In situ and genetic characterization of Gossypium barbadense populations from the states of Pará and Amapá, Brazil

The objective of this work was to characterize the populations of Gossypium barbadense in the states of Amapá and Pará, Brazil. In situ characterization was conducted through interviews with the owners of the plants and environmental observations. Leaf or petal tissue as well as seed samples were collected for genetic characterization by single sequence repeats markers and for storage in germplasm banks, respectively. The plants were maintained in dooryards and used mainly for medical purposes. The genetic analysis showed no heterozygous plants at the loci tested (f = 1), indicating that reproduction occurs mainly through selfing. The total genetic diversity was high (He = 0.39); and a high level of differentiation was observed between cotton plants from the two states (F ST = 0.36). Conventional methods of in situ maintenance of G. barbadense populations are not applicable. The conservation of the genetic variability of populations present in the two states could be achieved through germplasm collection and establishing of ex situ seed banks.

Diagnostic underestimation of atypical ductal hyperplasia and ductal carcinoma in situ at percutaneous core needle and vacuum-assisted biopsies of the breast in a Brazilian reference institution

Abstract Objective: To determine the rates of diagnostic underestimation at stereotactic percutaneous core needle biopsies (CNB) and vacuum-assisted biopsies (VABB) of nonpalpable breast lesions, with histopathological results of atypical ductal hyperplasia (ADH) or ductal carcinoma in situ (DCIS) subsequently submitted to surgical excision. As a secondary objective, the frequency of ADH and DCIS was determined for the cases submitted to biopsy. Materials and Methods: Retrospective review of 40 cases with diagnosis of ADH or DCIS on the basis of biopsies performed between February 2011 and July 2013, subsequently submitted to surgery, whose histopathological reports were available in the internal information system. Biopsy results were compared with those observed at surgery and the underestimation rate was calculated by means of specific mathematical equations. Results: The underestimation rate at CNB was 50% for ADH and 28.57% for DCIS, and at VABB it was 25% for ADH and 14.28% for DCIS. ADH represented 10.25% of all cases undergoing biopsy, whereas DCIS accounted for 23.91%. Conclusion: The diagnostic underestimation rate at CNB is two times the rate at VABB. Certainty that the target has been achieved is not the sole determining factor for a reliable diagnosis. Removal of more than 50% of the target lesion should further reduce the risk of underestimation.

Use of the EPR technique to determine thermal stability of some humified organic substances found in soil organic-mineral fractions

In this work, using the EPR spectroscopy, we analysed the thermal stability of some organic-mineral compounds found in a Gleysoil from Rio Janeiro. It was observed a complete disappearance of the EPR signal around 600 °C for the < 2 µm fraction and a residual EPR signal of semiquinone free radical for the 2-20 µm and 20-53 µm fractions at the same temperature. Also, the experiments showed that the 2-20 µm fraction had a larger concentration of semiquinone free radical per g of carbon and a smaller line width indicated a larger humification of this fraction. This is an evidence that the soil organic matter of this fraction (2-20 µm) is more stable than the other ones.

Combined application of continuous wavelet transform-zero crossing technique in the simultaneous spectrophotometric determination of perindopril and indapamid in tablets

Signal processing methods based on the combined use of the continuous wavelet transform (CWT) and zero-crossing technique were applied to the simultaneous spectrophotometric determination of perindopril (PER) and indapamide (IND) in tablets. These signal processing methods do not require any priory separation step. Initially, various wavelet families were tested to identify the optimum signal processing giving the best recovery results. From this procedure, the Haar and Biorthogonal1.5 continuous wavelet transform (HAAR-CWT and BIOR1.5-CWT, respectively) were found suitable for the analysis of the related compounds. After transformation of the absorbance vectors by using HAAR-CWT and BIOR1.5-CWT, the CWT-coefficients were drawn as a graph versus wavelength and then the HAAR-CWT and BIOR1.5-CWT spectra were obtained. Calibration graphs for PER and IND were obtained by measuring the CWT amplitudes at 231.1 and 291.0 nm in the HAAR-CWT spectra and at 228.5 and 246.8 nm in BIOR1.5-CWT spectra, respectively. In order to compare the performance of HAAR-CWT and BIOR1.5-CWT approaches, derivative spectrophotometric (DS) method and HPLC as comparison methods, were applied to the PER-IND samples. In this DS method, first derivative absorbance values at 221.6 for PER and 282.7 nm for IND were used to obtain the calibration graphs. The validation of the CWT and DS signal processing methods was carried out by using the recovery study and standard addition technique. In the following step, these methods were successfully applied to the commercial tablets containing PER and IND compounds and good accuracy and precision were reported for the experimental results obtained by all proposed signal processing methods.

Construção de célula eletroquímica para observação de amostras in situ em estereomicroscópio

The electrochemical study of glass like tungsten oxide derivatives requires the construction of special electrodes due to the fact that these glasses are not conductive. Electrodes modified with WO3 change their color when submitted to some potential perturbation. The color change of the electrochromic materials was observed in situ by coupling an electrochemical cell to a stereomicroscope. The constructed cell is versatile and may represent a great contribution to the electrochemical studies of materials, especially in the systems where it is interest to observe the working electrode surface during the electrochemical experiment.

Produção de biodiesel através de transesterificação in situ de sementes de girassol via catálise homogênea e heterogênea

The objective of this work is to show the results of the in situ transesterification of sunflower seed oil with methanol on basic homogeneous and heterogeneous catalysis for the production of biodiesel. In homogeneous catalysis, the activity of KOH and K2CO3 were evaluated using the same oil:methanol ratio of 1:90. KOH showed to be more active than K2CO3, leading to total conversion in biodiesel after 1h reaction time. In the heterogeneous catalysis the activity of K2CO3/Al2O3 was comparable to the activity of K2CO3 bulk: 53.0 and 66.6% resp. The properties of samples of biodiesel produced by homogeneous and heterogeneous catalysis were evaluated and are in accordance with the recommended fuel properties.

Um sistema microcontrolado para o monitoramento on-line, in situ e remoto de pH, condutividade e temperatura de águas

A portable microcontrolled system is proposed to monitor conductivity, temperature and pH in on-line, in situ and remote way from a water reservoir faraway 200 m. The system comprises two modules: one for data reception (located in laboratory) and another for data acquisition/transmission (located near water reservoir). It uses a microcontroller and a transceiver to remote data transmission/reception by radio frequency. Variations of water parameters were simultaneously monitored without interruption during a period of ten hours with a relative error about 4.0 %. The developed system showed simple, stable, accurate, robust and low-cost to determine parameters of water in field.

In situ synthesis of nanoclay filled polyethylene using polymer supported metallocene catalyst system

In situ ethylene polymerizations were performed using bis(cyclopentadiene)titanium dichloride supported on polyethersulfone as catalyst. The bis(cyclopentadiene)titanium dichloride supported on polyethersulfone catalyst activity estimated by ethylene polymerization was 360 kgPE/molTi/h. During polymerization the fillers used were montmorillionite nanoclays having surface modifications with 35-45 wt% dimethyl dialkyl(14-18)amine (FA) and 25-30 wt% trimethyl stearyl ammonium (FB). These fillers were pretreated with methylaluminoxine (MAO; cocatalyst) for better dispersion onto the polymer matrix. The formation of polyethylene within the whole matrix was confirmed by FTIR studies. It was found that the nature of nanofiller did not have any remarkable effect on the melting characteristics of the polymer. TGA study indicates that nanoclay FB filled polyethylene has higher thermal stability than nanoclay FA filled polyethylene. The melting temperature of the obtained polyethylenes was 142 ºC, which corresponds to that synthesized by the polyether sulfone supported catalyst.

Construção de uma câmara para monitoramento in situ do processo de secagem de geis e sólidos porosos

The present work deals with the design and construction of an equipment for studying the drying process of gels and solids. The equipment was built using mainly a commercial oven and others peripherals for programmed control of temperature, humidity and data acquisition. The system allows the in situ monitoring of the gel drying, registering the weight loss, and the shrinkage of sample and the oven temperatures. This set of allowed parameters makes possible to establish the main steps involved in the drying of meso and nanostructured porous materials.

Construction and application of a portable microcontrolled turbidimeter for the in situ determination of sulfate

This study reports on the construction of a turbidimeter employing light emitting diodes as radiation source at a wavelength of 405 nm, a photodiode as detector, a temperature sensor and a microcontroller used for data acquisition and processing. The turbidimeter was applied to determine sulfate concentrations in natural water employing barium chloride as reagent. Potential interferences and recovery studies were performed and an interference of 3.5 % and a recovery between 97.8 and 108 % were estimated. The analytical performance of in situ turbidimeter for the determination of sulfate was evaluated and compared with two commercial spectrophotometers and a good agreement was obtained.

Desenvolvimento e avaliação de eletrodos de difusão gasosa (EDG) para geração de H2O2 in situ e sua aplicação na degradação do corante reativo azul 19

This work reports the development of GDE for electrogeneration of H2O2 and their application in the degradation process of Reactive Blue 19 dye. GDE produced by carbon black with 20% polytetrafluoroethylene generated up to 500 mg L-1 of H2O2 through the electrolysis of acidic medium at -0.8 V vs Ag/AgCl. Reactive Blue 19 dye was degraded most efficiently with H2O2 electrogenerated in the presence of Fe(II) ions, leading to removal of 95% of the original color and 39% of TOC at -0.8 V vs Ag/AgCl.

Development of a simple analytical method for determining trihalomethanes in beer using a headspace solid-phase microextraction technique

We developed a simple, rapid, and solventless method for analyzing trihalomethanes in beer samples using headspace solid-phase microextraction. The effects of varying experimental parameters, such as extraction temperature and time, addition of sodium chloride, and agitation speed, on extraction yield were studied using a univariate experimental design. Limits of detection between 0.22 and 0.46 µg L- 1 and wide linear ranges were achieved for trihalomethanes. We measured the trihalomethane recoveries and precision (as the standard deviation of repeat measurements) and demonstrated the applicability of the proposed method by analyzing 32 beer samples.

Optimization of solvent mixtures for extraction from bark of Schinus terebinthifolius by a statistical mixture-design technique and development of a UV-Vis spectrophotometric method for analysis of total polyphenols in the extract

A statistical mixture-design technique was used to study the effects of different solvents and their mixtures on the yield, total polyphenol content, and antioxidant capacity of the crude extracts from the bark of Schinus terebinthifolius Raddi (Anacardiaceae). The experimental results and their response-surface models showed that ternary mixtures with equal portions of all the three solvents (water, ethanol and acetone) were better than the binary mixtures in generating crude extracts with the highest yield (22.04 ± 0.48%), total polyphenol content (29.39 ± 0.39%), and antioxidant capacity (6.38 ± 0.21). An analytical method was developed and validated for the determination of total polyphenols in the extracts. Optimal conditions for the various parameters in this analytical method, namely, the time for the chromophoric reaction to stabilize, wavelength of the absorption maxima to be monitored, the reference standard and the concentration of sodium carbonate were determined to be 5 min, 780 nm, pyrogallol, and 14.06% w v-1, respectively. UV-Vis spectrophotometric monitoring of the reaction under these conditions proved the method to be linear, specific, precise, accurate, reproducible, robust, and easy to perform.

Preconcentration of copper from natural water samples using ligand-less in situ surfactant-based solid phase extraction prior to FAAS determination

In the present work, a simple and rapid ligand-less, in situ, surfactant-based solid phase extraction for the preconcentration of copper in water samples was developed. In this method, a cationic surfactant (n-dodecyltrimethylammonium bromide) was dissolved in an aqueous sample followed by the addition of an appropriate ion-pairing agent (ClO4-). Due to the interaction between the surfactant and ion-pairing agent, solid particles were formed and subsequently used for the adsorption of Cu(OH)2 and CuI. After centrifugation, the sediment was dissolved in 1.0 mL of 1 mol L-1 HNO3 in ethanol and aspirated directly into the flame atomic absorption spectrometer. In order to obtain the optimum conditions, several parameters affecting the performance of the LL-ISS-SPE, including the volumes of DTAB, KClO4, and KI, pH, and potentially interfering ions, were optimized. It was found that KI and phosphate buffer solution (pH = 9) could extract more than 95% of copper ions. The amount of copper ions in the water samples varied from 3.2 to 4.8 ng mL-1, with relative standard deviations of 98.5%-103%. The determination of copper in water samples was linear over a concentration range of 0.5-200.0 ng mL-1. The limit of detection (3Sb/m) was 0.1 ng mL-1 with an enrichment factor of 38.7. The accuracy of the developed method was verified by the determination of copper in two certified reference materials, producing satisfactory results.

Detection of Rhynchosporium secalis in barley seeds from Argentina through polymerase chain reaction technique

Leaf scald of barley caused by Rhynchosporium secalis is an important disease in Argentina. The fungus is a necrotrophic pathogen which survives in stubble, seeds and weeds. Isolation of R. secalis from seeds on artificial media usually has not been successful due to the slow growth rate of the pathogen and strong inhibition by contaminants. The objective in this work was to detect R. secalis in different genotypes of barley seeds in Argentina using the polymerase chain reaction (PCR)-based diagnostic assay. Four barley genotypes were tested in 2004: Quilmes Ayelén, Quilmes Alfa, Barke and Maltería Pampa 1004. The previously described RS8 and RS9 primers were used for the detection of R. secalis in barley seeds. A 264-bp single band was obtained for each cultivar showing the presence of R. secalis. The use of specific primers was efficient in the detection of R. secalis in barley seeds in Argentina and could be used for routine diagnosis, epidemiology and seed transmission studies. This is the first report on the detection of R. secalis in barley seeds in Argentina.