Applications of the Rietveld method to quantify the crystalline phases of Portland cement clinker doped with nickel and chromium

The effects of chromium or nickel oxide additions on the composition of Portland clinker were investigated by X-ray powder diffraction associated with pattern analysis by the Rietveld method. The co-processing of industrial waste in Portland cement plants is an alternative solution to the problem of final disposal of hazardous waste. Industrial waste containing chromium or nickel is hazardous and is difficult to dispose of. It was observed that in concentrations up to 1% in mass, the chromium or nickel oxide additions do not cause significant alterations in Portland clinker composition. (C) 2008 International Centre for Diffraction Data.

Mineralogical characterization of a highly-weathered soil by the Rietveld Method

The mineralogical characterization through mineral quantification of Brazilian soils by X-ray diffraction data using the Rietveld Method is not common. A mineralogical quantification of an Acric Ferralsol from the Ponta Grossa region, state of Paraná, Brazil, was carried out using this Method with X-Ray Diffraction data to verify if this method was suitable for mineral quantification of a highly-weathered soil. The A, AB and B3 horizons were fractioned to separate the different particle sizes: clay, silt, fine sand (by Stokes Law) and coarse sand fractions (by sieving), with the procedure free of chemical treatments. X-ray Fluorescence, Inductively Coupled Plasma Atomic Emission Spectrometry, Infrared Spectroscopy and Mössbauer Spectroscopy were used in order to assist the mineral identification and quantification. The Rietveld Method enabled the quantification of the present minerals. In a general way, the quantitative mineralogical characterization by the Rietveld Method revealed that quartz, gibbsite, rutile, hematite, goethite, kaolinite and halloysite were present in the clay and silt fractions of all horizons. The silt fractions of the deeper horizons were different from the more superficial ones due to the presence of large amounts of quartz. The fine and the coarse sand fractions are constituted mainly by quartz. Therefore, a mineralogical quantification of the finer fraction (clay and silt) by the Rietveld Method was successful.

Quantitative analysis of aluminum dross by the Rietveld method

Aluminum white dross is a valuable material principally due to its high metallic aluminum content. The aim of this work is to develop a method for quantitative analysis of aluminum white dross with high accuracy. Initially, the material was separated into four granulometric fractions by means of screening. Two samples of each fraction were obtained, which were analyzed by means of X-ray fluorescence and energy dispersive spectroscopy in order to determine the elements present in the samples. The crystalline phases aluminum, corundum, spinel, defect spinel, diaoyudaoite, aluminum nitride, silicon and quartz low were identified by X-ray diffraction. The quantitative phase analysis was performed by fitting the X-ray diffraction profile with the Rietveld method using the GSAS software. The following quantitative results were found: 77.8% aluminum, 7.3% corundum, 2.6% spinel, 7.6% defect spinel, 1.8% diaoyudaoite, 2.9% aluminum nitride, and values not significant of quartz and silicon.

A Simple and Fast Method for the Production and Characterization of Methylic and Ethylic Biodiesels from Tucum Oil via an Alkaline Route

A simple, fast, and complete route for the production of methylic and ethylic biodiesel from tucum oil is described. Aliquots of the oil obtained directly from pressed tucum (pulp and almonds) were treated with potassium methoxide or ethoxide at 40 degrees C for 40 min. The biodiesel form was removed from the reactor and washed with 0.1 M HCl aqueous solution. A simple distillation at 100 degrees C was carried out in order to remove water and alcohol species from the biodiesel. The oxidative stability index was obtained for the tucum oil as well as the methylic and ethylic biodiesel at 6.13, 2.90, and 2.80 h, for storage times higher than 8 days. Quality control of the original oil and of the methylic and ethylic biodiesels, such as the amount of glycerin produced during the transesterification process, was accomplished by the TLC, GC-MS, and FT-IR techniques. The results obtained in this study indicate a potential biofuel production by simple treatment of tucum, an important Amazonian fruit.

Thermal lens and interferometric method for glass transition and thermo physical properties measurements in Nd(2)O(3) doped sodium zincborate glass

In this work the time resolved thermal lens method is combined with interferometric technique, the thermal relaxation calorimetry, photoluminescence and lifetime measurements to determine the thermo physical properties of Nd(2)O(3) doped sodium zincborate glass as a function of temperature up to the glass transition region. Thermal diffusivity, thermal conductivity, fluorescence quantum efficiency, linear thermal expansion coefficient and thermal coefficient of electronic polarizability were determined. In conclusion, the results showed the ability of thermal lens and interferometric methods to perform measurements very close to the phase transition region. These techniques provide absolute values for the measured physical quantities and are advantageous when low scan rates are required. (c) 2008 Optical Society of America

Evaluation of erythrocyte dysmorphism by light microscopy with lowering of the condenser lens: A simple and efficient method

Aim: To demonstrate that the evaluation of erythrocyte dysmorphism by light microscopy with lowering of the condenser lens (LMLC) is useful to identify patients with a haematuria of glomerular or non-glomerular origin. Methods: A comparative double-blind study between phase contrast microscopy (PCM) and LMLC is reported to evaluate the efficacy of these techniques. Urine samples of 39 patients followed up for 9 months were analyzed, and classified as glomerular and non-glomerular haematuria. The different microscopic techniques were compared using receiver-operator curve (ROC) analysis and area under curve (AUC). Reproducibility was assessed by coefficient of variation (CV). Results: Specific cut-offs were set for each method according to their best rate of specificity and sensitivity as follows: 30% for phase contrast microscopy and 40% for standard LMLC, reaching in the first method the rate of 95% and 100% of sensitivity and specificity, respectively, and in the second method the rate of 90% and 100% of sensitivity and specificity, respectively. In ROC analysis, AUC for PCM was 0.99 and AUC for LMLC was 0.96. The CV was very similar in glomerular haematuria group for PCM (35%) and LMLC (35.3%). Conclusion: LMLC proved to be effective in contributing to the direction of investigation of haematuria, toward the nephrological or urological side. This method can substitute PCM when this equipment is not available.

A device to improve the Schleger and Turner method for sweating rate measurements

The objective of this study was to test a device developed to improve the functionality, accuracy and precision of the original technique for sweating rate measurements proposed by Schleger and Turner [Schleger AV, Turner HG (1965) Aust J Agric Res 16:92-106]. A device was built for this purpose and tested against the original Schleger and Turner technique. Testing was performed by measuring sweating rates in an experiment involving six Mertolenga heifers subjected to four different thermal levels in a climatic chamber. The device exhibited no functional problems and the results obtained with its use were more consistent than with the Schleger and Turner technique. There was no difference in the reproducibility of the two techniques (same accuracy), but measurements performed with the new device had lower repeatability, corresponding to lower variability and, consequently, to higher precision. When utilizing this device, there is no need for physical contact between the operator and the animal to maintain the filter paper discs in position. This has important advantages: the animals stay quieter, and several animals can be evaluated simultaneously. This is a major advantage because it allows more measurements to be taken in a given period of time, increasing the precision of the observations and diminishing the error associated with temporal hiatus (e.g., the solar angle during field studies). The new device has higher functional versatility when taking measurements in large-scale studies (many animals) under field conditions. The results obtained in this study suggest that the technique using the device presented here could represent an advantageous alternative to the original technique described by Schleger and Turner.

Rankamaite from the Urubu pegmatite, Itinga, Minas Gerais, Brazil: Crystal chemistry and Rietveld refinement

A new occurrence of rankamaite is here described at the Urubu pegmatite, Itinga municipality, Minas Gerais, Brazil. The mineral forms cream-white botryoidal aggregates of acicular to fibrous crystals, intimately associated with simpsonite, thoreaulite, cassiterite, quartz, elbaite, albite, and muscovite. The average of six chemical analyses obtained by electron microprobe is (range in parentheses, wt%): Na(2)O 2.08 (1.95-2.13), K(2)O 2.61 (2.52-2.74), Al(2)O(3) 1.96 (1.89-2.00), Fe(2)O(3) 0.01 (0.00-0.03), TiO(2) 0.02 (0.00-0.06), Ta(2)O(5) 81.04 (79.12-85.18), Nb(2)O(5) 9.49 (8.58-9.86), total 97.21 (95.95-101.50). The chemical formula derived from this analysis is (Na(1.55)K(1.28))(Sigma 2.83)(Ta(8.45)Nb(1.64)Al(0.89)Fe(0.01)(3+)Ti(0.01))(Sigma 11.00)[O(25.02)(OH)(5.98)](Sigma 31.00). Rankamaite is an orthorhombic ""tungsten bronze"" (OTB), crystallizing in the space group Cmmm. Its unit-cell parameters refined from X-ray diffraction powder data are: a = 17.224(3), b = 17.687(3), c = 3.9361(7) angstrom, V = 1199.1(3) angstrom(3), Z = 2. Rietveld refinement of the powder data was undertaken using the structure of LaTa(5)O(14) as a starting model for the rankamaite structure. The structural formula obtained with the Rietveld analyses is: (Na(2.21)K(1.26))Sigma(3.37)(Ta(9.12)NB(1.30) Al(0.59))(Sigma 11.00)[O(26.29)(OH)(4.71)](Sigma 31.00). The tantalum atoms are coordinated by six and seven oxygen atoms in the form of distorted TaO(6) octahedra and TaO(2) pentagonal bipyramids, respectively. Every pentagonal bipyramid shares edges with four octahedra, thus forming Ta(5)O(14) units. The potassium atom is in an 11-fold coordination, whereas one sodium atom is in a 10-fold and the other is in a 12-fold coordination. Raman and infrared spectroscopy were used to investigate the room-temperature spectra of rankamaite.

Spectrophotometric determination of zinc in pharmaceutical and biological samples with di-2-pyridyl ketone benzoylhydrazone: A simple, fast, accurate and sensitive method

A simple, fast, accurate, and sensitive spectrophotometric method was developed to determine zinc(II). This method is based on the reaction of Zn(II) with di-2-pyridyl ketone benzoylhydrazone (DPKBH), at pH=5.5 and 50% (v/v) ethanol. Beers law was obeyed in the range 0.020-1.82 mu g mL(-1) with a molar apsorptivity of 3.64 x 10(4) L mol(-1) cm(-1), and a detection limit (3) of 2.29 mu g L-1. The action of some interfering ions was verified and the developed method applied to pharmaceutical and biological samples. The results were then compared with those obtained by using a flame atomic absorption technique.

Bending of stochastic Kirchhoff plates on Winkler foundations via the Galerkin method and the Askey-Wiener scheme

In this paper, the method of Galerkin and the Askey-Wiener scheme are used to obtain approximate solutions to the stochastic displacement response of Kirchhoff plates with uncertain parameters. Theoretical and numerical results are presented. The Lax-Milgram lemma is used to express the conditions for existence and uniqueness of the solution. Uncertainties in plate and foundation stiffness are modeled by respecting these conditions, hence using Legendre polynomials indexed in uniform random variables. The space of approximate solutions is built using results of density between the space of continuous functions and Sobolev spaces. Approximate Galerkin solutions are compared with results of Monte Carlo simulation, in terms of first and second order moments and in terms of histograms of the displacement response. Numerical results for two example problems show very fast convergence to the exact solution, at excellent accuracies. The Askey-Wiener Galerkin scheme developed herein is able to reproduce the histogram of the displacement response. The scheme is shown to be a theoretically sound and efficient method for the solution of stochastic problems in engineering. (C) 2009 Elsevier Ltd. All rights reserved.

Use of the DNA Checkerboard hybridization method for detection and quantitation of Candida species in oral microbiota

The DNA Checkerboard method enables the simultaneous identification of distinct microorganisms in a large number of samples and employs up to 45 whole genomic DNA probes to gram-negative and gram-positive bacterial species present in subgingival biofilms. Collectively, they account for 55%-60% of the bacteria in subgingival biofilms. In this study, we present the DNA Checkerboard hybridization as an alternative method for the detection and quantitation of Candida species in oral cavities. Our results reveal that DNA Checkerboard is sensitive enough and constitutes a powerful and appropriate method for detecting and quantifying Candida species found in the oral cavity.

Influence of heavy rare earth ions substitution on microstructure and magnetism of nanocrystalline magnetite

In this work we report results on the influence of heavy rare earth ions substitution on microstructure and magnetism of nanocrystalline magnetite. A series of Fe(2.85)RE(0.15)O(4) (RE = Gd, Dy, Ho, Tm and Yb) samples have been prepared by high energy ball milling. Structure/microstructure investigations of two selected samples Fe(2.85)Gd(0.15)O(4) and Fe(2.85)Tm(0.15)O(4), represent an extension of the previously published results on Fe(3)O(4)/gamma-Fe(2)O(3), Fe(2.85)Y(0.15)O(4) and Fe(2.55)In(0.45)O(4) [Z. Cvejic, S. Rakic, A. Kremenovic, B. Antic, C. Jovalekic. Ph. Colomban, Sol. State Sciences 8 (2006) 908], while magnetic characterization has been done for all the samples. Crystallite/particle size and strain determined by X-ray diffractometry and Transmission electron microscopy (TEM) confirmed the nanostructured nature of the mechanosynthesized materials. X-ray powder diffraction was used to analyze anisotropic line broadening effects through the Rietveld method. The size anisotropy was found to be small while strain anisotropy was large, indicating nonuniform distribution of deffects in the presence of Gd and Tm in the crystal structure. Superparamagnetic(SPM) behavior at room temperature was observed for all samples studied. The Y-substituted Fe(3)O(4) had the largest He and the lowest M(S). We discuss the changes in magnetic properties in relation to their magnetic anisotropy and microstructure. High field irreversibility (H>20kOe) in ZFC/FC magnetization versus temperature indicates the existence of high magnetocrystalline and/or strain induced anisotropy. (C) 2008 Elsevier B.V. All rights reserved.

Development and Validation of a Mice liar Electrokinetic Chromatography Method for Quantitative Determination of Butenolides in Piper malacophyllum (C. Presl) C. DC.

Introduction - A large number of natural and synthetic compounds having butenolides as a core unit have been described and many of them display a wide range of biological activities. Butenolides from P. malacophyllum have presented potential antifungal activities but no specific, fast, and precise method has been developed for their determination. Objective - To develop a methodology based on micellar electrokinetic chromatography to determine butenolides in Piper species. Methodology - The extracts were analysed in an uncoated fused-silica capillaries and for the micellar system 20 mmol/L SDS, 20% (v/v) acetonitrile (ACN) and 10 mmol/L STB aqueous buffer at pH 9.2 were used. The method was validated for precision, linearity, limit of detection (LOD) and limit of quantitation (LOQ) and the standard deviations were determined from the standard errors estimated by the regression line. Results - A micellar electrokinetic chromatography (MEKC) method for determination of butenolides in extracts gave full resolution for 1 and 2. The analytical curve in the range 10.0-50.0 mu g/mL (r(2) = 0.999) provided LOD and LOQ for 1 and 2 of 2.1/6.3 and 1.1/3.5 mu g/mL, respectively. The RSD for migration times were 0.12 and 1.0% for peak area ratios with 100.0 +/- 1.4% of recovery. Conclusions - A novel high-performance MEKC method developed for the analysis of butenolides 1 and 2 in leaf extracts of P. malacophyllum allowed their quantitative determined within an analysis time shorter than 5 min and the results indicated CE to be a feasible analytical technique for the quantitative determination of butenolides in Piper extracts. Copyright (C) 2010 John Wiley & Sons, Ltd.

Garlic (Allium sativum L.) and ready-to-eat garlic products: in vitro antioxidant activity

Garlic contains polyphenol and sulphur compounds, which are responsible for its antioxidant activity (AA). This study aimed at evaluating the AA of fresh garlic and its commercialised products and their shelf life. Fresh garlic (FG) and its products, i.e. chopped with salt (CGS), chopped without salt (CG), fried (FRG) and mixed garlic (FG with dehydrated garlic; MG) antioxidant activity was evaluated by three different methods: DPPH (1,1-diphenyl-2-picrylhydrazyl) assay, ß-carotene/linoleic acid assay and Rancimat® method. Amongst all the analysed products, fried garlic presented the highest antioxidant activity. The free radical-scavenging activity decreased during the shelf life of all analysed products that correlated with the decrease in the total polyphenol content. Our findings suggest that some compounds other than phenol may have contributed towards this outcome

Analysis of the tip roundness effects on the micro- and macroindentation response of elastic-plastic materials

In this work, the effects of indenter tip roundness oil the load-depth indentation curves were analyzed using finite element modeling. The tip roundness level was Studied based on the ratio between tip radius and maximum penetration depth (R/h(max)), which varied from 0.02 to 1. The proportional Curvature constant (C), the exponent of depth during loading (alpha), the initial unloading slope (S), the correction factor (beta), the level of piling-up or sinking-in (h(c)/h(max)), and the ratio h(max)/h(f) are shown to be strongly influenced by the ratio R/h(max). The hardness (H) was found to be independent of R/h(max) in the range studied. The Oliver and Pharr method was successful in following the variation of h(c)/h(max) with the ratio R/h(max) through the variation of S with the ratio R/h(max). However, this work confirmed the differences between the hardness values calculated using the Oliver-Pharr method and those obtained directly from finite element calculations; differences which derive from the error in area calculation that Occurs when given combinations of indented material properties are present. The ratio of plastic work to total work (W(p)/W(t)) was found to be independent of the ratio R/h(max), which demonstrates that the methods for the Calculation of mechanical properties based on the *indentation energy are potentially not Susceptible to errors caused by tip roundness.