1000 resultados para dissolução ácida


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Desenvolveu-se uma metodologia que dispensa a dissolução completa da amostra para determinar Hg em solos, sedimentos fluvial e marinho. O Hg é quantitativamente extraído do sedimento marinho usando-se HNO3 30% (v/v), ultra-som (120 s, 70 W) e granulometria ≤ 120 µm. Condições similares são eficientes para sedimento fluvial e solo, exceto o tempo de sonicação (180 s) e a adição de KCl 0,15% (m/v). As suspensões sonicadas são centrifugadas e o Hg é determinado no sobrenadante por FI-CV AAS. A validação da metodologia foi feita com CRMs: PACS-2, MESS-3 (NRCC); Buffalo River (NIST 8704), Montana Soil (NIST 2710) e RS-3 (não certificada). Os parâmetros de mérito do método são: massa característica de 25 pg; LD (3s) de 0,2 µg l–1; LQ (10s) de 0,012 µg g–1 (800 µl de solução obtida de 1 g de amostra em 20 ml de suspensão). Aplicou-se a metodologia à análise de amostras reais (solo, sedimentos fluvial e marinho), as quais também foram preparadas com digestão ácida (85 °C durante 3 h) em mistura oxidante (K2S2O8 1 a 2% (m/v) e HNO3 30% (v/v)). Concentrações concordantes foram obtidas. Utilizou-se calibração externa e, quando necessário, ajuste de matriz com KCl ou K2S2O8. Para investigar a extração de Hg orgânico utilizando ultra-som, adicionou-se MeHg aos CRMs. Aproximadamente 5% do MeHg adicionado transformam-se em Hg2+ pelo método proposto, enquanto que chega a 100% quando a amostra é digerida. Assim, propõe-se uma especiação química semiquantitativa entre Hg inorgânico e orgânico, pois o Hg orgânico pode ser obtido pela diferença entre Hg total (determinado pela digestão) e Hg inorgânico (determinado pelo método proposto).

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This project describes a methodology optimization that would allow for a more efficient microwave assisted digestion process for petroleum samples. With the possible chance to vary various factors at once to see if any one factor was significant enough in the answers, experimental planning was used. Microwave assisted digestion allows, through the application of potency, an increasing number of collisions between the HNO3 and H2O2 molecules, favoring sample opening for complex matrixes. For this, a 24 factorial experimental planning was used, varying potency, time and the volumes for HNO3 65% and H2O2 30%. To achieve the desired answers, several elements were monitored (C, Cu, Cr, Fe, Ni, Zn and V) through Inductively coupled plasma atomic emission spectroscopy (ICP-OES). With this initial study it was noticed that the HNO3 was not a significant factor for any of the statistical studies for any of the analytes and the other 3 factors and their interactions showed statistical significance. A Box Behnken experimental planning was used taking in consideration 3 factors: H2O2 volume, time (min) and Potency (W), Nitric Acid kept at 4mL for a mass of 0,1g of petroleum. The results were extremely satisfying showing higher efficiency in the digestion process and taking in a responsibility between the answers for each analyte and the carbon monitoring was achieved in the following conditions: 7mL of H2O2, 700 Watts of potency and a reaction time of 7 minutes with 4mL de HNO3 for a mass of 0,1g of petroleum. The optimized digestion process was applied to four different petroleum samples and the analytes determined by ICP-OES

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The experiment constituted in evaluating the acid silage prepared from Nile tilapia (Oreochromis niloticus) filletage industry residues. This silage was prepared in a filetage industry through the residues milling and 5% of ascetic acid addition and stock piling in a period up to until 201 days. Storaged silages in a period of 7, 12, 22, 27, 41, 48, 61, 75, 84, 91, 96, 110, 140, 151, 181, 187 and 201dias were evaluated. Bromatologics analyses of rude protein(PB), etereal extract (EE), humidity (UM), ashes (CZ) and microbiological analyses of Salmonella, total coliforms, faecals and Escherichia coli of the storaged silages in a period of 7, 91 and 201 days were realized. The pH was evaluated in all the storaged periods. Differences (P > 0.05) in the substance of PB, EE, UM and CZ were not observed. A linear increase in PH was observed, being stabilizing in plateau of 4.74. In relation to the microbiological analysis the presence of Salmonella, total coliforms, faecals and E. Coli were not found. Was concluded that the acid silage gotten from tilapia filetage residues produced with the use of 5% ascetic acid can be stored during 201 days without having Salmonella, total coliforms and faecals proliferation.

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A floração nos citros, assim como em outras fruteiras, é um dos fatores determinantes para a produção. A possibilidade de inibição ou redução da florada normal e alteração da época de produção para a lima 'Tahiti' é fator primordial para determinar sua rentabilidade econômica. O presente trabalho teve como objetivo avaliar o efeito do ácido giberélico sobre a florada, número de flores formadas, da lima ácida 'Tahiti', nas condições do Estado de São Paulo durante dois anos, buscando inibir a florada normal e observar o efeito desta inibição sobre produções temporãs. O delineamento experimental foi em blocos casualizados (5 blocos) com 3 plantas por tratamento. Foi utilizada uma planta como bordadura entre os tratamentos e uma linha de plantas entre os blocos. Os tratamentos foram: testemunha, 20, 40 e 80 mg/L de ácido giberélico (AG3) + 10 ml/L de espalhante adesivo, e o pH da água utilizada foi 6,2. As plantas foram tratadas com ácido giberélico durante o inverno (estação seca) após 50 dias sem irrigação no primeiro ano e 60 dias no segundo. O ácido giberélico reduziu o número de flores formadas (-81%) e aumentou a produção de frutos temporões (+59,77% ou +16,04 kg/pl).

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Foram avaliadas concentrações de 0; 10; 20; 40 e 80 mg/L do 3,5,6-TPA (Ácid 3,5,6-tricloro-2-piridil- oxiacético), em sua formulação éster, para desbaste de frutos novos da limeira-ácida-'Tahiti' (Citrus latifolia Tanaka), nas condições ecológicas do Estado de São Paulo. O 3,5,6-TPA, na concentração 10mg/L, foi o tratamento mais eficaz para uso na cultura. Concentrações maiores causaram severos danos às plantas. Essa concentração, aplicada logo após a florada de outubro, reduziu em 65% a produção do mês de fevereiro seguinte. Todavia, as produções dos meses subseqüentes não diferiram entre si. A concentração de 10mg/L causou alongamento dos frutos, aumento da espessura da casca e redução do Brix, na época da colheita.

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A proteína glial fibrilar ácida (GFAP), subunidade dos filamentos intermediários do citoesqueleto celular, está presente no citoplasma de astrócitos. Técnicas imunohistoquímicas com anticorpos primários anti-GFAP são geralmente empregadas para identificar astrócitos no sistema nervoso, permitindo verificar também sua hipertrofia. Vários estudos mostram a distribuição, a morfologia e a citoarquitetura de astrócitos em várias regiões do SNC do homem e de animais de laboratório. No entanto, em animais domésticos e, especialmente em equinos, poucas informações estão disponíveis. No presente trabalho, verificou-se a densidade e a morfologia de astrócitos imunorreativos à GFAP na substância branca da córtex cerebral de equinos com leucoencefalomalácia (LEM) comparando-se esses aspectos com o de equinos normais. Animais com LEM apresentaram hipertrofia de astrócitos em áreas próximas às lesões, representada pelo aumento do corpo celular, do núcleo e dos prolongamentos citoplasmáticos. O número de astrócitos apresentou-se reduzido e a imunorreatividade foi mais acentuada. Nos animais normais, verificou-se distribuição constante de astrócitos imunorreagentes com características de fibrosos. Alterações vasculares nos animais com LEM, como por exemplo degeneração de endotélio vascular, também foram observadas, podendo estar associadas às alterações astrocíticas.

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Seeds of Caesalpinea ferrea Mart. ex Tu. var. leiostachya Benth. present low and irregular germination due to dormancy caused by the impermeability of the tegument. With the purpose to determine an efficient method to accelerate and uniformize seed germination, they were submitted to different immersion periods (0, 5, 10, 15, 20, 25 and 30 minutes) in sulfuric acid (95-98%), influence emergency and vigor (first count, speed index, medium time and relative frequency of emergency, length and dry matter of the seedlings). The experiment was carried out under greenhouse conditions with an experimental design of completely randomized, with seven treatments and four replications. The pre-conditioning of the seeds with immersion in concentrated sulfuric acid was efficient to overcoming seed dormancy, by increasing the percentage and speed emergency, the first count of emergency, length and dry matter of seedlings and reduction in the medium time for emergency. The efficiency of this chemical treatment with concentrated sulfuric depends on the immersion time, and 10 to 20 minutes were the most adequate to provide larger emergency uniformity percentages and vigor.

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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This work describes the establishment of dissolution test conditions for 75 mg cinnarizine capsules using a multivariate approach. A 2³ full factorial design was carried out to achieve the best conditions and HCl 0.1 mol L-1 as dissolution medium, basket as apparatus at 100 rpm and collect time at 30 min were considered adequate. The quantification was carried out by spectrophotometry at 251 nm. Both dissolution procedure and analytical method were validated and all parameters were within the acceptable limits. Since there is no official monograph for this pharmaceutical product, this dissolution test could be applied for quality control routine.

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This work involved the synthesis, characterization and proposing the molecular structure of coordination compounds involving ligands pyrazine-2-carboxamide (PZA) and 4- hydrazide acidic pyridine carboxylic (INH) and metals of the first transition series (M = Co2+, Ni2+ and Cu2+). For the characterization of the compounds used were analytical techniques such as infrared absorption spectroscopy average (FT-IR) molar conductivity measurements, CHN elemental analysis, EDTA Complexometric, measurement of melting point, X-ray diffraction by powder method, Thermogravimetry (TG) and Differential Thermal Analysis (DTA) and Simultaneous Differential Scanning Calorimetry (DSC). The absorption spectra in the infrared region suggested that the ligand coordination to the metal center occurs through the carbonyl oxygen atom and nitrogen alpha pyrazine ring to those complexes formed with PZA. For INH complexes with metal-ligand coordination is through the carbonyl oxygen and nitrogen of the terminal hydrazide grouping. The conductivity measurements of the complexes in aqueous solution they suggest to all behavior of the type 1:2 electrolytes, and conduct of non-electrolytes in acetonitrile. The results obtained by CHN elemental analysis and EDTA Complexometric allowed to infer the stoichiometry of the compounds synthesized. For all of the complexes obtained was possible to record the melting points, neither of which melted near the melting temperature of the free ligands. The X-ray diffraction showed that the complexes of pyrazinamide exhibited diffraction lines, suggesting that these compounds are crystalline, while compounds of isoniazid, with the exception of cobalt, exhibited diffraction lines, indicating that they are crystalline. The results from the TG-DTA and DSC allowed information regarding the dehydration and thermal decomposition of these complexes

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In Fazenda Belém oil field (Potiguar Basin, Ceará State, Brazil) occur frequently sinkholes and sudden terrain collapses associated to an unconsolidated sedimentary cap covering the Jandaíra karst. This research was carried out in order to understand the mechanisms of generation of these collapses. The main tool used was Ground Penetrating Radar (GPR). This work is developed twofold: one aspect concerns methodology improvements in GPR data processing whilst another aspect concerns the geological study of the Jandaíra karst. This second aspect was strongly supported both by the analysis of outcropping karst structures (in another regions of Potiguar Basin) and by the interpretation of radargrams from the subsurface karst in Fazenda Belém. It was designed and tested an adequate flux to process GPR data which was adapted from an usual flux to process seismic data. The changes were introduced to take into account important differences between GPR and Reflection Seismic methods, in particular: poor coupling between source and ground, mixed phase of the wavelet, low signal-to-noise ratio, monochannel acquisition, and high influence of wave propagation effects, notably dispersion. High frequency components of the GPR pulse suffer more pronounced effects of attenuation than low frequency components resulting in resolution losses in radargrams. In Fazenda Belém, there is a stronger need of an suitable flux to process GPR data because both the presence of a very high level of aerial events and the complexity of the imaged subsurface karst structures. The key point of the processing flux was an improvement in the correction of the attenuation effects on the GPR pulse based on their influence on the amplitude and phase spectra of GPR signals. In low and moderate losses dielectric media the propagated signal suffers significant changes only in its amplitude spectrum; that is, the phase spectrum of the propagated signal remains practically unaltered for the usual travel time ranges. Based on this fact, it is shown using real data that the judicious application of the well known tools of time gain and spectral balancing can efficiently correct the attenuation effects. The proposed approach can be applied in heterogeneous media and it does not require the precise knowledge of the attenuation parameters of the media. As an additional benefit, the judicious application of spectral balancing promotes a partial deconvolution of the data without changing its phase. In other words, the spectral balancing acts in a similar way to a zero phase deconvolution. In GPR data the resolution increase obtained with spectral balancing is greater than those obtained with spike and predictive deconvolutions. The evolution of the Jandaíra karst in Potiguar Basin is associated to at least three events of subaerial exposition of the carbonatic plataform during the Turonian, Santonian, and Campanian. In Fazenda Belém region, during the mid Miocene, the Jandaíra karst was covered by continental siliciclastic sediments. These sediments partially filled the void space associated to the dissolution structures and fractures. Therefore, the development of the karst in this region was attenuated in comparison to other places in Potiguar Basin where this karst is exposed. In Fazenda Belém, the generation of sinkholes and terrain collapses are controlled mainly by: (i) the presence of an unconsolidated sedimentary cap which is thick enough to cover completely the karst but with sediment volume lower than the available space associated to the dissolution structures in the karst; (ii) the existence of important structural of SW-NE and NW-SE alignments which promote a localized increase in the hydraulic connectivity allowing the channeling of underground water, thus facilitating the carbonatic dissolution; and (iii) the existence of a hydraulic barrier to the groundwater flow, associated to the Açu-4 Unity. The terrain collapse mechanisms in Fazenda Belém occur according to the following temporal evolution. The meteoric water infiltrates through the unconsolidated sedimentary cap and promotes its remobilization to the void space associated with the dissolution structures in Jandaíra Formation. This remobilization is initiated at the base of the sedimentary cap where the flow increases its abrasion due to a change from laminar to turbulent flow regime when the underground water flow reaches the open karst structures. The remobilized sediments progressively fill from bottom to top the void karst space. So, the void space is continuously migrated upwards ultimately reaching the surface and causing the sudden observed terrain collapses. This phenomenon is particularly active during the raining season, when the water table that normally is located in the karst may be temporarily located in the unconsolidated sedimentary cap