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Síntese e aplicações de nanocristais semicondutores de ZnCdTe em matriz de grafeno / Synthesis and applications of ZnCdTe semiconductor nanocrystals in graphene matrixSantana, Paula de Cássia Andrade 21 February 2018 (has links)
Conselho Nacional de Pesquisa e Desenvolvimento Científico e Tecnológico - CNPq / In the present study, a new nanocomposite based on ZnCdTe semiconductor
nanocrystals synthesized in situ on reduced graphene oxide was obtained. The
characterization of the heterostructure was done by transmission electronic
microscopic and using spectroscopic emission and UV-Vis absorption
techniques, where it was possible to observe the growth of nanocrystals in the
rGO reduced graphene oxide matrix, as well as to estimate the value of the optical
band gap. Cyclic voltammetry was used as a complementary characterization
technique which was created to investigate the surface of the nanomaterial and
calculate the band gap, obtaining approximate value to the optic. The study of
the multifunctionality in applications of the obtained nanocomposite was carried
out using the material as base of an electrochemical sensor and also, as a
catalyst in the process of degradation of the methylene blue dye by exposure to
the ultrasound waves, using the sonocatalysis procedure. To evaluate the
electrochemical properties of the modified carbon paste electrodes with
nanocomposite were prepared, with an effective area equal to 0.30 cm2. The
modified electrode showed high sensitivity in the detection of the pesticide
carbendazim. The parameters for the best conditions of analysis were
established and a calibration curve was constructed with a behavior proportional
to the concentration of the electroactive species in a linear range of 9.98.10-8 to
1.20.10-5 mol L-1, with limit of detection and quantification equal to 9.20.10-8 and
2.80.10-7 mol L-1, respectively. The method developed was applied in real
samples of orange juice, which detected a concentration of 2.91.10-5 mol L-1 of
the analyte, above that allowed by the legislation, indicating a possible
contamination of the matrix. The sonocatalytic procedure demonstrated that the
presence of the nanocomposite as a catalyst in the dye degradation process
favored the dye degradation reaction speed in which it was possible to observe
its color change during the time of exposure to the ultrasonic energy. / No presente estudo, foi obtido um novo nanocompósito a base de nanocristais
semicondutores de ZnCdTe sintetizados in situ em óxido de grafeno reduzido.
As caracterizações da heteroestrutura foram realizadas através da microscopia
eletrônica de transmissão e utilizando as técnicas espectroscópicas de emissão
e absorção UV-Vis, em que foi possível observar o crescimento dos nanocristais
na matriz de óxido de grafeno reduzido, como também estimar o valor do band
gap óptico. A técnica de voltametria cíclica foi utilizada para investigar a
superfície do nanomaterial e calcular o band gap eletroquímico, obtendo-se valor
aproximado ao óptico. O estudo da multifuncionalidade em aplicações do
nanocompósito obtido foi realizado utilizando o material como base de um sensor
eletroquímico e também, como catalisador no processo de degradação do
corante azul de metileno por exposição as ondas de ultrassom, empregando o
procedimento de sonocatálise. Para avaliar as propriedades eletroquímicas,
eletrodos de pasta de carbono modificados com o nanocompósito foram
preparados, com uma área efetiva igual 0,30 cm2. O eletrodo modificado mostrou
elevada sensibilidade na detecção do pesticida carbendazim. Os parâmetros
para as melhores condições de análise foram estabelecidos e uma curva de
calibração foi construída com um comportamento proporcional a concentração
da espécie eletroativa em uma faixa linear de 9,98.10-8 a 1,20.10-5 mol L-1,
apresentando um limite de detecção e quantificação igual a 9,20.10-8 e 2,80.10-7
mol L-1, respectivamente. O método desenvolvido foi aplicado em amostras reais
de suco de laranja, o qual detectou uma concentração de 2,91.10-5 mol L-1 do
analito, este valor está acima do permitido pela legislação, indicando uma
possível contaminação da matriz. O procedimento sonocatalítico demonstrou
que a presença do nanocompósito como catalisador no processo de degradação
do corante favoreceu a velocidade da reação de degradação do corante no qual,
foi possível observar a sua mudança de cor do decorrer do tempo de exposição
à energia ultrassônica. / São Cristóvão, SE Read more
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Tratamento fotocatalítico de poluentes aquosos utilizando CdS ancorado em biofiltros / Photocatalytic treatment of aqueous pollutants using CdS anchored onto biofiltersNascimento, Cristiane da Cunha 26 February 2018 (has links)
The release of various organic and inorganic pollutants into the environment has
been considered a major global problem since it has effects on human health and other
forms of life. Among the various methods for treating this problem, heterogeneous
photocatalysis using semiconductor nanoparticles has been considered one of the most
promising. In this work, nanoparticles of cadmium sulfide anchored onto different
diatomite species were synthesized using a fast and simple method. Through the
UV/visible spectra, variations in the absorption maxima and spectral shifts to hight
wavelengthts were observed with the increase of the reaction time, whereas the XRD
data showed the formation of the hexagonal phase for the nanoparticles of cadmium
sulfide, while the morphological analyzes showed nanoparticles with an approximately
spherical shape. Also, the degradation of the methylene blue dye, ciprofloxacin and the
reduction of Cr(VI) to Cr(III) ion reduction were studied via photocatalysis. For the dye
degradation tests, studies were carried out under UVA and solar irradiation. It was
observed that the photocatalysis process was more effective during irradiation with
sunlight. For the photocatalytic tests with chromium and ciprofloxacin, it was noticed
that the photocatalysis is much more efficient when compared to the adsorption and
photolysis processes, showing a reduction rate around 86% for Cr(VI) to Cr(III), after
210 min of solar irradiation, and a pseudo-first order kinetics, whereas the degradation
of ciprofloxacin reached approximately 90% after 180 min of exposure with a secondorder
kinetic model. / A presença de diversos poluentes orgânicos e inorgânicos que são lançados
diretamente no meio ambiente, tem sido considerada um grande problema mundial, uma
vez que traz efeitos à saúde dos seres humanos e a outras formas de vida. Dentre os
diversos métodos de tratamento empregados, a fotocatálise heterogênea utilizando
nanopartículas semicondutoras tem sido considerada uma das mais promissoras. Neste
trabalho, nanopartículas de sulfeto de cádmio ancoradas em diferentes espécies de
diatomitas foram sintetizadas com diferentes tempos de síntese, por meio de um método
rápido e simples. Através dos espectros no UV/visível, notaram-se variações nos
máximos de absorção e descolamentos para maiores comprimentos de onda com o
aumento do tempo de reação, já os dados de DRX evidenciaram a formação da fase
hexagonal para as nanopartículas de sulfeto de cádmio, enquanto que as análises
morfológicas apresentaram nanopartículas de forma aproximadamente esféricas.
Adicionalmente, estudos de fotocatálise foram realizados na degradação do corante azul
de metileno, do antibiótico ciprofloxacina e na redução dos íons Cr(VI) a Cr(III). Para
os testes de degradação do corante foram realizados estudos sob irradiação UVA e solar.
Foi observado que o processo de fotocatálise foi mais efetivo durante a irradiação com a
luz solar. Já para os testes fotocatalíticos com o Cr(VI) e o ciprofloxacina, notou-se que
a fotocatálise é muito mais eficaz quando comparada aos processos de adsorção e
fotólise, apresentando uma redução do Cr(VI) a Cr(III) em torno de 86%, após 210 min
de irradiação solar,e uma cinética de pseudo-primeira ordem, enquanto que a
degradação do ciprofloxacina atingiu aproximadamente 90% após 180 min de exposição
solar, apresentando um modelo cinético de segunda ordem. / São Cristóvão, SE Read more
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Efeito da terapia fotodinâmica sobre biofilme de Enterococcus faecalis e estrutura dentinária / Effect of photodynamic therapy on Enterococcus faecalis biofilm and dentin structureAlves, Denise Ramos Silveira 05 May 2016 (has links)
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Previous issue date: 2016-05-05 / Fundação de Amparo à Pesquisa do Estado de Goiás - FAPEG / Objective: Evaluate the effect of photodynamic therapy (PDT) on Enterococcus faecalis biofilm in
infected root canals and on dentin structure.
Methods: Twenty-one root canals of a sample of 24 extracted single-rooted human teeth were
infected by E. faecalis for 60 days to form biofilm. The antimicrobial strategies tested were (n=3 in
each group): root canal preparation using NiTi rotary instruments, 2.5% NaOCl and 17% EDTA
irrigation, and PDT with 0.01% methylene blue (group I) or 0.01% malachite green (group II); root
canal preparation using NiTi rotary instruments, 2.5% NaOCl and 17% EDTA irrigation, and PDT
with 0.01% methylene blue (group III); PDT with 0.01% methylene blue without root canal
preparation (group IV); root canal preparation using NiTi rotary instruments, 22.5% NaOCl and
17% EDTA irrigation, and no PDT (group V); 2.5% NaOCl irrigation with no root canal
preparation, and 17% EDTA irrigation (group VI); positive control (group VII). Three roots were
not infected and were used as negative controls (group VIII). Samples for microbiological tests
were collected using three sterile paper points, later stored in BHI and incubated at 37o C for 48
hours at three time points: before (S1) and after (S2) root canal preparation, and after PDT
application (S3). Bacterial growth was analyzed according to turbidity of culture medium, presence
of bacteria, and spectrophotometric optical density (nm). Specimens were sectioned and prepared
for SEM analysis of dentin structure.
Results: Bacteria were found at S1, S2 and S3 in all experimental groups. Optical density of
culture media at S2 and S3 in groups I, II and III were lower than at S1, but not statistically
different. Optical density of culture media at S2 was 28.70% and 24.67% lower than at S1 in
groups I and II; after PDT, optical density was 90.00% (group I) and 37.30% (group II) lower. In
group III, it was 97.70% lower at S2 and an additional 92.00% lower after PDT. In group IV,
optical density increase 3.2%. Dentin analysis after PDT revealed areas of melting and
recrystallization, peritubular dentin projections, intertubular dentin erosion and fusion of dentinal
tubule openings, which made dentin surface irregular. Some dentinal tubules were obliterated, and
there were changes in the shape of their openings.
Conclusion: PDT applied after root canal preparation using manual or rotary files was not
effective in eliminating E. faecalis completely. PDT changed dentin structure and resulted in
dentin melting and recrystallization, as well as in dentinal tubule erosion and obliteration. / Objetivo: Avaliar o efeito da terapia fotodinâmica sobre biofilme de Enterococcus faecalis em
canais radiculares infectados e sobre a estrutura dentinária.
Metodologia: O estudo foi desenvolvido em vinte e quatro dentes humanos unirradiculares
extraídos, dos quais vinte e um canais radiculares foram infectados com E. faecalis por 60
dias para formação de biofilme. As estratégias antimicrobianas testadas foram (n=3): preparo
do canal radicular com instrumentos rotatórios de NiTi/ NaOCl 2,5%/ irrigação final EDTA
17%, e TFD com azul de metileno 0,01% (Grupo I) ou verde malaquita 0,01% (Grupo II);
preparo do canal radicular com instrumentos manuais de aço inox/ NaOCl 2,5%/ irrigação
final EDTA 17% e TFD com azul de metileno 0,01% (Grupo III); TFD com azul de metileno
0,01% sem preparo prévio do canal radicular (Grupo IV); preparo do canal radicular com
instrumentos rotatórios de NiTi/ NaOCl 2,5%/ irrigação final EDTA 17% sem emprego da TFD
(Grupo V); irrigação com hipoclorito de sódio 2,5% sem preparo do canal radicular/ irrigação
final EDTA 17% (Grupo VI); controle positivo (Grupo VII). Três espécimes não foram
contaminados, sendo utilizados como controle negativo (Grupo VIII). Coletas microbiológicas
foram realizadas, antes (CM1) e após (CM2) o preparo do canal radicular, e depois da
aplicação da TFD (CM3), utilizando três pontas de papel absorventes esterilizadas,
posteriormente armazenadas em BHI e a seguir , incubadas a 37o
C por 48 horas. O
crescimento bacteriano foi analisado pela turbidez do meio de cultura, sendo determinada a
presença ou ausência de bactérias, e pela densidade óptica do meio de cultura, interpretada
por espectrofotometria (nm). A seguir, os espécimes foram seccionados e preparados para
análise da estrutura dentinária por meio de imagens de MEV.
Resultados: A presença de bactérias foi verificada na CM1 , CM2 e CM3 de todos os grupos
experimentais. As medidas da densidade óptica dos meios de cultura das CM2 e CM3 nos
grupos experimentais I, II e III apresentaram redução quando comparada a CM1, porém não
significativa estatisticamente. Nos Grupos I e II a densidade óptica do meio de cultura foi
reduzida em 28.70% e 24,67% em CM2, respectivamente. Após a TFD, a redução da
densidade óptica foi 90,00% (Grupo I) e 37,70% (Grupo II). No Grupo III, a redução da
densidade óptica do meio de cultura foi de 97,70% na CM2, com redução adicional de 92,00%
após TFD. No Grupo IV foi verificado aumento da densidade óptica do meio de cultura em
3,2%. A análise da dentina evidenciou, nos grupos submetidos à TFD, áreas de derretimento
e recristalização, projeção da dentina peritubular, e regiões com erosão da dentina
intertubular e união das entradas dos túbulos dentinários, tornando a superfície dentinária
irregular. Obliteração de túbulos dentinários com alteração do contorno de suas entradas
também foi verificada.
Conclusão: A TFD, após preparo do canal radicular com sistema rotatório ou manual, não foi
efetiva na eliminação completa de E. faecalis, e alterou a estrutura dentinária, determinando
derretimento e recristalização de dentina, erosão e obliteração de túbulos dentinários. Read more
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Filmes sensíveis a pressão pela técnica de fotoluminescência. / Pressure sensitive films based on photoluminescence technique.Keth Rousbergue Maciel de Matos 20 May 2011 (has links)
O presente projeto tem como objetivo contribuir para o desenvolvimento de dispositivos para monitoração de pressão dinâmica do ar. Para isso, foram produzidos filmes sensíveis a pressão baseados na detecção de concentração de oxigênio por meio de processos de emissão fotoluminescente das moléculas de Azul de Metileno (MB) e Platina Octaetilporfirina (PtOEP). Nesse sentido, foi estudado o comportamento da emissão fotoluminescente dessas moléculas em interação com o gás de oxigênio. A concentração de oxigênio (do ar) sobre superfície sensível depende da pressão dinâmica de superfície. Desta forma, monitorando a fotoluminescência dos dispositivos submetidos a diferentes concentrações de oxigênio, pode-se determinar uma relação entre a pressão pontual da superfície analisada e a intensidade de emissão fotoluminescente do filme. Os dispositivos de monitoração de pressão dinâmica são constituídos de um filme de estado sólido contendo as moléculas sensíveis. Foram utilizados como substratos hospedeiros para o Azul de Metileno e para a Octaetilporfirina de Platina, os filmes de silício poroso oxidado e Poliestireno, respectivamente. É proposto um arranjo experimental que utiliza um fluorímetro para caracterizar as amostras produzidas e uma câmara de fluxo de gases. Os dispositivos apresentaram elevada sensibilidade e evidenciaram o potencial para desenvolvimento e integração de sensores baseados no silício poroso à microeletrônica. / This project aims to contribute to the development of devices for monitoring dynamic pressure of the air. In this sense, films were produced based on pressure-sensitive detection of oxygen concentration through processes of photoluminescence emission from the molecules of methylene blue (MB) and platinum octaethylporphyrin (PtOEP). Accordingly, it was studied the behavior of the photoluminescence emission of these molecules in interaction with the oxygen gas. The concentration of oxygen (of the air composition) on the sensitive surface depends on the surface dynamic pressure. Thus, monitoring the photoluminescence of the devices under different oxygen concentrations, it can be determined a relationship between the punctual pressure of the tested surface and the photoluminescence emission intensity of the film. The devices for monitoring dynamic pressure are made of a solid state film containing the sensitive molecules. Oxidized porous silicon and polystyrene films were used as hosts for the Methylene Blue and for the Platinum Octaethylporphyrin, respectively. It was proposed an experimental setup that uses a spectrofluorophotometer and a gas flow chamber to characterize the produced samples. The devices showed high sensitivity and potential for development and integration of the sensors based on porous silicon for microelectronics. Read more
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FORMULAÇÕES DE FOTOSSENSIBILIZADOR FENOTIAZÍNICO CONTENDO ETANOL OU CARREADOR DE OXIGÊNIO EM DIFERENTES pHs. EFEITO ANTIMICROBIANO EM BIOFILMES DE Pseudomonas aeruginosa / PHENOTHIAZINE PHOTOSENSITIZER FORMULATIONS CONTAINING ETHANOL OR OXYGEN CARRIER IN DIFFERENT pHs. ANTIMICROBIAL EFFECT IN Pseudomonas aeruginosa BIOFILMSMartins, Maritieli Righi 27 August 2014 (has links)
Our goal was to optimize the antimicrobial photodynamic effect of methylene blue (MB) by adding ethanol or oxygen carrier in the formulation. Pseudomonas aeruginosa PA01 biofilms were formed on acrylic disks for 5 days. Photoactivated formulations contained MB (250 μM) in: buffered water, 10% ethanol (buffer:ethanol, 90:10), 20% ethanol (buffer:ethanol, 80:20) and emulsion carrier (perfluorodecalin:buffer:triton-X100, 60:35:5). The buffer used was a Tris-HCl solution to a pH of 7.4; and sodium acetate/acetic acid to solutions at pH 5.6. Untreated biofilms and exposed to the buffer, 10% ethanol and 20% without polymerization were evaluated as controls. Production of singlet oxygen was measured by photo-oxidation of 1.3-difenilisobenzofuran (75μM). Data of photo-oxidation and CFU (log10) were evaluated by One-Way ANOVA and post hoc Tukey and Dunnett, respectively. Student t-test assessed differences between the same formulation with different pH. Increased production of singlet oxygen was determined on MB diluted in 10% ethanol and 20% at pH 7.4. However, these formulations showed no statistical difference compared to pH 5.6; or in comparison to the MB diluted in buffer. Average data of CFU log10 for compositions of pH 7.4 containing MB/ethanol 10%, MB/ethanol 20% and MB/carrier were 3.99 ± 1.74; 4.04 ± 1.82; 3.82 ± 1.63, respectively. The average microbial reduction of these formulations were 2.47 (P=0.03); 2.42 (P=0.03); and 2.64 (P=0.02), respectively. The other formulations had no significant antimicrobial effect. / Nosso objetivo foi otimizar o efeito fotodinâmico antimicrobiano do azul de metileno (AM) por meio da inclusão de etanol ou carreador de oxigênio na formulação. Biofilmes de Pseudomonas aeruginosa PA01 foram formados sobre discos de acrílico por 5 dias. Formulações fotoativadas continham AM (250 μM) em: água tamponada, etanol 10% (tampão:etanol, 90:10), etanol 20% (tampão:etanol, 80:20) e emulsão com carreador (perfluordecaleno:tampão:triton-X100, 60:35:5). O tampão utilizado foi o Tris-HCl para as soluções em pH 7,4; e acetato de sódio/ácido acético para as soluções em pH 5,6. Biofilmes sem tratamento e expostos ao tampão, etanol 10% e 20% sem fotoativação foram avaliados como controles. Produção de oxigênio singleto foi mensurada pela fotoxidação do 1,3-difenilisobenzofuran (75μM). Dados de foto-oxidação e UFC (log10) foram avaliados por One-Way ANOVA e post hoc Tukey e Dunnett, respectivamente. Teste t-Student avaliou diferenças entre a mesma formulação com diferente pH. Maior produção de oxigênio singleto foi verificada com AM diluído em etanol 10% e 20% no pH 7,4. Contudo, estas formulações não apresentaram diferença estatística em relação ao pH 5,6; ou em comparação ao AM diluído no tampão. Dados médios de UFC log10 para formulações com pH 7,4 contendo AM/etanol 10%, AM/etanol 20%, e AM/carreador foram de 3,99 ± 1,74; 4,04 ± 1,82; 3,82 ± 1,63, respectivamente. A redução microbiana média dessas formulações foi de 2,47 (P=0,03); 2,42 (P=0,03); e 2,64 (P=0,02), respectivamente. As demais formulações não apresentaram efeito antimicrobiano estatisticamente significante. Read more
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Sources environnementales de Mycobacterium ulcerans en Côte d'Ivoire / Environmental sources of Mycobacterium ulcerans in Ivory CoastTian, Roger Bi Diangoné 16 November 2015 (has links)
L’ulcère de Buruli est la troisième mycobactériose la plus prévalente dans le monde après la tuberculose et la lèpre. L’ulcère de Buruli sévit dans au moins 33 pays dont l’Afrique de l’Ouest qui présente la prévalence la plus élevée. Parmi ces pays dans lesquels l’ulcère de Buruli est rapporté, la Côte d’Ivoire dont nous sommes originaires présente la plus forte incidence de 36% déclarée à l’Organisation Mondiale de la Santé. L’ulcère de Buruli est causé par Mycobacterium ulcerans, une mycobactérie environnementale dont le réservoir et les sources de transmission à l’homme, ne sont pas élucidés. Notre revue de la littérature a porté sur les sources environnementales de cette mycobactérie en Afrique de l’Ouest. Sur cette base, nous avons réalisé une vaste campagne de prélèvements d’échantillons environnementaux en Côte d’Ivoire et détecté par PCR en temps réel M. ulcerans dans l’eau stagnante, le sol et les selles d’un mammifère herbivore Thryonomys swinderianus. Ensuite, nous avons prouvé expérimentalement que M. ulcerans pouvait survivre dans le sol pendant au moins quatre mois et que le sol était source d’infection expérimentale par M. ulcerans dans un modèle animal. Ces résultats suggèrent que, en Côte d’Ivoire, l’eau stagnante, le sol et cet animal pourraient jouer un rôle dans le cycle de vie de la bactérie. Dans le second travail, nous avons valorisé des plantes tropicales aquatiques par l’utilisation de leurs extraits dans le milieu de culture de M. ulcerans, mycobactérie à croissance lente pour accélérer sa croissance. Dans le troisième travail, nous avons montré l’efficacité in vitro et dans un modèle animal, du bleu de méthylène contre M. ulcerans. / Buruli ulcer is the third mycobacteriosis in the world after tuberculosis, leprosy. Buruli ulcer is widespread in at least 33 countries including West Africa which has the highest prevalence. Among the countries in which Buruli ulcer is reported, Ivory Coast which we come from has the highest incidence of 36% reported in the World Health Organization. Buruli ulcer is caused by Mycobacterium ulcerans, an environmental mycobacterium whose reservoir and source of transmission to humans, are not understood. Our review of the literature focused on environmental sources of this mycobacterium in West Africa, which converge stagnant aquatic environment. On this basis, we conducted an extensive campaign of environmental sampling in Ivory Coast and detected by real-time PCR M. ulcerans in stagnant water, soil and feces of an herbivorous mammal Thryonomys swinderianus. Then we experimentally proved that M. ulcerans could survive in the soil for at least four months. These results suggest that, in Ivory Coast, stagnant water, soil and animal could play a role in the life cycle of the bacterium. In the second work, we have upgraded aquatic tropical plants by the use of extracts in the culture medium of M. ulcerans, slow growing mycobacteria to accelerate its growth. In the third work, we proposed the methylene blue, less expensive, easy to access as an alternative treatment for Buruli ulcer. It is appropriate to resume the experiment on methylene blue by other teams of researchers and after reproducing our experimental data, suggest the topical use of purified, non-toxic methylene blue in human clinical. Read more
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Etude physico-chimique des possibilités de valorisation des sables argileux non conformes dans des mélanges bitumineux routiers / A mineralogical approach to use the non-qualified fine aggregates in asphalt concrete pavementChen, Chi-Wei 29 March 2016 (has links)
Ma thèse de doctorat doit contribuer à la diminution du gaspillage des ressources naturelles (en particuliers les sables naturels) en étendant leur acceptabilité dans les enrobés bitumineux. La compréhension de l’effet des particules nocives, notamment la fraction argileuse contenue dans les sables, sur le comportement des mélanges bitumineux est visé. Pour évaluer le niveau de nocivité des particules fines, le test d'adsorption du bleu de méthylène noté MB (EN13043, NF EN 933-9) est appliqué, mais un tel test a été modifié à quatre reprises au cours des 22 dernières années tandis que la valeur de bleu limite, utilisée pour déterminer la conformité ou non du sable, n’a pas été modifiée. Le projet de thèse vise à modifier cette valeur limite pour étendre la gamme de sable utilisable. Cet objectif sera atteint grâce à l’identification de la composition minéralogique des sables, une recherche sur la meilleure manière de quantifier les phases qui composent les sables et une meilleure compréhension du rôle de la fraction fine sur la durabilité et les pathologies des mélanges bitumineux. Le travail de thèse est organisé en différentes tâches : 1. Tester le protocole de mesure de la valeur de bleu. Nous voulons comprendre l'effet de différents facteurs (tels que l'échantillonnage, la cinétique des additions de bleu, la température de séchage du sable avant l’essai ...) sur la mesure de la valeur de bleu. Le développement d'un appareil automatique ou d'une nouvelle méthode (qui sera validée par comparaison avec les résultats obtenus à partir de la méthode standardisée) est prévu.2. Établir une corrélation entre la valeur de bleu (ou d'autres paramètres à trouver) et la quantité de phases minérales présentes dans les sables. Un jeu de données a d’ores et déjà été établi au cours de mon stage de master. Pour atteindre cet objectif, les différentes méthodes de quantification (utilisant en particuliers la diffraction de rayons X) doivent être testées et comparées.3. Corréler la valeur de bleu couplée à la nature minéralogique des particules fines avec le comportement mécanique des mélanges sable/bitume. Nous allons étudier la dégradation en présence d’eau des propriétés du matériau bitumineux (par exemple l'adhésion du liant bitumineux sur granulat) et le rôle de la couche de particules fines qui entourent les grains de sable sur les propriétés mécaniques de ce matériau. Nous espérons comprendre en particulier l'effet de la présence d’argile gonflante dans les matériaux constitutifs de la chaussée bitumineuse.4. Améliorer le comportement des granulats non conformes par l’application d’un traitement. Après l'identification de l'origine des pathologies (nous faisons l'hypothèse que les argiles gonflantes jouent un rôle majeur), nous proposons d'appliquer un traitement en ajoutant de la chaux (ou de traiter en ajoutant des déchets qui contiendraient des substances actives comme la chaux), et de tester également l’utilisation de polymères ou du greffage avec des composés organiques des argiles comme traitement / Siliceous fines (clays) in fine aggregates used for AC pavement stimulate the moisture entering the bitumen-aggregates interface in AC mixture and create channels for water penetration. MB adsorption for qualifying fine aggregates is in accordance with the layer charge and the accessibility of consisted mineralogy in fine aggregates. However, the correlation between MB qualification for fine aggregates and fine aggregates triggering moisture susceptibility of AC mixture has not ever been addressed; moreover, the questions from MB adsorption still remain to be solved. In order to evaluate the stripping and to clarify MB adsorption on fine aggregates from a mineralogical perspective, the most common clays in natural aggregates, kaolinite, illite and montmorillonite, were extracted from their clay rocks, and used to prepare thin clay film, artificial fine aggregates and asphalt concrete mixtures consist of artificial fine aggregates. Moreover, the 5 blinded fine aggregates received from quarries without any given information were applied as the blinded experiments to confirm the practicability with mineralogical diversity. The mineralogical analysis was identifying and quantifying the mineral phases in extracted clay and fine aggregates by using X-Ray diffraction, and the quantitative results were judged by complementary test. MB adsorption was studied using drop method, UV-Photometer method and cation exchange capacity from clays and aggregates. Water-bitumen-clay interaction was studied using the sessile drop and the Oliensis spot tests on those thin clay films. The water intrusion routes in AC mixture was investigated immersing AC mixture in solution with chemical probe, whereas Duriez tests allowed measuring the moisture susceptibility of AC mixtures containing varied clay mineralogy in fine aggregates. The results show that clay mineralogy is in relation to water-bitumen-clay interaction, and it is agreed by moisture susceptibility of AC mixture indicated by Duriez test. With the dispersive nature bitumen used in this study, cohesive failure is in the light of kaolinite-AC mixture in the presence of water, whereas swelling property is responsible for the stripping in illite- and montmorillonite- AC mixture. In order to exclude the physical interferences on MB adsorption, the vale of 100% of MB adsorption on fine aggregates referred to CEC value is necessary to apply, and MB value measured from drop method efficiently excludes the significant impacts from layer charge, pH value and exchangeable cations. Although MB adsorption is in relation to clay mineralogy, this test does not sufficiently indicate the stripping of AC mixture occurred by clay in fine aggregates. There are still rooms to use the non-qualified fine aggregates for the use of AC pavement. As Rietveld method from X-Ray diffraction derives the most reasonable quantitative results, the X-Ray powder diffraction and the X-Ray orientated EG treated K-saturated clay diffraction are proposed for analyzing clay mineralogy and its swelling property for judging the use of non-qualified fine aggregates for AC mixture.MB2 and Duriez0.8 surfaces can be established on clay mineralogical map since we discovered MB adsorption and moisture susceptibility are related to clay mineralogy in fine aggregates. The fine aggregates which is not qualified by MB adsorption is going to confirm the possibility for the use of AC pavement by the mineralogical analysis through X-Ray diffraction. By adopting the quantitative results of clay on mineralogical map with Duriez0.8 surface and the swelling property of clays in fine aggregates, the use of fine aggregates for AC pavement can be properly judged according to water-bitumen-aggregates interaction and stripping which has been proved in this study Read more
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Compact photocatalytic reactors for water treatment : mass and photon transfer issues / Conception, caractérisation et application d'un réacteur photocatalytique compact pour le traitement de l'eau en espace restreintZhou, Shuzhen 19 December 2014 (has links)
Le but de ce travail est de concevoir, opérer et caractériser un réacteur photo-catalytique compact qui opère en régime non limité par le transfert de matière et le transfert de la lumière. Plus particulièrement, il s'agit de traiter de l'eau polluée par un principe pharmaceutique, le diclofénac (DCF) dans un pilote à l'échelle du laboratoire et, essentiellement, de fournir les données quantitatives pour le dimensionnement d'un pilote industriel. La fabrication du dépôt du photocatalyseur TiO2, la désactivation, les transferts interne et externe de matière et l'extinction lumineuse dans la couche de TiO2 ont été étudiés expérimentalement. Les paramètres opératoires – débits, concentration initiale de MB et d'oxygène, intensité lumineuse, épaisseur du dépôt – ont été variés. Un modèle de simulation du réacteur a été construit qui incorpore les transferts externe et interne de matière et l'extinction lumineuse dans le cas d'une molécule modèle, le bleu de méthylène (MB). Enfin, à l'aide d'outils de résolution numérique, les paramètres du modèle ont été déterminées. Cette méthodologie a ensuite été appliquée partiellement à la molécule cible, le DCF, en combinant hydrogénation et photocatalyse. Pour le dépôt de catalyseur (TiO2-P25), la méthode de dépôt par gouttes a été sélectionnée car conduisant à une large gamme d'épaisseurs. La densité du catalyseur déposé a été déterminée ce qui a permis de mettre au point une méthode d'évaluation rapide de l'épaisseur du film par simple pesée. Le coefficient d'extinction du rayonnement UV utilisé dans ce travail à travers le film de TiO2 a été déterminé et comparé favorablement avec les données de la bibliographie. Le composé DCF a été dégradé par hydrogénation et par oxydation photocatalytique. L'hydrogénation se révèle être une méthode de choix pour l hydrodéchloration et l'hydrodéaromatisation du DCF dans l'eau en présence d'un catalyseur au ruthénium déposé sur charbon actif (5%Ru, 59.7% H2O, type H 101B Degussa) à 60°C et 25 bars. Les résultats de cette recherche peuvent potentiellement s'appliquer à d'autres secteurs industriels où des systèmes compacts sont nécessaires / In this work, we aim to overcome photon transfer limitations and mass transfer limitations to design, operate and characterize a compact photocatalytic reactor to remove the pharmaceutical pollutant diclofenac (DCF) in a laboratory pilot reactor, and further to produce metrics for the design of a full scale industrial pilot. Metrics include rate law for pollutant degradation, optimal photocatalytic film thickness, catalyst deactivation law, light distribution, geometry, etc. under process conditions. Catalyst deposition, kinetics, catalyst deactivation; external and internal mass transfer and UV light diffusion in TiO2 film, etc. were studied with a model molecule methylene blue (MB) and operation parameters - flow rate, initial concentration of MB, light intensity, thickness of catalyst film, dissolved oxygen, etc - on MB photocatalytic degradation were investigated. A reactor model was built considering the mass transfer and light extinction issues. Numerical integration was performed to fit the experimental data to determine the intrinsic rate constant and order of light intensity. This methodology was then applied albeit partially to the targeted DCF, combined photocatalysis together with hydrogenation technology. Drop-coating method was chosen mainly for catalyst deposition and a wide range of catalyst (TiO2 P25) film was got with this method. A method to get and use the density of the catalyst film was performed to determine the thickness of deposited catalyst film. The extinction coefficients of the Pyrex glass and TiO2-P25 film were measured experimentally and compatible with literature data. DCF was degraded by photocatalysis and hydrogenation. Hydrogenation was proved to be effective for hydrodechlorination and hydrodearomatisation of DCF in water in the presence of Ru/C catalyst (5% Ru, Type H 101B Degussa) at 60°C and around 25 bars. This research can also be applied to other industrial sectors (off-shore platforms, “inside-thecity” production units, etc.) where such compact process may be required Read more
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Otimização da inativação fotodinâmica de E. coli por fotossensibilizadores veiculados por nanopartículas de sílica / Optimization of the photodynamic inactivation of E. coli by photosensitizers carried by silica nanoparticlesLarissa Souza Amaral 03 February 2016 (has links)
A nanotecnologia tem sido aplicada para o desenvolvimento de materiais para diversas aplicações inclusive na inativação de patógenos. As nanopartículas de sílica (npSi) destacam-se pela alta área superficial, facilidade na alteração da superfície para aumento da eficiência adsortiva, penetrabilidade e toxicidade para bactérias gram-negativas sendo biocompatíveis para células de mamíferos e mais foto-estáveis que a maioria dos compostos orgânicos. Devido as suas vantagens, as npSi podem ser usadas para veicular fotossensibilizadores (FSs) uma vez que permitem sua utilização em solução aquosa em que os FSs geralmente são insolúveis. Além disso, o uso de FSs em vez de antibióticos, permite a inativação microbiológica pela Terapia Fotodinâmica sem que as bactérias adquiram resistência por mecanismos genéticos. Esse processo ocorre pela interação entre um FS, luz e oxigênio molecular produzindo oxigênio singleto que é extremamente reativo danificando estruturas celulares. O objetivo desse estudo foi otimizar a fotoinativação dinâmica de E .coli utilizando Azul de Metileno (AM) e Azul de Toluidina O (ATO) veiculados por npSi. As npSi foram preparadas pela metodologia sol-gel, caracterizadas por microscopia eletrônica de varredura (MEV) e submetidas à adsorção de AM e ATO em sua superfície. A presença de AM e ATO na superfície das npSi foram analisadas por espectroscopia no infravermelho; espectroscopia de fluorescência por raio-X e análise termogravimétrica. O planejamento experimental, iniciado pelo fatorial 23 e modelado ao composto central em busca das condições ótimas foi adotado pela primeira vez nessa aplicabilidade, visando a fotoinativação de E. coli empregando AM e ATO em solução e em seguida com npSi. AM e ATO veiculados por npSi permitem a fotoinativação em concentrações mais baixas de FS (20 e 51% respectivamente), causando desestruturação da integridade bacteriana demonstrada por MEV. Os resultados sugerem que a veiculação de AM e ATO por npSi é extremamente efetiva para a fotoinativação dinâmica de E. coli e que o planejamento composto central pode levar à completa inativação das bactérias. / Nanotechnology has been applied to the development of materials for several apllications inclusive inactivation of pathogens. The silica nanoparticles (npSi) are distinguished by high surface area, ease of change the surface in order to increase the adsorption efficiency, penetrability and toxicity in gram-negative bacteria being biocompatible with mammalian cells and more photo-stable than most the organic compounds. Due to its advantages, npSi can be used to carry photosensitizers (PSs) since they allow its use in aquous solution in which PSs are frequently insoluble. Furthermore, the use of PSs instead of antibiotics, allows the microbiological inactivation by Photodynamic Therapy without bacteria to develop resistance by genetic mechanisms. This process occurs by the interaction among a PS, light and molecular oxygen producing singlet oxygen, which is extremely reactive, causing damage to cellular structures. The aim of this study was to optimize the photoinactivation of E. coli using Methylene Blue (MB) and Toluidine Blue O (TBO) carried by npSi using the central composite design. The npSi were prepared by sol-gel method, characterized by scanning electron microscopy (SEM) and subjected to adsorption of MB and TBO on its surface. The presence of FSs on the surface of npSi were analyzed by infrared spectroscopy, fluorescence X-ray spectroscopy and thermogravimetric analysis. The experimental design, initiated by the factorial 23 and modeled by the central composite in search of the optimal conditions was adopted for the first-time for this applicability, aiming the E. coli photoinactivation employing MB and TBO in solution and then with npSi. MB and TBO carried by npSi allowed the photoinactivation in lower concentrations of PS (20 and 51% respectively), causing disruption of bacterial integrity demonstrated by SEM. The results suggest that MB and TBO carried by npSi are extremely effective for dynamic photoinactivation of E. coli and the central composite design can lead to complete inactivation of bacteria. Read more
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Avaliação histopatológica do tratamento do carcinoma espinocelular cutâneo em camundongos usando terapia fotodinâmica mediada por azul de metileno. / Histopathological evaluation of the treatment of cutaneous squamous cell carcinoma in mice using photodynamic therapy mediated by methylene blue.Ana Paula da Silva 18 August 2014 (has links)
A terapia fotodinâmica (TFD) é uma modalidade clínica para tratar uma variedade de neoplasias, doenças de pele e representa um promissor tratamento estético. O presente trabalho avaliou os aspectos histopatológicos e moleculares do tratamento pela TFD mediada por azul de metileno (TFD-AM) no modelo experimental in vivo do Carcinoma Espinocelular Cutâneo (CEC) e na pele sadia de camundongos Swiss. O protocolo da TFD foi de uma única sessão, com aplicação da solução de AM a 1% seguido por irradiação com laser diodo na dose total de 24 J/cm2 nos tecidos tumorais e sadios. Os animais foram sacrificados em dois períodos, 24 horas e 15 dias após TFD. Alterações morfológicas foram pouco marcantes nos tecidos tumorais tratados, entretanto, foram mais pronunciadas nos tecidos sadios. Podemos concluir que os efeitos de uma única sessão da TFD mediada pelo AM na dose aplicada não conferiu melhora no tratamento do CEC. Estes resultados motivam novos estudos com ajustes no protocolo para melhorar a eficácia desta terapia. / Photodynamic therapy (PDT) is a clinical method for treating a variety of tumors, skin disorders and represents a promising cosmetic treatment. This study evaluated the histopathological and molecular aspects of the treatment by PDT mediated by methylene blue (PDT-MB) in vivo experimental model of cutaneous squamous cell carcinoma (SCC) and in healthy skin of swiss mice. The PDT protocol was a single session with the application of MB 1% solution followed by irradiation with diode laser at a total dose of 24 J/cm2 in tumor and healthy tissue. The animals were sacrificed at two periods, 24 hours and 15 days after PDT. Morphological changes were less marked in the tumor tissues treated, however, were more pronounced in healthy tissues treated. We can conclude that the effects of a single session of PDT mediated by MB in applied dose conferred no improvement in the treatment of SCC. These results motivate further studies with adjustments in the protocol to improve the effectiveness of this therapy. Read more
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