Chemical vapor deposition of multi-walled carbon nanotubes from nickel/yttria-stabilized zirconia catalysts

Multi-walled carbon nanotubes (MWNT) were produced by chemical vapor deposition using yttria-stabilized zirconia/nickel (YSZ/Ni) catalysts. The catalysts were obtained by a liquid mixture technique that resulted in fine dispersed nanoparticles of NiO supported in the YSZ matrix. High quality MWNT having smooth walls, few defects, and low amounts of by-products such as amorphous carbon were obtained, even from catalysts with large Ni concentrations (> 50 wt.%). By adjusting the experimental parameters, such as flux of the carbon precursor (ethylene) and Ni concentration, both the MWNT morphology and the process yield could be controlled. The resulting YSZ/Ni/MWNT composites can be interesting due to their mixed ionic-electronic transport properties, which could be useful in electrochemical applications.

Reversible intermittent flow-injection determination of mercury in sediments and vinasses by cold vapor atomic absorption spectrometry

A reversible intermittent pow-injection procedure is proposed for the automated determination of mercury in sediments and vinasses by cold vapor atomic absorption spectrometry, CVAAS. Solutions of sample and stannous chloride are carried by two air streams and sequentially injected into the generator/separator chamber in a segmented asynchronous merging zone configuration. The intermittent flow in the forward direction carries the mercury vapor through the flow cell, and in the backward direction, if aspirates the the remaining solution from the vessel to waste. We investigated composition and concentration of reagents, pow rates, commutation times, reactor configuration, and conditions for mercury release. The accuracy was checked by mercury determination in a certified sediment and spiked vinasses and river waters. The system handles about 100 samples per hour (0.50-5.00 mu g L-1), consuming ca. 2.5 mL of sample and 50 mg of SnCl2 per determination; Good recoveries (92-103%) were obtained with spiked samples. Results are precise (RSD <3% for 2.5 mu g Hg L-1, n = 12) and in agreement with values for certified reference material at 95% confidence level. (C) 1999 John Wiley & Sons, Inc.

A fast microwave-assisted, acid-vapor, steam-cleaning procedure for autosampler cups

A new and fast procedure is proposed for cleaning autosampler cups using acid-vapor steam-cleaning with a miniaturized assembly in a microwave-heated sealed Teflon vessel. A glass cactus-shaped holder was made to support six polyethylene autosampler cups (volume, 2.0 mt) inside a 100 mt microwave vessel. Regent-grade nitric acid was added to the vessels, and the system was heated in a microwave oven for 5 min at 300 W. Chromium was determined by graphite-furnace atomic-absorption spectrophotometry. The blank values were lower with cleaned cups compared to untreated cups (i.e., as received from supplier). The quantification limits, estimated from detection limits established with Milli-Q water, were 0.66 and 0.95 mu g Cr L-1 for cleaned and untreated auto-sampler cups, respectively. (C) 1998 Elsevier B.V. B.V. All rights reserved.

Effect of maltodextrin and arabic gum in water vapor sorption thermodynamic properties of vacuum dried pineapple pulp powder

Moisture equilibrium data of pineapple pulp (PP) powders with and without additives - 18% maltodextrin (MD) or 18% gum Arabic (GA) - were determined at 20, 30, 40 and 50 degrees C by using the static gravimetric method in a water activity range of 0.06-0.90. The obtained isotherms were sigmoid, typical type 111, and the Guggenhein-Anderson-de Boer (GAB) model was fitted to the experimental data of equilibrium moisture content versus water activity. Addition of additives was shown to affect the isotherms in such a way that, at the same water activity, samples PP + GA and PP + MD presented lower equilibrium moisture content and were not so affected by varying temperature. The net isosteric heats of sorption of pulp powders with additives were higher (less negative) than those of pineapple pulp powders, suggesting that there are more active polar sites in the product without addition of GA or MD. An empirical exponential relationship could describe the heat of sorption dependence on the material moisture content. (C) 2007 Elsevier Ltd. All rights reserved.

Plasma enhanced chemical vapor deposition of titanium(IV) ethoxide-oxygen-helium mixtures

Thin films were deposited by plasma enhanced chemical vapor deposition from titanium (IV) ethoxide (TEOT)-oxygen-helium mixtures. Actinometric optical emission spectroscopy was used to obtain the relative plasma concentrations of the species H, CH, O and CO as a function of the percentage of oxygen in the feed, R(ox). The concentrations of these species rise with increasing R(ox) and tend to fall for R(ox) greater than about 45%. As revealed by a strong decline in the emission intensity of the actinometer Ar as R(ox) was increased, the electron mean energy or density (or both) decreased as greater proportions of oxygen were fed to the chamber. This must tend to reduce gas-phase fragmentation of the monomer by plasma electrons. As the TEOT flow rate was fixed, however, and since the species H and CH do not contain oxygen, the rise in their plasma concentrations with increasing R(ox) is explained only by intermediate reactions involving oxygen or oxygen-containing species. Transmission infrared (IRS) and X-ray photoelectron (XPS) spectroscopies were employed to investigate film structure and composition. The presence of CH(2), CH(3), C=C, C-O and C=O groups was revealed by IRS. In addition, the presence of C-O and C=O groups was confirmed by XPS, which also revealed titanium in the +4 valence state. The Ti content of the films, however, was found to be much less than that of the monomer material itself. (C) 2007 Elsevier B.V. All rights reserved.

Spectroscopy and electrochemical characterization of Langmuir-Blodgett and physical vapor thin films of 29-membered diazocrown ether 1 with two n-octyl substituents

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

Diverse Amorphous Carbonaceous Thin Films Obtained by Plasma Enhanced Chemical Vapor Deposition and Plasma Immersion Ion Implantation and Deposition

Diverse amorphous hydrogenated carbon and similar films containing additional elements were produced by Plasma Enhanced Chemical Vapor Deposition (PECVD) and by Plasma Immersion Ion Implantation and Deposition (PIIID). Thus a-C:H, a-C:H:F, a-C:H:N, a-C:H:Cl and a-C:H:O:Si were obtained, starting from the same feed gases, using both techniques. The same deposition system supplied with radiofrequency (RF) power was used to produce all the films. A cylindrical stainless steel chamber equipped with circular electrodes mounted horizontally was employed. RF power was fed to the upper electrode; substrates were placed on the lower electrode. For PIIID negative high tension pulses were also applied to the lower electrode. Raman spectroscopy confirmed that all the films are amorphous. Chemical characterization of each pair of films was undertaken using Infrared Reflection Absorption Spectroscopy and X-ray Photoelectron Spectroscopy. The former revealed the presence of specific structures, such as C-H, C-O, O-H. The latter allowed calculation of the ratio of hetero-atoms to carbon atoms in the films, e. g. F:C, N:C, and Si:C. Only relatively small differences in elemental composition were detected between films produced by the two methods. The deposition rate in PIIID is generally reduced in relation to that of PECVD; for a-C:H:Cl films the reduction factor is almost four.

Development of chemical vapor deposition diamond burrs using hot filament

The fabrication of boring tools (burrs) for dentistry with the use of a hot-filament chemical vapor deposition (CVD) system, to form the diamond abrading structure, is reported here. The diamond was synthesized from a methane/freon gas mixture diluted in hydrogen. Comparative drilling tests with conventional diamond burrs and the CVD diamond burrs in borosilicate glasses demonstrated a lifetime more than 20 times larger for the CVD diamond burrs. Also, heat flow experiments in dentine showed that the CVD diamond burrs induce temperature gradients of the same order as the conventional ones. These characteristics of the CVD diamond burrs are highly desirable for odontological applications where the burrs' lifetime and the low temperature processing are essential to the quality and comfort of the treatment. © 1996 American Institute of Physics.

Determination of mercury in agroindustrial samples by flow-injection cold vapor atomic absorption spectrometry using ion exchange and reductive elution

A flow-injection system with a Chelite-S® cationic resin packed minicolumn is proposed for the determination of trace levels of mercury in agroindustrial samples by cold vapor atomic absorption spectrometry. Improved sensitivity and selectivity are attained since mercuric ions are on-line concentrated whereas other potential interferents are discarded. With on-line reductive elution procedure, concentrated hydrochloric acid could be replaced by 10% w/v SnCl2, in 6 M HCl as eluent. The reversed-intermittent stream either carries the atomic mercury, to the flow cell in the forward direction or removes the residue from reactor/gas liquid separator to a discarding flask in the opposite direction. Concentration and volume of reagent, acidity, flow rates, commutation times and potential interfering species were investigated. For 120 s preconcentration time, the proposed system handles about 25 samples h-1 (50.0 500 ng l-1), consuming about 10 ml sample and 5 mg SnCl2 per determination. The detection limit is 0.8 ng l-1 and the relative standard deviation (RSD) (n = 12) of a 76.7 ng l-1 sample is about 5%. Results are in agreement with certified value of standard materials at 95% confidence level and good recoveries (97-128%) of spiked samples were found. (C) 2000 Elsevier Science B.V.

Morphology changes induced by laser irradiation on disperse red 13 films prepared by physical vapor deposition

Surface morphology changes induced by argon laser irradiation (514 nm) on disperse red 13 (DR13) films prepared by physical vapor deposition (PVD) were investigated. Atomic force microscopy was used to characterize the irradiated sample for different periods of irradiation. Needle-shape structures are observed which are attributed to the symmetry of DR13 molecules. The film becomes increasingly closely packed with the irradiation, with lower root mean square roughness for long exposure times. This is due to photoisomerization of DR13 molecules and probably heating of the sample, which can provide the required mobility for the molecular rearrangement. The rearrangement is such that voids in the film are filled in upon irradiating the sample, thus decreasing the film roughness and increasing the packing.

Injeção subaracnóidea inadvertida de corticoíde em tratamento de dor crônica da coluna lombar. Relato de caso

BACKGROUND AND OBJECTIVES: Before epídural steroids were used in chronic lumbar pain, subarachnoid injection of these agents was the treatment of choice. Although still preconized by some authors, this technique may lead to severe complications with neurological sequelae. This report aimed at describing a case of accidental subarachnoid injection of steroid associated to local anesthetics during epidural puncture to treat lumbar pain. CASE REPORT: Male patient, 46 years old, followed byneuro-surgery for presenting right sciatic pain for 9 month, refractory to clinical treatment due to L 4-L 5 disk protrusion confirmed by CT scan, without neurological deficit. Epidural puncture for pain treatment was performed in L 4-L 5 with 17G needle and 10 mL solution were injected containing 4 mL of 0.25% bupivacaine, 80 mg methylprednisolone and 4 mL of 0.9% saline. Although there has not been CSF reflux, 5 minutes after injection there were sensory block in T 4 and motor block in T 6, associated to blood pressure and heart rate decrease. CONCLUSIONS: Accidental subarachnoid injections with the association of steroids for pain relief may cause adverse effects. There are several risks, varying from mild transient symptoms to nervous injuries, including spinal cord injuries. Our patient had no sequelae from the accidental subarachnoid injection, probably because it has been a single injection.

GPS performance in the quantification of integrated water vapor in Amazonian regions

The Amazonian regions are characterized by large space-time variability in the humidity fields due to the intense convective process in those areas associated with the great humidity potential generated by high temperatures. An experiment denominated RACCI/DRY-TO-WET (RAdiation, Cloud, and Climate Interactions in the Amazonia during the DRY-TO-WET Transition Season) was carried out in the Brazilian Amazonian Region in 2002. The IWV values from GPS and other techniques, such as radiosondes, radiometer and humidity sounding satellites were used in this experiment to supply subsidies to evaluate the aerosols influence in the associated processes modifications to seasonality of atmospheric water vapor. Those regions are one of the most humid of the planet, where IWV (Integrated Water Vapor) average values are in the order of 50 kg/m2. As according the literature the IWV quantification using GPS has not been explored in those circumstances, the objective this paper is to present the preliminary results obtained in the evaluation of the GPS performance in Amazonian Regions when comparing with other techniques. The tendency measurement values indicated that the IWV values from GPS tend to be larger than those from radiosondes and smaller than those from radiometer. On the other hand, IWV values from GPS are very close of the average values supplied by radiosondes and radiometer. Due to the great amount of atmospheric water vapor existent in this region, the results obtained in the experiment in percentile terms are quite better than those found in the literature, which are around of 10%.

Effects of copper vapor laser radiation on the root canal wall of human teeth: A scanning electron microscope study

Objective: The aim of this study is to analyze the effects of copper vapor laser radiation on the radicular wall of human teeth. Materials and Methods: Immediately after the crowns of 10 human uniradicular teeth were cut along the cement-enamel junction, a chemical-surgical preparation of the radicular canals was completed. Then the roots were longitudinally sectioned to allow for irradiation of the surfaces of the dentin walls of the root canals. The hemi-roots were separated into two groups: one (control) with five hemi-roots that were not irradiated, and another (experimental) with 15 hemi-roots divided into three subgroups that were submitted to the following exposure times: 0.02,0.05, and 0.1 s. A copper vapor laser (510.6 nm) with a total average power of 6.5 W in green emission, frequency of 16.000 Hz, and pulse duration of 30 ns was used. Results: The results obtained by scanning electron microscope analysis showed the appearance of a cavity in the region of laser beam impact, with melting, recrystallization, and cracking on the edges of the dentin of the cavity due to heat diffusion. Conclusions: We determined that the copper vapor laser produces significant morphologic changes in the radicular wall of human teeth when using the parameters in this study. However, further research should be done to establish parameters that are compatible with dental structure in order to eliminate thermal damages. © Mary Ann Liebert, Inc.