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 digestão de sedimento de curtume visando a extração do cromo por microemulsão

Leather tanneries generate effluents with high content of heavy metals, especially chromium, which is used in the mineral tanning process. Microemulsions have been studied in the extraction of heavy metals from aqueous solutions. Considering the problems related with the sediment resulting from the tanning process, due to its high content in chromium, in this work this sediment was characterized and microemulsion systems were applied for chromium removal. The extraction process consists in the removal of heavy metal ions present in an aqueous feeding solution (acid digestion solution) by a microemulsion system. First three different solid sludge digestion methods were evaluated, being chosen the method with higher digestion capacity. For this digestion method, seeking its optimization, was evaluated the influence of granule size, temperature and digestion time. Experimental results showed that the method proposed by USEPA (Method A) was the most efficient one, being obtained 95.77% of sample digestion. Regarding to the evaluated parameters, the best results were achieved at 95°C, 14 Mesh granule size, and 60 minutes digestion time. For chromium removal, three microemulsion extraction methods were evaluated: Method 1, in a Winsor II region, using as aqueous phase the acid digestion solution; Method 2, in a Winsor IV region, being obtained by the addition of the acid digestion solution to a microemulsion phase, whose aqueous phase is distilled water, until the formation of Winsor II system; and Method 3, in a Winsor III region, consisting in the formation of a Winsor III region using as aqueous phase the acid digestion solution, diluted in NaOH 0.01N. Seeking to optimize the extraction process only Method 1 (Systems I, II, and VIII) and Method 2 (System IX) were evaluated, being chosen points inside the interest regions (studied domains) to study the influence of contact time and pH in the extraction percentiles. The studied systems present the following compositions: System I: Surfactant Saponified coconut oil, Cosurfactant 1-Butanol, Oil phase Kerosene, Aqueous phase 2% NaCl solution; System II: Aqueous phase Acid digestion solution with pH adjusted using KOH (pH 3.5); System VIII: Aqueous phase - Acid digestion solution (pH 0.06); and System IX Aqueous phase Distilled water (pH 10.24), the other phases of Systems II, VIII and IX are similar to System I. Method 2 showed to be the more efficient one regarding chromium extraction percentile (up to 96.59% - pH 3.5). Considering that with Method 2 the microemulsion region only appears in the Winsor II region, it was studied Method 3 (System X) for the evaluation and characterization of a triphasic system, seeking to compare with a biphases system. System X is composed by: Surfactant Saponified coconut oil, Cosurfactant 1-Butanol, Oil phase Kerosene, Aqueous phase Acid digestion solution diluted with water and with its pH adjusted using 0.01N NaOH solution. The biphasic and triphasic microemulsion systems were analyzed regarding its viscosity, extraction efficiency and drop effective diameter. The experimental results showed that for viscosity studies the obtained values were low for all studied systems, the diameter of the drop is smaller in the Winsor II region, with 15.5 nm, reaching 46.0 nm in Winsor III region, being this difference attributed to variations in system compositions and micelle geometry. In chromium extraction, these points showed similar results, being achieved 99.76% for Winsor II system and 99.62% for Winsor III system. Winsor III system showed to be more efficient due to the obtaining of a icroemulsion with smaller volume, with the possibility to recover the oil phase in excess, and the use of a smaller proportion of surfactant and cosurfactant (C/S)

Extração e análise da fração lipídica da microalga monoraphidium sp., síntese e caracterização do seu biodiesel

The cultivation of microalgae biomass in order to produce biodiesel arises as an extremely promising aspect, in that the microalgae culture includes short cycle of reproduction, smaller areas for planting and residual biomass rich in protein content. The present dissertation evaluates the performance and features, through spectrometry in the region of infrared with transformed Fourier (FTIR) and spectrometry in the region of UVvisible (UV-Vis), of the extracted lipid material (LM) using different techniques of cell wall disruption (mechanical agitation at low and at high spin and agitation associated with cavitation). The technique of gas chromatography (GC) brought to light the success of alkaline transesterification in the conversion of oil into methyl monoesters (MME), which was also analyzed by spectroscopic techniques (FTIR, proton magnetic resonance (1H NMR) and carbon (13C NMR). Through thermogravimetric analysis (TGA) were analyzed the lipid material (LM), biodiesel and the microalgae biomass. The method which provided the best results concerning the efficiency in extraction of the LP of Monoraphidium sp. (12,51%) was by mechanical agitation at high spin (14 000 rpm), for 2 hours being the ideal time, as shown by the t test. The spectroscopic techniques (1H NMR, 13C NMR and FTIR) confirmed that the structure of methyl monoesters and the chromatographic data (CG) revealed a high content of saturated fatty acid esters (about 70%) being the major constituent eicosanoic acid (33,7%), which justifies the high thermal stability of microalgae biodiesel. The TGA also ratified the conversion rate (96%) of LM into MME, pointing out the quantitative results compatible with the values obtained through GC (about 98%) and confirmed the efficiency of the extraction methods used, showing that may be a good technique to confirm the extraction of these materials. The content of LM microalgae obtained (12,51%) indicates good potential for using such material as a raw material for biodiesel production, when compared to oil content which can be obtained from traditional oil for this use, since the productivity of microalgae per hectare is much larger and requires an extremely reduced period to renew its cultivation

Eficiência de extração de cobre e níquel utilizando sistemas microemulsionados bifásicos e trifásicos

The environmental impact due to the improper disposal of metal-bearing industrial effluents imposes the need of wastewater treatment, since heavy metals are nonbiodegradable and hazardous substances that may cause undesirable effects to humans and the environment. The use of microemulsion systems for the extraction of metal ions from wastewaters is effective when it occurs in a Winsor II (WII) domain, where a microemulsion phase is in equilibrium with an aqueous phase in excess. However, the microemulsion phase formed in this system has a higher amount of active matter when compared to a WIII system (microemulsion in equilibrium with aqueous and oil phases both in excess). This was the reason to develop a comparative study to evaluate the efficiency of two-phases and three-phases microemulsion systems (WII and WIII) in the extraction of Cu+2 and Ni+2 from aqueous solutions. The systems were composed by: saponified coconut oil (SCO) as surfactant, n-Butanol as cosurfactant, kerosene as oil phase, and synthetic solutions of CuSO4.5H2O and NiSO4.6H2O, with 2 wt.% NaCl, as aqueous phase. Pseudoternary phase diagrams were obtained and the systems were characterized by using surface tension measurements, particle size determination and scanning electron microscopy (SEM). The concentrations of metal ions before and after extraction were determined by atomic absorption spectrometry. The extraction study of Cu+2 and Ni+2 in the WIII domain contributed to a better understanding of microemulsion extraction, elucidating the various behaviors presented in the literature for these systems. Furthermore, since WIII systems presented high extraction efficiencies, similar to the ones presented by Winsor II systems, they represented an economic and technological advantage in heavy metal extraction due to a small amount of surfactant and cosurfactant used in the process and also due to the formation of a reduced volume of aqueous phase, with high concentration of metal. Considering the reextraction process, it was observed that WIII system is more effective because it is performed in the oil phase, unlike reextraction in WII, which is performed in the aqueous phase. The presence of the metalsurfactant complex in the oil phase makes possible to regenerate only the surfactant present in the organic phase, and not all the surfactant in the process, as in WII system. This fact allows the reuse of the microemulsion phase in a new extraction process, reducing the costs with surfactant regeneration

Paralelização em GPU da segmentação vascular com extração de Centerlines por Height Ridges

The vascular segmentation is important in diagnosing vascular diseases like stroke and is hampered by noise in the image and very thin vessels that can pass unnoticed. One way to accomplish the segmentation is extracting the centerline of the vessel with height ridges, which uses the intensity as features for segmentation. This process can take from seconds to minutes, depending on the current technology employed. In order to accelerate the segmentation method proposed by Aylward [Aylward & Bullitt 2002] we have adapted it to run in parallel using CUDA architecture. The performance of the segmentation method running on GPU is compared to both the same method running on CPU and the original Aylward s method running also in CPU. The improvemente of the new method over the original one is twofold: the starting point for the segmentation process is not a single point in the blood vessel but a volume, thereby making it easier for the user to segment a region of interest, and; the overall gain method was 873 times faster running on GPU and 150 times more fast running on the CPU than the original CPU in Aylward

Dinâmica sazional de fungos micorrízicos arbusculares (Glomeromycota) em cerradão e brejo de altitude na Chapada do Araripe, CE

Arbuscular mycorrhizal fungi (AMF) are obligatory symbiotic organisms that associate with roots of a large number of plant taxa, and are found in all terrestrial ecosystems. These fungi promote greater tolerance to environmental stresses to associated plant, favoring the establishment of plant communities, especially where soil fertility is a limiting factor, as in the Caatinga, an exclusively Brazilian domain that has been focus of research due to its great biodiversity that can help clarify the history of vegetation in South America. Because of the ecological importance of AMF, the limited number of jobs and the potential diversity of the Caatinga, this work aims to inventory the diversity and determine AMF communities in areas with different faces occurrent in FLONA Araripe, Ceará (CE). The sample collection occurred in four periods at the beginning and end of the dry season (August and December 2011, respectively) and rainy (February and June 2012, respectively) in an area of marsh and woodland altitude of the Araripe, Crato, CE. The glomerosporos were extracted by wet sieving and centrifugation in water and sucrose (50%) mounted between slide and coverslip using PVLG and PVLG + Reagent Melzer. In total, we found 46 species of AMF distributed in eight families and 16 genera: Acaulospora (6), Ambispora (1), Cetraspora (2), Dentiscutata (5), Fuscutata (2), Gigaspora (6), Glomus (13) Intraornatospora (1), Kuklospora (1), Orbispora (1), Paradentiscutata (1), Quatunica (1), Racocetra (1), Scutellospora (2), Septoglomus (2) and a new genus. analysis showed that ecological each area of study has its own seasonal dynamics, with an area of woodland with a greater diversity of species throughout the year, while the marsh elevation showed greater variation in species found among the collection periods, showing that vegetation and rainfall has strong influence on the seasonal dynamics of AMF, as well as the availability of nutrients and soil pH so

Fungos gasteroides (Basidiomycota, Agaricomycetes) de três áreas de semiárido no Estado do Ceará, Brasil

Gasteroid fungi include several distinct lineages of basidiomycetes that were grouped by presenting some striking features in common like angiocarpic development and passive release of basidiospores. For a long period these fungi were accomodate in Gasteromycetes class. However, biochemistry and molecular studies showed the polyphyly of this group and curriently this class lies devoid of taxonomic value. These organisms influence the ecology of the various biomes, however, are poorly studied and knowledge of their diversity in neotropical ecosystems remains insufficient, despite studies that have been developed in recent years. The Brazilian semiarid region has many areas with an unexplored mycobiota. Ceará State has many areas of extreme biological importance and for this study three protected areas were chosen: Área de Proteção Ambiental da Serra da Ibiapaba, Parque Nacional de Ubajara and Área de Proteção Ambiental de Baturité. Therefore, the aim of this study was to inventory gasteroid fungi ocorring in these three areas in the semiarid region of Ceará. The expeditions, herborization and analysis of specimes were based in traditional methodology used to identify gasteroid fungi. Were identified 16 species belong to 5 families: Agaricaceae, Clathraceae, Geastraceae, Nidulariceae and Phallaceae. Morganella nuda Alfredo & Baseia is recorded for the second time in the world, Blumenavia angolensis (Welw. & Curr) Dring and Mutinus elegans (Mont.) E. Fisch. corresponds to a first record in the Brazilian Northeastern. Except for Abrachium floriforme (Baseia & Calonge) Baseia & T.S. Cabral and Geastrum lloydianum Rick, all remaining species are new records for Ceará, increasing the list of gasteroid fungi in the region of 3 for 17 species. Identified species were deposited in the collection of the Herbarium of Universidade Federal do Rio Grande do Norte. Although these areas have proved conducive to the study of gasteroid fungi, more efforts are still needed to increase knowledge of these fungi in the region