Determinação de chumbo em álcool combustível por voltametria de redissolução anódica utilizando um eletrodo de pasta de carbono modificado com resina de troca iônica Amberlite IR 120

Um método envolvendo a pré-concentração e redissolução anódica em condições de voltametria de pulso diferencial empregando um eletrodo de pasta de carbono modificado (EPCM) com uma resina de troca iônica Amberlite IR120 foi proposto para a determinação de íons chumbo em álcool combustível. O procedimento é baseado em um pico de oxidação do analito observado em -0,53 V(vs. Ag/AgCl) em solução de HCl. As melhores condições experimentais encontradas foram: 5% (m/m) da Amberlite IR120 para a construção do eletrodo, solução de HCl 0,1 mol L-1, velocidade de varredura de 10 mVs-1, tempo de pré-concentração de 15 min e amplitude de pulso de 100 mV. Utilizando essas condições, o EPCM apresentou uma resposta linear entre a corrente de pico anódica e a concentração de íons chumbo para o intervalo entre 9,9 x 10-9 e 1,2 x 10-6 mol L-1 e um limite de detecção de 7,2 x 10-9 mol L-1. Valores de recuperação entre 96 % e 102 % foram encontrados para amostras de álcool combustível enriquecidas com Pb2+ em níveis de 10-7 mol L-1. O efeito da presença de outros íons concomitantes sobre a resposta voltamétrica do eletrodo também foi avaliado.

A Simple and Green Analytical Method for the Determination of Formaldehyde

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Estudo de alguns esfeitos na precipitação de partículas esféricas de sílica via microemulsão inversa

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

Determinação espectrofotométrica de citrato de sildenafil em formulações farmacêuticas

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

Aproveitamento de um fosfato natural parcialmente solubilizado pelas culturas do arroz, milho e soja: I. Resultados preliminares

Em solos pouco ácidos, pobres em P disponível, dois dos quais anteriormente com vegetação de cerrado, foram conduzidos ensaios destinados a comparar a eficiência de um fosfato natural parcialmente acidulado com ácido sulfúrico (FAPS) com a do super simples (SS) e a do fosfato de Araxá original. Usaram-se as culturas de arroz de sequeiro, milho e soja. Verificou-se que: (1) o FAPS deu produções que não diferiram estatísticamente das obtidas com o SS sendo maiores que as conseguidas com o FA; (2) os resultados das análises de solos e da diagnose foliar indicam que o FAPS funcionou como fonte de P, Ca e S.

Curva de sobrevivência e estimativa de entropia em Lucilia cuprina (Diptera, Calliphoridae)

Lucilia cuprina (Wiedemann, 1830) is a cosmopolite blowfly species of medical and veterinary importance because it produces myiasis, mainly in ovine. In order to evaluate the demographic characteristics of this species, survivorship curves for 327 adult males and 323 adult females, from generation F1 maintained under experimental conditions, were obtained. Entropy was utilized as the estimator of the survival pattern to quantify the mortality distribution of individuals as a function of age. The entropy values 0.216 (males) and 0.303 (females) were obtained. These results denote that, considering the survivorship interval until the death of the last individual for each sex, the males present a tendency of mortality in more advanced age intervals, in comparison with the females.

Controle químico do aguapé (Eichhornia crassipes)

Foram testados os produtos 2,4-D, sulfentrazone, glyphosate, diquat, imazapyr, imazapic, metsulfuron-metil e sulfosate. Conduziram-se seis ensaios em condições controladas de casa de vegetação, visando estudar a eficácia no controle de Eichhornia crassipes (Mart.) Solms. em todos os ensaios, as plantas de aguapé foram cultivadas em caixas com substrato como material de fundo e água completando o volume; os herbicidas foram aplicados com pulverizador costal a CO2. No primeiro ensaio, foram testados os herbicidas diquat, glyphosate, imazapyr e sulfentrazone. O diquat e o glyphosate foram altamente eficazes no controle de E. crassipes, com ação mais rápida do primeiro produto. Imazapyr e sulfentrazone indicaram que maior intensidade de controle poderá ser obtida em maior tempo de observação. No segundo ensaio, foram testados diquat, glyphosate, imazapyr, imazapic, 2,4-D, metsulfuron-metil e sulfosate. Diquat, glyphosate, imazapyr e 2,4-D foram eficazes no controle do aguapé. Diquat e 2,4-D mostraram ação mais rápida. O imazapyr apresentou lenta evolução, e o glyphosate, ação intermediária. Os herbicidas imazapic, sulfosate e metsulfuron, em função do tempo de avaliação, não mostraram eficácia satisfatória. No terceiro ensaio, foram estudados imazapyr e glyphosate aplicados três, seis e nove horas antes da incidência de chuva simulada. O glyphosate apresentou maior eficácia que o imazapyr e o glyphosate não sofreu influência do intervalo entre a aplicação e a ocorrência de chuva. No entanto, o desenvolvimento inicial dos sintomas foi mais rápido em intervalos maiores. No quarto ensaio foi estudado o diquat, aplicado nos períodos noturno e diurno, o qual foi eficiente no controle do aguapé na dose de 1,0 L ha-1 ou acima. Aplicações noturnas apenas proporcionaram ação mais rápida do produto, não influenciando o controle final. No quinto ensaio foi estudado o diquat em aplicações diurnas ou noturnas e em intervalos de 30, 60 e 120 minutos entre a aplicação e a ocorrência de chuva simulada, tendo ele mostrado elevada atividade herbicida contra o aguapé, com eficácia maior na dose de 2,00 L ha-1. A ação do produto foi maior em aplicações noturnas, período em que houve maior importância da extensão do intervalo entre a aplicação do produto e a ocorrência da primeira chuva. O último ensaio foi realizado em campo, para estudo da ação do imazapyr aplicado sobre plantas de aguapé crescidas em caixas de cimento-amianto. Todas as doses estudadas proporcionaram controle total da planta daninha. As doses mais elevadas apresentaram efeitos mais rápidos.

Evaluation of extracts from Coccoloba mollis using the Salmonella/microsome system and in vivo tests

The common everyday use of medicinal plants is an ancient, and still very widespread practice, whereby the need for studies on their possible toxicity and mutagenic properties. The species Coccoloba mollis has been much used in phytotherapy, mainly in cases involving loss of memory and stress. In order to investigate its genotoxic and mutagenic potential, ethanolic extracts from the leaves and roots underwent Salmonella/microsome assaying (TA98 and TA100 strains, with and without exogenous metabolism - S9), besides comet and micronucleus tests in vivo.There was no significant increase in the number of revertants/plate of Salmonella strains in any of the analyzed root-extract concentrations, although the extract itself was extremely toxic to the Salmonella TA98 strain in the tests carried out with S9 (doses varying from 0.005 to 0.5 µg/plate). on the other hand, the leaf-extract induced mutations in the TA98 strain in the absence of S9 in the highest concentration evaluated, although at very low mutagenic potency (0.004 rev/µg). Furthermore, there was no statistically significant increase in the number of comets and micronuclei, in treatments involving Swiss mice. It was obvious that extracts of Coccoloba mollis, under the described experimental conditions, are not mutagenic.

Extraction and clean-up procedure for analysis of organochlorine pesticide residues in ethoxylated lanolin

In the present study an evaluation was made of a method for the determination of organochlorine pesticide residues in ethoxylated lanolin. Samples were homogenized with Celite, transferred to chromatographic columns, prepacked with silica gel deactivated to 10%. The pesticide elution was processed with n-hexane-dichloromethane and the concentrated eluate was analyzed using gas-liquid chromatography (GC) with electron capture detection (ECD). The composition of the elution solvent was a significant factor for the recovery of the pesticides. Mean recoveries obtained for fortified samples ranged from 87 to 94% for p,p'-DDE, dieldrin, endrin, p,p'-DDD and p,p'-DDT. Optimization of the experimental conditions resulted in a small-scale method that combines extraction and cleanup in a single step. (C) 2000 Elsevier B.V. S.A. All rights reserved.

Evaluation and application of bismuth as an internal standard for the determination of lead in wines by simultaneous electrothermal atomic absorption spectrometry

A method for the direct determination of Pb in wines by simultaneous multi-element atomic absorption spectrometry (SIMAAS) using a transversely heated graphite atomizer, Zeeman-effect background corrector and internal standardization is proposed. Bismuth was used as an internal standard and Pd(NO3)(2) plus Mg(NO3)(2) as chemical modifier,to stabilize both the analyte and the internal standard. The implementation of two pyrolysis steps avoided any build-up of carbonaceous residues on the graphite platform. All diluted samples (1 + 1 v/v) in 0.2% v/v HNO3 and reference solutions (5.0-50 mug l(-1) Ph in 0.2% v/v HNO3) were spiked with 25 mug l(-1) Bi. For a 20 mul aliquot dispensed into the graphite tube, a good correlation (r = 0.9997) was obtained between the ratio of the analyte signal to the internal standard signal and the analyte concentration of the reference solutions. The electrothermal behaviour of Pb and Bi in red, white and rose wines were compared. In addition, absorbance variations due to changes in experimental conditions, such as atomizer temperature, integration time, injected sample volume, radiation beam intensity, graphite tube surface, dilution and sample composition, were minimized by using Bi as internal standard. Relative standard deviations of measurements based on integrated absorbance varied from 0.1 to 3.4% and from 0.5 to 7.3% (n = 12) with and without internal standard correction, respectively. Good recoveries (91-104%) for Pb spikes were obtained. The characteristic mass was 45 pg Pb and the limit of detection based on integrated absorbance was 0.9 mug l(-1) Pb. Internal standardization increased the lifetime of the tube by 25%. Direct determinations of Pb in wines with and without internal standardization approaches were in agreement at the 95% confidence level. The repeatability and the tube lifetime were improved when using Bi as internal standard. The improvement in accuracy using an internal standard was only observed when the analytical results were affected by errors.

Physical activity and postural control in the elderly: Coupling between visual information and body sway

Background: Aging is characterized by a decline in the postural control performance, which is based on a coherent and stable coupling between sensory information and motor action. Therefore, changes in postural control in elderlies can be related to changes in this coupling. In addition, it has been observed that physical activity seems to improve postural control performance in elderlies. These improvements can be due to changes in the coupling between sensory information and motor action related to postural control. Objective: the purpose of this study was to verify the coupling between visual information and body sway in active and sedentary elderlies. Methods: Sixteen sedentary elderlies ( SE), 16 active elderlies ( AE) and 16 young adults ( YA) were asked to stand upright inside a moving room in two experimental conditions: ( 1) discrete movement and ( 2) continuous movement of the room. Results: In the continuous condition, the results showed that the coupling between the movement of the room and body sway was stronger and more stable for SE and AE compared to YA. In the discrete condition, SE showed larger body displacement compared to AE and YA. Conclusions: SE have more difficulty to discriminate and to integrate sensory information than AE and YA indicating that physical activity may improve sensory integration. Copyright (C) 2005 S. Karger AG, Basel.

Laboratory essays on solid residues from an area of sand mining activities at Analandia, São Paulo, Brazil, and implications to the water resources quality

This investigation reports the results of tests performed in a laboratory with solid waste samples from an area belonging to Sibelco Mineracao Ltd., which is located around Analandia municipality, nearly in the center of São Paulo State, Brazil. Dissolution and leaching essays were realized under different experimental conditions in four samples collected from the mining front and decantation pool, with the aim of evaluating the possibility of release of several constituents to the liquid phase.

Flow injection amperometric determination of procaine in pharmaceutical formulation using a screen-printed carbon electrode

A rapid and simple method for procaine determination was developed by flow injection analysis (FIA) using a screen-printed carbon electrode (SPCE) as amperometric detector. The present method is based on the amine/hydroxylamine oxidation from procaine monitored at 0.80 V on SPCE in sodium acetate solution pH 6.0. Using the best experimental conditions assigned as: pH 6.0, flow rate of 3.8 mL min(-1), sample volume of 100 mu L and analytical path of 30 cm it is possible to construct a linear calibration curve from 9.0 x 10(-6) to 1.0 x 10(-4) mol L-1. The relative standard deviation for 5.0 x 10(-5) mol L-1 procaine (15 repetitions using the same electrode) is 3.2% and detection limit calculated is 6.0 x 10(-6) mol L-1. Recoveries obtained for procaine gave a mean values from 94.8 to 102.3% and an analytical frequency of 36 injections per hour was achieved. The method was successfully applied for the determination of procaine in pharmaceutical formulation without any pre-treatment, which are in good accordance with the declared values of manufacturer and an official method based on spectrophotometric analysis. (c) 2006 Elsevier B.V. All rights reserved.

BaTiO3 obtained through metallic stearate precursors

Metallic stearates were used as precursors to obtain BaTiO3. Barium and titanium stearate mixtures were homogenized in ball mill containing some amount of ammonium stearate. The mixture of the precursors was evaluated by simultaneous TG/ DTA and TMA, and residues from thermal decomposition were characterized by XRD and SEM. It could be verified that the residues from the thermal decomposition in both oxidant and inert atmospheres were the BaTiO3 but with characteristic morphological and crystalline aspects depending on the experimental conditions in which the mixtures of precursors were obtained. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Determination of selenium in nutritionally relevant foods by graphite furnace atomic absorption spectrometry using arsenic as internal standard

A method has been developed for the direct determination of Se in nutritionally relevant foods by graphite furnace atomic absorption spectrometry. Tungsten/rhodium carbide coating on the integrated platform of a transversely heated graphite atomizer or W coating with co-injection of Pd(NO3)(2) were used as a permanent modifiers. Samples and reference solutions were spiked with 500 mu g L-1 As and absorbance variations due to changes in experimental conditions were minimized. For 20 mu L aqueous analytical solutions delivered into the graphite tube, analytical curves in the 5.0-40 mu g L-1 with good linear correlation were established. Pyrolysis and atomization temperatures were evaluated using pyrolysis and atomization curves, respectively. The optimized heating program (temperature, ramp time, hold time) of the graphite tube of the Perkin-Elmer SIMAA 6000 atomic absorption spectrometer was: dry steps (110 degrees C, 5 s, 10 s; 130 degrees C, 15 s, 15 s); air-assisted pyrolysis step (600 degrees C, 20 s, 40 s; 20 degrees C, 1 s, 40 s); pyrolysis step (1300 degrees C, 10 s, 20 s); atomization step (2100 degrees C, 0 s, 4 s); clean step (2550 degrees C, 1 s, 5 s). The method was applied for Se determination in coconut water, coconut milk, soybean milk, cow milk, tomato juice, mango juice, grape juice and drinking water samples and four standard reference materials and results were in agreement at 95% confidence level. The lifetime of the tube was 500 firings and the relative standard deviations of measurements of typical samples containing 25 mu gL(-1) Se were 3.0% and 6.0% (n = 12) with and without internal standardization, respectively. The limits of detection were in the 0.35 mu g L-1-0.7 mu g Se L-1 range. The accuracy of the proposed method was evaluated by an addition-recovery experiment and all recovered values were in the 98-109% range. (c) 2004 Elsevier Ltd. All rights reserved.