Determination of lead in medicinal plants by high-resolution continuum source graphite furnace atomic absorption spectrometry using direct solid sampling

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

Comparative extraction of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/F-s) from a variety of solid samples

Extraction experiments with spiking of C-13(12)-PCDD/Fs were performed with a variety of PCDD/Fs contaminated samples. The extraction recovery of PCDD/Fs was mainly influenced by PCDD/Fs concentration and the sample matrix. Generally, the first soxhlet extraction with toluene has suitable recovery. From the selected samples, only FAMS4 and 5 which are fly ashes with high concentration, the recovery of the first soxhlet extraction with 24 hr. is low, but PCDD/Fs were almost completely removed after 72 hr. Copyright (C) 1996 Elsevier Science Ltd

Feasibility of using in situ fusion for the determination of Co, Cr and Mn in Portland cement by direct solid sampling graphite furnace atomic absorption spectrometry

In situ fusion on the boat-type graphite platform has been used as a sample pretreatment for the direct determination of Co, Cr and Mn in Portland cement by solid sampling graphite furnace atomic absorption spectrometry (SS-GF AAS). The 3-field Zeeman technique was adopted for background correction to decrease the sensitivity during measurements. This strategy allowed working with up to 200 mu g of sample. The in situ fusion was accomplished using 10 mu L of a flux mixture 4.0% m/v Na(2)CO(3) + 4.0% m/v ZnO + 0.1% m/v Triton (R) X-100 added over the cement sample and heated at 800 degrees C for 20 s. The resulting mould was completely dissolved with 10 mu L of 0.1% m/v HNO(3). Limits of detection were 0.11 mu g g(-1) for Co, 1.1 mu g g(-1) for Cr and 1.9 mu g g(-1) for Mn. The accuracy of the proposed method has been evaluated by the analysis of certified reference materials. The values found presented no statistically significant differences compared to the certified values (Student`s t-test, p<0.05). In general, the relative standard deviation was lower than 12% (n = 5). (C) 2009 Elsevier B.V. All rights reserved.

Quantificação de metais potencialmente tóxicos em mexilhão dourado (Limnoperna fortunei) por espectrometria de absorção atômica com fonte contínua e alta resolução empregando amostragem direta de sólidos

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Quantificação de metais potencialmente tóxicos em mexilhão dourado (Limnoperna fortunei) por espectrometria de absorção atômica com fonte contínua e alta resolução empregando amostragem direta de sólidos

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Evaluation of solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for direct determination of chromium in medicinal plants

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

Analytical procedures for cadmium determination in facial make-up samples by graphite furnace AAS

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

COMPARATIVE EVALUATION OF THERMAL CONDUCTIVITY OF ZIRCONIA SOLID AND HONEYCOMB STRUCTURES

Porous zirconia ceramic monoliths have been extensively used in thermo-structural applications due to their inherent low thermal conductivity in combination with their adaptability to form complicated shapes through advanced ceramic processing techniques. However, extruded cellular honeycomb structures made from these materials have been less explored for thermal management applications. There exist large potential applications due to their unique configurations, resulting in better heat-management mechanisms. Some of the studies carried out on zirconia honeycombs are safeguarded through patents due to its technical importance, or the information is not in the public domain. In the present study, for the sake of comparison, honeycomb specimens with varying wall thicknesses and unit cell lengths maintaining almost same bulk density of around 90% theoretical and relative density of 0.34-0.37 were prepared and subjected to thermal conductivity evaluation along with the solid samples with relative density of 1.0 using monotonic heating regime methodology. In addition, the effect of channel shape was also evaluated using square and triangular channeled honeycombs with the same relative densities. The results obtained from these specimens were correlated with their configurations to bring out the advantages accrued by using the honeycomb with these configurations. It was observed that a significant decrease in thermal conductivity was achieved in honeycombs, which can be attributed to the behavior of various heat transfer mechanisms that are operative at high temperatures in combination with the considerable reduction in thermal mass and the consequent conduction through the solids.

Applications of a nuclear technique for depth-sensitive hydrogen analysis : trapped H in lunar samples and the hydration of terrestrial obsidian

The resonant nuclear reaction ¹⁹F(p,αy)¹⁶O has been used to perform depth-sensitive analyses for both fluorine and hydrogen in solid samples. The resonance at 0.83 MeV (center-of-mass) in this reaction has been applied to the measurement of the distribution of trapped solar protons in lunar samples to depths of ~1/2µm. These results are interpreted in terms of a redistribution of the implanted H which has been influenced by heavy radiation damage in the surface region. Fluorine determinations have been performed in a 1-µm surface layer on lunar and meteoritic samples using the same ¹⁹F(p,αy)¹⁶O resonance. The measurement of H depth distributions has also been used to study the hydration of terrestrial obsidian, a phenomenon of considerable archaeological interest as a means of dating obsidian artifacts. Additional applications of this type of technique are also discussed.

Dietary switching of collembola in grassland soil food webs

Soil food webs are characterised by complex direct and indirect effects among the organisms. Consumption of microorganisms by soil animals is considered as an important factor that contributes to the stability of communities, though cascading effects within the food web can be difficult to detect. In a greenhouse experiment, an addition of a high number the fungal feeding collembola Folsomia quadrioculata was applied to grassland soil food webs in monocultures of three plant species: Plantago lanceolato (forb), Lotus corniculatus (legume) and Holcus lanatus (grass). The abundance of microorganisms, determined as the abundances of phospholipid fatty acids (PLFAs) and the abundances of resident invertebrates, nematodes and collembolans, did not change due to the addition of E quadrioculata. Trophic positions of collembolans were determined by analyses of natural abundances of N-15 stable isotopes. The use of food resources by microorganisms and collembolans was determined by C-13 analysis of microbial PLFAs and solid samples of collembolans. delta C-13 values of the resident collembola Folsomia fimetaria were lower in the presence of E quadrioculata than in the control food webs indicating a use of more depleted C-13 food resources by E fimetaria. The delta N-15 values of E fimetaria did not change at the addition of E quadrioculata thus no change of trophic levels was detected. The switch of E fimetaria to a different food resource could be due to indirect interactions in the food web as the two collembolan species were positioned on different trophic positions, according to different delta N-15 values. (c) 2008 Elsevier Ltd. All rights reserved.

Polytypism and Silicon carbide : a solid state nuclear magnetic resonance study

A survey of predominantly industrial silicon carbide has been carried out using Magic Angle Spinning nuclear magnetic resonance (MAS nmr); a solid state technique. Three silicon carbide polytypes were studied; 3C, 6H, and 15R. The 13C and 29 Si MAS nmr spectra of the bulk SiC sample was identified on the basis of silicon (carbon) site type in the d iff ere n t pol Y t Y pes • Out to 5.00 A fro mac en t r a lsi 1 i con (0 r carbon) atom four types of sites were characterized using symmetry based calculations. This method of polytype analysis was also considered, in the prelminary stages, for applications with other polytypic material; CdBr 2 , CdI 2 , and PbI 2 " In an attempt to understand the minor components of silicon carbide, such as its surface, some samples were hydrofluoric acid washed and heated to extreme temperatures. Basically, an HF removable species which absorbs at -110 ppm (Si0 2 ) in the 29 Si MAS nmr spectrum is found in silicon carbide after heating. Other unidentified peaks observed at short recycle delays in some 29 Si MAS nmr spectra are considered to be impurities that may be within the lattice. These components comprise less than 5% of the observable silicon. A Tl study was carried out for 29 Si nuclei in a 3C ii polytype sample, using the Driven Equilibrium Single-Pulse Observation of T1 (DESPOT) technique. It appears as though there are a number of nuclei that have the same chemical shift but different T1 relaxation times. The T1 values range from 30 seconds to 11 minutes. Caution has to be kept when interpreting these results because this is the first time that DESPOT has been used for solid samples and it is not likely in full working order. MAS nmr indicates that the 13C and 29 Si ~sotropic chemical shifts of silicon carbide appear to have a reciprocal type of relationship_ Single crystal nmr analysis of a 6H sample is accordance with this finding when only the resultant isotropic shift is considered. However, single crystal nmr also shows that the actual response of the silicon and carbon nuclear environment to the applied magnetic field at various angles is not at all reciprocal. Such results show that much more single crystal nmr work is required to determine the actual behavior of the local magnetic environment of the SiC nuclei.

Studies on Electrical and Thermal Properties of Certain Selected Photonic Materials

The present thesis is centered around the study of electrical and thermal properties of certain selected photonic materials.We have studied the electrical conduction mechanism in various phases of certain selected photonic materials and those associated with different phase transitions occurring in them. A phase transition leaves its own impressions on the key parameters like electrical conductivity and dielectric constant. However, the activation energy calculation reveals the dominant factor responsible for conduction process.PA measurements of thermal diffusivity in certain other important photonic materials are included in the remaining part of the research work presented in this thesis. PA technique is a promising tool for studying thermal diffusivities of solid samples in any form. Because of its crucial role and common occurrence in heat flow problems, the thermal diffusivity determination is often necessary and knowledge of thermal diffusivity can intum be used to calculate the thermal conductivity. Especially,knowledge of the thermal diffusivity of semiconductors is important due to its relation to the power dissipation problem in microelectronic and optoelectronic devices which limits their performances. More than that, the thermal properties, especially those of thin films are of growing interest in microelectronics and microsystems because of the heat removal problem involved in highly integrated devices. The prescribed chapter of the present theis demonstrates how direct measurement of thermal diffusivity can be carried out in thin films of interest in a simple and elegant manner using PA techniques. Although results of only representative measurements viz; thermal diffusivity values in Indium, Aluminium, Silver and CdS thin films are given here, evaluation of this quantity for any photonic and / electronic material can be carried out using this technique in a very simple and straight forward manner.