976 resultados para ASSISTED HYDROTHERMAL METHOD
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A microwave-assisted extraction (MAE) procedure to isolate phenolic compounds from almond skin byproducts was optimized. A three-level, three-factor Box–Behnken design was used to evaluate the effect of almond skin weight, microwave power, and irradiation time on total phenolic content (TPC) and antioxidant activity (DPPH). Almond skin weight was the most important parameter in the studied responses. The best extraction was achieved using 4 g, 60 s, 100 W, and 60 mL of 70% (v/v) ethanol. TPC, antioxidant activity (DPPH, FRAP), and chemical composition (HPLC-DAD-ESI-MS/MS) were determined by using the optimized method from seven different almond cultivars. Successful discrimination was obtained for all cultivars by using multivariate linear discriminant analysis (LDA), suggesting the influence of cultivar type on polyphenol content and antioxidant activity. The results show the potential of almond skin as a natural source of phenolics and the effectiveness of MAE for the reutilization of these byproducts.
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The inner surface of fused-silica capillaries has been coated with a dense/homogeneous coating of commercial multi-wall carbon nanotubes (MWCNTs) using a stable ink as deposit precursor. Solubilization of the MWCNTs was achieved in water/ethanol/dimethylformamide by the action of a surfactant, which can switch between a neutral or an ionic form depending on the pH of the medium, which thus becomes the driving force for the entire deposition process. Careful control of the experimental conditions has allowed us to selectively deposit CNTs on the inner surface of insulating silica capillaries by a simple, reproducible, and easily adaptable method.
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A novel approach is presented to determine mercury in urine samples, employing vortex-assisted ionic liquid dispersive liquid–liquid microextraction and microvolume back-extraction to prepare samples, and screen-printed electrodes modified with gold nanoparticles for voltammetric analysis. Mercury was extracted directly from non-digested urine samples in a water-immiscible ionic liquid, being back-extracted into an acidic aqueous solution. Subsequently, it was determined using gold nanoparticle-modified screen-printed electrodes. Under optimized microextraction conditions, standard addition calibration was applied to urine samples containing 5, 10 and 15 μg L−1 of mercury. Standard addition calibration curves using standards between 0 and 20 μg L−1 gave a high level of linearity with correlation coefficients ranging from 0.990 to 0.999 (N = 5). The limit of detection was empirical and statistically evaluated, obtaining values that ranged from 0.5 to 1.5 μg L−1, and from 1.1 to 1.3 μg L−1, respectively, which are significantly lower than the threshold level established by the World Health Organization for normal mercury content in urine (i.e., 10–20 μg L−1). A certified reference material (REC-8848/Level II) was analyzed to assess method accuracy finding 87% and 3 μg L−1 as the recovery (trueness) and standard deviation values, respectively. Finally, the method was used to analyze spiked urine samples, obtaining good agreement between spiked and found concentrations (recovery ranged from 97 to 100%).
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The effect of volcanic activity on submarine hydrothermal systems has been well documented along fast- and intermediate-spreading centers but not from slow-spreading ridges. Indeed, volcanic eruptions are expected to be rare on slow-spreading axes. Here we report the presence of hydrothermal venting associated with extremely fresh lava flows at an elevated, apparently magmatically robust segment center on the slow-spreading southern Mid-Atlantic Ridge near 5°S. Three high-temperature vent fields have been recognized so far over a strike length of less than 2 km with two fields venting phase-separated, vapor-type fluids. Exit temperatures at one of the fields reach up to 407°C, at conditions of the critical point of seawater, the highest temperatures ever recorded from the seafloor. Fluid and vent field characteristics show a large variability between the vent fields, a variation that is not expected within such a limited area. We conclude from mineralogical investigations of hydrothermal precipitates that vent-fluid compositions have evolved recently from relatively oxidizing to more reducing conditions, a shift that could also be related to renewed magmatic activity in the area. Current high exit temperatures, reducing conditions, low silica contents, and high hydrogen contents in the fluids of two vent sites are consistent with a shallow magmatic source, probably related to a young volcanic eruption event nearby, in which basaltic magma is actively crystallizing. This is the first reported evidence for direct magmatic-hydrothermal interaction on a slow-spreading mid-ocean ridge.
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Originally presented as the author's thesis (M.A.), University of Illinois at Urbana-Champaign.
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Complete and precise characterization of a quantum dynamical process can be achieved via the method of quantum process tomography. Using a source of correlated photons, we have implemented several methods, each investigating a wide range of processes, e.g., unitary, decohering, and polarizing. One of these methods, ancilla-assisted process tomography (AAPT), makes use of an additional ancilla system, and we have theoretically determined the conditions when AAPT is possible. Surprisingly, entanglement is not required. We present data obtained using both separable and entangled input states. The use of entanglement yields superior results, however.
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The first success in the preparation of rare earth hydroxycarbonate thin films has been achieved. Cerium hydroxycarbonate films were prepared by a hydrothermal deposition method, the sample of a single orthorhombic phase was deposited at a lower temperature while those of orthorhombic and hexagonal phases were obtained at higher temperatures. The crystals in the films could be ellipsoidal, prismatic, or rhombic, depending on the deposition conditions applied. The thin films could be candidates for developing novel optical materials and for advanced ceramics processing. (C) 2003 Elsevier Science B.V. All rights reserved.
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A rapid method has been developed for the quantification of the prototypic cyclotide kalata B I in water and plasma utilizing matrix-assisted laser desorption ionisation time-of-flight (MALDI-TOF) mass spectrometry. The unusual structure of the cyclotides means that they do not ionise as readily as linear peptides and as a result of their low ionisation efficiency, traditional LC/MS analyses were not able to reach the levels of detection required for the quantification of cyclotides in plasma for pharmacokinetic studies. MALDI-TOF-MS analysis showed linearity (R-2 > 0.99) in the concentration range 0.05-10 mu g/mL with a limit of detection of 0.05 mu g/mL (9 fmol) in plasma. This paper highlights the applicability of MALDI-TOF mass spectrometry for the rapid and sensitive quantification of peptides in biological samples without the need for extensive extraction procedures. (c) 2005 Elsevier B.V. All rights reserved.
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A dry matrix application for matrix-assisted laser desorption/ionization mass spectrometry imaging (MALDI MSI) was used to profile the distribution of 4-bromophenyl-1,4-diazabicyclo(3.2.2)nonane-4-carboxylate, monohydrochloride (BDNC, SSR180711) in rat brain tissue sections. Matrix application involved applying layers of finely ground dry alpha-cyano-4-hydroxycinnamic acid (CHCA) to the surface of tissue sections thaw mounted onto MALDI targets. It was not possible to detect the drug when applying matrix in a standard aqueous-organic solvent solution. The drug was detected at higher concentrations in specific regions of the brain, particularly the white matter of the cerebellum. Pseudomultiple reaction monitoring imaging was used to validate that the observed distribution was the target compound. The semiquantitative data obtained from signal intensities in the imaging was confirmed by laser microdissection of specific regions of the brain directed by the imaging, followed by hydrophilic interaction chromatography in combination with a quantitative high-resolution mass spectrometry method. This study illustrates that a dry matrix coating is a valuable and complementary matrix application method for analysis of small polar drugs and metabolites that can be used for semiquantitative analysis.
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We propose and experimentally demonstrate a new method to extend the range of Brillouin optical time domain analysis (BOTDA) systems. It exploits the virtual transparency created by second-order Raman pumping in optical fibers. The idea is theoretically analyzed and experimentally demonstrated in a 50 km fiber. By working close to transparency, we also show that the measurement length of the BOTDA can be increased up to 100 km with 2 meter resolution. We envisage extensions of this technique to measurement lengths well beyond this value, as long as the issue of relative intensity noise (RIN) of the primary Raman pump can be avoided. © 2010 Optical Society of America.
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This study examined the effects of computer assisted instruction (CAI) 1 hour per week for 18 weeks on changes in computational scores and attitudes of developmental mathematics students at schools with predominantly Black enrollment. Comparisons were made between students using CAI with differing software--PLATO, CSR or both together--and students using traditional instruction (TI) only.^ This study was conducted in the Dade County Public School System from February through June 1991, at two senior high schools. The dependent variables, the State Student Assessment Test (SSAT), and the School Subjects Attitude Scales (SSAS), measured students' computational scores and attitudes toward mathematics in 3 categories: interest, usefulness, and difficulty, respectively.^ Univariate analyses of variance were performed on the least squares mean differences from pretest to posttest for testing main effects and interactions. A t-test measured significant main effects and interactions. Results were interpreted at the.01 level of significance.^ Null hypotheses 1, 2, and 3 compared versions of CAI with the control group, for changes in mathematical computation scores measured with the SSAT. It could not be concluded that changes in standardized mathematics test scores of students using CAI with differing software 1 hour per week for 18 class hours combined with TI were significantly higher than changes in test scores for students receiving TI only.^ Null hypotheses 4, 5, and 6 tested the effects of CAI for attitudes toward mathematics for experimental groups against control groups measured with the SSAS. Changes in attitudes toward mathematics of students using CAI with differing software 1 hour per week for 18 class hours combined with TI were not significantly higher than attitude changes for students receiving TI only.^ Teacher effect on students' computational scores was a more influential variable than CAI. No interaction was found between gender and learning method on standardized mathematics test scores (null hypothesis 7). ^
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Simulations suggest that photomixing in resonant laser-assisted field emission could be used to generate and detect signals from DC to 100 THz. It is the objective of this research to develop a system to efficiently couple the microwave signals generated on an emitting tip by optical mixing. Four different methods for coupling are studied. Tapered Goubau line is found to be the most suitable. Goubau line theory is reviewed, and programs are written to determine loss on the line. From this, Goubau tapers are designed that have a 1:100 bandwidth. These tapers are finally simulated using finite difference time domain, to find the optimum design parameters. Tapered Goubau line is an effective method for coupling power from the field emitting tip. It has large bandwidth, and acceptable loss. Another important consideration is that it is the easiest to manufacture of the four possibilities studied, an important quality for any prototype.
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The objective was to develop and validate a method for estimating food intake of nursing home residents. The study was conducted with certified nursing assistants (CNAs) at a 180-bed nursing facility. CNAs assisted in the development of the new method by providing feedback on existing estimation methods. Four simulated resident trays were used to estimate both food intake and overall meal intake. Twelve CNAs' intake estimates for 34 simulated food items (n=384 estimates) were compared to weighed values. Eightyfive percent of the 384 intake estimates for the simulated food items were correct; Cohen's kappa was 0.80, p
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Electron beam-induced deposition (EBID) is a direct write process where an electron beam locally decomposes a precursor gas leaving behind non-volatile deposits. It is a fast and relatively in-expensive method designed to develop conductive (metal) or isolating (oxide) nanostructures. Unfortunately the EBID process results in deposition of metal nanostructures with relatively high resistivity because the gas precursors employed are hydrocarbon based. We have developed deposition protocols using novel gas-injector system (GIS) with a carbon free Pt precursor. Interconnect type structures were deposited on preformed metal architectures. The obtained structures were analysed by cross-sectional TEM and their electrical properties were analysed ex-situ using four point probe electrical tests. The results suggest that both the structural and electrical characteristics differ significantly from those of Pt interconnects deposited by conventional hydrocarbon based precursors, and show great promise for the development of low resistivity electrical contacts.
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Introduction: Computer-Aided-Design (CAD) and Computer-Aided-Manufacture (CAM) has been developed to fabricate fixed dental restorations accurately, faster and improve cost effectiveness of manufacture when compared to the conventional method. Two main methods exist in dental CAD/CAM technology: the subtractive and additive methods. While fitting accuracy of both methods has been explored, no study yet has compared the fabricated restoration (CAM output) to its CAD in terms of accuracy. The aim of this present study was to compare the output of various dental CAM routes to a sole initial CAD and establish the accuracy of fabrication. The internal fit of the various CAM routes were also investigated. The null hypotheses tested were: 1) no significant differences observed between the CAM output to the CAD and 2) no significant differences observed between the various CAM routes. Methods: An aluminium master model of a standard premolar preparation was scanned with a contact dental scanner (Incise, Renishaw, UK). A single CAD was created on the scanned master model (InciseCAD software, V2.5.0.140, UK). Twenty copings were then fabricated by sending the single CAD to a multitude of CAM routes. The copings were grouped (n=5) as: Laser sintered CoCrMo (LS), 5-axis milled CoCrMo (MCoCrMo), 3-axis milled zirconia (ZAx3) and 4-axis milled zirconia (ZAx4). All copings were micro-CT scanned (Phoenix X-Ray, Nanotom-S, Germany, power: 155kV, current: 60µA, 3600 projections) to produce 3-Dimensional (3D) models. A novel methodology was created to superimpose the micro-CT scans with the CAD (GOM Inspect software, V7.5SR2, Germany) to indicate inaccuracies in manufacturing. The accuracy in terms of coping volume was explored. The distances from the surfaces of the micro-CT 3D models to the surfaces of the CAD model (CAD Deviation) were investigated after creating surface colour deviation maps. Localised digital sections of the deviations (Occlusal, Axial and Cervical) and selected focussed areas were then quantitatively measured using software (GOM Inspect software, Germany). A novel methodology was also explored to digitally align (Rhino software, V5, USA) the micro-CT scans with the master model to investigate internal fit. Fifty digital cross sections of the aligned scans were created. Point-to-point distances were measured at 5 levels at each cross section. The five levels were: Vertical Marginal Fit (VF), Absolute Marginal Fit (AM), Axio-margin Fit (AMF), Axial Fit (AF) and Occlusal Fit (OF). Results: The results of the volume measurement were summarised as: VM-CoCrMo (62.8mm3 ) > VZax3 (59.4mm3 ) > VCAD (57mm3 ) > VZax4 (56.1mm3 ) > VLS (52.5mm3 ) and were all significantly different (p presented as areas with different colour. No significant differences were observed at the internal aspect of the cervical aspect between all groups of copings. Significant differences (p< M-CoCrMo Internal Occlusal, Internal Axial and External Axial 2 ZAx3 > ZAx4 External Occlusal, External Cervical 3 ZAx3 < ZAx4 Internal Occlusal 4 M-CoCrMo > ZAx4 Internal Occlusal and Internal Axial The mean values of AMF and AF were significantly (p M-CoCrMo and CAD > ZAx4. Only VF of M-CoCrMo was comparable with the CAD Internal Fit. All VF and AM values were within the clinically acceptable fit (120µm). Conclusion: The investigated CAM methods reproduced the CAD accurately at the internal cervical aspect of the copings. However, localised deviations at axial and occlusal aspects of the copings may suggest the need for modifications in these areas prior to fitting and veneering with porcelain. The CAM groups evaluated also showed different levels of Internal Fit thus rejecting the null hypotheses. The novel non-destructive methodologies for CAD/CAM accuracy and internal fit testing presented in this thesis may be a useful evaluation tool for similar applications.