Comparison of various NMR methods for the indirect detection of nitrogen-14 nuclei via protons in solids

We present an experimental comparison of several through-space Hetero-nuclear Multiple-Quantum Correlation experiments, which allow the indirect observation of homo-nuclear single- (SQ) or double-quantum (DQ) ¹⁴N coherences via spy ¹H nuclei. These ¹H-{¹⁴N} D-HMQC sequences differ not only by the order of ¹⁴N coherences evolving during the indirect evolution, t1, but also by the radio-frequency (rf) scheme used to excite and reconvert these coherences under Magic-Angle Spinning (MAS). Here, the SQ coherences are created by the application of center-band frequency-selective pulses, i.e. long and low-power rectangular pulses at the ¹⁴N Larmor frequency, ν0(¹⁴N), whereas the DQ coherences are excited and reconverted using rf irradiation either at ν0(¹⁴N) or at the ¹⁴N overtone frequency, 2ν0(¹⁴N). The overtone excitation is achieved either by constant frequency rectangular pulses or by frequency-swept pulses, specifically Wide-band, Uniform-Rate, and Smooth-Truncation (WURST) pulse shapes. The present article compares the performances of four different ¹H-{¹⁴N} D-HMQC sequences, including those with ¹⁴N rectangular pulses at ν0(¹⁴N) for the indirect detection of homo-nuclear (i) ¹⁴N SQ or (ii) DQ coherences, as well as their overtone variants using (iii) rectangular or (iv) WURST pulses. The compared properties include: (i) the sensitivity, (ii) the spectral resolution in the ¹⁴N dimension, (iii) the rf requirements (power and pulse length), as well as the robustness to (iv) rf offset and (v) MAS frequency instabilities. Such experimental comparisons are carried out for γ-glycine and l-histidine.HCl monohydrate, which contain ¹⁴N sites subject to moderate quadrupole interactions. We demonstrate that the optimum choice of the ¹H-{¹⁴N} D-HMQC method depends on the experimental goal. When the sensitivity and/or the robustness to offset are the major concerns, the D-HMQC sequence allowing the indirect detection of ¹⁴N SQ coherences should be employed. Conversely, when the highest resolution and/or adjusted indirect spectral width are needed, overtone experiments are the method of choice. The overtone scheme using WURST pulses results in broader excitation bandwidths than that using rectangular pulses, at the expense of reduced sensitivity. Numerically exact simulations also show that the sensitivity of the overtone ¹H-{¹⁴N} D-HMQC experiment increases for larger quadrupole interactions.

Cyanobacteria and Cyanotoxin in the Billings Reservoir (São Paulo, SP, Brazil)

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Caracterização de Efluente Têxtil e Proposta de Tratamento

Textile industry deals with a high diversity of processes and generation of wastewaters with a high content of pollutant material. Before being disposed of in water bodies, a pre-treatment of the effluent is carried out, which is sometimes ineffective. In order to be properly treated, physical and chemical properties of the effluent must be known, as well as the pollutant agents that might be present in it. This has turned out to be a great problem in the textile industry, for there is a variety of processes and the pollutant load is very diversified. The characterization of the effluent allows the identification of most critical points and, as a consequence, the most appropriate treatment procedure to be employed, may be chosen. This study presents the results obtained after characterizing the effluent of a textile industry that comprises knitting, dyeing and apparel sections, processing mainly polyester/cotton articles. In this work, twenty samples of the effluent were collected, and related to the changes in production. From the results, a statistical evaluation was applied, determined in function of the rate of flow. The following properties and pollutants agents were quantitatively analysed: temperature; pH; sulfides; chlorine; alcalinity; chlorides; cianides; phenols; color; COD (Chemical Oxygen Demand); TOC (Total Organic Carbon); oil and grease; total, fixed and volatile solids; dissolved, fixed and volatile solids; suspended, fixed and volatile solids; setteable solids and heavy metals such as cadmium, copper, lead, chromium, tin, iron, zinc and nickel. Analyses were carried out according to ABNT NBR 13402 norm, based upon Standard Methods for the Examination of Water and Wastewater. As a consequence, a global treatment proposal is presented, involving clean production practices as contaminant load reducer, followed by conventional (biological) treatment

Avaliação da eficiência de filtros anaeróbios na remoção de coliformes fecais e ovos de helmintos

The technology of anaerobic reactors for sanitary wastewater treatment has been extensively developed in Brazil, and today it is practically consolidated. They present several advantages, such as low construction and operating costs, and low sludge production, the anaerobic reactors are an attractive alternative to minimize problematic lack of basic sanitation in urban areas, and also of the rural areas. The anaerobic filters have been widely used in Brazil. It produces an effluent with low concentration of organic matter and solids suspended, besides conserving the nutrients, therefore, it is good for use in irrigation, but the practice must be associated with knowledge of the pathogens presence. The main objective of this study was to evaluate the efficiency of anaerobic filters in removal faecal coliforms and helminth eggs, and to verify if the effluent can be used for agricultural purposes, according to the World Organization of Health (WHO, 1989). The protocol used to enumerate helminths eggs was the modified Bailenger method, (Ayres and Mara, 1996) recommended by WHO for evaluation of raw effluent and treated effluent. The membrane filtration method was utilized to determine the concentrations of faecal coliforms. Three different systems of sewer treatment composed by anaerobic filters were analyzed. The results, in a general analysis, showed that all the researched systems reached a larger removal than 93% to helminth eggs, resulting in an effluent with smaller average than 1 egg/L. One of these systems, Sistema RN, reached a larger removal than 99%, confirming the good performance of the anaerobic filters in removal helminths eggs. Even with low concentrations of eggs in the influent, the filters were capable to remove this parameter efficiently. About faecal coliforms, it was observed for all the researched systems an effluent with 106 CFU/100mL. The high concentrations to faecal coliforms in the effluent just allow reuse for restricted irrigation, in agreement with the guidelines of WHO. Although the researched systems have not removed faecal coliforms efficiently, the results indicated a good efficiency of the anaerobic filters in removal helminth eggs

Estudos dos aspectos qualitativos e quantitativos da água e do sedimento no baixo curso do Rio Pitimbu (RN)

Urban growth of metropolitan areas has produced impacts of considerable importance on environment and water resources. Such impacts are in general associated with human activities, such as basin area uncontrolled development. In this context, Pitimbu river watershed, located at Natal metropolitan area, has been affected by uncontrolled development caused by urban expansion. Indeed, such effects have been reflected on water quantity and quality, which may produce social consequences. Pitimbu river is an important water supplier for human consumption, actually supplying a 2600 m3/h water discharge. This study aims to analyze the qualitative and quantitative aspects of water and sediment on Pitimbu river lowland portion. For this purpose, physical-chemical water properties were analyzed, and sediment macro invertebrates benthonic were monitored in two cross sections in a period between November 8th, 2007 and October 3rd, 2008. Monitoring methodology consisted of water and sediment sampling for laboratory analysis. Water quality analysis included Dissolved Oxygen, Oxygen Biochemical Demand, Nitrate, pH and Alkalinity, Suspended and Total Solids. The analysis of heavy metals in the sediment included Cadmium, Cobalt, Copper, Chrome, Silver and Nickel. Dry season water discharge data were measured and used to adjust recession function parameters, whose values reveal quick recession and strong river-aquifer unconfined interaction. Water quality analysis revealed the absence of degradation by organic composites. However, DO and BOD levels indicate that more consistent results could be provided if sampling time interval were reduced. Biomonitoring showed signs of aquatic ecosystem degradation by the absence of sensitive and abundance of resistant benthic organisms. Obtained results demonstrate the urgent need of effective management measures to provide environmental protection. The increase of environmental degradation will certainly make impracticable the use of water for human consumption

Desempenho de reatores aeróbios de leito fluidizado com circulação interna na remoção de matéria carbonácea tratando diferentes águas residuárias

The organic matter. (OM) removal efficiency in the biochemical oxygen demand (BOD) and chemical oxygen demand (COD) forms for domestic wastewater and semi-intensive fish culture effluents by using three phase aerobic fluidized bed reactors with circulation in concentric tubes was studied. Three different ratios between external and internal areas by different internal diameter configurations (100, 125 and 150mm) to the same external diameter of 250mm were used; sand for filters and granulated activated carbon were used as supporting media. The reactors were tested for three hydraulic retention times: 11.5min to the R100, and 3h for the R125 and R150 reactors. The results demonstrated that this kind of reactors had good performance in the BOD and COD removal for different concentrations of waste waters. BOD mean removal efficiencies obtained were: 47% at the R100 reactor, 57% and 93% of raw and filtered BOD respectively at R125, 48 and 89% of raw and filtered BOD at R150. The COD mean calculated removal efficiencies were: 75% at the R100 reactor, 56 and 86% of raw and filtered COD at R125, and 54 and 86% of raw and filtered COD at R150. In the case of domestic wastewater it is necessary to provide a solids removal system at the reactor outflow in order to increase the removal of suspended OM from the final effluent.

Electrofluid dynamic (EFD) energy conversion in gas flows with suspended nanoparticles

This work presents simulations of the Electrofluid Dynamic energy conversion process in slender channel devices having very small particles (in both micro and nano scales) as charge carriers. Solutions are discussed for a system composed by coupled differential equations, which includes the equation for the total current along the channel, the equations for total energy and momentum of the mixture (gas and solid particles), the continuity equation and the equations for energy and momentum of a single particle. Results for suspended particles of higher diameters have been previously published in the Literature, but the simulations here presented exhibit an appreciable increase in the values for output currents.

Electrofluid dynamic (EFD) energy conversion in gas flows with suspended nanoparticles

This work presents simulations of the Electrofluid Dynamic energy conversion process in slender channel devices having very small particles (in both micro and nano scales) as charge carriers. Solutions are discussed for a system composed by coupled differential equations, which includes the equation for the total current along the channel, the equations for total energy and momentum of the mixture (gas and solid particles), the continuity equation and the equations for energy and momentum of a single particle. Results for suspended particles of higher diameters have been previously published in the Literature, but the simulations here presented exhibit an appreciable increase in the values for output currents.

Tratamento de águas residuárias de suinocultura em reator UASB e filtro anaeróbio em série seguidos de filtro biológico percolador

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

Flotation of blocolloids suspended in liquid phases of different compositions and pH values

The flotation capacity was determined for cells of yeasts strains belonging to the genera Hansenula, Candida and Saccharomyces. A heterogeneous group of yeasts, comprising strains from the three genera, was identified as showing high flotation capacities (degrees of flotation above 50%), which were practically not affected by variations in medium pH in both the synthetic medium and 2% molasses. Thus, the flotation capacity of the cells in this yeast group seemed strongly dependent on the liquid phase properties and/or growth medium composition, more than on the simple variation in pH of the cell suspensions. A second group of strains, belonging to the Saccharomyces genus, including also brewing yeast strains, was identified as having lower flotation capacities (degrees of flotation below 50% at pH 1.5), which showed no alterations or variations significantly affected by the medium pH. Foam volumes obtained with Saccharomyces strains were greater in synthetic media than in molasses owing to the higher air flow rates required for flotation in molasses. The flotation efficiency decreased in molasses in all cases as well as the foam volume, except in the case of Hansenula cells, which showed an increased foam volume. This was probably due to variations in product excretion by the different yeasts and/or differences in cell wall composition.

Photoacoustic procedure for measuring thermal parameters of transparent solids

An application of photoacoustic technique is developed for determining the thermal diffusivity coefficient and the thermal conductivity of transparent materials. The backing material which supports the sample is made optically opaque, i.e., it entirely absorbs the incident light, and the converted heat diffuses through the sample heating the gas in contact with its opposite surface. The method is illustrated by fitting voltage amplitude and phase signals versus the chopping frequency in the photoacoustic cell, according to a theoretical model of heat diffusion. Thermal parameters obtained for three polymers compare very well with results from the literature. (C) 1995 American Institute of Physics.

Hollow silica particles from microemulsion

Silica particles were obtained by addition of diluted soluble sodium silicate in sodium 1,2 bis (2-ethylhexyloxycarbonyl)-1-ethenesulfonate reverse microemulsions, in which aqueous phase was nitric acid solution and the water/surfactant ratio (W) was 5 or 10. Products, whether washed or not, were dried at 100 degrees C and suspended in different solvents: heptane, water, kerosene or pentane for making SEM measurements. Thermal treatments of washed silica samples were carried out at 900 degrees C and 1200 degrees C. Silica particles of sizes from 1 to 10 mu m were obtained at room temperature without changing their shape due to thermal treatment and crystallization. SEM micrographs show hollow particles suggesting that silica preferably polymerizes on microemulsion droplet interface where ionic strength of nitric acid aqueous solution is favourable for silica polymerization reaction. (C) 1999 Elsevier B.V. B.V. All rights reserved.

Solids rheology for dehydrated food and biological materials

Mechanical properties of food products and biological materials are greatly affected by the drying process and are considered one of the most important quality attributes of dehydrated products. The aim of this work was to review theoretical principles and mathematical modeling, analyzing the measurement techniques and major experimental results that exist in the literature about rheological properties of dehydrated foods and biological materials. Different methods of measuring rheological parameters (fundamental and empiric or imitative) are discussed and major experimental results, as well as the rheological models used in their analysis, published in recent years are presented.

An implicit BEM formulation to model strong discontinuities in solids

A boundary element method (BEM) formulation to predict the behavior of solids exhibiting displacement (strong) discontinuity is presented. In this formulation, the effects of the displacement jump of a discontinuity interface embedded in an internal cell are reproduced by an equivalent strain field over the cell. To compute the stresses, this equivalent strain field is assumed as the inelastic part of the total strain. As a consequence, the non-linear BEM integral equations that result from the proposed approach are similar to those of the implicit BEM based on initial strains. Since discontinuity interfaces can be introduced inside the cell independently on the cell boundaries, the proposed BEM formulation, combined with a tracking scheme to trace the discontinuity path during the analysis, allows for arbitrary discontinuity propagation using a fixed mesh. A simple technique to track the crack path is outlined. This technique is based on the construction of a polygonal line formed by segments inside the cells, in which the assumed failure criterion is reached. Two experimental concrete fracture tests were analyzed to assess the performance of the proposed formulation.