas: a grande geração de resíduos; a carência por sistemas de tratamento adequado desses resíduos; e a crescente demanda por energia. A busca por alternativas para lidar com essas questões vem mobilizando os setores público e privado no sentido de explorar soluções ainda não praticadas na maior parte do mundo em desenvolvimento. A Política Nacional de Resíduos Sólidos (PNRS), instituída pela Lei nº 12.305/2010, estabeleceu um novo paradigma na gestão de resíduos sólidos no Brasil. Entre as mudanças apresentadas, uma das mais relevantes é a exclusividade de destinação de apenas rejeitos aos aterros sanitários, sendo os rejeitos entendidos como os resíduos que não mais apresentam possibilidade de tratamento. O cumprimento dessa lei irá requerer o estudo de alternativas de tratamento de resíduos gerados na fase anterior à sua disposição final. Entre as soluções possíveis está o seu aproveitamento energético, também previsto na PNRS. Nesse contexto, esta dissertação busca analisar duas tecnologias de tratamento de resíduos digestão anaeróbia e incineração e verificar suas respectivas viabilidades econômicas, tendo como objeto o cenário brasileiro, com foco especial no estado de São Paulo. Os resultados obtidos indicam que, respeitando-se as diretrizes da PNRS, entre os métodos de tratamento de resíduos sólidos urbanos analisadas, a digestão anaeróbia se mostrou mais viável do que a incineração para as regiões estudadas. Tais resultados tomaram como pressuposto que a PNRS é uma lei que deverá ser cumprida e exigida tal como se apresenta, e seu cumprimento implicará numa mudança significativa do modo como é feita a gestão de resíduos sólidos no país. Adicionalmente, as análises realizadas apontaram que, além dos aspectos econômicos, aspectos ambientais, sociais e culturais também são de fundamental importância na tomada de decisão por uma opção tecnológica adequada dos RSU. / Three issues of the XXI century society can be pointed out: The increasing volume of waste generation, the lack of adequate waste treatment systems and the increasing demand of energy. The search for alternatives to deal with these issues is calling the attention of both public and private agents who are engaged in exploring solutions not yet in place in most part of developing countries. The National Policy on Solid Waste (PNRS), established by the Law # 12,305/2010, set a new paradigm for the solid waste management in Brazil. Amongst the proposed changes, one of the most relevance is the destination of the so-called \"rejects\" to landfill, in which \"rejects\" stands for the residues that can no longer be processed. To abide by this law will require the analysis of alternatives for treating the residues prior to their final disposal. Amongst the possible solutions, there is the utilization of residues to generate electric energy. In this context, this master\'s thesis examines the two of the most used technologies in the developed world anaerobic digestion and incineration and evaluation their economic feasibility in the Brazilian scenario, particularly in the State of São Paulo. The analysis took as an assumption that the PNRS is a law that shall be enforced as it was stated, and that its compliance will require in a significant change in the way the solid waste management is done within the country. For the regions analyzed, our results showed that, under the PNRS requirements, the anaerobic digestion appeared to be more feasible than the incineration technology. Additionally, our work also indicates that, beyond the economic aspects, other issues such as environmental, social and cultural ones are fundamental for the decision making regarding the best technology applied in urban solid waste process.

Esse trabalho investigou a influência de diferentes origens e pré-tratamentos do inóculo na produção de biohidrogênio em reatores anaeróbios de leito fixo e fluxo ascendente. Aparas de polietileno de baixa densidade foram usadas como material suporte para fixação da biomassa e os reatores foram operados com 2 h de tempo de detenção hidráulica (TDH) e a 25ºC, alimentados com efluente sintético a base de sacarose. Duas fontes de inóculo foram estudadas: lodo anaeróbio de reator UASB aplicado ao tratamento de água residuária de abatedouro de aves (D) e lodo anaeróbio de reator UASB aplicado ao tratamento de água residuária de suinocultura (S); além da autofermentação (A), quando não há nenhum inóculo no reator. Além disso, dois tipos de pré-tratamento térmico (T) e ácido (A) foram avaliados. Os rendimentos de hidrogênio foram de 2,1, 2,0, 2,0,1,0, 1,0, 0,7, 0,7 mol \'H IND.2\' mol-1 sacarose quando os reatores foram inoculados com A, DT, DA, D, SA, ST e S, respectivamente. Nessa nomenclatura, a primeira letra se refere à origem do inóculo e a segunda, ao pré-tratamento. Embora hidrogênio (20-78%) e dióxido de carbono (21-55%) tenham sido os principais produtos no biogás, metano foi detectado nos reatores inoculados com D, DA, S, ST e SA no início e no final da operação. A produção volumétrica máxima de hidrogênio (61,6 mL \'H IND.2\' h-1.L-1) foi obtida quando DA foi usado com inóculo. Porém, o menor valor (15,1 mL \'H IND.2\' h-1.L-1) foi observado usando o inóculo S. Quando o reator não foi inoculado (A), a produção volumétrica de hidrogênio foi 47,3 mL \'H IND.2\' h-1.L-1. Etanol, ácido butírico e acético foram os principais produtos \'metabólicos detectados na fase líquida. Em resumo, os resultados demonstraram que há influência da origem e do pré-tratamento do inóculo em todos os parâmetros analisados. Inóculos sem pré-tratamento resultaram em menor rendimento de hidrogênio do que os observados nos experimentos com inóculos pré-tratados devido a seleção das bactérias produtoras de hidrogênio (BPH). Ademais, embora o pré-tratamento térmico tenha gerado os maiores valores de rendimento, o pré-tratamento ácido resultou em uma operação mais estável com os maiores valores médios. A autofermentação teve desempenho semelhante aos DT e DA e pode ser uma alternativa para a produção biológica de hidrogênio, pois seleciona as BPH naturalmente. / This paper investigated the influence of different inoculums and pretreatment of seed sludge on the biohydrogen production in up-flow anaerobic fixed-bed reactors. Particles of low-density polyethylene were used as support for biomass attachment and the reactor was operated with hydraulic retention time (HRT) of 2 h at 25ºC, fed with a sucrose-based synthetic wastewater. Two sources of inoculums were studied: anaerobic sludge from an UASB (up-flow anaerobic sludge blanket) reactor applied to treat poultry slaughterhouse wastewater (Sl) and anaerobic sludge from an UASB reactor treating swine wastewater (Sw), besides the autofermentation (A), with no inoculation of the reactor. In addition, two kinds of pretreatment heat (He) and acid (Ac) shock were evaluated. Hydrogen yields were 2.1, 2.0, 2.0,1.0, 1.0, 0.7, 0.7, mol \'H IND.2\' mol-1 sucrose when the reactors were inoculated with A, SlHe, SlAc, SwAc, Sl, Sw, and SwHe, respectively. In this nomenclature, the first two letters refer to source and the others refer to pretreatment. Although hydrogen (20-78%) and carbon dioxide (21-55%) have been the main gaseous products in the biogas, methane was detected in Sl, SlAc, Sw, SwHe and SwAc at the beginning and in the last days of the operation. Optimal \'H IND.2\' production rate (61.6 mL \'H IND.2\' h-1 L-1) was obtained when SlAc was used as seed sludge. On the other hand, the smallest value (15.1 mL \'H IND.2\' h-1 L-1) were observed using Sw inoculums. When the reactor was not inoculated (A), \'H IND.2\' production rate was 47.3 mL \'H IND.2\' h-1 L-1. Ethanol, butyric acid and acetic acid were the main soluble products detected in the liquid phase. In summary, the results have demonstrated that there are influences of the source and the pretreatment of the seed sludge in all parameters analyzed. Inoculums without pretreatment resulted in hydrogen productivity lower than those observed for experiments with pretreated inoculums due the selection of hydrogen producing bacteria (HPB). Furthermore, although the heat shock has generated the highest values of hydrogen yield, the acid-shock provided more stable operation with the highest average values. Besides, the autofermentation had almost the same performance than SlAc and SlHe and could be an alternative for biological hydrogen production due to natural selection of HPB.

Nesta tese foi estudada a influência da recirculação do percolado, ajustando as melhores taxas e freqüências, para degradação da fração orgânica dos resíduos sólidos urbanos, em sistema de batelada de uma e duas fases (híbrido). Foram utilizados reatores de 3,45 litros preenchidos com resíduo sólido urbano padrão (FORSUp), percolado como inóculo e um filtro anaeróbio como reator metanogênico. Foram testadas as taxas de recirculação do inóculo de 1%, 2,5%, 5%, 10%, 20%, 30% e 50% e seu monitoramento feito por análises físico-químicas e microbiológicas. O reator que apresentou melhores valores de produção de metano e redução de DQO foi aquele com taxa de recirculação de 20% do percolado metanogênico. Na segunda etapa foram operados três digestores de 50L, alimentados com a FORSUp com as melhores taxas de recirculação determinadas na primeira etapa desse trabalho e a obtida no trabalho de Salgado (2003). Um reator simulou o reator acidogênico de um sistema de duas fases, no qual 20% de seu inóculo foi injetado em um filtro anaeróbio (com tempo de detenção hidráulico de 24 horas). Um outro sistema com taxa de 10% de recirculação de percolado foi operado como reator de uma fase. Outro reator, inoculado com a mesma quantidade de FORSUp e percolado, porém, não se realizou qualquer recirculação do seu inóculo (controle), servindo para comparar os digestores de uma e duas fases. O sistema de duas fases, comparado aos demais reatores, confirmou que a taxa de recirculação de 20%, obteve maior eficiência na partida, com elevada produção de metano e maior percentual de degradação de sólidos. Os exames microscópicos realizados em amostras de percolado desses reatores revelaram predominância de organismos de morfologia com características de Methanococcus e Methanosarcina. Concluiu-se que a taxa de recirculação de percolado influi significativamente nos reatores degradando a matéria orgânica. O estudo cinético confirmou que o processo de digestão obedece a cinética das reações em série, com elevados valores de k´1 / This thesis studied the influence of the leachate recirculation, adjusting to the best rates and frequencies, for degradation of the organic fraction of the urban solid wastes, in one and two-phases (hybrid) system. Bioreactors of 3.45 L were used and filled out with OFMSW pattern, leachate as seed and an anaerobic filter as methanogenic reactor. The performance of the reactors was analyzed varying recirculation rates (1, 2.5, 5, 10, 20, 30 and 50 % in volume of seed). Leachate samples from these reactors were examined through microscopical examinations and physical-chemical analyses to evaluate its performance. The reactor with 20% recirculation rate, got larger efficiency in the departure, methane production and percentage of solid degradation, compared to the others reactors. In the second stage, three 50L digesters were operated and fed with standard OFMSW with the best recirculation rates of the first stage and the best rate obtained in Salgado (2003). A bioreactor simulated the acidogenic reactor of a two-phase system, in which 20% of its seed was injected in anaerobic filter (with hydraulic detention time of 24 hours). Another system, with 10% of recirculation rate of leachate was operated in a one-phase reactor. Once more bioreactor, inoculated like others, however, without any recirculation were studied to compare with one and two-phase reactor. The two-phase system confirmed that the 20% recirculation rate, compared to the others reactors, obtained better efficiency with high methane production and solid degradation. The microscopical examinations in the leachate samples from this reactor presented predominance of organisms with characteristical morphology from Methanococcus and Methanosarcina. It was concluded that the leachate recirculation has significant influence in the degradation of organic matter bioreactors. The kinetic study confirmed that the anaerobic process for OFMSW proceed the in series kinetics, with high constants values of first order