Dans le cadre de l’évaluation multicritère des systèmes en protection intégrée contre les adventices (PIC-Adventices), cette étude a eu pour objectif d’étudier l’impact de la combinaison de pratiques alternatives à l’usage d’herbicides sur les émissions de N2O par les sols. L’étude a été conduite sur quatre systèmes de culture, un système de référence en agriculture raisonnée (S1) et trois systèmes PIC-Adventices (S2, S3, S5), sur le site expérimental Dijon-Epoisses (47°20'N, 5°2'E). La mise en place de dispositifs de mesure à haute résolution, alliant la méthode des chambres d’accumulation de gaz en surface du sol aux analyses de gaz par infrarouge, a permis d’estimer l’intensité des émissions de N2O pour les sols argilo-calcaires caractéristiques de la plaine dijonnaise, avec des flux moyens compris entre -6 et 257 g N-N2O ha-1 jour-1. Cette intensité s’est avérée étroitement liée à certains paramètres environnementaux (température, part de porosité occupée par l’eau, teneur en azote), et certaines pratiques agricoles, induisant des différences significatives entre les systèmes. Les émissions de N2O ont notamment été affectées par le mode de gestion des sols et la nature des cultures constituant la succession de chaque système. L’absence de travail du sol depuis 2008 dans le système S2 s’est traduite par une amplification des émissions de N2O d’un facteur multiplicatif d’au moins six par rapport aux autres systèmes pour l’année 2012. Par ailleurs, ces émissions équivalentes à 0.7 t C-CO2 ha-1 pourraient avoir compensé la séquestration de carbone additionnelle induite par le travail réduit du sol pendant la période de mesure. De la même manière, la dégradation des résidus de culture légumineuse, dans les systèmes S3 et S5 ont respectivement stimulé les émissions de N2O en 2011 et en 2012, en comparaison avec le système de référence S1. Par ailleurs, le suivi mensuel de la taille des communautés microbiennes du sol a également permis de mettre en évidence une variabilité temporelle liée aux pratiques culturales (travail du sol, récolte), en plus de la variabilité saisonnière. En revanche, dans cette étude les variations de taille des communautés microbiennes nitrifiantes et dénitrifiantes ne sont pas apparues comme un facteur d’explication de la variabilité des émissions de N2O, quel que soit le système. Enfin, l’approche par la modélisation des émissions de N2O sur les quatre systèmes, à l’aide des modèles NOE et DNDC, a permis d’identifier les principaux facteurs de régulation de ces émissions. De surcroît, le modèle NOE a bien identifié le système de culture S2, sans travail du sol, comme étant le système le plus émetteur de N2O, conformément aux observations de terrain. Cette étude renforce donc la pertinence de la modélisation pour estimer et analyser les émissions de N2O dans différents systèmes de culture. / In the context of the multicriteria evaluation of Integrated Weed Management (IWM) cropping systems, our study highlights the impacts of the combination of alternative agricultural practices to herbicide reliance on N2O emissions from soils. The study was located at the INRA experimental site of Dijon-Epoisses (47 ° 20'N, 5 ° 2'E) and considered 4 cropping systems, a reference system designed to maximize financial returns (S1) and three IWM systems (S2, S3, S5). The setup of high resolution measuring devices, combining the non-steady state chamber method with infrared gas analysis, allowed to estimate the intensity of N2O emissions from the calcareous clay soil, which is specific of Dijon plain, with average fluxes laying between -6 and 257 g N2O-N ha-1 day-1. The intensity of fluxes was closely related to environmental parameters (temperature, water filled pore space, inorganic N amount) and particular agricultural practices, leading to significant differences between systems. N2O emissions were notably affected by soil management and nature of crops. The conversion of S2 system to no-till in 2008 increased the N2O emissions, fluxes being at least 6 times more important than those emitted by the other cropping systems, during the year 2012. Moreover, these emissions, equivalent to 0.7 ha-1 C-CO2 ha-1, could have offset the soil additional carbon sequestration induced by reduced tillage during the studying period. Similarly, the degradation of legume crop residues in the S3 and S5 systems respectively enhanced N2O emissions in 2011 and 2012, by comparison with the S1 reference system. Elsewhere, the monthly monitoring of the soil microbial communities sizes has also helped to highlight temporal variability induced by the agricultural practices (tillage, harvest) as well as the seasonal variability. However, in this study the fluctuations of nitrifying and denitrifying communities sizes observed did not explain the variability of N2O emissions, whatever the considered cropping system. Finally, the modeling of N2O emitted from the 4 cropping systems, using NOE and DNDC models, allowed to identify the mains factors regulating the emissions. In addition, the NOE model accurately identified the S2 system, without tillage, as the most N2O emitter, in accordance with field observations. Thus, our study reinforces the relevance of modeling to estimate and explain N2O emissions in different cropping systems.

Os processos de amonificação e nitrificação no solo são de fundamental importância para a disponibilidade de N-mineral às plantas. Recentemente, foi demonstrado que a cana-de-açúcar tem preferência na absorção de NH4 + à NO3 -, podendo apresentar maior produtividade quando fertilizada apenas com Namoniacal. Da mesma forma, estudos indicaram que gramíneas do gênero Brachiaria podem inibir a nitrificação no solo por meio da exsudação radicular de compostos denominados braquiolactanas. Portanto, é oportuno avaliar as taxas de amonificação (TAB) e nitrificação brutas (TNB) de N pela técnica da diluição do isótopo 15N em solos cultivados com cana-de-açúcar e braquiária. Devido à escassez de trabalhos voltados à estimativa da TAB e TNB em solos tropicais, adaptações na metodologia são requeridas. Objetivou-se, então, realizar ajustes nos protocolos para determinação da TAB e TNB, para, posteriormente, quantificar as referidas taxas em solos sob cultivo de cana-de-açúcar e de algumas espécies de gramíneas para pastagem. Primeiramente, avaliou-se o tempo necessário de agitação de amostras líquidas contendo um sistema de microdifusão para captura do N-mineral presente. Os resultados indicaram que a máxima recuperação isotópica de 15N-mineral e de N-15NH4 + ocorreu em 24 h de agitação. Em sequência foram avaliadas duas técnicas para recuperação do N-15NO3 - (eliminação prévia do N-NH4 + e diluição isotópica) presente em extratos de KCl contendo N-15NO3 - e 15N-mineral. Ambas foram eficientes, sendo recomendada técnica que preconiza a eliminação prévia do N-NH4 +, pela boa operacionalidade proporcionada. A última adaptação efetuada se refere à abundância de 15N no composto marcado a ser aplicado no solo, visto que em estudos com solos temperados, são utilizados compostos altamente enriquecidos no isótopo. Foi constatado que para solos tropicais (agricultáveis e cultivados com cana-de-açúcar, no caso) não há necessidade de alta marcação com 15N nos compostos. Por fim, foi quantificada a TAB e TNB de solos cultivados com cana-de-açúcar e pastagens, com as devidas adaptações metodológicas efetuadas. A TAB dos solos de cana-de-açúcar e pastagem foi superior à TNB. Os solos de pastagem cultivados unicamente com a espécie B. humidicola apresentaram alto conteúdo de N-NH4 + e valores extremamente baixos de N-NO3 - e TNB, indicando inibição biológica da nitrificação. A ação inibitória da nitrificação em solos com ocupação de B. humidicola pode ser uma estratégia interessante para o plantio de cana-de-açúcar, com base na hipótese de preferência de absorção por NH4 + à NO3 - pela cultura. / The ammonification and nitrification processes of soils are of fundamental importance because they release mineral N to the plants. It was recently shown that sugarcane has a preference to uptake NH4 + instead of NO3 -, and may have higher yield when is fertilized with only NH4 +-N. Similarly, studies indicated that some Brachiaria species can inhibit soil nitrification through root exudation of free fatty acids. Therefore, it is appropriate to assess the gross rates of ammonification (GRA) and gross nitrification (GRN) by 15N pool dilution technique Therefore, it is appropriate to assess the gross rates of ammonification (GRA) and gross nitrification (GRN) by the 15N pool dilution technique in soils cropped with sugarcane and pasture. Due to the lack of studies related to the estimate of GRA and GRN in tropical soils, adjustments in methodology are required. Thus, the objectives were to perform some adjustments in the protocols of GRA and GRN to subsequently quantify such rates in soils under sugarcane and some pasture grasses. First, it was assessed the time needed for shaking liquid samples containing a microdiffusion system to capture the mineral N present. Results indicate that the maximum isotopic recovery of 15NH4 +-N and mineral-15N occurred within 24 h of shaking. Following, two methods of recovery the added 15NO3 --N (prior removal of NH4 +-N and isotope dilution procedure) to samples containing KCl were tested. Both methods were effective, but the technique that advocates removal of NH4 +-N is recommended, due to the good operability. The last adjustment made refers to the 15N abundance of labelled compound, since studies with temperate soils usually use highly enriched compounds in the isotope. It was observed that for tropical soils (arable and under sugarcane, in this case) there is no need to use highly enriched 15N-coumpounds. Finally, GRA and GRN were quantified in soils under sugarcane and pasture, applying the adjustments previously made. GRA in soils from sugarcane and pasture was higher compared to GRN. The soils under B. humidicola showed high content of NH4 +-N and extremely low values of NO3 --N and GRN, indicating biological nitrification inhibition. Nitrification inhibition in soils occupied by B. humidicola may be an interesting strategy for sugarcane planting, on the assumption of preference to uptake NH4 + rather than NO3 - in this crop.

Il est de plus en plus admis que pour comprendre le fonctionnement des écosystèmes, une approche aérienne associée à une approche souterraine est nécessaire en raison des rétroactions entre plantes et sol. La structure des communautés végétales peut affecter le fonctionnement du sol en altérant la quantité et la qualité des ressources intégrant le sol. Les contrôles abiotiques des processus microbiens du sol sont largement documentés, mais les potentiels effets de la composition de la communauté végétale et des traits racinaires sont peu connus. L'étude a été menée sur des prairies méditerranéennes du sud de la France. Nous avons sélectionné 12 communautés contrastées le long d'un gradient de disponibilité des ressources du sol principalement lié à la texture du sol. Les objectifs de cette thèse sont d'évaluer i) la réponse de la composition floristique et des traits foliaires et racinaires mesurés au niveau de la communauté le long gradient édaphique et à travers les saisons, et ii) leurs effets sur trois processus microbiens du sol impliqués dans les cycles du carbone (C) et de l'azote (N) : la respiration potentielle (SIR), la nitrification (NEA) et la dénitrification (DEA). Dans les sols sableux (parcelles peu productives), la communauté végétale possède une stratégie de conservation au niveau des feuilles et une stratégie d'acquisition des ressources au niveau des racines suggérant une forte plasticité des traits racinaires en réponse à la limitation des ressources ; les taux de SIR et NEA sont élevés. Un patron opposé est observé dans les sols argileux des milieux productifs. La DEA ne varie pas le long du gradient. Aucun effet de la richesse spécifique, de l'équitabilité ou de la biomasse végétale sur la SIR ou la NEA n'a été trouvé. Cependant, nous avons démontré qu'il y a une forte influence de la composition fonctionnelle des communautés végétales (abondance des graminoïdes), et surtout des traits racinaires. Nos résultats les plus novateurs montrent que la NEA et dans une moindre mesure la SIR sont positivement corrélés à la concentration en N des racines de la communauté et négativement corrélés à leur ratio C/N, tandis que les traits foliaires analogues ont seulement un effet mineur sur les activités microbiennes. Ces résultats suggèrent que la qualité chimique des racines est le principal pilote des activités du sol et que cela est maintenu à travers les saisons. D'importantes variations saisonnières de la composition floristique des communautés, de leurs traits racinaires et des activités microbiennes, excepté la DEA, ont été mises en avant. Les variations saisonnières des traits racinaires sont interprétées comme un changement relatif de la proportion de racines jeunes/vieilles et suggèrent une asynchronie entre la croissance aérienne et souterraine. Pour la première fois, nous montrons qu'en conditions naturelles, les changements saisonniers des traits fonctionnels racinaires peuvent être impliqués dans le pilotage de la NEA et de la SIR. Ce résultat démontre la nécessité d'études plus approfondies pour comprendre le rôle des traits racinaires comme pilote du fonctionnement du sol. / It is increasingly recognized that the understanding of ecosystem functioning requires a combined above- and belowground approach, because of the importance of feedbacks between plants and soil. Plant community structure may affect soil functioning by altering the quantity and the quality of resources entering the soil. Abiotic controls on soil microbial processes are well documented, but potential effects of plant composition and root traits are poorly understood. The study was conducted in Mediterranean grasslands located in southern France. We selected 12 contrasting communities along a gradient of soil resource availability, which is mainly driven by soil texture. The aims of the thesis were to evaluate: i) the response of plant composition and leaf and root traits measured at the community level along the soil gradient and across seasons, ii) their effect on three soil microbial processes involved in carbon (C) and nitrogen (N) cycling, i.e. substrate-induced respiration (SIR), nitrifying (NEA) and denitrifying enzyme activities (DEA). In sandy soils (unproductive plots) plant communities had a conservation strategy at the leaf level and an acquisitive strategy at the root level suggesting a strong plasticity of root traits in response to resource limitation; rates of SIR and NEA were higher. Opposite pattern was observed in clay productive soils. DEA did not vary along the gradient. We did not find evidence of a species richness, evenness, or plant biomass effect on SIR and NEA. However, we demonstrated that they were strongly influenced by plant functional composition (abundance of graminoids), and particularly by root traits. Our most innovative finding evidences that NEA, and to a lesser extent SIR, were positively correlated with root nitrogen (N) concentration and negatively correlated with C/Ncom, whereas analogous leaf traits have only minor effect on microbial activities. Our results suggested that the chemical quality of roots is the main driver of soil activities and this was confirmed across the seasons. We highlight strong seasonal variations in plant community composition, root traits and soil microbial activity, except DEA. Seasonal variations in root traits were interpreted as a relative change in the proportion of young versus old roots and suggested an asynchrony between above– and belowground growth. We showed for the first time evidences that in natural conditions, seasonal changes in root functional traits could be implicated in driving NEA and SIR. This result demonstrates the need to further develop studies allowing a better understanding of the role of root traits as soil functioning drivers.

Made available in DSpace on 2017-07-10T19:24:42Z (GMT). No. of bitstreams: 1 Juliana Bortoli Rodrigues Mees.pdf: 1255432 bytes, checksum: bf00dbf45cce28fdbe504091e6363048 (MD5) Previous issue date: 2010-02-01 / Agro-industries stand out as large polluters in Brazil, particularly because of the large amounts of waste rich in organic substances, nutrients (especially nitrogen and phosphorus), solids, oils and greases. In this category, slaughterhouses and bird cold storage processing plants are known for their high pollution potential. The removal of nitrogen from wastewater is usually accomplished using biological conventional processes, by nitrification plus denitrification, involving aerobic and anaerobic phases that are generally carried out in separate reactors or by different aeration intervals. The sequencing batch reactor (SBR) uses multiple steps in the same reactor, which include filling, reaction, settling, withdrawal and idling. This study aimed to investigate how carbon:nitrogen ratios (COD/NO2 --N+NO3 --N) 3, 6 and 9, adjusted by manipueira (wastewater from cassava industry) and cycle time (CT) of 8,12 and 16 hours affects the nitrogen and organic matter removal from poultry wastewater, operating a sequencing batch reactor containing suspended biomass, in two different conditions: condition I, with the reaction step consisted by aerobic/anoxic phases and condition II, anoxic I/aerobic/anoxic II phases. It was also intended to optimize and validate the process of nitrogen removal in this type of effluent, to evaluate the reactor stability using Shewhart control charts for individual measures, and to study the kinetics behavior of organic matter (COD) and nitrogen (NH4 +-N, NO2 --N and NO3 --N) degradation. The conditions I and II were evaluated through factorial planning (32) and, in order to optimize the conditions obtained with the initial factorial design, it was used a central composite rotational design (CCRD) with four assays in levels -1 and +1, four assays on the axial points levels (-1.414 and +1.414) and five replicates at the central point (0). The nitrification process performance was evaluated by the efficiency of ammonia nitrogen removal (%), the pre-denitrification and denitrification processes by the efficiencies of nitrite and nitrate removal (%) and the whole process by total inorganic nitrogen removal (%). During the nitrification and denitrification processes, parameters like temperature, pH, alkalinity, redox potential, salinity and conductivity were monitored. The highest removal percentages of total inorganic nitrogen were obtained, for conditions I and II, at the cycle time range between 12 and 16 hours and the C/N ratio of 3 to 6, which showed average efficiencies of 80.76 and 85.57% in condition I, and 90.99 and 91.09% in condition II, respectively. Although the condition II obtained a higher removal percentage of total inorganic nitrogen, only condition I presented a regression statistically significant and predictive, with Fcal/Ftab values higher than 4 for all steps involved in nitrogen removal. Optimizing the condition I, the highest percentages of nitrogen removal were achieved with the cycle time of 16 hours and C/N ratio of 6, validated experimentally, achieving an overall removal of inorganic nitrogen of 85.83±0.87 %. Evaluating the reactor stability, the results of the 20 trials carried out with optimum conditions showed a total inorganic nitrogen average removal of 84.32±1.59% (CV=1.89%) and organic matter removal of 53.65±8.48% (CV=15.81%), considering the complete process (nitrification plus denitrification), being the process under statistical control. The evaluation of the kinetic behavior of nitrogen conversion indicated a possible reduction in the cycle time of the anoxic phase, since percentages of NO2 --N and NO3 -N removal higher than 90% were obtained in just one hour of denitrification. / As agroindústrias destacam-se como grandes poluidoras, devido, especialmente, às elevadas vazões com que geram seus efluentes ricos em carga orgânica, nutrientes (principalmente nitrogênio e fósforo), sólidos, óleos e graxas. Neste setor enquadram-se os abatedouros e frigoríficos de aves. A remoção de nitrogênio das águas residuárias é geralmente realizada por processos biológicos convencionais, que contemplam a nitrificação seguida da desnitrificação, envolvendo fases aeróbias e anaeróbias, separadas em diferentes reatores ou por diferentes intervalos de aeração. Os reatores em bateladas sequenciais (RBS) utilizam múltiplas etapas no mesmo reator, que incluem enchimento, reação, sedimentação, descarte e repouso. Esta pesquisa teve por objetivo investigar os efeitos da relação carbono:nitrogênio (DQO/N-NO2 -+N-NO3 -); 3, 6 e 9, ajustada pela adição de manipueira e do tempo de ciclo (TC); 8, 12 e 16 horas, na remoção de nitrogênio e matéria orgânica de efluente avícola, operando um RBS, em escala de bancada, com biomassa em suspensão em duas condições distintas, condição I com a etapa de reação composta pelas fases aeróbia/anóxica e condição II anóxica I/aeróbia/anóxica II. Objetivouse também, otimizar e validar o processo de remoção de nitrogênio, avaliar a estabilidade do reator através de gráficos de controle Shewhart para medidas individuais e, efetuar o estudo do comportamento cinético de degradação da matéria orgânica (DQO) e nitrogenada (N-NH4 +, N-NO2 - e N-NO3 -). Para avaliação das condições I e II elaborou-se um planejamento fatorial completo (32) e para otimização das condições obtidas com o planejamento fatorial inicial, utilizou-se um delineamento composto central rotacional (DCCR), com quatro ensaios nos níveis -1 e +1, quatro ensaios nos níveis dos pontos axiais (-1,414 e +1,414) e cinco repetições no ponto central (0). Avaliou-se o desempenho da nitrificação através da eficiência de remoção do nitrogênio amoniacal (%), o desempenho da pré-desnitrificação e desnitrificação através da eficiência de remoção de nitrito e nitrato (%) e a eficiência do processo completo pela remoção de nitrogênio inorgânico total (%), além do monitoramento de parâmetros, como a temperatura, pH, alcalinidade, potencial redox, salinidade e condutividade elétrica. Os maiores percentuais de remoção de nitrogênio inorgânico total foram obtidos, para ambas as condições I e II, usando as faixas de TC de 12 a 16 horas e relação C/N de 3 a 6, com valores médios de eficiências de 80,76 e 85,57% na condição I e, 90,99 e 91,09% na condição II, respectivamente. Apesar da condição II ter apresentado um percentual de remoção de nitrogênio inorgânico total superior, apenas a condição I apresentou uma regressão estatisticamente significativa e preditiva, com valores de Fcal/Ftab superiores a 4, para todas as etapas envolvidas na remoção de nitrogênio. Otimizando-se a condição I, os maiores percentuais de remoção de nitrogênio foram alcançados com o tempo de ciclo de 16h e a relação C/N de 6, validados experimentalmente, alcançando uma remoção global de nitrogênio inorgânico de 85,83±0,87%. Na avaliação da estabilidade do reator, os resultados dos 20 ensaios realizados com a condição ótima apontaram valores médios de remoção de nitrogênio inorgânico total de 84,32±1,59% (CV=1,89%) e, de matéria orgânica de 53,65±8,48% (CV= 15,81%), no processo completo (nitrificaçãodesnitrificação), estando o processo sob controle estatístico. A avaliação do comportamento cinético de conversão do nitrogênio indicou uma possível redução no tempo de ciclo da fase anóxica, uma vez que foram alcançadas remoções de N-NO2 -e N-NO3 - superiores a 90%, em apenas uma hora de desnitrificação.

Made available in DSpace on 2017-05-12T14:48:05Z (GMT). No. of bitstreams: 1 Juliana Bortoli Rodrigues Mees.pdf: 1255432 bytes, checksum: bf00dbf45cce28fdbe504091e6363048 (MD5) Previous issue date: 2010-02-01 / Agro-industries stand out as large polluters in Brazil, particularly because of the large amounts of waste rich in organic substances, nutrients (especially nitrogen and phosphorus), solids, oils and greases. In this category, slaughterhouses and bird cold storage processing plants are known for their high pollution potential. The removal of nitrogen from wastewater is usually accomplished using biological conventional processes, by nitrification plus denitrification, involving aerobic and anaerobic phases that are generally carried out in separate reactors or by different aeration intervals. The sequencing batch reactor (SBR) uses multiple steps in the same reactor, which include filling, reaction, settling, withdrawal and idling. This study aimed to investigate how carbon:nitrogen ratios (COD/NO2 --N+NO3 --N) 3, 6 and 9, adjusted by manipueira (wastewater from cassava industry) and cycle time (CT) of 8,12 and 16 hours affects the nitrogen and organic matter removal from poultry wastewater, operating a sequencing batch reactor containing suspended biomass, in two different conditions: condition I, with the reaction step consisted by aerobic/anoxic phases and condition II, anoxic I/aerobic/anoxic II phases. It was also intended to optimize and validate the process of nitrogen removal in this type of effluent, to evaluate the reactor stability using Shewhart control charts for individual measures, and to study the kinetics behavior of organic matter (COD) and nitrogen (NH4 +-N, NO2 --N and NO3 --N) degradation. The conditions I and II were evaluated through factorial planning (32) and, in order to optimize the conditions obtained with the initial factorial design, it was used a central composite rotational design (CCRD) with four assays in levels -1 and +1, four assays on the axial points levels (-1.414 and +1.414) and five replicates at the central point (0). The nitrification process performance was evaluated by the efficiency of ammonia nitrogen removal (%), the pre-denitrification and denitrification processes by the efficiencies of nitrite and nitrate removal (%) and the whole process by total inorganic nitrogen removal (%). During the nitrification and denitrification processes, parameters like temperature, pH, alkalinity, redox potential, salinity and conductivity were monitored. The highest removal percentages of total inorganic nitrogen were obtained, for conditions I and II, at the cycle time range between 12 and 16 hours and the C/N ratio of 3 to 6, which showed average efficiencies of 80.76 and 85.57% in condition I, and 90.99 and 91.09% in condition II, respectively. Although the condition II obtained a higher removal percentage of total inorganic nitrogen, only condition I presented a regression statistically significant and predictive, with Fcal/Ftab values higher than 4 for all steps involved in nitrogen removal. Optimizing the condition I, the highest percentages of nitrogen removal were achieved with the cycle time of 16 hours and C/N ratio of 6, validated experimentally, achieving an overall removal of inorganic nitrogen of 85.83±0.87 %. Evaluating the reactor stability, the results of the 20 trials carried out with optimum conditions showed a total inorganic nitrogen average removal of 84.32±1.59% (CV=1.89%) and organic matter removal of 53.65±8.48% (CV=15.81%), considering the complete process (nitrification plus denitrification), being the process under statistical control. The evaluation of the kinetic behavior of nitrogen conversion indicated a possible reduction in the cycle time of the anoxic phase, since percentages of NO2 --N and NO3 -N removal higher than 90% were obtained in just one hour of denitrification. / As agroindústrias destacam-se como grandes poluidoras, devido, especialmente, às elevadas vazões com que geram seus efluentes ricos em carga orgânica, nutrientes (principalmente nitrogênio e fósforo), sólidos, óleos e graxas. Neste setor enquadram-se os abatedouros e frigoríficos de aves. A remoção de nitrogênio das águas residuárias é geralmente realizada por processos biológicos convencionais, que contemplam a nitrificação seguida da desnitrificação, envolvendo fases aeróbias e anaeróbias, separadas em diferentes reatores ou por diferentes intervalos de aeração. Os reatores em bateladas sequenciais (RBS) utilizam múltiplas etapas no mesmo reator, que incluem enchimento, reação, sedimentação, descarte e repouso. Esta pesquisa teve por objetivo investigar os efeitos da relação carbono:nitrogênio (DQO/N-NO2 -+N-NO3 -); 3, 6 e 9, ajustada pela adição de manipueira e do tempo de ciclo (TC); 8, 12 e 16 horas, na remoção de nitrogênio e matéria orgânica de efluente avícola, operando um RBS, em escala de bancada, com biomassa em suspensão em duas condições distintas, condição I com a etapa de reação composta pelas fases aeróbia/anóxica e condição II anóxica I/aeróbia/anóxica II. Objetivouse também, otimizar e validar o processo de remoção de nitrogênio, avaliar a estabilidade do reator através de gráficos de controle Shewhart para medidas individuais e, efetuar o estudo do comportamento cinético de degradação da matéria orgânica (DQO) e nitrogenada (N-NH4 +, N-NO2 - e N-NO3 -). Para avaliação das condições I e II elaborou-se um planejamento fatorial completo (32) e para otimização das condições obtidas com o planejamento fatorial inicial, utilizou-se um delineamento composto central rotacional (DCCR), com quatro ensaios nos níveis -1 e +1, quatro ensaios nos níveis dos pontos axiais (-1,414 e +1,414) e cinco repetições no ponto central (0). Avaliou-se o desempenho da nitrificação através da eficiência de remoção do nitrogênio amoniacal (%), o desempenho da pré-desnitrificação e desnitrificação através da eficiência de remoção de nitrito e nitrato (%) e a eficiência do processo completo pela remoção de nitrogênio inorgânico total (%), além do monitoramento de parâmetros, como a temperatura, pH, alcalinidade, potencial redox, salinidade e condutividade elétrica. Os maiores percentuais de remoção de nitrogênio inorgânico total foram obtidos, para ambas as condições I e II, usando as faixas de TC de 12 a 16 horas e relação C/N de 3 a 6, com valores médios de eficiências de 80,76 e 85,57% na condição I e, 90,99 e 91,09% na condição II, respectivamente. Apesar da condição II ter apresentado um percentual de remoção de nitrogênio inorgânico total superior, apenas a condição I apresentou uma regressão estatisticamente significativa e preditiva, com valores de Fcal/Ftab superiores a 4, para todas as etapas envolvidas na remoção de nitrogênio. Otimizando-se a condição I, os maiores percentuais de remoção de nitrogênio foram alcançados com o tempo de ciclo de 16h e a relação C/N de 6, validados experimentalmente, alcançando uma remoção global de nitrogênio inorgânico de 85,83±0,87%. Na avaliação da estabilidade do reator, os resultados dos 20 ensaios realizados com a condição ótima apontaram valores médios de remoção de nitrogênio inorgânico total de 84,32±1,59% (CV=1,89%) e, de matéria orgânica de 53,65±8,48% (CV= 15,81%), no processo completo (nitrificaçãodesnitrificação), estando o processo sob controle estatístico. A avaliação do comportamento cinético de conversão do nitrogênio indicou uma possível redução no tempo de ciclo da fase anóxica, uma vez que foram alcançadas remoções de N-NO2 -e N-NO3 - superiores a 90%, em apenas uma hora de desnitrificação.

Nitrogen is the major component of biosphere. Paradoxically, nitrogen pollution is the concern globally. Ammonia pollution is due to its unceasing rejection into nature such as groundwater, current water and the atmosphere. This phenomenon constitutes a threat for the humanity, land and aquatic flora, and consequently disturbs the balance of natural ecosystem. Recently, that situation has lead to develop various techniques and/or technologies for ammonia removal from municipal and industrial wastewaters. Particularly in the environmental biotechnology area, two main objectives were recently aimed in many research activities: the development of new configurations of competitive bioreactors and the monitoring of partial nitrification process, which are the fundamental basis of this thesis project. In this study, the partial ammonium oxidation process, also called nitrite route, was studied in a 60 litre jet-loop submerged membrane bioreactor pilot plant. The research was organized around six chapters. An exhaustive literature review of the state-of- art of the biological nitrification process and the membrane technologies was performed. The materials and measurement methods were presented. The colorimetric method, the chromatography analysis, the biomass estimation by the suspended solids (SS), the aggregates size measurement, the gas holdup, the gas-liquid mass transfer, the bubbles gas diameter determination, the medium rheology aspects, etc., and the complete equipment of the bioreactor were studied in detail. The plant automation functioning was also studied. Membrane module (Mitsubishi Sterapore-L) characterization was carried out and three characteristic parameters were estimated: the membrane intrinsic resistance Rm, the membrane permeability Lp and the membrane porosity εm. Estimations revealed good agreement between experimental results and theoretical methods based on the Darcys law and the Carman-Kozeny law applicable in microfiltration system. Hydrodynamics and aeration aspects were studied. The mixing in the jet-loop system was characterized by the mixing time (tmix) and the circulation time (tc), respectively. The results showed that the characteristic times (tmix and tc) decrease with an increase in input gas flowrate and the circulated liquid flowrate. A model correlation involving the air and the combined liquid effects was proposed to describe the circulation time evolution. The classical non-steady state clean water test was used to determine the gas-liquid mass transfer coefficient (kLa). It was found to be influenced by the combined action of air and recirculated-liquid flowrates and a correlation has been proposed to describe their influence. The interpretation of kLa results and the system mixing data showed that the developed reactor corresponds to a near perfect mixing tank. This criterion was satisfactorily verified by literature data. The gas holdup (εg) was directly measured by the volume expansion method. In the absence of liquid circulation, εg ranged between 1 and 4% for the investigated range of gas liquid superficial velocities. It was found to increase linearly with the air superficial velocity, which corresponds to the bubbly flow regime. However, in the presence of liquid flowrate, εg slightly increased (from 1 to 6%) with increase in the superficial liquid velocity. A model has been proposed to correlate εg and the air and the recirculated-liquid velocities. The average diameter of the bubbles gas (dB) in the system was also estimated by the Leibson theoretical model based on the Reynolds number at the orifice of the gas distributor. Finally, biological aspects were studied. Respirometry measurements were conducted to characterize the process medium. The mass transfer, the gas holdup and the medium viscosity were determined. The obtained data allowed estimating the α factor and the β factor, respectively. The interaction of the growth of microorganisms into the process and the membrane performance was also investigated and a correlation model was proposed to describe membrane fouling with time. The optimal conditions for ammonium partial oxidation were determined using process monitoring and simulation. Dissolved oxygen (DO), temperature (T) and hydraulic retention time (HRT) were selected to achieve a high nitrite accumulation in the system. The results obtained showed that the selected parameters should be fixed at DO ≈ 2 mgO2.l-1, HRT ≈ 6 7 h and T = 30°C, respectively. The partial nitrification was simulated by the use of the TwoPopNitrification model included into the BioWin 2.2 software. For these simulations, a sequencing ammonia oxidation assumption was adopted: the nitrozation followed by the nitration step, respectively. The corresponding kinetics and stoichiometric constants were estimated by combining literature data and experimental nitrification results. For these estimates, the ammonium oxidation was monitored on several process samples taken at different times. The estimates were also delivered by monitoring the ammonium oxidation on the process operated in the batch mode. The plotting of simulations and experimental results revealed good agreement. In order to investigate the process performance in terms of biological stability, a long time period (≈ 600 days) was simulated. The results showed that a high stable nitrite accumulation (> 95%) could be achieved when the above optimal conditions are imposed to the system. However, after a long time, the accumulated nitrite is converted into nitrate and then the system is disrupted. For the simulated experimental conditions, the process disruption period was located between 180 and 350 days. At this period, a corresponding theoretical purge flowrate was found to range between 0.15 10-3 m3.d-1 and 3.0 10-3 m3.d-1. Simulations also showed that increasing the purge flowrate decreases the sludge retention time and then favours nitrite accumulation into the process. That is an interesting strategy to increase the performance of the biological partial nitrification process.

L’assainissement d’effluents résiduaires urbains par filtres plantés de roseaux (FPR) rencontre, depuis plus de trois décennies, un engouement croissant en raison de ses remarquables performances de traitement ainsi que de considérations technico-économiques et écologiques. Néanmoins, des objectifs de traitement de plus en plus contraignants, ainsi qu’un marché de plus en plus concurrentiel, amènent la nécessité d’une meilleure connaissance des processus afin d’en optimiser la conception en fonction du contexte. Une attention toute particulière a été portée au traitement de l’azote, au cours de cette étude, en raison de l’aspect particulièrement contraignant de son élimination. Ces travaux se sont articulés autour de trois axes principaux permettant l’évaluation des principaux mécanismes d’élimination de l’azote (nitrification, dénitrification et adsorption, respectivement). Un premier volet, conduit sur unités pilotes alimentées en effluents domestiques réels, s’est attaché à identifier l’impact respectif de divers critères de dimensionnement et opérationnels (profondeur de filtration, surface de filtration, charges hydrauliques et organiques) afin de proposer des consignes de conception adaptées aux objectifs de traitement sur l’azote ammoniacal ainsi que la matière organique et la pollution particulaire. Une seconde partie de l’étude, mené à échelle pilote à partir d’effluents semi-synthétiques, s’est quant à elle focalisée sur le processus de dénitrification afin de mettre en exergue les critères majeurs (composition des effluents, paramètres de conception et fonctionnement) pour l’atteinte de performances poussées sur le traitement des nitrates. Enfin, un dernier axe de recherche, effectué en laboratoire en colonne, a visé à évaluer l’effet de l’adsorption d’ammonium sur matériaux filtrants réactifs (zéolithe) en vue d’optimiser par la suite le temps de rétention de cette espèce au regard des cinétiques de dégradation biologique. Une synthèse des connaissances acquises au cours de cette étude a donné lieu à des conseils de conception ainsi qu’à des recommandations pour d’éventuelles études complémentaires. / The treatment of domestic wastewater by constructed wetlands (CWs) meets, from more than three decades, an increasing interest because of its high treatment efficiency as well as technological, economic and ecological issues. However, with treatment objectives that are growing ever stricter and an increasingly competitive market, fine knowledge of removal processes is required in order to optimize design in regards with context. A particular attention was paid to nitrogen removal, through this study, because of its particularly coercive dimension in treatment process. This work is partitioned in three axes which enable the assessment of the main mechanisms ensuring nitrogen removal (nitrification, denitrification and sorption, respectively). A first part, conducted in pilot-scaled units fed in real domestic wastewater, aimed at identifying the respective effects of various design and operational parameters (filtration height, filtration area, hydraulic and organic loads) in order to provide design recommendations for an efficient removal of ammonium as well as organic matter and suspended solids. A second part of this work, carried out in pilot-scaled units fed with semi-synthetic wastewater, focused on denitrification process in order to highlight driving parameters (influent composition, design and operational parameters) of full nitrate removal. Last but not least, a third research axis, conducted in column-scaled units, assessed the ammonium adsorption onto reactive material (i.e. zeolite) in order to optimize the retention time of ammonium within the system in regards with nitrification kinetic. These results were then summarized in order to provide design guidelines as well as recommend further complementary experiments.

Dans ce travail, le traitement des nutriments et plus particulièrement celui de l’azote en procédé de granulation aérobie a été étudié. L’approche expérimentale a dans un premier temps eu pour objet de comparer la stabilité des caractéristiques physiques et microbiologiques d’agrégats développés dans deux réacteurs fonctionnant en alternances de phases anaérobie / aérobie ou anoxie / aérobie. L’opération d’un procédé de granulation aérobie en alternance de phases anoxie / aérobie a favorisé la stabilisation des performances de traitement de l’azote et notamment celle de la nitrification. Le développement d’une boue hybride comprenant une fraction de flocs et de granules a été observé. Dans le but d’évaluer comment le caractère hybride de la boue obtenue en conditions anoxie/aérobie oriente les performances et vitesses de transformation de l’azote, une caractérisation ex-situ des limitations au transfert d’oxygène au sein des flocs, granules et boue hybride a été réalisée par respirométrie. En complément, la localisation des espèces nitrifiantes par la technique d’hybridation fluorescente in situ (FISH) a été réalisée. Les résultats obtenus indiquent que la présence de flocs au sein d’une boue granulaire permet d’augmenter la vitesse de la nitrification, en particulier pour de faibles concentrations en oxygène dissous. D’autre part, il est ici mis en évidence la nécessité de contrôler simultanément le ratio floc/granules et la taille des granules en vue de l’optimisation du traitement de l’azote.Enfin un outil mathématique permettant de décrire les phénomènes réactionnels ayant lieu au sein d’une biomasse hybride a été développé. Celui-ci a été employé dans le but d’optimiser le fonctionnement du procédé hybride par l’évaluation de l’effet des propriétés physiques de la biomasse, et plus particulièrement de la proportion de granules en présence, pouvant conduire à une élimination efficace de l’azote et à l’augmentation de la robustesse du procédé vis-à-vis de diminutions ponctuelles de l’oxygène dissous / In this work, the treatment of nutrients, especially that of nitrogen in aerobic granulation process was studied.The experimental approach has initially been intended to compare the stability and the physical and microbiological characteristics of aggregates developed in two reactors operating in alternating anaerobic / aerobic or anoxic / aerobic conditions. The presence of a pre-anoxic phase promoted the stabilization of nitrogen removal performances and especially those of nitrification. The development of a hybrid sludge process containing a fraction of flocs and granules was observed.In order to evaluate and quantify the influence of the simultaneous presence of flocs and granules in the nitrifying activity of the hybrid sludge developed in the alternating anoxic / aerobic conditions, the nitrification rate and oxygen limitation of flocs, granules and hybrid sludge was assessed using respirometric assays at different dissolved oxygen concentrations. The spatial distribution of nitrifying bacteria was investigated using fluorescence in situ hybridization (FISH). Results indicated that the presence of flocs with granules could increase the rate of nitrification to transitory reductions of aeration. On the other hand, the optimization of nitrogen removal requires the simultaneous control of the floc to granule ratio and granule size.Finally, a mathematical model to describe the reaction phenomena taking place in the hybrid biomass was developed. It was used in order to optimize the operation of the hybrid process through the evaluation of the effect of physical properties of biomass, specifically the ratio of granules and flocs in the reactor that can lead to efficient removal of nitrogen and increase the robustness of the process

Os processos de amonificação e nitrificação no solo são de fundamental importância para a disponibilidade de N-mineral às plantas. Recentemente, foi demonstrado que a cana-de-açúcar tem preferência na absorção de NH4 + à NO3 -, podendo apresentar maior produtividade quando fertilizada apenas com Namoniacal. Da mesma forma, estudos indicaram que gramíneas do gênero Brachiaria podem inibir a nitrificação no solo por meio da exsudação radicular de compostos denominados braquiolactanas. Portanto, é oportuno avaliar as taxas de amonificação (TAB) e nitrificação brutas (TNB) de N pela técnica da diluição do isótopo 15N em solos cultivados com cana-de-açúcar e braquiária. Devido à escassez de trabalhos voltados à estimativa da TAB e TNB em solos tropicais, adaptações na metodologia são requeridas. Objetivou-se, então, realizar ajustes nos protocolos para determinação da TAB e TNB, para, posteriormente, quantificar as referidas taxas em solos sob cultivo de cana-de-açúcar e de algumas espécies de gramíneas para pastagem. Primeiramente, avaliou-se o tempo necessário de agitação de amostras líquidas contendo um sistema de microdifusão para captura do N-mineral presente. Os resultados indicaram que a máxima recuperação isotópica de 15N-mineral e de N-15NH4 + ocorreu em 24 h de agitação. Em sequência foram avaliadas duas técnicas para recuperação do N-15NO3 - (eliminação prévia do N-NH4 + e diluição isotópica) presente em extratos de KCl contendo N-15NO3 - e 15N-mineral. Ambas foram eficientes, sendo recomendada técnica que preconiza a eliminação prévia do N-NH4 +, pela boa operacionalidade proporcionada. A última adaptação efetuada se refere à abundância de 15N no composto marcado a ser aplicado no solo, visto que em estudos com solos temperados, são utilizados compostos altamente enriquecidos no isótopo. Foi constatado que para solos tropicais (agricultáveis e cultivados com cana-de-açúcar, no caso) não há necessidade de alta marcação com 15N nos compostos. Por fim, foi quantificada a TAB e TNB de solos cultivados com cana-de-açúcar e pastagens, com as devidas adaptações metodológicas efetuadas. A TAB dos solos de cana-de-açúcar e pastagem foi superior à TNB. Os solos de pastagem cultivados unicamente com a espécie B. humidicola apresentaram alto conteúdo de N-NH4 + e valores extremamente baixos de N-NO3 - e TNB, indicando inibição biológica da nitrificação. A ação inibitória da nitrificação em solos com ocupação de B. humidicola pode ser uma estratégia interessante para o plantio de cana-de-açúcar, com base na hipótese de preferência de absorção por NH4 + à NO3 - pela cultura. / The ammonification and nitrification processes of soils are of fundamental importance because they release mineral N to the plants. It was recently shown that sugarcane has a preference to uptake NH4 + instead of NO3 -, and may have higher yield when is fertilized with only NH4 +-N. Similarly, studies indicated that some Brachiaria species can inhibit soil nitrification through root exudation of free fatty acids. Therefore, it is appropriate to assess the gross rates of ammonification (GRA) and gross nitrification (GRN) by 15N pool dilution technique Therefore, it is appropriate to assess the gross rates of ammonification (GRA) and gross nitrification (GRN) by the 15N pool dilution technique in soils cropped with sugarcane and pasture. Due to the lack of studies related to the estimate of GRA and GRN in tropical soils, adjustments in methodology are required. Thus, the objectives were to perform some adjustments in the protocols of GRA and GRN to subsequently quantify such rates in soils under sugarcane and some pasture grasses. First, it was assessed the time needed for shaking liquid samples containing a microdiffusion system to capture the mineral N present. Results indicate that the maximum isotopic recovery of 15NH4 +-N and mineral-15N occurred within 24 h of shaking. Following, two methods of recovery the added 15NO3 --N (prior removal of NH4 +-N and isotope dilution procedure) to samples containing KCl were tested. Both methods were effective, but the technique that advocates removal of NH4 +-N is recommended, due to the good operability. The last adjustment made refers to the 15N abundance of labelled compound, since studies with temperate soils usually use highly enriched compounds in the isotope. It was observed that for tropical soils (arable and under sugarcane, in this case) there is no need to use highly enriched 15N-coumpounds. Finally, GRA and GRN were quantified in soils under sugarcane and pasture, applying the adjustments previously made. GRA in soils from sugarcane and pasture was higher compared to GRN. The soils under B. humidicola showed high content of NH4 +-N and extremely low values of NO3 --N and GRN, indicating biological nitrification inhibition. Nitrification inhibition in soils occupied by B. humidicola may be an interesting strategy for sugarcane planting, on the assumption of preference to uptake NH4 + rather than NO3 - in this crop.

Les nanoparticules métalliques manufacturées (NPs) sont des polluants émergents dont la concentration augmente dans les sols en raison de leur utilisation croissante dans de nombreux produits commerciaux de la vie courante (cosmétiques, aliments, peintures…). Des études in vitro ont montré la toxicité des NPs pour les microorganismes, mais il existe encore peu de données sur l'écotoxicité et le devenir de ces contaminants dans les sols. L'objectif de cette thèse est donc d'évaluer l'influence des paramètres abiotiques du sol sur (i) les caractéristiques physico-chimiques et le transfert des NPs, et (ii) sur la toxicité des NPs pour les communautés microbiennes du sol, en particulier pour des groupes fonctionnels microbiens impliqués dans le cycle du carbone et de l'azote. Nous avons mis en évidence que les propriétés du sol influençaient l'agrégation et la charge de surface des NPs de dioxyde de titane (TiO2) et d'oxyde de cuivre (CuO). Dans les six sols agricoles étudiés, nous avons observé un transport très faible des NPs testées lors d'une expérimentation en colonnes de sols. Nous avons mis en évidence une absence de toxicité des NPs de TiO2 sur les communautés microbiennes, sauf dans un sol limono-argileux à forte teneur en matière organique. Dans ce sol, des effets négatifs ont été observés après 90 jours d'exposition sur les activités microbiennes, sur l'abondance des microorganismes nitrifiants et la diversité des bactéries et des archées. Des études complémentaires en colonnes de sol, ont permis de mettre en évidence des effets délétères des NPs plus importants que la nitrification lors d'une contamination chronique au TiO2 que lors d'une contamination aigüe / Manufactured metallic nanoparticles (NPs) are emerging pollutants of soils due to their increasing utilization in numerous commercial products (cosmetics, food, paint…). In vitro studies have demonstrated NPs toxicity on microorganisms but data are still scarce on the fate and ecotoxicity of these contaminants in soils. The objective of this thesis was to assess the influence of soil properties on (i) the physicochemical characteristics and the transport of NPs, and (ii) on the NPs toxicity on soil microbial communities, especially on microbial functional groups involved in carbon and nitrogen cycles. This work highlighted that soil properties influenced the aggregation and the surface charges of titanium dioxide NPs (TiO2-NPs) and copper oxide NPs (CuO-NPs). In the six agricultural soils studied, we observed a very low transport of the two NPs in a soil column experiment. We observed a low toxicity of TiO2-NPs for soil microbial communities, except in a silty-clay soil with a high organic matter content. In this soil, microbial activities (soil respiration, nitrification and denitrification) and nitrifier abundances were strongly decreased and archaeal and bacterial community structure were altered after 90 days of exposure. Furthermore in this soil, we observed decreases of nitrification activity, even for very low TiO2-NPs concentrations (0.05 mg kg-1) which were explained by a high sensitivity of ammonia-oxidizing archaea (AOA) involved in this process. Additional studies in soil columns demonstrated that chronic contamination with TiO2-NPs caused more deleterious effects on nitrification than acute contamination