Evaluation of sample treatment for the simultaneous flow injection hydride generation and determination of As, Bi, Sb and Se by GRAS

A new method was developed for the simultaneous determination of As, Bi, Sb, and Se by flow injection hydride generation graphite furnace atomic absorption spectrometry. An alternative two-step sample treatment procedure was used. The sample was heated (80degreesC) for 10 min in 6 M HCl to reduce Se(VI) to Se(IV), followed by the addition of 1% (m/v) thiourea solution to reduce arsenic and antimony from the pentavalent to the trivalent states.With this procedure, all analytes were converted to their most favorable and sensitive oxidation states to generate the corresponding hydrides. The pre-treated sample solution was then processed in the flow system for in situ trapping and atomization in a graphite tube coated with iridium. The impermanent modifier remained stable up to 300 firings and new coating out significant were possible wit changes in the analytical performance.The accuracy was checked for As, Bi, Sb, and Se determination in water standard reference materials NIST 1640 and 1643d and the results were in agreement with the certified values at a 95% confidence level. Good recoveries (94-104%.) of spiked mineral waters and synthetic As(V), Sb(Ill), mixtures of As(Ill), Sb(V), Se(VI), and Se(IV) were also found. Calculated characteristic masses were 32 mug As, 79 mug Bi, 35 mug Sb, and 130 pg Se, and the corresponding limits of detection were 0.06, 0.16, 0.19, and 0.59 mug L-1, respectively. The repeatability for a typical solution containing 5 mug L-1 As, Bi, Sb, and Se was in the 1-3% range.

Influence of simultaneous addition of MnO2 and CoO on properties of SnO2-based ceramics

This paper reports on a study of the: effect of replacing CoO by MnO2 on the sintering and electrical propel-ties of the 98.95% SnO2 + (1 - x)% CoO + x% MnO2 + 0.05% Ta2O5 system. All the samples were compacted into pellets and sintered at 1300 degrees C for 1 h, when they reached densities of about 98% of the theoretical density. An X-ray diffraction (XRD) analysis showed no other detectable phases other than SnO2. Current-voltage characterization indicated varistor behavior in the systems. The non-linear coefficient (alpha) and breakdown electric field (Eb) increased as the amount of MnO2 was increased. The results are explained in terms of an electric barrier modification, due to the presence of adsorbed negative oxygen species at the grain boundary inter face. (C) 2000 Elsevier B.V. B.V. All rights reserved.

Direct electron paramagnetic resonance monitoring of the peptide synthesis coupling reaction in polymeric support

This work demonstrates, for the first time. a time-resolved electron paramagnetic resonance (EPR) monitoring of a chemical reaction occurring in a polymeric structure. The progress of the coupling of a N-alpha-tert-butyloxycarbonyl-2.2.6.6-tetramethylpiperidine-1-oxyl-4-amino-4-carboxylic acid (Boc-TOAC) spin probe to a model peptide-resin was followed through EPR spectra. Progressive line broadening of EPR peaks was observed, indicative of an increased population of immobilized spin probe molecules attached to the solid support. The time for spectral stabilization of this process coincided with that determined in a previous Coupling study. thereby validating this in situ quantitative monitoring of the reaction. In addition, the influence of polymer swelling degree and solvent viscosity, as well as of the steric hindrance within beads. on the rate of coupling reaction was also addressed. A deeper evaluation of the latter effect was possible by determining unusual polymer parameters such as the average site-site distance and site-concentration within resin beads in each solvent system. (c) 2006 Elsevier Ltd. All rights reserved.

Growth of SnO nanobelts and dendrites by a self-catalytic VLS process

This article reports on the growth of SnO nanobelts and dendrites by a carbothermal reduction process. The materials were synthesized in a sealed tube furnace at 1210 degrees C and at 1260 degrees C for 2 h. in a dynamic nitrogen atmosphere of 40 seem. After synthesis, gray-black materials were collected downstream in the tube and the samples were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy-dispersive X-ray spectroscopy (EDX). The results showed that the gray-black materials were composed of nanobelts, which grew in the [110] direction of the orthorhombic structure of SnO. Some of the belts also presented dendritic growth. The dendrites grew in the (110) planes of the SnO structure, and no defects were observed at the junction between the nanobelts and the dendrites. A self-catalytic vapor-liquid-solid (VLS) process was proposed to explain the growth of the SnO nanobelts and dendrites.

Effect of Different Solvent Ratios (Water/Ethylene Glycol) on the Growth Process of CaMoO4 Crystals and Their Optical Properties

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

All-on-four concept and immediate loading for simultaneous rehabilitation of the atrophic maxilla and mandible with conventional and zygomatic implants

We report the simultaneous rehabilitation of an edentulous patient with a hybrid (zygomatic and conventional implants) all-on-four implant-supported prosthesis for the maxilla and a standard (conventional implants) all-on-four implant-supported prosthesis for the mandible. The transfer impression was made with a multifunctional guide and the upper and lower prostheses were placed 24 h postoperatively. Clinical and radiographic examinations showed no infection or bony resorption 2 years later. Simultaneous maxillary and mandibular rehabilitation with all-on-four immediate loading is a viable, fast and effective option for edentulous patients. (C) 2009 Published by Elsevier Ltd on behalf of The British Association of Oral and Maxillofacial Surgeons.

Selection of radio transmitter and attachment method for post-release monitoring of captive-bred reintroduced Red-billed Curassow Crax blumenbachii, Brazil

Long-term monitoring of reintroduced individuals is a central component of many endangered species reintroduction programs. Radio-telemetry techniques are rarely used to monitor reintroduced captive-bred Cracids and few data exist regarding possible adverse effects of radio-tagging Cracids. In this study, we identify an appropriate radio transmitter design and develop a suitable attachment method that minimizes anthropogenic influence and enables long-term, post-release monitoring (2-3 years) of reintroduced captive-bred Red-billed Curassows in the Brazilian Atlantic Rainforest. We also review studies about the effects of different VHF radio transmitter models on survival, reproduction, behavior, and physiology of Galliformes.

Monitoring the covariance matrix with the VMAX chart

In this article, we propose a new statistic to control the covariance matrix of bivariate processes. This new statistic is based on the sample vat-lances of the two quality characteristics, shortly VMAX statistic. The points plotted on the chart correspond to the maximum of the values of these two variances. The reasons to consider the VMAX statistic instead of the generalized variance vertical bar S vertical bar are faster detection of process changes and better diagnostic feature, that is, with the VMAX statistic It is easier to identify the out-of-control variable.

Structural refinement, growth process, photoluminescence and photocatalytic properties of (Ba1-xPr2x/3)WO4 crystals synthesized by the coprecipitation method

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

Evaluation of different rhodium modifiers and coatings on the simultaneous determination of As, Bi, Pb, Sb, Se and of Co, Cr, Cu, Fe, Mn in milk by electrothermal atomic absorption spectrometry

Different kinds of modifiers and coatings on the integrated platform of transversely heated graphite atomizer (THGA) have been tested for the simultaneous determination of two group of elements: the first, the more volatile, formed by arsenic, bismuth, lead, antimony and selenium; the second, the less volatile, formed by cobalt, chromium, cupper, iron and manganese in milk by electrothermal atomic absorption spectrometry. Different Rh-modifiers were studied, such as Rh-coated platforms (Rh), carbide plus rhodium coated platforms (W-Rh, Zr-Rh), carbide-coated platforms (W and Zr) with co-injection of RhCl3, solutions and uncoated platforms with injection of solutions of Pd(NO3)(2), Mg(NO3)(2), and RhCl3. Milk samples were diluted 1:10 in 1.0% HNO3 and injected into the tube. The mass of modifier deposited and co-injected in the tube and the use of end capped tubes were also evaluated in order to improve the electrothermal behavior of analytes. Integrated platform pretreated with W plus co-injection RhCl3 for first group and pretreated with W-Rh for second group were elected. For 20 mu L injected samples the analytical curves in the 5.0-20.0 mu g L-1 concentration range have good linear correlation coefficients (r > 0.998). Relative standard deviations (n = 12) are < 6% and the calculated characteristic masses are between 5 pg and 62 pg.

Degradation of the antibiotic amoxicillin by photo-Fenton process - Chemical and toxicological assessment

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

Fresh autogenous rib cartilage graft to the malar process of rats with and without removal of the perichondrium: a histological study.

A comparison was made of autogenous grafts of rib cartilage with and without removal of the perichondrium, applied to the malar process of rats. Seventy-two male albino rats were divided into two groups according to the kind of graft received by each animal. The experimental periods were 5, 10, 20, 30, 60 and 120 postoperative days. The results showed that, in the control group, the grafts maintained their vitality for the whole experimental period and the perichondrium was biologically integrated into the host bed. Appositional growth was also observed. The treated animals showed intense resorption of the grafts and more intense bone neoformation. The newly formed bone was in intimate contact with the graft in both groups.

Joint X̄ and R Charts with Variable Sample Sizes and Sampling Intervals

Recent studies have shown that the X̄ chart with variable sampling intervals (VSI) and/or with variable sample sizes (VSS) detects process shifts faster than the traditional X̄ chart. This article extends these studies for processes that are monitored by both the X̄ and R charts. A Markov chain model is used to determine the properties of the joint X and R charts with variable sample sizes and sampling intervals (VSSI). The VSSI scheme improves the joint X̄ and R control chart performance in terms of the speed with which shifts in the process mean and/or variance are detected.

Concept of Matching Parallelepiped and its use in the correspondence problem

In this paper, the concept of Matching Parallelepiped (MP) is presented. It is shown that the volume of the MP can be used as an additional measure of `distance' between a pair of candidate points in a matching algorithm by Relaxation Labeling (RL). The volume of the MP is related with the Epipolar Geometry and the use of this measure works as an epipolar constraint in a RL process, decreasing the efforts in the matching algorithm since it is not necessary to explicitly determine the equations of the epipolar lines and to compute the distance of a candidate point to each epipolar line. As at the beginning of the process the Relative Orientation (RO) parameters are unknown, a initial matching based on gradient, intensities and correlation is obtained. Based on this set of labeled points the RO is determined and the epipolar constraint included in the algorithm. The obtained results shown that the proposed approach is suitable to determine feature-point matching with simultaneous estimation of camera orientation parameters even for the cases where the pair of optical axes are not parallel.

Simultaneous determination of As, Cu, Mn, Sb, and Se in drinking water by GFAAS with transversely heated graphite atomizer and longitudinal zeeman-effect background correction

A method has been developed for the direct and simultaneous determination of As, Cu, Mn, Sb, and Se in drinking water by electrothermal atomic absorption spectrometry (ETAAS) using a transversely heated graphite tube atomizer (THGA) with longitudinal Zeeman-effect background correction. The thermal behavior of analytes during the pyrolysis and atomization stages was investigated in 0.028 mol L-1 HNO3, 0.14 mol L-1 HNO3 and 1 + 1 (v/v) diluted water using mixtures of Pd(NO3)2 + Mg(NO3)2 as the chemical modifier. With 5 μg Pd + 3 μg Mg as the modifier, the pyrolysis and atomization temperatures of the heating program of the atomizer were fixed at 1400°C and 2100°C, respectively, and 20 μL of the water sample (sample + 0.28 mol L-1 HNO3, 1 + 1, v/v), dispensed into the graphite tube, analytical curves were established ranging from 5.00 -50.0 μg L-1 for As, Sb, Se; 10.0 - 100 μg L-1 for Cu; and 20.0 - 200 μg L-1 for Mn. The characteristic masses were around 39 pg As, 17 pg Cu, 60 pg Mn, 43 pg Sb, and 45 pg Se, and the lifetime of the tube was around 500 firings. The limits of detection (LOD) based on integrated absorbance (0.7 μg L-1 As, 0.2 μg L-1 Cu, 0.6 μg L-1 Mn, 0.3 μg L-1 Sb, 0.9 μg L-1 Se) exceeded the requirements of the Brazilian Food Regulations (decree # 310-ANVS from the Health Department), which established the maximum permissible level for As, Cu, Mn, Sb, and Se at 50 μg L-1, 1000 μg L-1, 2000 μg L-1, 5 μg L-1, and 50 μg L-1, respectively. The relative standard deviations (n = 12) were typically < 5.3% for As, < 0.5% for Cu, < 2.1% for Mn, < 11.7% for Sb, and < 9.2% for Se. The recoveries of As, Cu, Mn, Sb, and Se added to the mineral water samples varied from 102-111%, 91-107%, 92-109%, 89-97%, and 101-109%, respectively. Accuracy for the determination of As, Cu, Mn, Sb, and Se was checked using standard reference materials NIST SRM 1640 - Trace Elements in Natural Water, NIST SRM 1643d - Trace Elements in Water, and 10 mineral water samples. A paired t-test showed that the results were in agreement with the certified values of the standard reference materials at the 95% confidence level.