Comparação entre metodologias de extração de HPAs em água utilizando um planejamento fatorial com quantificação no CG/EM

PAHs (Polycyclic Aromatic Hydrocarbons) are a group of organic substances which receive considerable attention because of the carcinogenic and mutagenic properties of some of them. It is therefore important to determine the PAHs in different environmental matrices. Several studies have shown the use of gas chromatography coupled to mass spectrometry as a technique for quantification of PAHs by presenting excellent detection limits. This study aimed to develop an analytical methodology for the determination of 16 PAHs listed by the USEPA, test two methods for extraction of PAHs in water from a 23 factorial design, quantify them through the analytical technique coupled to gas chromatography mass spectrometry (GC/MS) using the method developed, and finally apply the results in chemometrics. The sample was synthesized and subjected to tests of the 23 factorial design, which has the factors: the type of extraction technique (ultrasound and digester), the ratio solvent / sample (1:1 and 1:3) and the type of solvent (dichloromethane / hexane and acetone / dichloromethane). The responses of eight combinations of the factorial design were obtained from the quantification by external calibration in GC/MS. The quantification method was developed from an optimized adaptation of the USEPA Method 8270. We used the full scan mode as a way of acquiring the mass spectra of 16 PAHs. The time in which the samples were subjected to ultrasound was fixed at 10 min and held an investigation to establish the conditions of power and time in the digester. We had the best response in the investigation of the digester power of 100 watts and the time of six minutes. The factorial design of liquid-liquid extraction showed that the most representative factors were: the use of the digester as extraction technique, the ratio solvent / sample 1:1 and the use of a 1:1 mixture of dichloromethane / hexane as a solvent more suitable. These results showed that the 1:1 mixture of dichloromethane / hexane is an excellent mixture to recover the extraction of PAHs an aqueous sample using the microwave digester. The optimization of the method of separation, identification and quantification of PAHs in the GC/MS was valid for 16 PAHs present in each chromatogram of the samples

Estudo da viabilização do uso da mistura híbrida ferrocarbonila / ferrita de NI0,5Zn0,5Fe2o4 como material absorvedor de radiação eletromagnética

Were synthesized ferrites of NiZn on systems Ni0,5Zn0,5Fe2O4, the precursors citrate method. The decomposition of the precursors was studied by thermogravimetric analysis and spectroscopy in the infrared region, the temperature of 350°C/3h. The evolution of the phases formed after calcinations at 350ºC/3h, 600, 1000 and 1100ºC/2h was accompanied by X-ray diffraction using the Rietveld refinement method for better identification os structures formed. Was observed for samples calcined at different temperatures increased crystallinity with increasing calcination temperature, being observed for the samples calcined at 900 and 1100 º C/2h was the precipitation of a secondary phase, the phase hematite. The ferrocarbonila of industrial origin was analyzed by X-ray diffraction and Rietveld for the identification of its structure. The carbonyl iron was added NiZn ferrite calcined at 350ºC/3h, 600, 900, 1000 and 1100ºC/2h to the formation of hybrid mixtures. They were then analyzed by Xray diffraction and Rietveld. The NiZn ferrite and ferrocarbonila as well as the hybrid mixtures were subjected to analysis of scanning electron microscopy, magnetic measurements and reflectivity. The magnetic measurements indicated that the ferrite, the ferrocarbonila, as well as hybrid mixtures showed characteristics of soft magnetic material. The addition of ferrocarbonila in all compositions showed an increase in the results of magnetic measurements and reflectivity. Best result was observed in the increase of the magnetization for the hybrid mixture of Ferrocarbonila / ferrite of NiZn calcined at 600ºC/2h. The mixture Ferrocarbonila / ferrite calcined 1000°C/2h presented better absorption of electromagnetic radiation in the microwave

Secagem de misturas de polpa de frutas tropicais em leito de jorro

Drying of fruit pulps in spouted beds of inert particles has been indicated as a viable technique to produce fruit powders. Most of the processes employed to produce dried fruit pulps and juices, such as Foam Mat, encapsulation by co-crystallization and spray drying utilize adjuvant and additives (such as thickeners, coating materials, emulsifiers, acidulants, flavors and dyes), which is not always desirable. The fruit pulp composition exerts an important effect on the fruit powder production using a spouted bed. In the study by Medeiros (2001) it was concluded that lipids, starch and pectin contents play an important role on the process performance, enhancing the powder production; however, the drying of fruit pulps containing high content of reducing sugars (glucose and fructose) is practically unviable. This work has the objective of expanding the studies on drying of fruit pulps in spouted bed with aid of adjuvant (lipids, starch and pectin) aiming to enhance the dryer performance without jeopardizing the sensorial quality of the product. The optimum composition obtained by Medeiros (2001) was the basis for preparing the mixtures of pulps. The mixture formulations included pulps of mango (Mangifera indica), umbu (Spondias tuberosa) and red mombin (Spondia purpurea) with addition of cornstarch, pectin and lipids. Different products were used as lipids source: olive and Brazil nut oils, coconut milk, heavy milk, powder of palm fat and palm olein. First of all, experiments were conducted to define the best formulation of the fruit pulps mixture. This definition was based on the drying performance obtained for each mixture and on the sensorial characteristics of the dry powder. The mixture formulations were submitted to drying at fixed operating conditions of drying and atomizing air flow rate, load of inert particles, temperature and flow rate of the mixture. The best results were obtained with the compositions having powder of palm fat and palm olein in terms of the drying performance and sensorial analysis. Physical and physicochemical characteristics were determined for the dry powders obtained from the mixtures formulations. Solubility and reconstitution time as well as the properties of the product after reconstitution were also evaluated. According to these analyses, the powder from the mixtures formulations presented similar characteristics and compatible quality to those produced in other types of dryers. Considering that the palm olein is produced in Brazil and that it has been used in the food industry substituting the palm fat powder, further studies on drying performance were conducted with the composition that included the palm olein. A complete factorial design of experiments 23, with three repetitions at the central point was conducted to evaluate the effects of the air temperature, feeding flow rate and intermittence time on the responses related to the process performance (powder collection efficiency, material retained in the bed and angle of repose of the inert particles after the process) and to the product quality (mean moisture content, loss of vitamin C and solubility). Powder production was uniform for the majority of the experiments and the higher efficiency with lower retention in the bed (59.2% and 1.8g, respectively) were obtained for the air temperature of 80°C, mixture feed rate of 5ml/min in intervals of 10 min. The statistical analysis of the results showed that the process variables had individual or combined significant influences on the powder collection efficiency, material retention in the bed, powder moisture content and loss of vitamin C. At the experimental ranges of this work, the angle of repose and solubility were not influenced by the operating variables. From the results of the experimental design, statistical models were obtained for the powder moisture content and loss of vitamin C

Estudo das características magnéticas e absorvedoras das ferritas de nizn, niznmn, mnzn, nimg, nicuzn e nicuznmg obtidas via método do citrato precursor

Were synthesized systems Ni0,5Zn0,5Fe2O4, i0,2Zn0,5Mn0,3Fe2O4, Mn0,5Zn0,5Fe2O4, Ni0,5Mg0,5Fe2O4, Ni0,2Cu0,3Zn0,5Fe2O4 and Ni0,2Cu0,3Zn0,5Mg0,08Fe2O4, the precursors citrate method. The decomposition of the precursors was studied by thermogravimetric analysis and spectroscopy in the infrared region, the temperature of 350°C/3h. The evolution of the phases formed after calcinations at 350, 500, 900 and 1100ºC/3h was accompanied by X-ray diffraction using the Rietveld refinement to better identify the structures formed. The materials were also analyzed by scanning electron microscopy, magnetic measurements and analysis of the reflectivity of the material. The samples calcined at different temperatures showed an increase of crystallinity with increasing calcination temperature, verifying that for some compositions at temperatures above 500°C precipitates of second phase such as hematite and CuO. The compositions of manganese present in the structure diffusion processes slower due to the ionic radius of manganese is greater than for other ions substitutes, a fact that delays the stabilization of spinel structure and promotes the precipitation of second phase. The compositions presented with copper precipitation CuO phase at a temperature of 900 and 1100ºC/3h This occurs according to the literature because the concentration of copper in the structure is greater than 0.25 mol%. The magnetic measurements revealed features of a soft ferrimagnetic material, resulting in better magnetic properties for the NiZn ferrite and NiCuZnMg at high temperatures. The reflectivity measurements showed greater absorption of electromagnetic radiation in the microwave band for the samples calcined at 1100ºC/3h, which has higher crystallite size and consequently the formation of multi-domain, increasing the magnetization of the material. The results of absorption agreed with the magnetic measurements, indicating among the ferrites studied, those of NiZn and NiCuZnMg as better absorbing the incident radiation.

Síntese, caracterização e estudo das propriedades magnéticas de ortoferritas de lantânio dopadas com manganês

Orthoferrites AFeO3 (A = rare earth) are an important class of perovskite oxides that exhibit weak ferromagnetism. These materials find numerous applications as chemical sensors, cathodes for fuel cells and catalysis, which make them interesting from the standpoint of science and technology. Their structural, electrical and magnetic properties are dependent on many factors such as the preparation method, heat treatment conditions, chemical composition and replacement of cations in sites A and/or B. In this paper, LaFe1-xMnxO3 (0 ≤ x ≤ 1) orthoferrites-type was prepared by Pechini method and Microwave-assisted combustion reaction in order to evaluate the influence of synthesis route on the formation of oxide, as well as the effect of parcial replacement of iron by manganese and heat treatment on the magnetic properties. The precursor powders were calcined at 700°C, 900°C, 1100°C and 1300°C for 4 hours and they were characterized by the techniques: Thermogravimetric analysis (TGA), X ray diffraction (XRD), Refinement by Rietveld method, Scanning electron microscopy (SEM), Reduction temperature programmed (RTP) and Magnetic hysteresis measurements performed at room temperature. According to the XRD patterns, the formation of perovskite phase with orthorhombic structure was observed for the systems where 0 ≤ x ≤ 0.5 and rhombohedral for x = 1. The results also showed a decrease of lattice parameters with the parcial replacement of iron by manganese and consequently a reduction in cell volume. The hysteresis curves exhibited weak ferromagnetism for the systems prepared by both synthesis methods. However, a dependence of magnetization as a function of dopant content was observed for samples produced by Pechini method. As for the systems prepared by combustion reaction, it was found that the secondary phases exert a strong influence on the magnetic behavior

Reforma a vapor catalítica do metano: Otimização da produção e seletividade em hidrogênio por absorção in situ do CO2 produzido

Topics of research related to energy and environment have significantly grown in recent years, with the need of its own energy as hydrogen. More particularly, numerous researches have been focused on hydrogen as energy vector. The main portion of hydrogen is presently obtained by reforming of methane or light hydrocarbons (steam, oxy, dry or auto reforming). During the methane steam reforming process the formation of CO2 undesirable (the main contributor to the greenhouse effect) is observed. Thus, an oxide material (sorbent) can be used to capture the CO2 generated during the process and simultaneously shifting the equilibrium of water gas shift towards thermodynamically more favorable production of pure hydrogen. The aim of this study is to develop a material with dual function (catalyst/sorbent) in the reaction of steam reforming of methane. CaO is well known as CO2 sorbent due to its high efficiency in reactions of carbonation and easy regeneration through calcination. However the kinetic of carbonation decreases quickly with time and carbonation/calcination cycles. A calcium aluminate (Ca12Al14O33) should be used to avoid sintering and increase the stability of CaO sorbents for several cycles. Nickel, the industrial catalyst choice for steam reforming has been added to the support from different manners. These bi-functional materials (sorbent/catalyst) in different molar ratios CaO.Ca12Al14O33 (48:52, 65:35, 75:25, 90:10) were prepared by different synthesis methodologies, among them, especially the method of microwave assisted self-combustion. Synthesis, structure and catalytic performances of Ni- CaO.Ca12Al14O33 synthesized by the novel method (microwave assisted selfcombustion) proposed in this work has not being reported yet in literature. The results indicate that CO2 capture time depends both on the CaO excess and on operating conditions (eg., temperature and H2O/CH4 ratio). To be efficient for CO2 sorption, temperature of steam reforming needs to be lower than 700 °C. An optimized percentage corresponding to 75% of CaO and a ratio H2O/CH4 = 1 provides the most promising results since a smaller amount of water avoids competition between water and CO2 to form carbonate and hydroxide. If this competition is most effective (H2O/CH4 = 3) and would have a smaller amount of CaO available for absorption possibly due to the formation of Ca(OH)2. Therefore, the capture time was higher (16h) for the ratio H2O/CH4 = 1 than H2O/CH4 = 3 (7h) using as catalyst one prepared by impregnating the support obtained by microwave assisted self-combustion. Therefore, it was demonstrated that, with these catalysts, the CO2 sorption on CaO modifies the balance of the water gas-shift reaction. Consequently, steam reforming of CH4 is optimized, producing pure H2, complete conversion of methane and negligible concentration of CO2 and CO during the time of capture even at low temperature (650 °C). This validates the concept of the sorption of CO2 together with methane steam reforming

Síntese e caracterização de ferritas de níquel dopadas com cobalto e efeito da substituição nas suas propriedades magnéticas

The ferrite composition Ni1 - xCoxFe2O4 (0 ≤ x ≤ 0.75) were obtained by the method of microwave assisted synthesis and had their structural and magnetic properties evaluated due to the effect of the substitution of Ni by Co. The compounds were prepared: according to the concept of chemical propellants and heated in the microwave oven with power 7000kw. The synthesized material was characterized by absorption spectroscopy in the infrared (FTIR), Xray diffraction (XRD) using the Rietveld refinement, specific surface area (BET) , scanning electron microscopy (SEM) with aid of energy dispersive analysis (EDS) and magnetic measurements (MAV). The results obtained from these techniques confirmed the feasibility of the method of synthesis employed to obtain the desired spinel structure, the ferrite, nickel ferrite as for nickel doped with cobalt. The results from XRD refinement ally showed the formation of secondary phases concerning stages α - Fe2O3, FeO, (FeCo)O e Ni0. On the other hand, there is an increase in crystallite size with the increase of cobalt in systems, resulting in an increased crystallinity. The results showed that the BET systems showed a reduction in specific surface area with the increase of cobalt and from the SEM, the formation of irregular porous blocks and that the concentration of cobalt decreased the agglomerative state of the system. The magnetic ferrites studied showed different characteristics according to the amount of dopant used, ranging from a very soft magnetic material (easy magnetization and demagnetization ) - for the system without cobalt - a magnetic material with a little stiffer behavior - for systems containing cobalt. The values of the coercive field increased with the increasing growth of cobalt, and the values of saturation magnetization and remanence increased up to x = 0,25 and then reduced. The different magnetic characteristics presented by the systems according to the amount of dopant used, allows the use of these materials as intermediates magnetic

Uma nova proposta de antena planar multibanda para comunicações móveis

The great interest observed in wireless communication systems has required the development of new configurations of microstrip antennas, because they are easily built and integrated to other microwave circuit components, which is suitable for the construction and development of planar antenna arrays and microwave integrated circuits. This work presents a new configuration of tapered microstrip antenna, which is obtained by impressing U-slots on the conducting patch combined with a transmission line matching circuit that uses an inset length. It is shown that the use of U-slots in the microstrip antenna conducting patch excites new resonating modes, that gives a multiband characteristic for the slotted microstrip antenna, that is suitable for applications in communication systems that operates several frequencies simultaneously. Up to this date, the works reported in the literature deals with the use of Uslotted microstrip rectangular antennas fed by a coaxial probe. The properties of a linear array of microstrip patch tapered antennas are also investigated. The main parameters of the U slotted tapered microstrip antennas are investigated for different sizes and locations of the slots impressed on the conducting patch. The analysis of the proposed antenna is performed by using the resonant cavity and equivalent transmission line methods, in combination with a parametric study, that is conducted by the use of the Ansoft Designer, a commercial computer aided microwave software well known by its accuracy and efficiency. The mentioned methods are used to evaluate the effect in the antennas parameters, like resonant frequency and return loss, produced by variations of the antenna structural parameters, accomplished separately or simultaneously. An experimental investigation is also developed, that consists of the design, construction and measurement of several U slotted microstrip antenna prototypes. Finally, theoretical and simulated results are presented that are in agreement with the measured ones. These results are related to the resonating modes identification and to the determination of the main characteristics of the investigated antennas, such as resonant frequency, return loss, and radiation pattern

Densificação e microestrutura de um compósito Mo-Cu preparado a partir de um pó de heptamolibidato de amônia e cobre

The Cu-Mo system is a composite used in the electrical industry as material for electrical contact and resistance welding electrode as well as the heat sink and microwave absorber in microelectronic devices. The use of this material in such applications is due to the excellent properties of thermal and electrical conductivity and the possibility of adjustment of its coefficient of thermal expansion to meet those of materials used as substrates in the semiconductor micoreletrônic industry. Powder metallurgy through the processes of milling, pressing shaping and sintering is a viable technique for consolidation of such material. However, the mutual insolubility of both phases and the low wettability of liquid Cu on Mo impede its densification. However, the mutual insolubility of both phases and the low wettability of liquid Cu on Mo impede its densification. The mechanical alloying is a technique for preparation of powders used to produce nanocrystalline composite powder with amorphous phase or extended solid solution, which increases the sinterability immiscible systems such as the Mo-Cu. This paper investigates the influence of ammonium heptamolybdate (HMA) and the mechanical alloying in the preparation of a composite powder HMA-20% Cu and the effect of this preparation on densification and structure of MoCu composite produced. HMA and Cu powders in the proportion of 20% by weight of Cu were prepared by the techniques of mechanical mixing and mechanical alloying in a planetary mill. These were milled for 50 hours. To observe the evolution of the characteristics of the particles, powder samples were taken after 2, 10, 15, 20, 30 and 40 hours of milling. Cylindrical samples 5 to 8 mm in diameter and 3 to 4 mm thickness were obtained by pressing at 200 MPa to the mixed powders so as to ground. These samples were sintered at 1200 ° C for 60 minutes under an atmosphere of H2. To determine the effect of heating rate on the structure of the material during the decomposition and reduction of HMA, rates of 2, 5 and 10 ° C / min were used .. The post and the structures of the sintered samples were characterized by SEM and EDS. The density of the green and sintered bodies was measured using the geometric method (weight / volume). Vickers microhardness with a load of 1 N for 15 s were performed on sintered structures. The density of the sintered structures 10 ° C / min. reached 99% of theoretical density, how the density of sintered structures to 2 ° C / min. reached only 90% of the theoretical density

Transportadores sólidos de oxigênio à base de níquel e cobre suportados em aluminatos para combustão do metano pela tecnologia de recirculação química

In recent years, solid carriers suitable oxygen have been developed for use in different chemical processes recirculation. The success of this technology is directly related to the chemical reactivity and the oxygen storage capacity of the carrier. Thus, research into the development of new materials that can be applied to the process becomes extremely important. Possible candidates are the carriers based on nickel and copper for presenting favorable thermodynamic properties. In this work, aluminates type MAl2O4 (M = Mg and Ca) and M0,9B0,1Al2O4 (B = Ni and Cu) that are used as supports were synthesized by combustion reactions assisted by microwave and calcined at 900°C/2h. Then, the carriers were impregnated with 10% (m/m) of nickel or copper, and subsequently calcined at 600°C/2h to obtain the solid oxygen carriers, which were characterized by X-ray diffraction (XRD) Microscopy scanning electron microscopy (SEM) and temperature programmed reduction (TPR). Reactions simulating the combustion process by chemical recirculation were performed by cycles reduction/oxidation, in order to evaluate the reactivity of carriers. XRD analysis revealed diffraction peaks of the spinel type structures. In the doped substrates were verified the presence of secondary phases, suggesting that all the metal was incorporated into the spinel structure. In solid oxygen carriers, the NiO and CuO phases were observed after impregnation of active phases on different media. The results of evaluations of chemical cycles reduction/oxidation revealed that TSO's impregnated with nickel in various media were more active and are potential candidates for use in the chemical recirculation technology

Síntese de carreadores de oxigênio à base de Ni e Co para estudo do processo de Chemical Looping usando CH4 como combustível

Increasing energy demand is being met largely by fossil fuel reserves, which emit CO2, SOx gases and various other pollutants. So does the search for fuels that emit fewer pollutants and have the same energy efficiency. In this context, hydrogen (H2) has been increasingly recognized as a potential carrier of energy for the near future. This is because the H2 can be obtained by different routes and has a wide application area , in addition to having clean burning, generating only H2O as a product of combustion , and higher energy density per unit mass . The Chemical Looping Reforming process (CLR) has been extensively investigated in recent years, it is possible to regenerate the catalyst by applying cycles of reduction and oxidation. This work has as main objective to develop catalysts based on nickel and cobalt to study the reactivity of reform with chemical recycling process. The catalysts were prepared by three different methods: combustion assisted by microwave, wet impregnation and co-precipitation. All catalysts synthesized have the same amount by weight of the active phases (60% w / w). The other 40 % m/m consists in La2O3 (8% w / w), Al2O3 (30% w / w) and MgO (2%). Oxygen carriers have been named as follows: N or C, nickel or cobalt, followed by the number 3 or 6, meaning 30 to 60% of active phase in the oxide form and C, CI or CP, which means self-combustion assisted by microwave, self-combustion assisted by microwave followed by wet impregnation and co-precipitation. The oxygen carriers were then characterized by the techniques of X-ray diffraction (XRD), surface area (BET), temperature programmed reduction (TPR) and scanning electron microscopy (SEM). The characterization results showed that the different synthesis methods have led to obtaining different morphologies and structures. Redox tests using CH4 as reducing agent and sintetic air as oxidant agent was done with N6C and C6C, N6CI and C6CI and N6CP and C6CP oxygen carriers. The tests revealed different behaviors, depending on active phase and on synthesis procedure. N6C oxygen carrier produced high levels of H2. The C6CI oxygen carrier produced CO2 and H2O without carbon deposits.

Projeto de absorvedores de micro-ondas integrados com superfícies seletivas em frequência

Considering the fact that, the use of wireless communication systems has grown too fast, investigations concerning absorbers of electromagnetic waves has called closer attention of researchers. It is applicable from indoor systems to military applications. Paralleling with this growth, some extremely relevant investigations through Frequency Selective Surfaces (FSS) allows its filter property to be applicable in several systems, for example: reflector antennas, band-pass radomes, and absorbers, which are the main objective of this work. Therefore, the main goal of this work concerns to design micro-waves absorbers through FSS. Thus, the methodology consists basically in two steps: the first step concerns a theoretical and numerical analysis of the structures involved in the process of absorption, the second step, the analysis of the cascaded structures. In order to carry out the analysis, the Equivalent Circuit Method will be used. This method provides characteristics of transmission from the structure, for a plane wave incidence and it requires an extremely limited computing resource in relation if compared to full wave analyses method. Hence, it is useful to allow fast predictions of the development of the structures. Furthermore, a spreading matrix will be used in order to cascade the conductive FSS and the resistive FSS achieving absorption characteristics in the designed band. The experimental results used for the analysis are found in the literature due to the difficulty of building soon, given that it is not a simple construction technique. To conclude, a mathematical development through the Equivalent Circuit Method of a FSS modeling with cross-dipole geometry and a resistive FSS will be presented, as well as the cascading involving the two structures. The same setting is used with a square loop geometry. Besides it, the next steps will be discussed in the conclusion.

Caracterização de superfícies seletivas de frequência de periódicas e não-periódicas

The past years have seen a great interest in the use of frequency selective surfaces (FSS), as spatial filters, in many microwave applications. Among these, we highlight applications in telecommunication systems (such as satellite communications and radar), high gain antennas (combined with planar antennas) and (home and industrial) microwave ovens. The FSS is usually composed of two-dimensional periodic arrays, with equally spaced elements, which may be metallic patches (printed on dielectric substrates) or aperture (holes in thin metal surfaces). Using periodic arrays, the FSS have been able to meet the demands of the telecommunications industry. However, new demands are finding technological limitations. In this context, adverse filtering requirements have forced designers to use FSS optimization methods to find specific formats of FSS elements. Another alternative that has been used to increase the selectivity of the FSS is the cascaded FSS, a simple technique that has as main drawback the increased dimensions of the structure, as well as its weight. This work proposes the development of a new class of selective surfaces frequency (FSS) composed of quasi-periodic (or non-periodic) arrangements. The proposed FSS have no array periodicity, in relation with the spatial position of their elements. The frequency responses of these structures were simulated using commercial softwares that implement full-wave methods. For the purpose of validation of this study, FSS prototypes were built and measured, being possible to observe a good agreement between simulated and measured results. The main conclusions of this work are presented, as well as suggestions for future works.

Características bioativas, funcionais e efeito protetor do resíduo desidratado de camu-camu (Myrciaria dubia H.B.K. (McVaugh)) sobre doenças degenerativas utilizando modelos in vivo C. elegans

Camu-camu (Myrciaria dubia H.B.K. (McVaugh)) is a native Amazon fruit, recognized worldwide as one of the main natural sources of ascorbic acid. Due to its great acidity, this fruit is generally consumed after processing into juice or as ingredient in food preparations. As a co-product of the camu-camu processing, a significant amount of agroindustrial residue is generated. Despite the studies showing the bioactive value and biological potential of the fruit, few studies have approached the possible processing techniques, transformation and preservation of camu-camu fruits and its agroindustrial pomace. Therefore, the present work has the objective of evaluating two different drying processes applied to camu-camu pomace (peel and seeds with residual pulp), freeze drying and hot air drying, in order to obtain a functional fruit product. This thesis was divided into three stages: the first one shows the studies related to the freeze drying and hot air drying, where we demonstrated the impact of the selected drying techniques on the bioactive components of camu-camu, taking the fresh pomace as the control group. Among the investigated conditions, the groups obtained at 50ºC and 4 m/s (SC50) and 80ºC and 6 m/s (SC80) were selected as for further studies, based on their ascorbic acid final content and Folin-Ciocalteau reducing capacity. In addition to SC50 and SC80, the fresh pomace (RF) and freeze dried (RL) samples were also evaluated in these further stages of the research. Overall, the results show higher bioactive concentration in the RF samples, followed by RL, SC50 and SC80. On the second step of the research, the antioxidant, antimicrobial and antienzymatic activities were evaluated and the same tendency was observed. It was also reported, for the first time in the literature, the presence of syringic acid in dried camu-camu pomace. In the third and final stage of the research, it was investigated the effect of dried camu-camu on aging and neuroprotective disorders, using the in vivo model C.elegans. It was observed that camu-camu extracts were able to modulate important signaling genes relevant to thermal and oxidative stresses (p < 0.05). The polar acid, polar basic and polar neutral fractions obtained from the low molecular extracts of SC50 were able to extend the lifespan of wild type N2 C. elegans in 20% and 13% (p < 0.001). Results also showed that the paralysis induced by the β1-42 amyloid was significantly (p < 0.0001) retarded in CL4176 worms. Similarly, the camu-camu extracts attenuated the dopaminergic induction associated to Parkinson’s disease. Finally, a global analysis of the data presented here reveal that the camu-camu pomace, a co-product obtained from the industrial processing of a native Brazilian fruit, is a relevant natural source of health relevant compounds. This thesis, shows for the first time, the multifunctionality of camu-camu pomace, a natural resource still underexploited for scientific, commercial and technological purposes.

Síntese, estrutura e propriedades de polímeros de coordenação à base de íons lantanídeos e ácidos benzenodicarboxílicos

Metal Organic Frameworks (MOFs) are hybrids materials, often crystalline, consisting of metal or metal clusters, connected by polytopic organic ligands repetitively, leading to structures, usually porous. In this work, MOFs based on lanthanide ions (La3+ and Gd3+) and dicarboxylate type of ligands (isophthalic and terephthalic acids), were synthesized by hydrothermal, solvothermal and hydro(solvo)thermal methods. The effects of the synthetic route as well as the type of heating, conventional or by microwave, on the structure and properties of MOFs were studied. The powder samples obtained were characterized by X-ray diffraction, infrared spectroscopy, thermal analysis and scanning electron microscopy. The results suggest that the addition of an organic or inorganic base is needed to promote the deprotonation of the ligand, since in the samples prepared by the hydrothermal method, without the use of a base, no formation of the metalorganic framework was observed. On the other hand, the presence of DMF as solvent or cosolvent, afforded the deprotonation of the ligand with the consequent formation of MOFs. At least two different crystalline structures were identified for the samples prepared with terephthalic acid. These samples are isostructural with those reported for phases Eu(1,3-BDC)DMF, Eu2(1,4-BDC)3 (DMF)2 and Tb(1,4-BDC)H2O. The presence of water in the reaction medium in the hydro(solvo)thermal method, provoked the growth of the structure different from that observed in the absence of water. This can be explained by the difference in the coordination mode of water and DMF to lanthanide ions. Although not identified by XRD, the samples prepared with isophthalic acid, also present metalorganic structures, which was confirmed by the presence of the characteristic displacement of the carbonyl group band in their infrared spectra, compared to the spectrum of the pure ligand. This shift was also observed in the samples prepared with terephthalic acid. Thermal analisys shows that the metal organic frameworks do not collapse occurs at a temperature below 430°C.The analysis of scanning electron microscopy suggests that the morphology of powders is highly dependent on the type of heating used, conventional or by microwave.