A cubic silsesquioxane modified with purpald®: Preparation, characterization and a voltammetric application for determination of sulfite

A novel composite formed by interaction of a octa(3-chloropropyl)octasilsesquioxane modified with Purpald®, and its subsequent reaction with silver and hexacyanoferrate (III) (AgHSP), was synthesized and initially characterized by Fourier transform infrared spectra (FTIR) and cyclic voltammetry. The cyclic voltammogram of the modified graphite paste electrode with AgHSP, showed one redox couple with formal potential Eθ'=0.64V (vs Ag/AgCl, KNO3, 1.0 mol L-1; v = 20 mV s-1), attributed to the Fe2+(CN)6/ Fe3+(CN)6 process. The redox couple presents an electrocatalytic response for determination of sulfite. The modified electrode showed a linear response from 7.0×10-5 to 1.0×10-3 mol L-1 with the corresponding equation Y(μA) = 18.05 + 29.983×103 [sulfite], and a correlation coefficient of r=0.999. The method showed a detection limit of 0.115×10-4 mol L-1 with a relative standard deviation of ± 4% (n = 3) and amperometric sensitivity of 29.983×10-3A mol L-1. The modified electrode showed a excellent stability and good reproducibility during experiments. © 2013 by ESG.

Evaluation of sample preparation procedures and krypton as an interference standard probe for arsenic speciation by HPLC-ICP-QMS

Different conditions of extraction using water, a methanol-water mixture and nitric acid solutions were evaluated for speciation of As(iii), As(v), DMA and MMA in plant samples that previously received As(v) after being sown and emergence was investigated. Microwave-assisted extraction (MAE) using diluted nitric acid solutions was also performed for arsenic extraction from chicken feed samples. The separation and determination of arsenic species were performed using HPLC-ICP-MS. The interference standard method (IFS) using 83Kr+ as the IFS probe was employed to minimize spectral interferences caused by polyatomic species, such as 40Ar 35Cl+. The extraction procedures tested presented adequate extraction efficiencies (90%), and the four arsenic species evaluated were found in plant samples. Extractions with diluted nitric acid solution at 90 °C were the most efficient strategy, with quantitative recoveries for all four As species in plant tissues. On the other hand, the methanol-water mixture was the solvent with the lowest extraction efficiency (50-60%). For chicken feed samples, MAE at 100 °C for 30 min resulted in an extraction efficiency of 97% and only As(v) was found, without any species interconversion. The IFS method contributed to improving precision and limits of detection and quantification for all tested extraction procedures. Significant improvements on accuracy were obtained by applying the IFS method and recoveries between 77 and 94%, and 82 and 93% were obtained for plant extracts and chicken feed samples, respectively. This journal is © 2013 The Royal Society of Chemistry.

Zoneamento geoambiental do município de São João da Boa Vista (SP)

Pós-graduação em Geociências e Meio Ambiente - IGCE

Flow-batch analyser for preparation of calibration standard mixtures in simultaneous multicomponent spectrometric analysis

ABSTRACT: The application of multivariate calibration techniques to multicomponent analysis by UV-VIS molecular absorption spectrometry is a powerful tool for simultaneous determination of several chemical species. However, when this methodology is accomplished manually, it is slow and laborious, consumes high amounts of reagents and samples, is susceptible to contaminations and presents a high operational cost. To overcome these drawbacks, a flow-batch analyser is proposed in this work. This analyser was developed for automatic preparation of standard calibration and test (or validation) mixtures. It was applied to the simultaneous determination of Cu²⁺, Mn²⁺ and Zn²⁺ in polyvitaminic and polymineral pharmaceutical formulations, using 4-(2-piridilazo) resorcinol as reagent and a UV-VIS spectrophotometer with a photodiode array detector. The results obtained with the proposed system are in good agreement with those obtained by flame atomic absorption spectrometry, which was employed as reference method. With the proposed analyser, the preparation of calibration and test mixtures can be accomplished about four hours, while the manual procedure requires at least two days. Moreover, it consumes smaller amounts of reagents and samples than the manual procedure. After the preparation of calibration and test mixtures, 60 samples^-1 can be carried out with the proposed flow-batch analyser.

Uranium-lead dating method at the Pará-Iso isotope geology laboratory, UFPA, Belém – Brazil

ABSTRACT: Analytical procedures for U-Pb isotope dilution analyses at the Pará-Iso isotope geology laboratory of the Federal University of Pará (UFPA) are described in detail. The procedures are applied to zircon, titanite, rutile, apatite, columbite-tantalite and whole rock. Reagent preparation and chemical processing are done in clean-room conditions. Samples are dissolved using Teflon™ microcapsules in steel jacket Teflon™ Parr Instrument™ bomb or Teflon™ screw cap containers. U and Pb are separated using anion exchange AG 1x8 resin columns. Typical blanks for mineral sample amounts of 0.01 to 1.0 mg are less than 1 pg U and 20-30 pg Pb. Isotope analysis of the U and Pb from the same filament are carried out using a Finnigan MAT 262 mass-spectrometer in static and dynamic modes. The current analytical level is demonstrated on analyses of international standard zircon 91500 with three different ²³⁵U-²⁰⁵Pb and ²³⁵U-²⁰⁸Pb isotope tracers and whole rock standards. Results of analyses of two zircon samples are also presented.

Use of synthetic aperture radar for recognition of Coastal Geomorphological Features, land-use assessment and shoreline changes in Bragança coast, Pará, Northern Brazil

Imagens de radar de abertura sintética (SAR) vem sendo bem mais utilizadas do que antes nas aplicações de geociências em regiões tropicais úmidas. Nesta investigação, uma imagem RADARSAT-1, na banda C, polarização HH adquirida em 1998 foi usada para o mapeamento costeiro e avaliação da cobertura da terra na área de Bragança, norte do Brasil. Imagem do radar aerotransportado GEMS-1000, na banda X, polarização HH, adquirida em 1972 durante o projeto RADAM foi também utilizada para avaliar as variações costeiras ocorridas nas últimas três décadas. A pesquisa tem confirmado a utilidade da imagem RADARSAT-1 para o mapeamento geomorfológico e avaliação da cobertura da terra, particularmente em costas de manguezal de macromaré. Além disso, um novo método para estimar as variações da linha de costa baseado na superposição de vetores extraídos de diferentes imagens SAR, com alta acurácia geométrica, tem mostrado que a planície costeira de Bragança tem estado sujeita a severa erosão responsável pelo recuo de aproximadamente 32 km² e acreção de 20 km², resultando em uma perda de área de manguezal de aproximadamente 12 km². Como perspectiva de aplicação, dados SAR orbitais e aerotransportados provaram ser uma importante fonte de informação tanto para o mapeamento geomorfológico, quando para o monitoramento de modificações costeiras em ambientes tropicais úmidos.

Preparation of refractory calcium aluminate cement using the sonochemical process

Calcium aluminate cements (CAC) were prepared using the sonochemical process, followed by heat treatment. A study was made of the action of ultrasonic waves and the influence of thermal treatment conditions on two initial molar compositions of 1:1 and 1:2 of calcia:alumina. The aqueous suspension containing the raw materials (A-50 alumina and CaO) was subjected to an ultrasonic bath, followed by drying and burning at 1000, 1200 and 1300 ºC. These cements were characterized by SEM, XRD and the mechanical strength was evaluated by splitting tensile tests, using commercial cement as a reference. Furthermore, the phases were semi-quantified using the Rietveld method. The results show that hydration and sonochemical action increased the reactivity of the raw materials during firing and that phase formation is dependent on the thermal treatment conditions. The CAC cements were obtained at temperatures at least 200 ºC lower than those used in conventional methods, indicating the potential of this route of synthesis.

Rapid preparation of alpha-FeOOH and alpha-Fe2O3 nanostructures by microwave heating and their application in electrochemical sensors

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

A cubic silsesquioxane modified with purpald (r) : preparation, characterization and a voltammetric application for determination of sulfite

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

A novel hybrid composite formed by reaction of 4,5-diphenyl-2-imidazolethiol with hexacyanoferrate (iii) and subsequent reaction with copper (ii): preparation, characterization and a voltammetric application for determination of l-glutatione

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

Bacterial cellulose as a template for preparation of hydrotalcite-like compounds

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

Preparation and characterization of PEG-coated silica nanoparticles for oral insulin delivery

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

Unusual broadening of the NIR luminescence of Er3+-doped Nb2O5 nanocrystals embedded in silica host: Preparation and their structural and spectroscopic study for photonics applications

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

Preparation and Characterization of Chitosan Nanoparticles for Zidovudine Nasal Delivery

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

Elaboração de mapa de susceptibilidade de corridas de massa/detritos e ondas de cheia, aplicado a empreendimentos dutoviários, na bacia hidrográfica do Ribeirão da Prata (SP)

Given the intense expansion of the industries in Brazil and the discovery of hydrocarbons in the pre-salt layer of the Santos and Campos Basin, there is a need to expand the distribution of oil and gas network in the country. The present work aims to present the development of susceptibility map by two distinct methods of two events (debris flows and full wave), applied to the establishment of pipelines on Ribeirão da Prata Basin. The research area covers two municipalities: São João da Boa Vista and Águas da Prata, in total 145 km2. In the paper was used the methodology proposed by Zaine (2011) for the physiographic subdivision method, which uses geological maps, geomorphological maps, digital terrain models and aerial photographs, used to extract the main elements of the physical environment, as rivers, lines, ridges, tops forms and valley forms and historical processes. Thus, the basin was divided into 11 physiographic zones, considering the following elements: thickness of soil, rock type, geomorphology, amplitude, ridges orientation, erosion occurences and mass movements. Were subsequently performed location maps of dams, that had as main purpose to localize major dams in the study area along with their area and perimeter of the reservoir, and land use map that subdivided the area in woody vegetation, permanent culture, temporary culture and urban area. Along with the preparation of the auxiliar maps was conducted a field campaign with three days and approximately 2 points per km2, which aimed to better understand the physical environment and check the main peculiarities of the study area. Criteria have been established for susceptibility maps physiographic subdivision and land use, and a survey of criteria weights used in each map for both processes under study. For the preparation of susceptibility maps were adopted two different methods, which treat the weighted average and the multiplicand. The weighted average method it is...