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Sample records for rietveld method caracterizacao

  1. A modified Rietveld method to model highly anisotropic ceramics

    Tutuncu, G.; Motahari, M.; Daymond, M.R.; Ustundag, E.

    2012-01-01

    High energy X-ray diffraction was employed to probe the complex constitutive behavior of a polycrystalline ferroelectric material in various sample orientations. Pb(Zn,Nb)O 3 –Pb(Zr,Ti)O 3 (PZN–PZT) ceramics were subjected to a cyclic bipolar electric field while diffraction patterns were taken. Using transmission geometry and a two-dimensional detector, lattice strain and texture evolution (domain switching) were measured in multiple sample directions simultaneously. In addition, texture analysis suggests that non-180° domain switching is coupled with lattice strain evolution during uniaxial electrical loading. As a result of this material’s high strain anisotropy, the full-pattern Rietveld method was inadequate to analyze the diffraction data. Instead, a modified Rietveld method, which includes an elastic anisotropy term, yielded significant improvements in the data analysis results.

  2. Characterization of barium titanate powder doped with sodium and potassium ions by using Rietveld refining; Caracterizacao do po de titanato de bario dopado com ions sodio e potasio com o refinamento de Rietveld

    Andrade, M.C.; Assis, J.T.; Pereira, F.R., E-mail: mcalixto@iprj.uerj.b [Universidade do Estado do Rio de Janeiro (IPRJ/UERJ), Nova Friburgo, RJ (Brazil). Instituto Politecnico; Araujo, J.C. [Universidade do Estado do Rio de Janeiro (FFP/UERJ), Sao Goncalo, RJ (Brazil). Fac. de Formacao de Professores; Moreira, E.L.; Moraes, V.C.A.; Lopes, A.R. [Centro Brasileiro de Pesquisas Fisicas (CBPF/MCT), Rio de Janeiro, RJ (Brazil)

    2009-07-01

    A solid-reaction synthesis of doped barium titanate was done by employing barium carbonates, sodium, potassium and titanium oxides with classic procedures. Rietveld refining of X ray diffraction data of perovskite samples with tetragonal symmetry was applying and show good agreement. Besides, the treatment performed from 600 deg C produces nanocrystals of barium titanate with average size of 33 nm. The presence of endothermic peaks related to BaTiO{sub 3} formation at relatively low temperatures was determined by thermal analysis. A pseudo-Voigt Thompson-Cox-Hastings function was used to fit the standard samples of barium titanate. The Rietveld method has showed be efficient to detect the influences of temperature and doping on barium titanate microstructures. (author)

  3. Chemical analysis of superconductor material by Rietveld method; Analise quimica de material superconductor atraves do metodo de Rietveld

    Garcia Junior, E.S.; Gomes Junior, G.G.; Ogasawara, T., E-mail: georges@metalmat.ufrj.b [Universidade Federal do Rio de Janeiro (COPPE/UFRJ), RJ (Brazil). Coordenacao dos Programas de Pos-Graduacao de Engenharia. Dept. de Eng. Metalurgica e Materiais; Bispo, E.R.; Polasek, A. [Centro de Pesquisas de Energia Eletrica (CEPEL), Rio de Janeiro, RJ (Brazil); Amorim, H.S. [Universidade Federal do Rio de Janeiro (IF/UFRJ), RJ (Brazil). Inst. de Fisica

    2010-07-01

    Among the main superconducting systems, the system Bi-Sr-Ca-Cu-O is extremely important because it presents two stages of high superconducting critical temperature. To manufacture samples of the superconducting phase (Bi, Pb){sub 2}Sr{sub 2}Ca{sub 2}Cu{sub 3}Ox (Bi-2223) were used oxides and carbonates of high purity. The mixture was calcined and sintered for 100-200h in air. To characterize the material we used X-ray diffraction, SEM / EDS and measurement of critical temperature (Tc). The Rietveld method was used for structure refinement, and quantification of phases and to estimate the chemical composition of samples in order to obtain greater control of chemical composition using only the data of X-ray diffraction. The results were compared with the refinement results of X-ray fluorescence and was observed a discrepancy of about 8%. This result indicates that the Rietveld method can be an interesting alternative to perform chemical analysis. (author)

  4. Full quantitative phase analysis of hydrated lime using the Rietveld method

    Lassinantti Gualtieri, Magdalena; Romagnoli, Marcello; Miselli, Paola; Cannio, Maria; Gualtieri, Alessandro F.

    2012-01-01

    Full quantitative phase analysis (FQPA) using X-ray powder diffraction and Rietveld refinements is a well-established method for the characterization of various hydraulic binders such as Portland cement and hydraulic limes. In this paper, the Rietveld method is applied to hydrated lime, a non-hydraulic traditional binder. The potential presence of an amorphous phase in this material is generally ignored. Both synchrotron radiation and a conventional X-ray source were used for data collection. The applicability of the developed control file for the Rietveld refinements was investigated using samples spiked with glass. The results were cross-checked by other independent methods such as thermal and chemical analyses. The sample microstructure was observed by transmission electron microscopy. It was found that the consistency between the different methods was satisfactory, supporting the validity of FQPA for this material. For the samples studied in this work, the amount of amorphous material was in the range 2–15 wt.%.

  5. Full quantitative phase analysis of hydrated lime using the Rietveld method

    Lassinantti Gualtieri, Magdalena, E-mail: magdalena.gualtieri@unimore.it [Dipartimento Ingegneria dei Materiali e dell' Ambiente, Universita Degli Studi di Modena e Reggio Emilia, Via Vignolese 905/a, I-41100 Modena (Italy); Romagnoli, Marcello; Miselli, Paola; Cannio, Maria [Dipartimento Ingegneria dei Materiali e dell' Ambiente, Universita Degli Studi di Modena e Reggio Emilia, Via Vignolese 905/a, I-41100 Modena (Italy); Gualtieri, Alessandro F. [Dipartimento di Scienze della Terra, Universita Degli Studi di Modena e Reggio Emilia, I-41100 Modena (Italy)

    2012-09-15

    Full quantitative phase analysis (FQPA) using X-ray powder diffraction and Rietveld refinements is a well-established method for the characterization of various hydraulic binders such as Portland cement and hydraulic limes. In this paper, the Rietveld method is applied to hydrated lime, a non-hydraulic traditional binder. The potential presence of an amorphous phase in this material is generally ignored. Both synchrotron radiation and a conventional X-ray source were used for data collection. The applicability of the developed control file for the Rietveld refinements was investigated using samples spiked with glass. The results were cross-checked by other independent methods such as thermal and chemical analyses. The sample microstructure was observed by transmission electron microscopy. It was found that the consistency between the different methods was satisfactory, supporting the validity of FQPA for this material. For the samples studied in this work, the amount of amorphous material was in the range 2-15 wt.%.

  6. Quantitative phase analysis of uranium carbide from x-ray diffraction data using the Rietveld method

    Singh Mudher, K.D.; Krishnan, K.

    2003-01-01

    Quantitative phase analysis of a uranium carbide sample was carried out from the x-ray diffraction data by Rietveld profile fitting method. The method does not require the addition of any reference material. The percentage of UC, UC 2 and UO 2 phases in the sample were determined. (author)

  7. Quantitative determination of the crystalline phases of the ceramic materials utilizing the Rietveld method

    Kniess, C.T.; Prates, P.B.; Lima, J.C. de; Kuhnen, N.C.; Riella, H.G.; Maliska, A.M.

    2009-01-01

    Ceramic materials have properties defined by their chemical and micro-structural composition. The quantification of the crystalline phases is a fundamental stage in the determination of the structure, properties and applications of a ceramic material. Within this context, this study aims is the quantitative determination of the crystalline phases of the ceramic materials developed with addition of mineral coal bottom ash, utilizing the X ray diffraction technique, through the method proposed by Rietveld. For the formulation of the ceramic mixtures a {3,3} simplex-lattice design was used, giving ten formulations of three components (two different types of clays and coal bottom ash). The crystalline phases identified in the ceramic materials after sintering at 1150 deg C during two hours are: quartz, tridimite, mullite and hematite. The proposed methodology utilizing the Rietveld method for the quantification relating to crystalline phases of the materials was shown to be adequate and efficient. (author)

  8. Application of the Rietveld method to assess chromium(VI) speciation in chromite ore processing residue

    Chrysochoou, Maria; Dermatas, Dimitris

    2007-01-01

    The Rietveld method allows the quantification of crystalline phases and amorphous material identified by X-ray powder diffraction (XRPD) and other diffraction methods. The method assists in determining the speciation of contaminants in solid matrices both qualitatively and quantitatively in a statistically defensible approach, as it does not focus on a microscale. Rietveld was applied to chromite ore processing residue (COPR), a cementitious waste containing hexavalent chromium. Calcium aluminum chromium oxide hydrates (CACs) were the crystalline phases identified by XRPD that bind Cr 6+ in COPR according to their chemical formula. Rietveld quantification, combined with mass balances on Cr 6+ , showed that CACs may bind Cr 6+ in variable percentages, ranging from 25% to 85%. Analysis of duplicate samples showed that material variability is the predominant factor of uncertainty in evaluating the role of CACs in Cr 6+ speciation, provided that a consistent quantification strategy is pursued. The choice of strategy was performed on the basis of the pertinent literature, preliminary analyses of the equipment and the software settings, and mass balances. The correlation between the average CAC-bound Cr 6+ concentration and the total Cr 6+ for five samples (R 2 = 0.94), extracted from different zones and soil borings, suggests that CACs are a primary sink for Cr 6+ in COPR

  9. Study of crystallite size of yttria-stabilized zirconia powders by Rietveld method

    Leite, Wellington Claiton; Brinatti, Andre Mauricio; Ribeiro, Mauricio Aparecido; Andrade, Andre Vitor Chaves de; Chinelatto, Adriana Scoton Antonio; Chinelatto, Adilson Luiz

    2009-01-01

    The yttria-stabilized zirconia (YSZ) is used in a great variety of applications, for example, electrolytes of solid oxide fuel cells and oxygen sensors. In the study of YSZ, the particle size powders and sintering processes are important to define the final properties of the zirconia products. The objectives of this work were to determine the phases and the crystalline size using X-Ray Diffraction (XRD) data and the Rietveld Method (RM) of the YSZ powders obtained by chemical synthesis based on the Pechini method. It was used ZrOCl 2.8 H 2 O and Y(NO 3 ) 3.5 H 2 O as precursors reagents. After calcination at 550 deg C during 24 hours, the powder was analyzed by XRD and scanning electronic microscopy (SEM). From XRD and using Rietveld method were verified that there is only cubic phase with lattice parameter a = 5.1307(1) Å and the space group Fm3m. Due to substitution of the Zr atoms in the Y atoms sites, there were vacancies in 17.72 % of O atoms sites. However, the percentage of substitution of Zr atoms in Y atoms sites in the structure not was determinate because the curves of atomic scattering of them are very similar. Using Scherrer equation and considering anisotropy effect, the average crystalline size was determinate: 10,43 nm (c axis) and 10,39 (b axis). This spherical symmetry also observed for SEM. (author)

  10. Study the oxidation kinetics of uranium using XRD and Rietveld method

    Zhang Yanzhi; Guan Weijun; Wang Qinguo; Wang Xiaolin; Lai Xinchun; Shuai Maobing, E-mail: yanzhizh@163.com [China Academy of Engineering Physics, PO Box 919-71, Mianyang, Sichuan, 621900 (China)

    2010-03-15

    The surface oxidation of uranium metal has been studied by X-ray diffraction (XRD) and Rietveld method in the range of 50{approx}300deg. C in air. The oxidation processes are analyzed by XRD to determine the extent of surface oxidation and the oxide structure. The dynamics expression for the formation of UO{sub 2} was derived. At the beginning, the dynamic expression was nonlinear, but switched to linear subsequently for uranium in air and humid oxygen. That is, the growth kinetics of UO{sub 2} can be divided into two stages: nonlinear portion and linear portion. Using the kinetic data of linear portion, the activation energy of reaction between uranium and air was calculated about 46.0 kJ/mol. However the content of oxide as a function of time was linear in humid helium ambience. Contrast the dynamics results, it prove that the absence of oxygen would accelerate the corrosion rate of uranium in the humid gas. We can find that the XRD and Rietveld method are a useful convenient method to estimate the kinetics and thermodynamics of solid-gas reaction.

  11. Study the oxidation kinetics of uranium using XRD and Rietveld method

    Zhang, Yanzhi; Guan, Weijun; Wang, Qinguo; Wang, Xiaolin; Lai, Xinchun; Shuai, Maobing

    2010-03-01

    The surface oxidation of uranium metal has been studied by X-ray diffraction (XRD) and Rietveld method in the range of 50~300°C in air. The oxidation processes are analyzed by XRD to determine the extent of surface oxidation and the oxide structure. The dynamics expression for the formation of UO2 was derived. At the beginning, the dynamic expression was nonlinear, but switched to linear subsequently for uranium in air and humid oxygen. That is, the growth kinetics of UO2 can be divided into two stages: nonlinear portion and linear portion. Using the kinetic data of linear portion, the activation energy of reaction between uranium and air was calculated about 46.0 kJ/mol. However the content of oxide as a function of time was linear in humid helium ambience. Contrast the dynamics results, it prove that the absence of oxygen would accelerate the corrosion rate of uranium in the humid gas. We can find that the XRD and Rietveld method are a useful convenient method to estimate the kinetics and thermodynamics of solid-gas reaction.

  12. Separation of the overlapping effects in spectra for WDXRF using the Rietveld method

    Salvador, Vera Lucia Ribeiro

    2005-01-01

    This work presents a new methodology for the overlapping spectra separation obtained by the technique of wavelength dispersion X-ray fluorescence (WDXRF). This methodology allows to improve the conventional analytic results and to facilitate the determination of chemical species of a same element without chemical separation, by means of the separation of coming spectra of electronic transitions of valence electrons or chemical effects in internal electrons. With the software 'GSAS-EXPGUI' and the method of Rietveld overcomes the problem of overlapping lines of the present species in the sample and it facilitates the determination of the same ones simultaneously, without the need of samples patterns and calibration curves, what means an expressive gain in relation to other techniques. The preparation of the surface of the sample for the collection of the spectrum represents a critical stage for the acting of the analysis whose effects can be minimized being used the refinement of Rietveld, that allows the determination of the relationships of the intensities of the lines put upon by means of mathematical models, what establishes the basic conditions for obtaining of more precise results in the quantitative analysis. In the case of the determination of chemical species it can separate, for example Cr (III), Cr (VI) and Fe (II), Fe(III) that present overlapping of almost 100%. (author)

  13. A research of the mineralogy phases of clinker in a spanish cement using the method of Rietveld

    Castanon Ana M; Garcia Granda Santiago; Guerrero Ana M; Gomez Fernandez Fernando

    2012-01-01

    In order to introduce continuously a quality control method in a Spanish cement factory to improve the final product feature new research methodology is being developed. The Rietveld method [1] has been successfully used to analyze the composition of the main phases of clinker. Using this methodologies, research has been carried out to quantize appropriately the minor phase of free lime which is extremely important in the clinker quality. This method leads to satisfactory results on samples with contents in CaO from 3%. These results are possible combining X- ray diffraction and fluorescence techniques as well as the chemical analysis data. Clinker, the Rietveld method, free lime.

  14. The use of the Rietveld method as an evaluation tool in the stages of production of nanostructured hard metal

    Batista, A.C.; Perpetuo, G.J.; Oliveira, H.C.P. de; Silva, T.R.G. da

    2014-01-01

    The processing of the composite WC-10% Co, with nanometric grain size was analyzed aiming at identifying changes undergone by the material during mixing and compaction steps. Use the X-ray diffraction and the Rietveld method to obtain accurate data on the behavior of powders before these steps. This paper describes the use of the Rietveld method as an evaluation tool to obtain information about the behavior of powders of WC and Co steps during mixing and compaction prior to sintering of the composite. (author)

  15. Effect of data quality on quantitative phase analysis (QPA) using the Rietveld method

    Scarlett, N.; Madsen, I.; Lwin, T.

    1999-01-01

    Full text: Quantitative phase analysis using the Rietveld method has become a valuable tool in modern X-ray diffraction. XRD is a recognised research tool and has been successfully employed in the developmental stages of many industrial processes. It is now becoming increasingly important as a means of process control either (i) in site quality control laboratories or (ii) even on-line. In on-line applications, the optimisation of data collection regimes is of critical importance if rapid turn-around, and hence timely process control, is to be achieved. This paper examines the effect of data quality on the quantification of phases in well characterised suites of minerals. A range of data collection regimes has been systematically investigated with a view to determining the minimum data required for acceptable quantitative phase analyses. Data has been collected with variations in the following process factors: 1st step, width ranging from 0.01 to 0.3 deg 2θ ;2nd step, counting time ranging from 0.0125 to 4 sec/step 3rd step, upper limit in the scan range varying from 40 to 148 deg 2θ. The data has been analysed using whole-pattern (Rietveld) based methods using two distinctly different analytical approaches: (i) refinement of only pattern background and individual scale factors for each phase; (ii) refinement of unit cell dimensions, overall thermal parameters, peak width and shape in addition to the background and scale factors. The experimental design for this work included a ternary design of the three component phases (fluorite, CaF 2 ; zincite, ZnO; corundum, Al 2 O 3 ) to form seven mixtures of major and minor phases of different scattering powers and the combination of the three process factors (variables) to form a factorial plan. The final data generation plan is a combination/crossing of the three process variable factorial plan with the three component mixture plan. It allows a detailed data analysis to provide information on the effect of the process

  16. Quantitative determination of phases in ZrO2 (MgO) (Y2O3) using the Rietveld method

    Castro, Antonio Carlos de

    2007-01-01

    The key objective of this work is the crystallographic characterization of the zircon co-doped with Yttria and magnesium with the application of the Rietveld method for quantitative phase analysis of zircon polymorph (zircon monoclinic, tetragonal, and cubic). Samples of zircon polymorph were obtained from zircon doped with Yttria and magnesium at defined molar concentrations. The zircon polymorph stability during subeutetoid aging at 1350 deg C were investigated to determine ZrO 2 - MgO - Y 2 0 3 phases degradation and to define the solid solutions stability environment. ZrO 2 powders doped with 8 mol por cent of MgO and 1 mol por cent of Y 2 O 3 , and 9 mol por cent of MgO and 0 mol por cent of Y 2 O 3 have been prepared by chemical route using the co-precipitation method. These samples have been calcinate at 550 deg C, sintered at 1500 deg C and characterized by the Rietveld method using the X-ray diffraction data. The variation of the lattice parameter, changes in the phase composition and their microstructures are discussed. The application of the Rietveld method for quantitative phase analysis of zircon polymorph (zircon tetragonal and cubic) reveals no formation of tetragonal phase and indicating that the matrix is the cubic phase with low concentration of monoclinic phase.(author)

  17. Tailoring diffraction technique Rietveld method on residual stress measurements of cold-can oiled 304 stainless steel plates

    Parikin; Killen, P.; Anis, M.

    2003-01-01

    Tailoring of diffraction technique-Rietveld method on residual stress measurements of cold-canailed stainless steel 304 plates assuming the material is isotopic, the residual stress measurements using X-ray powder diffraction is just performed for a plane lying in a large angle. For anisotropic materials, the real measurements will not be represented by the methods. By Utilizing of all diffraction peaks in the observation region, tailoring diffraction technique-Rietveld analysis is able to cover the limitations. The residual stress measurement using X-ray powder diffraction tailored by Rietveld method, in a series of cold-canailed stainless steel 304 plates deforming; 0, 34, 84, 152, 158, 175, and 196 % reduction in thickness, have been reported. The diffraction data were analyzed by using Rietveld structure refinement method. Also, for all cold-canailed stainless steel 304 plates cuplikans, the diffraction peaks are broader than the uncanailed one, indicating that the strains in these cuplikans are inhomogeneous. From an analysis of the refined peak shape parameters, the average root-mean square strain, which describes the distribution of the inhomogeneous strain field, was calculated. Finally, the average residual stresses in cold-canailed stainless steel 304 plates were shown to be a combination effect of hydrostatic stresses of martensite particles and austenite matrix. The average residual stresses were evaluated from the experimentally determined average lattice strains in each phase. It was found the tensile residual stress in a cuplikan was maximum, reaching 442 MPa, for a cuplikan reducing 34% in thickness and minimum for a 196% cuplikan

  18. Crystal structure analysis of LaMnO_3 with x-ray diffraction technique using the Rietveld method

    Engkir Sukirman; Wisnu Ari Adi; Yustinus Purwamargapratala

    2010-01-01

    Crystal structure analysis of LaMnO_3 using the Rietveld method has been carried out. The LaMnO_3 sample was synthesized with high energy mechanical milling from the raw materials of La_2O_3 and MnO_2 with the appropriate mol ratio. Milling were performed for 10 hours, pelletized and hereinafter sintered at 1350 °C for 6 hours. The sample characterizations covered the crystal structure and electric-magnetic properties of the materials by X-ray diffraction technique using the Rietveld method and the four point probe, respectively. The Rietveld refinement results based on the X-rays diffraction data indicate that the sample of LaMnO_3 is single phase with the crystal system: orthorhombic, the space group: Pnma No. 62 and the lattice parameters: a = 55.4405(9) Å; b = 7.717(1) Å dan c = 5.537(1) Å. The material owns Magnetic Resonance (MR) respond of 7 %, the mean value of crystallite size, D = 17 nm and lattice strain, e = - 0.5 %. So, the material go through a compressive strain, and according to the Nanda's strain model, it becomes a type G antiferromagnetic insulator. Because the insulator properties of the material does not change although being hit by the external magnetic field, hence the MR respond is only caused by the order of electron spin. Therefore at room temperature, LaMnO_3_._0 just exhibits a small MR respond. (author)

  19. Investigation on the evolution of microstructure and texture of electroplated Ni–Ti composite coating by Rietveld method

    Zhao, Yuantao, E-mail: zhaoyuantao@sjtu.edu.cn; Cai, Fei, E-mail: caifei32@126.com; Wang, Chengxi, E-mail: sjtucxw@sjtu.edu.cn; Chai, Ze, E-mail: zechaisjtu@163.com; Zhu, Kaiyuan, E-mail: xrd125@163.com; Xu, Zhou, E-mail: xuzhou@sjtu.edu.cn; Jiang, Chuanhai, E-mail: chjiang-sjtu@hotmail.com

    2015-10-30

    Highlights: • Ni–Ti composite coatings were prepared by electroplating. • Morphology and Ti content of Ni–Ti coatings were studied upon SEM and EDXS. • Microstructures of Ni–Ti coatings were studied upon the Rietveld method. • The texture of Ni–Ti coatings was studied upon the pole figure. - Abstract: Rietveld refinement was utilized to investigate the evolution of microstructure and texture of the Ni–Ti composite coatings electroplated at different applied current densities. Scanning Electron Microscope and Energy Dispersive Spectroscopy were utilized to investigate the morphology and chemical composition of the coatings. Relative texture coefficients (RTC) and measured pole figures were utilized to investigate the texture evolution of the coatings. The results showed that the surface morphology of the coatings changed from a colonial structure to a polyhedral one. And the incorporated Ti content decreased with increasing applied current density. As the applied current density increased, the crystallite sizes increased and their distribution got less uniform, and the microstrain and dislocation density decreased. The results of simulated pole figures obtained from Rietveld refinement illustrated that the texture of the coatings changed from no obvious texture to a strong [2 0 0] fiber texture with increasing applied current density. The texture evolution obtained from simulated pole figures was confirmed by the result of RTC and the measured pole figures. The evolutions of the microstructure and texture were derived from the change of the applied current density and incorporated Ti content in the Ni–Ti composite coatings.

  20. A research of the mineralogy phases of clinker in a spanish cement using the method of Rietveld

    Castanon, Ana M; Garcia, Granda Santiago; Guerrero, Ana M; Gomez Fernandez, Fernando

    2012-01-01

    In order to introduce continuously a quality control method in a Spanish cement factory to improve the final product feature new research methodology is being developed. The Rietveld method [1] has been successfully used to analyze the composition of the main phases of clinker. Using this methodologies, research has been carried out to quantize appropriately the minor phase of free lime which is extremely important in the clinker quality. This method leads to satisfactory results on samples with contents in CaO from 3%. These results are possible combining X- ray diffraction and fluorescence techniques as well as the chemical analysis data.

  1. Mineralogical characterization of a highly-weathered soil by the Rietveld Method Caracterização mineralógica de um solo altamente intemperizado pelo Método de Rietveld

    André Maurício Brinatti

    2010-08-01

    Full Text Available 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.A caracterização mineralógica por meio da quantificação dos minerais presentes em solos brasileiros por difração de raios X usando o Método de Rietveld é, ainda, pouco comum. Neste trabalho foi realizada a quantificação mineralógica de um Latossolo Vermelho ácrico da região de Ponta Grossa, Paraná, Brasil, utilizando o Método de Rietveld com dados de Difração de Raios X e também verificado se o método foi adequado na quantificação mineral de um solo altamente intemperizado. Os horizontes A

  2. Rietveld analysis system RIETAN (translation)

    Izumi, Fujio

    1991-09-01

    This is the manual of the RIETAN system (a Rietveld analysis program) which is originally written in Japanese by Fujio Izumi. The manual consists of two parts. Part I is a general description of the fundamental concepts and methods of the RIETAN system. Part II is the user's manual of the RIETAN which mainly describes in detail how to create user's data sets, procedures of Rietveld analysis and how to read the results of analysis. (author)

  3. Crystal phase analysis of SnO2-based varistor ceramic using the Rietveld method

    Moreira, M.L.; Pianaro, S.A.; Andrade, A.V.C.; Zara, A.J.

    2006-01-01

    A second addition of l mol% of CoO to a pre calcined SnO 2 -based ceramic doped with 1.0 mol% of CoO, 0.05 mol% of Nb 2 O 5 and 0.05 mol% of Cr 2 O 3 promotes the appearance of a secondary phase, Co 2 SnO 4 , besides the SnO 2 cassiterite phase, when the ceramic was sintered at 1350 deg. C/2 h. This was observed using X-ray powder diffraction, scanning electron microscopy and energy dispersive X-ray techniques. Rietveld refinement was carried out to quantify the phases present in the ceramic system. The results of the quantitative analysis were 97 wt.% SnO 2 and 3 wt.% Co 2 SnO 4 . The microstructural analysis showed that a certain amount of cobalt ion remains into cassiterite grains

  4. Application of the Rietveld method in structural analysis of catalysts based on CuO/CeO2

    Neiva, L.S.; Ribeiro, M.A.; Bispo, A.; Simoes, A.N.; Gama, L.

    2011-01-01

    This work has as aim to synthesize catalysts composed by CuO/CeO 2 by means two distinct methods of synthesis, they are: combustion synthesis and Pechini. The catalysts composed by CuO/CeO 2 were synthesized with CuO in condition of dopant element. The value of the CuO concentration ranged between 0 and 0.5 mol. Has been done a structural analysis related to how the kind of synthesis method used influences over physical characteristic of the catalytic material. The obtained catalysts were characterized by X-ray diffraction with refinement by Rietveld method. According to results, the synthesized catalysts showed crystalline structures formed mostly by CeO 2 phase, as expected, since this is the host matrix for the dopant element. The catalysts obtained by the Pechini method presented structures with a smaller amount of segregated phases formed by CuO, according to the results of the structural analysis. (author)

  5. Homogeneity characterisation of (U,Gd)O2 sintered pellets by X-ray diffraction powder analysis applying Rietveld method

    Leyva, Ana G.; Vega, Daniel R.; Trimarco, Veronica G.; Marchi, Daniel E.

    1999-01-01

    The (U,Gd)O 2 sintered pellets are fabricated by different methods. The homogeneity characterisation of Gd content seems to be necessary as a production control to qualify the process and the final product. The micrographic technique is the most common method used to analyse the homogeneity of these samples, this method requires time and expertise to obtain good results. In this paper, we propose an analysis of the X-ray diffraction powder patterns through the Rietveld method, in which the differences between the experimental data and the calculated from a crystalline structure model proposed are evaluated. This result allows to determine the cell parameters, that can be correlated with the Gd concentration, and the existence of other phases with different Gd ratio. (author)

  6. Rietveld analysis using powder diffraction data with anomalous scattering effect obtained by focused beam flat sample method

    Tanaka, Masahiko, E-mail: masahiko@spring8.or.jp; Katsuya, Yoshio, E-mail: katsuya@spring8.or.jp; Sakata, Osami, E-mail: SAKATA.Osami@nims.go.jp [Synchrotron X-ray Station at SPring-8, National Institute for Materials Science 1-1-1 Kouto, Sayo, Hyogo 679-5198 (Japan)

    2016-07-27

    Focused-beam flat-sample method (FFM) is a new trial for synchrotron powder diffraction method, which is a combination of beam focusing optics, flat shape powder sample and area detectors. The method has advantages for X-ray diffraction experiments applying anomalous scattering effect (anomalous diffraction), because of 1. Absorption correction without approximation, 2. High intensity X-rays of focused incident beams and high signal noise ratio of diffracted X-rays 3. Rapid data collection with area detectors. We applied the FFM to anomalous diffraction experiments and collected synchrotron X-ray powder diffraction data of CoFe{sub 2}O{sub 4} (inverse spinel structure) using X-rays near Fe K absorption edge, which can distinguish Co and Fe by anomalous scattering effect. We conducted Rietveld analyses with the obtained powder diffraction data and successfully determined the distribution of Co and Fe ions in CoFe{sub 2}O{sub 4} crystal structure.

  7. Rietveld analysis using powder diffraction data with anomalous scattering effect obtained by focused beam flat sample method

    Tanaka, Masahiko; Katsuya, Yoshio; Sakata, Osami

    2016-01-01

    Focused-beam flat-sample method (FFM) is a new trial for synchrotron powder diffraction method, which is a combination of beam focusing optics, flat shape powder sample and area detectors. The method has advantages for X-ray diffraction experiments applying anomalous scattering effect (anomalous diffraction), because of 1. Absorption correction without approximation, 2. High intensity X-rays of focused incident beams and high signal noise ratio of diffracted X-rays 3. Rapid data collection with area detectors. We applied the FFM to anomalous diffraction experiments and collected synchrotron X-ray powder diffraction data of CoFe_2O_4 (inverse spinel structure) using X-rays near Fe K absorption edge, which can distinguish Co and Fe by anomalous scattering effect. We conducted Rietveld analyses with the obtained powder diffraction data and successfully determined the distribution of Co and Fe ions in CoFe_2O_4 crystal structure.

  8. Synthesis of Zr-Si-O-N phases by carbonitriding reaction. Characterization of crystalline phases using the Rietveld method

    Mazzoni A.D.

    2001-01-01

    Full Text Available Zirconium compounds are of great interest for ceramic application due to their excellent thermal and mechanical properties. Zirconium phases of the system Zr-O-C-N were obtained using carbonitriding reactions of zircon mineral (ZrO2.SiO2, under different reaction conditions. The reaction products were studied by X-ray diffraction (XRD using the Rietveld method. Silicon was employed as internal standard. Zirconium compounds formed were m-ZrO2 (monoclinic, beta"-zirconium oxynitride and a cubic Zr(C,N,O phase whose lattice parameter a o depends on the composition. The crystallite sizes of the three zirconium phases were determined also by XRD. The minority phases present are the ones of the Si-O-N-C system. The reaction conditions employed allows to obtain reaction products with low or without silicon content.

  9. Influence of the milling time in the microstructural parameters of TA2O5-Al powder refined by Rietveld method

    Brito, R.A.; Mendes, M.W.D.; Alves Junior, C.; Costa, F.A. da; Gomes, U.U.

    2009-01-01

    Mechanical alloying (MA) is a solid-state powder processing technique involving repeated welding, fracturing, and re-welding of powder particles in a high energy mill. This process is used for producing of fine powders containing unique microstructures. The process starts with mixing of the powders in the desired proportion. Then, the mixture is milled using the established time in the high-energy mill. The powder particles are submitted to repeated cycles of cold working and fracture, and the final product correspond to a composite powder, containing characteristics different of the initial constituents. Ta 2 O 5 -Al powders were milled in a planetary ball mill for different times in order to evaluate the influence of the milling time in their microstructural parameters like crystallite size and micro deformation. The microstructural parameters were obtained by the Rietveld Method. The results showed that the microstructural parameters were influenced by the increase of the milling time. (author)

  10. Study of the superconducting compound Hg,Re-1223 by X-Ray diffraction with application of Rietveld method

    Putvinskis, Rodrigo

    2008-01-01

    The objective of this work was to study the crystal structure of the superconductor compound of nominal composition Hg 0,82 Re 0,18 Ba 2 Ca 2 Cu 3 O 8+δ and general formula Hg,Re- 1223 and different oxygen contents, by the X-ray diffraction technique, by using the Rietveld method. The studied samples present different oxygen stoichiometry because during the synthesis process, had been heat treated under different oxygen/argon gas mixtures in the ratios: 5:95, 10:90 and 15:85. The results of structural refinement for the samples show that different oxygen contents imply in different cell parameters, atomic positions and distances for the main phase of each sample. The segregation of two superconducting phases with the same crystal structure, but slightly different cell parameters was confirmed for the studied samples both by Rietveld analysis and anomalous X-ray diffraction experiments. It was also confirmed that one of the segregated phases does not incorporate Re cations its composition. The main phase, who incorporates the Re cations, is here called Hg,Re-1223 and the Re-free secondary phase is called Hg- 1223. It was found that the superconducting phases present different crystallite sizes and the sample treated under gas flow composed of 10% oxygen and 90% argon presents the highest fraction of superconducting phases. From these results it was possible to conclude that the sample produced from the precursor compound treated under flow of O 2 /Ar gas at the ratio 10/90 presents the better results for the synthesis of this superconducting compound. (author)

  11. Refinement of the crystal structure of lead titanate with different degrees of imperfection of cationic and anionic sublattices by the Rietveld method

    Akimov, A.I.; Savchuk, G.K.; Rubtsov, V.A.; Letko, A.K.

    2003-01-01

    The parameters of the crystal structure of lead titanate with different degrees of imperfection of the anionic and cationic sublattices are refined by the Rietveld method. The experiments are carried out on a DRON-4 diffractometer (CuK α radiation; 20 deg. d 5.0-6.0%

  12. Synthesis and refinement of ferroelectric ceramic BaBi4Ti4O15 (BBT) using Rietveld Methods

    Silva, P.M.O.; Sales, A.J.M.; Carneiro, J.C.S.; Sancho, E.O.; Sales, J.C.; Sombra, A.S.B.

    2012-01-01

    The lead zirconate titanate (PZT) has potential application in nonvolatile ferroelectric memory and capacitors, however this material is linked to environmental pollution. In order to remedy this problem, we propose the synthesis of the compound, BaBi 4 TI 4 O 15 (BBT) because of similarity to PZT. The phase of the BBT has been prepared by the method of solid state. Reagents (BaCO 3 , Bi 2 O 3 and TiO 2 ) were ground for 6 hours at 360 rpm in a planetary ball mill and suffered high energy heat treatment for 2 hours at temperatures of 850, 900, 950 and 1000 ° C. The calcined powder was characterized by X-ray diffraction (XRD) and refined by the program DBWSTools 2.3 Beta based on the Rietveld method. The results obtained confirmed the refinement of the single-phase with tetragonal structure BaBi 4 TI 4 O 15 for all samples. The sample calcined at 950 °C presented the best densification (7.508 g/cm³). (author)

  13. Influence of diopside: feldspar ratio in ceramic reactions assessed by quantitative phase analysis (X-ray diffraction - Rietveld method)

    Kuzmickas, L.; Andrade, F.R.D.; Szabo, G.A.J.; Motta, J.F.M.; Cabral Junior, M.

    2013-01-01

    White ceramics were produced with raw mixtures prepared with varying proportions of diopside-rich rock (0 to 20 wt.%) and potassic feldspar (40 to 20 wt.%), and fixed proportions of kaolinite (40 wt.%) and quartz (20 wt.%), fired in a temperature range from 1170 to 1210 deg C. The phases identified in the experimental ceramics were quartz, anorthite, mullite and glass, and their relative mass proportions were determined by X-ray diffraction (Rietveld method). The addition of diopside as a partial substitute for potassic feldspar causes the formation of a calcium silicate, analogous of the natural anorthite (CaSi 2 Al 2 O 8 ) in the ceramics, with proportional reduction in its glass and mullite contents. Water absorption and porosity of the ceramic bodies clearly decrease with increasing firing temperature, while the effect of the raw mixture composition on the physical and mechanical properties of the ceramics is less evident. Diopside-rich rock has low iron content (1.5 wt.% Fe 2 O 3 ) and, therefore, promotes white burning. (author)

  14. Influence of diopside: feldspar ratio in ceramic reactions assessed by quantitative phase analysis (X-ray diffraction - Rietveld method)

    Kuzmickas, L.; Andrade, F.R.D.; Szabo, G.A.J. [Universidade de Sao Paulo (IGc/USP), SP (Brazil). Inst. de Geociencias. Dept. de Mineralogia e Geotecnia; Motta, J.F.M.; Cabral Junior, M., E-mail: lukuzmickas@gmail.com, E-mail: dias@usp.br, E-mail: gajszabo@usp.b, E-mail: motta.jf@gmail.com, E-mail: marsis@ipt.br [Instituto de Pesquisas Tecnologicas (IPT), Sao Paulo, SP (Brazil). Secao de Recursos Minerais e Tecnologia Ceramica

    2013-04-15

    White ceramics were produced with raw mixtures prepared with varying proportions of diopside-rich rock (0 to 20 wt.%) and potassic feldspar (40 to 20 wt.%), and fixed proportions of kaolinite (40 wt.%) and quartz (20 wt.%), fired in a temperature range from 1170 to 1210 deg C. The phases identified in the experimental ceramics were quartz, anorthite, mullite and glass, and their relative mass proportions were determined by X-ray diffraction (Rietveld method). The addition of diopside as a partial substitute for potassic feldspar causes the formation of a calcium silicate, analogous of the natural anorthite (CaSi{sub 2}Al{sub 2}O{sub 8}) in the ceramics, with proportional reduction in its glass and mullite contents. Water absorption and porosity of the ceramic bodies clearly decrease with increasing firing temperature, while the effect of the raw mixture composition on the physical and mechanical properties of the ceramics is less evident. Diopside-rich rock has low iron content (1.5 wt.% Fe{sub 2}O{sub 3}) and, therefore, promotes white burning. (author)

  15. A Study on the quantification of hydration and the strength development mechanism of cementitious materials including amorphous phases by using XRD/Rietveld method

    Yamada, Kazuo; Hoshino, Seiichi; Hirao, Hiroshi; Yamashita, Hiroki

    2008-01-01

    X-ray diffraction (XRD)/Rietveld method was applied to measure the phase composition of cement. The quantative analysis concerning the progress of hydration was accomplished in an error of about the maximum 2-3% in spite of including amorphous materials such as blast furnace slag, fly ash, silica fume and C-S-H. The influence of the compressive strength on the lime stone fine powder mixture material was studied from the hydration analysis by Rietveld method. The two stages were observed in the strength development mechanism of cement; the hydration promotion of C 3 S in the early stage and the filling of cavities by carbonate hydrate for the longer term. It is useful to use various mixture materials for the formation of the resource recycling society and the durability improvement of concrete. (author)

  16. Quantitative phase analysis of alumina/calcium-hexaluminate composites using neutron diffraction data and the Rietveld method

    Asmi, D.; Low, I.M.; O'Connor, B.H.; Kennedy, S.J.

    2000-01-01

    Full text: The Al 2 O 3 -CaO system is the basis of an important class of high-temperature refractories in the steel industry. It contains a number of stable intermediate compounds which include C 3 A, C 12 A 7 , CA, CA 2 , and CA 6 . These calcium aluminates are also important constituents of high alumina cement and have been used to produce high-strength and high-toughness ceramic-polymer composite materials. More recently, alumina composites containing 30 wt% CA 6 platelets have been developed by An et al which show characteristics of self-reinforcement and enhanced toughening through crack-bridging. In this paper, we describe the use of high-temperature neutron diffraction to monitor the in-situ phase formation and abundances of calcium aluminates (CA, CA 2 , and CA 6 ) in alumina composites containing 5-50 wt % CA 6 .at temperatures in the range 1000 - 1600 deg C. These composites were produced using reaction sintering of alumina and calcium oxide. For comparison purposes, control samples of pure α-alumina and CA 6 were also produced. Determination of relative phase abundances in these materials has been performed using the standardless Rietveld refinement method. Results show that the relative phase abundance of calcium aluminates in the composites increased with temperature and in proportion with the amount of calcium oxide present. The formation temperatures of CA, CA 2 , and CA 6 have been observed to occur at 1000 deg , 1200 deg, and ∼1350 deg C respectively, which agree well with results obtained from x-ray diffraction, synchrotron radiation diffraction and differential thermal analysis

  17. Application of the Rietveld method in structural analysis of catalysts based on CuO/CeO{sub 2}; Aplicacao do metodo de Rietveld na analise estrutural de catalisadores a base de CuO/CeO{sub 2}

    Neiva, L.S.; Ribeiro, M.A.; Bispo, A.; Simoes, A.N.; Gama, L., E-mail: lsoutoneiva@yahoo.com.br [Universidade Federal de Campina Grande (UFCG), PB (Brazil). Departamento de Engenharia de Materiais

    2011-07-01

    This work has as aim to synthesize catalysts composed by CuO/CeO{sub 2} by means two distinct methods of synthesis, they are: combustion synthesis and Pechini. The catalysts composed by CuO/CeO{sub 2} were synthesized with CuO in condition of dopant element. The value of the CuO concentration ranged between 0 and 0.5 mol. Has been done a structural analysis related to how the kind of synthesis method used influences over physical characteristic of the catalytic material. The obtained catalysts were characterized by X-ray diffraction with refinement by Rietveld method. According to results, the synthesized catalysts showed crystalline structures formed mostly by CeO{sub 2} phase, as expected, since this is the host matrix for the dopant element. The catalysts obtained by the Pechini method presented structures with a smaller amount of segregated phases formed by CuO, according to the results of the structural analysis. (author)

  18. Assessment of firing conditions in old fired-clay bricks. The contribution of X-ray powder diffraction with the Rietveld method and small angle neutron scattering

    Viani, Alberto; Sotiriadis, Konstantinos; Len, A.; Šašek, Petr; Ševčík, Radek

    2016-01-01

    Roč. 116, June (2016), s. 33-43 ISSN 1044-5803 R&D Projects: GA MŠk(CZ) LO1219 Keywords : fired- clay brick * Rietveld method * small angle neutron scattering * X-ray diffraction * firing temperature Subject RIV: AL - Art, Architecture, Cultural Heritage Impact factor: 2.714, year: 2016 http://www.sciencedirect.com/science/article/pii/S1044580316300870

  19. Quantitative study of Portland cement hydration by X-ray diffraction/Rietveld analysis and independent methods

    Scrivener, K.L.; Fuellmann, T.; Gallucci, E.; Walenta, G.; Bermejo, E.

    2004-01-01

    X-ray diffraction (XRD) is a powerful technique for the study of crystalline materials. The technique of Rietveld refinement now enables the amounts of different phases in anhydrous cementitious materials to be determined to a good degree of precision. This paper describes the extension of this technique to a pilot study of the hydration of a typical Portland cement. To validate this XRD-Rietveld analysis technique, its results were compared with independent measures of the same materials by the analysis of backscattered electron images (BSE/IA) and thermogravimetric analysis (TGA). In addition, the internal consistency of the measurements was studied by comparing the XRD estimates of the amounts of hydrates formed with the amounts expected to form from the XRD estimates of the amounts of anhydrous materials reacted

  20. Structural analysis of a carbonated hydroxyapatite by the Rietveld method using different profile functions; Analise estrutural de uma hidroxiapatita carbonatada pelo metodo de Rietveld aplicando funcoes de perfil diferentes

    Araujo, Jorge C. de [Universidade do Estado do Rio de Janeiro (UERJ), RJ (Brazil). Dept. de Matematica], e-mail: jcaraujo@iprj.uerj.br; Moreira, Elizabeth L.; Moraes, Valeria Conde Alves [Centro Brasileiro de Pesquisas Fisicas (CBPF), Rio de Janeiro, RJ (Brazil)], e-mail: beth@cbpf.br, e-mail: conde@cbpf.br; Moreira, Ana Paula D. [Universidade Federal Fluminense (UFF), Niteroi, RJ (Brazil). Inst. de Quimica. Dept. de Quimica Analitica], e-mail: duarteap@gmail.com

    2008-10-15

    The crystal structure of the synthetic hydroxyapatite with 12.8 ({+-} 0,64) wt. % CO{sub 3}{sup 2-} ion content was analyzed by X-ray diffraction using the Rietveld refinement method employing Pearson VII and pseudo-Voigt functions to fit the X-ray profile. The results obtained for unit cell parameters when compared to pattern hydroxyapatite showed a decrease in the a (=b) parameter and an increase in the c parameter without significant difference between the functions employed. The separation of the anisotropic broadening of reflections originated from unit cell strains indicated that this effect is dominant in reflection line broadening, principally to hkl plans with an interatomic distance lower than 2,24 angstrom. Modifications in the atomic coordinates of C atom were noted mainly in PO{sub 4}{sup 3-} (B site) and OH{sup -} (A site) sites. The average crystallite size in the crystallography axis directions (002 and 300) suggests equi axial morphology. The results obtained to CO{sub 3}{sup 2}- content were 11.72 ({+-} 0,64) wt. % to Pearson VII and 13.20 ({+-} 0,64) wt. % to pseudo-Voigt function. The refinement of the occupancy factors to C atoms in both sites PO{sub 4}{sup 3-}(B) and OH{sup -} (A) indicated higher insertion in phosphate site than hydroxide site. However, the relative occupancy of the C atom observed in the B site is lower than in the A site. (author)

  1. Refinement by Rietveld method of a rolled sheet Al-Mg-Si 6063 alloy with preferential orientation

    Carrio, J.A.G.; Hattori, C.S.; Miranda, L.F.; Domingues Junior, N.I.; Lima, N.B.; Couto, A.A.; Aguiar, A.A.

    2010-01-01

    The Rietveld refinement of a sample with preferential orientation was accomplished using data of X ray diffraction of a rolled 6063 aluminum alloy. The refinement of the preferential orientation by spherical harmonic was accomplished using a symmetry of sample mmm (rolling) until the order of 8 and was compared with experimental pole figures. The four pole figures presented indicate a sharp texture of the planes (111), (200), (220) and (311). The calculated pole figures obtained from the refinement of the X ray diffraction spectrum can incur in mistakes of preferential orientation. This happens because the measure is restricted to the planes parallel to the surface without inference to the symmetry of the sample. (author)

  2. Application of the Rietveld method in powders of strontium-doped lanthanum manganite calcined in different temperatures

    Chiba, R.; Vargas, R.A.; Martinez, L.G.; Andreoli, M.; Seo, E.S.M.

    2010-01-01

    The strontium-doped lanthanum manganite (LSM) is a ceramic material used as cathode in device called High Temperature Solid Oxide Fuel Cell. In this work, the LSM was synthesized by the citrate technique with the objective to get powders without the formation of secondary phases, such as lanthanum oxide and the lanthanum hydroxide, harmful for the functional performance of the device. The definitive calcination temperatures had been 700, 900 and 1100 deg C, due the decomposition of the polymeric precursors to present stabilization from 480 deg C. The analysis by X-ray diffraction of the calcined powders in different temperatures shows the formation only of phase LSM of hexagonal crystalline structure, type pseudo-perovskite. Using the refinement of Rietveld was determined the parameters and volumes of unity cells, atomic positions and occupations. These results confirm that the chemical compositions obtained are similar to the nominal. (author)

  3. Assessment of firing conditions in old fired-clay bricks: The contribution of X-ray powder diffraction with the Rietveld method and small angle neutron scattering

    Viani, Alberto, E-mail: viani@itam.cas.cz [Institute of Theoretical and Applied Mechanics AS CR, Centre of Excellence Telč, Batelovská 485, CZ-58856 Telč (Czech Republic); Sotiriadis, Konstantinos [Institute of Theoretical and Applied Mechanics AS CR, Centre of Excellence Telč, Batelovská 485, CZ-58856 Telč (Czech Republic); Len, Adél [Wigner Research Centre for Physics HAS, Konkoly-Thege 29-33, 1121 Budapest (Hungary); Šašek, Petr; Ševčík, Radek [Institute of Theoretical and Applied Mechanics AS CR, Centre of Excellence Telč, Batelovská 485, CZ-58856 Telč (Czech Republic)

    2016-06-15

    Full characterization of fired-clay bricks is crucial for the improvement of process variables in manufacturing and, in case of old bricks, for restoration/replacement purposes. To this aim, five bricks produced in a plant in Czech Republic in the past have been investigated with a combination of analytical techniques in order to derive information on the firing process. An additional old brick from another brickyard was also used to study the influence of different raw materials on sample microstructure. The potential of X-ray diffraction with the Rietveld method and small angle neutron scattering technique has been exploited to describe the phase transformations taking place during firing and characterize the brick microstructure. Unit-cell parameter of spinel and amount of hematite are proposed as indicators of the maximum firing temperature, although for the latter, limited to bricks produced from the same raw material. The fractal quality of the surface area of pores obtained from small angle neutron scattering is also suggested as a method to distinguish between bricks produced from different raw clays. - Highlights: • Rietveld method helps in describing microstructure and physical properties of bricks. • XRPD derived cell parameter of spinel is proposed as an indicator of firing temperature. • SANS effectively describes brick micro and nanostructure, including closed porosity. • Fractal quality of pore surface is proposed as ‘fingerprint’ of brick manufacturing.

  4. PETROGRAPHY AND APPLICATION OF THE RIETVELD METHOD TO THE QUANTITATIVE ANALYSIS OF PHASES OF NATURAL CLINKER GENERATED BY COAL SPONTANEOUS COMBUSTION

    Pinilla A. Jesús Andelfo

    2010-06-01

    Full Text Available

    Fine-grained and mainly reddish color, compact and slightly breccious and vesicular pyrometamorphic rocks (natural clinker are associated to the spontaneous combustion of coal seams of the Cerrejón Formation exploited by Carbones del Cerrejón Limited in La Guajira Peninsula (Caribbean Region of Colombia. These rocks constitute remaining inorganic materials derived from claystones, mudstones and sandstones originally associated with the coal and are essentially a complex mixture of various amorphous and crystalline inorganic constituents. In this paper, a petrographic characterization of natural clinker, aswell as the application of the X-ray diffraction (Rietveld method by mean of quantitative analysis of its mineral phases were carried out. The RIQAS program was used for the refinement of X ray powder diffraction profiles, analyzing the importance of using the correct isostructural models for each of the existing phases, which were obtained from the Inorganic Crystal Structure Database (ICSD. The results obtained in this investigation show that the Rietveld method can be used as a powerful tool in the quantitative analysis of phases in polycrystalline samples, which has been a traditional problem in geology.

  5. Crystal structures of new cuprates containing CO3 analyzed by the Rietveld method of neutron powder diffraction

    Miyazaki, Y.; Yamane, H.; Kajitani, T.; Hiraga, K.; Hirai, T.; Morii, Y.; Funahashi, S.

    1993-01-01

    New compounds containing CO 3 groups, Sr 2 CuO 2 (CO 3 ), (C 0.4 Cu 0.6 )Sr 2 (Y 0.86 Sr 0.14 )Cu 2 O 7 and (C 0.35 Cu 0.65 )Sr 2 (Y 0.73 Ce 0.27 ) 2 Cu 2 O 9 , were prepared as stable phases at 1273-1303 K in a flowing gas of O 2 -CO 2 . The crystal structures of these compounds were refined by means of the Rietveld analysis for neutron powder diffraction data collected using a high resolution powder diffractometer (HRPD) in the JRR-3M reactor hall of the Japan Atomic Energy Research Institute (JAERI). Positions of CO 3 groups were satisfactorily determined. The distances of C-O bonds in the CO 3 groups were around 1.3A and the O-C-O angles were almost equal to the ideal bond angle of 120deg. (author)

  6. Study of effect of sintering time on the 2223 phase growth Bi-Pb-Sr-Ca-Cu-O superconductor by Rietveld method

    Parikin; Prasuad, W; Gunawan

    1996-01-01

    It has been reported that the sintering time is as important for the preparation of superconductor as the sintering temperature and method. This paper reports on the finding of the optimum sintering time in the preparation of the 2223 phase bismuth (Bi) superconductor. The samples were synthesized with nominal composition 1.84 : 0.34 : 1.91 : 2.03 : 3.06 from raw materials by solid state reaction and sintered at 860 o C for five days. The resintering were done three times, i.e. 24, 48 and 96 hours. The Rietveld analysis shows that the 2223 phase grows continuously as a function of the sintering time. The highest percentage of the 2223 phase (80.64%) were obtained at 96 hours sintering time. The result suggests that the 2223 phase can be obtained effectively by sintering with sufficiently long time

  7. Mineralogical analysis of clays in hardsetting soil horizons, by X-ray fluorescence and X-ray diffraction using Rietveld method

    Prandel, L.V.; Saab, S.C.; Brinatti, A.M.; Giarola, N.F.B.; Leite, W.C.; Cassaro, F.A.M.

    2014-01-01

    Diffraction and spectroscopic techniques have been shown to be suitable for obtaining physical and mineralogical properties in polycrystalline soil samples, and also in their precursor compounds. For instance, the X-ray fluorescence (XRF) spectroscopy allows obtaining the elemental composition of an investigated sample, while the X-ray diffraction (XRD) technique permits obtaining qualitative and quantitative composition of the soil minerals through the Rietveld method (RM). In this study Yellow Latosol (Oxisol), Yellow Argisol (Ultisol) and Gray Argisol (Ultisol) soil samples, classified as “hardsetting soils”, extracted from areas located at Northeast and Southeast of Brazilian coast were investigated. The soils and their fractions were analyzed in an EDX-700 and an XRD-6000 (Cu K α radiation). XRF results indicate high percentages of Si and Al, and small percentage of Fe and Ti in the investigated samples. The DRX data and RM indicate that there was a predominance of kaolinite and halloysite minerals (kaolin group minerals) in the clay fractions, which are presumably responsible for the formation of kaolinitic plasma in these soils. Also, the obtained results showed that the XRF, XRD techniques and RM were very helpful for investigating the mineralogical composition of a hardsetting soil. - Highlights: ► Elemental composition of soil samples through X-Ray fluorescence. ► Mineralogical quantification through X-ray diffraction and Rietveld method. ► Oxisol and Ultisol, Brazil ‘Barreiras’ formation. ► High amounts of Si and Al oxides and low amounts of Fe and Ti oxides. ► Predominance of kaolinite in the clay fraction

  8. Quantitative determination of phases in ZrO{sub 2} (MgO) (Y{sub 2}O{sub 3}) using the Rietveld method; Determinacao quantitativa de fases em ZrO{sub 2} - MgO - Y{sub 2}O{sub 3} utilizando o metodo de Rietveld

    Castro, Antonio Carlos de

    2007-07-01

    The key objective of this work is the crystallographic characterization of the zircon co-doped with Yttria and magnesium with the application of the Rietveld method for quantitative phase analysis of zircon polymorph (zircon monoclinic, tetragonal, and cubic). Samples of zircon polymorph were obtained from zircon doped with Yttria and magnesium at defined molar concentrations. The zircon polymorph stability during subeutetoid aging at 1350 deg C were investigated to determine ZrO{sub 2} - MgO - Y{sub 2}0{sub 3} phases degradation and to define the solid solutions stability environment. ZrO{sub 2} powders doped with 8 mol por cent of MgO and 1 mol por cent of Y{sub 2}O{sub 3}, and 9 mol por cent of MgO and 0 mol por cent of Y{sub 2}O{sub 3} have been prepared by chemical route using the co-precipitation method. These samples have been calcinate at 550 deg C, sintered at 1500 deg C and characterized by the Rietveld method using the X-ray diffraction data. The variation of the lattice parameter, changes in the phase composition and their microstructures are discussed. The application of the Rietveld method for quantitative phase analysis of zircon polymorph (zircon tetragonal and cubic) reveals no formation of tetragonal phase and indicating that the matrix is the cubic phase with low concentration of monoclinic phase.(author)

  9. The Rietveld method applied to the quantitative mineralogical analysis of some soil samples from Argentina Aplicación del método de Rietveld al análisis mineral��gico cuantitativo de algunas muestras de suelos de la Argentina

    Stella M Zabala

    2007-07-01

    Full Text Available The mineralogical quantification of soils species is mainly obtained by analysis of X-ray diffraction (XRD patterns. The classic method, for these analyses, is limited to semi quantitative determinations due to the overlapping of different specie's peaks and processes of absorption of the constituents, the wide range of particle size distribution, etc. The use of the Rietveld method for XRD quantitative analysis, in mixtures of minerals, has allowed to improve the accuracy of the quantitative results and to extend it to complex systems, as soils, transforming it in a meaningful tool for soils investigation. In this work, quantitative results obtained by the application of classic and Rietveld methods, are compared in different soils samples from Argentina. A set of mixtures of minerals with similar composition to three studied samples, was also quantified by Rietveld method, with absolute error lower than 3%. Obtained results indicate that quantitative analysis by Rietveld method, can improve the results found by XRD classic method and may be used for the quantitative determination of soil minerals.La cuantificación mineralógica de componentes del suelo es obtenida principalmente por análisis de espectros de difracción de rayos X (DRX. El método clásico aplicado para dicho análisis está limitado a determinaciones semi-cuantitativas debido a la superposición de picos de las distintas especies y procesos de absorción de los constituyentes, el amplio rango de distribución de tamaño de partícula, etc. El uso del método de Rietveld para el análisis cuantitativo por DRX, en mezclas de minerales, ha permitido mejorar la exactitud de los resultados cuantitativos y extenderlo a sistemas complejos, como lo son los suelos, transformándose en una herramienta significativa para su investigación. En este trabajo se comparan los resultados cuantitativos obtenidos por la aplicación del método clásico y de Rietveld, a diferentes muestras de

  10. Rietica - a visual Rietveld program

    Hunter, B.A.

    2000-01-01

    online help explains the fundamentals of the Rietveld method, the layout of the program, the input file structure, and the visual interface

  11. Rietveld analysis, powder diffraction and cement

    Peterson, V.

    2002-01-01

    Full text: Phase quantification of cement is essential in its industrial use, however many methods are inaccurate and/or time consuming. Powder diffraction is one of the more accurate techniques used for quantitative phase analysis of cement. There has been an increase in the use of Rietveld refinement and powder diffraction for the analysis and phase quantification of cement and its components in recent years. The complex nature of cement components, existence of solid solutions, polymorphic variation of phases and overlapping phase peaks in diffraction patterns makes phase quantification of cements by powder diffraction difficult. The main phase in cement is alite, a solid solution of tricalcium silicate. Tricalcium silicate has been found to exist in seven modifications in three crystal systems, including triclinic, monoclinic, and rhombohedral structures. Hence, phase quantification of cements using Rietveld methods usually involves the simultaneous modelling of several tricalcium silicate structures to fit the complex alite phase. An industry ordinary Portland cement, industry and standard clinker, and a synthetic tricalcium silicate were characterised using neutron, laboratory x-ray and synchrotron powder diffraction. Diffraction patterns were analysed using full-profile Rietveld refinement. This enabled comparison of x-ray, neutron and synchrotron data for phase quantification of the cement and examination of the tricalcium silicate. Excellent Rietveld fits were achieved, however the results showed that the quantitative phase analysis results differed for some phases in the same clinker sample between various data sources. This presentation will give a short introduction about cement components including polymorphism, followed by the presentation of some problems in phase quantification of cements and the role of Rietveld refinement in solving these problems. Copyright (2002) Australian X-ray Analytical Association Inc

  12. Structural determination of new solid solutions [Y2-x Mx ][Sn2-x Mx ]O7-3x/2 (M = Mg or Zn by Rietveld method

    Mohamed Douma

    2010-12-01

    Full Text Available New [Y2-x Mx][Sn2-x Mx]O7-3x/2 (0 ≤x≤ 0.30 for M = Mg and 0 ≤x≤ 0.36 for M = Zn solid solutions with the pyrochlore structure were synthesized via high-temperature solid-state reaction method. Powder X-ray diffraction (PXRD patterns and Fourier transform infrared (FT-IR spectra showed that these materials are new non-stoichiometric solid solutions with the pyrochlore type structure. The structural parameters for the solids obtained were successfully determined by Rietveld refinement based on the analysis of the PXRD diagrams. Lattice parameter (a of these solid solutions decreases when x increases in both series. All samples obtained have the pyrochlore structure Fd-3m, no. 227 (origin at center -3m with M2+ (M = Mg2+ or Zn2+ cations in Y3+ and Sn4+ sites, thus creating vacancies in the anionic sublattice.

  13. Measurements of Residual Stresses In Cold-Rolled 304 Stainless Steel Plates Using X-Ray Diffraction with Rietveld Refinement Method

    Parikin; Killen, P; Rafterry, A.

    2009-01-01

    The determination of the residual stresses using X-ray powder diffraction in a series of cold-rolled 304 stainless steel plates, deforming 0, 34, 84, 152, 158, 175 and 196 % reduction in thickness has been carried out. The diffraction data were analyzed using the Rietveld structure refinement method. The analysis shows that for all specimens, the martensite particles are closely in compression and the austenite matrix is in tension. Both the martensite and austenite, for a sample reducing 34% in thickness (containing of about 1% martensite phase) the average lattice strains are anisotropic and decrease approximately exponential with an increase in the corresponding percent reduction (essentially phase content). It is shown that this feature can be qualitatively understood by taking into consideration the thermal expansion mismatch between the martensite and austenite grains. Also, for all cold-rolled stainless steel specimens, the diffraction peaks are broader than the unrolled one (instrumental resolution), indicating that the strains in these specimens are inhomogeneous. From an analysis of the refined peak shape parameters, the average root-mean square strain, which describes the distribution of the inhomogeneous strain field, was predicted. The average residual stresses in cold-rolled 304 stainless steel plates showed a combination effect of hydrostatic stresses of the martensite particles and the austenite matrix. (author)

  14. X-ray diffraction analysis of stan nite, wurtz-stan nite and pseudo-cubic quaternary compounds by Rietveld method

    Quintero, M.; Quintero, E.; Moreno, E.; Alvarez, S.; Rincon, C.; Grima, P.; Bocaranda, P.; Rivero, D. [Universidad de Los Andes, Centro de Estudios de Semiconductores, 5101 Merida (Venezuela, Bolivarian Republic of); Marquina, J. [Universidad de Los Andes, Centro de Estudios Avanzados en Optica, 5101 Merida (Venezuela, Bolivarian Republic of); Henao, J. A.; Macias, M. A., E-mail: mquinterg@gmail.com [Universidad Industrial de Santander, Facultad de Ciencias, Escuela de Quimica, Grupo de Investigacion en Quimica Estructural, Apdo. Aereo 678, Bucaramanga (Colombia)

    2014-07-01

    Room temperature X-ray powder diffraction measurements were carried out on nine polycrystalline samples of the Cu{sub 2}B{sup II}C{sup IV}X{sub 4} (B=Mn, or Fe, or Co; C=Si, or Ge, or Sn; X=S, or Se or Te) magnetic semiconductor compounds. The diffraction patterns were used to show the equilibrium conditions and to derive crystalline parameters values. The results showed that four of these compounds have a tetragonal stan nite structure with space group 142 m(N{sup o} 121), two and orthorhombic wurtz-stan nite structure with space group Pmn2{sub 1}(N{sup o} 31) and three of them and orthorhombic pseudo-cubic structure with space group F222 (N{sup o} 22). In each case, the structure was refined using the Rietveld method. When the obtained atomic parameter values for the tetragonal compounds were plotted as a function of molecular weight W, it was found that the values of the atomic positions, the cation-anion bond distances, tetragonal distortion and internal distortion of the compounds containing S and /or Se lay on different lines. Also, it was found that when the experimental points of the cation-anion bond distances d{sub Cu-VI}, d{sub II-VI} and d{sub IV-VI} were plotted against the effective lattice parameter a{sub c} = (V/N){sup 1/3}, a linear variation of these distances with a{sub c} was obtained. Values of the ionic energy gap C{sub i} and homopolar energy gap E{sub h} using the Phillips-Van Vechten scheme, with the present experimental crystallographic results as well as using the atomic data, were determined. It was found that the observed and predicted values of C{sub i} and E{sub h} lie on the same straight line. (Author)

  15. Rietveld originals : Handle with care!

    Zijlstra, H.

    2009-01-01

    The work of architect Gerrit Th. Rietveld (1888 – 1964) is appreciated throughout the world. Many of the well-known buildings he designed have survived to the present. Some have been restored or refurbished, depending on the condition of the building, current needs of the building users, etc.

  16. A summary of available Rietveld and related software resources

    Cranswick, L.M.D

    1999-01-01

    Full text: There is a wide variety of Rietveld software available from both commercial and academic institutions. These resources will be reviewed along with the importance of validating Rietveld quantitative analysis results and gaining skills in complementary areas. This part of the workshop will mention a number of relevant programs and their main functionality: Rietveld software, Rietveld utilities, Rietveld friendly software and other powder diffraction utilities. Some of the main benefits of appreciating the availability of a wide range of software include: cross validation of results, data quality and diffractometer alignment, exploring new areas of research and analysis, solving new problems, nuances that occur as part of Rietveld analysis. Copyright (1999) Australian X-ray Analytical Association Inc

  17. Profile agreement indices in Rietveld and pattern-fitting analysis

    Hill, R.J.; Fischer, R.X.

    1990-01-01

    Two definitions of profile agreement indices are now in common use for estimating the degree of fit in Rietveld refinement and in structure-independent pattern-fitting methods of powder diffraction analysis. In the original program written by Rietveld, the background was subtracted and the 'non-peak' regions of the pattern were removed from further consideration in a preliminary data-reduction stage prior to structure refinement. However, the agreement indices used in many of the more recent programs retain the background counts in the observed step intensities and include all portions of the pattern in the sums. These latter definitions are strongly dependent on the signal-to-noise ratio and on the relative amount of 'background-only' regions and do not, therefore, provide a sound basis for comparing the degree of fit of peak profile and crystal structure model refinements in the general case. The extent of this dependence is illustrated quantitatively using conventional and synchrotron X-ray and constant-wavelength and time-of-flight neutron data sets with different inherent background levels and peak densities. The unweighted background-corrected peak-only profile agreement index R' p =Σ i vertical strokeY io -Y ic vertical stroke/Σ i vertical strokeY io -Y ib vertical stroke (and, to a lesser extent, its weighted equivalent) is recommended as the most appropriate criterion of fit for comparative work between diffraction patterns of all kinds. (orig.)

  18. Rietveld refinement with time-of-flight powder diffraction data from pulsed neutron sources

    David, W.I.F.; Jorgensen, J.D.

    1990-10-01

    The recent development of accelerator-based pulsed neutron sources has led to the widespread use of the time-of-flight technique for neutron powder diffraction. The properties of the pulsed source make possible unusually high resolution over a wide range of d spacings, high count rates, and the ability to collect complete data at fixed scattering angles. The peak shape and other instrument characteristics can be accurately modelled, which make Rietveld refinement possible for complex structures. In this paper we briefly review the development of the Rietveld method for time-of-flight diffraction data from pulsed neutron sources and discuss the latest developments in high resolution instrumentation and advanced Rietveld analysis methods. 50 refs., 12 figs., 14 tabs

  19. Quantitative phase analysis of a highly textured industrial sample using a Rietveld profile analysis

    Shin, Eunjoo; Huh, Moo-Young; Seong, Baek-Seok; Lee, Chang-Hee

    2001-01-01

    For the quantitative phase analysis on highly textured two-phase materials, samples with known weight fractions of zirconium and aluminum were prepared. Strong texture components prevailed in both zirconium and aluminum sheet. The diffraction patterns of samples were measured by the neutron and refined by the Rietveld method. The preferred orientation correction of diffraction patterns was carried out by means of recalculated pole figures from the ODF. The present Rietveld analysis of various samples with different weight fractions showed that the absolute error of the calculated weight fractions was less than 7.1%. (author)

  20. Mathematical aspects of Rietveld refinement and crystal structure ...

    Administrator

    The core mathematics, goodness-of-fit parameters of Rietveld refinement technique is introduced for structural ... transducers in medical and solar applications (Obmann ..... Prince 1985 in Structure and statistics in crystallography (ed.).

  1. Rietveld analysis and electronic bands structure on Tc superconductors systems

    Aldea, N.; Tiusan, C. V.; Sandu, V.

    1999-01-01

    A procedure for simultaneous refinement of structural and micro-structural disorder parameters for polycrystalline YBa 2 Cu 3 O 7-x system is proposed. It is based on Rietveld method combined with Fourier analysis for broadened peaks Another purpose of this paper consists in electronic structure determination studied by using the self-consistent Tight Binding Linear Muffin-Tin Orbital Atomic Spheres Approximation TB-LMTO-ASA methods. The Rietveld method uses an analytical function that describes the profiles, usually pseudo-Voigt (pV) or Pearson VII (PVII). The parameters of the analytical profiles describe its amplitude, position and peak shape. The full width at half maximum (FWHM) is supposed to vary with the diffraction angle in agreement with the Caglioti, Paoletti and Ricci's relationship. The best structural parameters are determined in the least squares sense by the minimisation a classical residual using the Marquardt method. In this case, the peak profiles were modelled by the pseudo-Voigt function corrected by the instrumental asymmetry. The physical information obtained are: scale factor, lattice parameters, atomic position and displacements, atomic occupation numbers, temperature factor (isotropy or anisotropy), preferred orientation parameter, crystalline size and micro-strain along different crystallographic directions, distributions of crystallite size and micro-strain functions. This procedure was implemented on computer code and it has a friendly graphical interface based on pull down menus technique. From the experimental point of view the X-ray diffraction data were collected using a horizontal powder diffractometer in the Bragg-Brentano (BB) geometry with a Ni filtered CuKα, λ = 1.54178 A, at room temperature using a DRON 2 set-up. The diffraction profiles were measured with a proportional gas detector, a single channel pulse-height discrimination and a standard associated counting circuit. The electronic band calculations are based on the TB

  2. Possibilities and limitations of parametric Rietveld refinement on high pressure data. The case study of LaFeO3

    Etter, Martin; Mueller, Melanie; Dinnebier, Robert E.; Hanfland, Michael

    2014-01-01

    Parametric Rietveld refinement is a powerful technique to apply directly physical or empirical equations to the refinement of in situ powder diffraction data. In order to investigate the possibilities and limitations of parametric Rietveld refinements for high pressure data four competitive crystallographic approaches were used to carry out a full structural investigation of the orthoferrite LaFeO 3 (Pbnm at ambient conditions) under high pressure up to 47 GPa. Approach A with traditional Rietveld refinement using atomic coordinates, Approach B where the Rietveld refinement was done by using the rigid body method, Approach C where symmetry modes were used and Approach D where the newly developed method of the rotational symmetry mode description for a rigid body was used. For all approaches sequential as well as parametric refinements were carried out, confirming a second order phase transition of LaFeO 3 to a higher symmetric phase (space group Ibmm) at around 21.1?GPa and an isostructural first order phase transition at around 38 GPa. Limitations due to non-hydrostatic conditions as well as the possibilities of a direct modeling of phase transitions with parametric Rietveld refinement are discussed in detail. (orig.)

  3. Characterization of barium titanate powder doped with sodium and potassium ions by using Rietveld refining

    Andrade, M.C.; Assis, J.T.; Pereira, F.R.

    2009-01-01

    A solid-reaction synthesis of doped barium titanate was done by employing barium carbonates, sodium, potassium and titanium oxides with classic procedures. Rietveld refining of X ray diffraction data of perovskite samples with tetragonal symmetry was applying and show good agreement. Besides, the treatment performed from 600 deg C produces nanocrystals of barium titanate with average size of 33 nm. The presence of endothermic peaks related to BaTiO 3 formation at relatively low temperatures was determined by thermal analysis. A pseudo-Voigt Thompson-Cox-Hastings function was used to fit the standard samples of barium titanate. The Rietveld method has showed be efficient to detect the influences of temperature and doping on barium titanate microstructures. (author)

  4. The IPNS rietveld analysis software package for TOF [time-of-flight] powder diffraction data: Recent developments

    Rotella, F.J.; Richardson, J.W. Jr.

    1987-01-01

    A system of FORTRAN programs for the analysis of time-of-flight (TOF) neutron powder diffraction data via the Rietveld method at IPNS has been modified recently, making it possible to analyze data that exhibit diffraction maxima broadened due to anisotropic strain and that can be modeled by individual atomic anharmonic thermal vibrations. The observation of noncrystalline scattering in data from some powder samples has led to the development of software to fit such scattering by a function related to a radial distribution function through Fourier-filtering techniques. The ''user friendliness'' of the IPNS Rietveld package has been enhanced by the development of ''RIETVELD,'' a menu-based VAX/VMS command language routine for interactive file manipulation and program execution

  5. Synthesis and characterization of NiO nanoparticles by Pechini method; Sintese e caracterizacao de nanoparticulas de NiO pelo metodo Pechini

    Nascimento, A; Ribeiro, M A; Costa, A C.F.M.; Gama, L [Universidade Federal de Campina Grande (UFCG), PB (Brazil). Dept. de Engenharia de Materiais; Bernardi, M I.B. [Universidade de Sao Paulo (IFSC/USP), Sao Carlos, SP (Brazil). Inst. de Fisica

    2009-07-01

    In recent years, ultrafine magnetic particles of NiO have attracting the attention because of its unknown behavior, enormous scientific potential and technological application. Some of its more important properties are accented magnetic moments, double dynamic exchange, quantization of wave of spin and etc. In this context, this work has for objective to synthesize and to characterize nanoparticles of NiO for the Pechini method. The powder was analyzed by X-rays diffraction. The results of scanning electron microscopy, adsorption of nitrogen. The analysis of X-rays diffraction of the sample showed single-phase peaks of NiO, with crystallite size close to 38 nm. The surface area was 6.44 m{sup 2}/g. The image from scanning electron microscopy shows soft homogeneous agglomerates. The Pechini synthesis was efficient in the production of powders of NiO nano metrics and single-phase. (author)

  6. Possibilities and limitations of parametric Rietveld refinement on high pressure data. The case study of LaFeO{sub 3}

    Etter, Martin; Mueller, Melanie; Dinnebier, Robert E. [Max-Planck-Institut fuer Festkoerperforschung, Stuttgart (Germany); Hanfland, Michael [European Synchrotron Radiation Facility (ESRF), Grenoble (France)

    2014-04-01

    Parametric Rietveld refinement is a powerful technique to apply directly physical or empirical equations to the refinement of in situ powder diffraction data. In order to investigate the possibilities and limitations of parametric Rietveld refinements for high pressure data four competitive crystallographic approaches were used to carry out a full structural investigation of the orthoferrite LaFeO{sub 3} (Pbnm at ambient conditions) under high pressure up to 47 GPa. Approach A with traditional Rietveld refinement using atomic coordinates, Approach B where the Rietveld refinement was done by using the rigid body method, Approach C where symmetry modes were used and Approach D where the newly developed method of the rotational symmetry mode description for a rigid body was used. For all approaches sequential as well as parametric refinements were carried out, confirming a second order phase transition of LaFeO{sub 3} to a higher symmetric phase (space group Ibmm) at around 21.1?GPa and an isostructural first order phase transition at around 38 GPa. Limitations due to non-hydrostatic conditions as well as the possibilities of a direct modeling of phase transitions with parametric Rietveld refinement are discussed in detail. (orig.)

  7. Structural and electrochemical characterization of calcium cobaltites (Ca{sub 3}Co{sub 4}O{sub 9}) obtained by the modified Pechini Method; Caracterizacao estrutural e eletroquimica de cobaltita de calcio (Ca{sub 3}Co{sub 4}O{sub 9}) obtida pelo Metodo Pechini modificado

    Silva, R.M.; Aquino, F. de M.; Macedo, D. A. de, E-mail: rinaldo_mendesa@hotmail.com [Universidade Federal da Paraiba (UFPB), Joao Pessoa, PB (Brazil)

    2016-07-01

    This work deals with the synthesis and characterization of calcium cobaltite (Ca{sub 3}Co{sub 4}O{sub 9}, C349), a p-type semiconductor with high Seebeck coefficient (S), high electrical conductivity and low thermal conductivity that has emerged as thermoelectric material. The synthesis method used to obtain the compound C349 uses commercial gelatin as complexing and polymerizing agent. The obtained material was characterized by X-ray diffraction with Rietveld refinement of the diffraction data. The results indicated that the modified Pechini method using gelatin allows to obtain powders of calcium cobaltite (with monoclinic structure) associated with a small content (2% by volume) of Co{sub 3}O{sub 4} with cubic structure. Impedance spectroscopy measurements in air indicated that the composite C349/Co{sub 3}O{sub 4} is a promising material for use as solid oxide fuel cell cathode.(author)

  8. Determination of phases of {alpha} - Fe{sub 2}O{sub 3}: SiO{sub 2} compound by the Rietveld refinement

    Palomares S, S.A. [Istituto Materiali Speciali per Elettronica e Magnetismo (MASPEC), Parco Area delle Scienze 37A-43010 Loc. Fontanni, Parma (Italy); Ponce C, S.; Martinez, J.R. [Facultad de Ciencias, Universidad Autonoma de San Luis Potosi, 78000 San Luis Potosi (Mexico); Ruiz, F. [Instituto Potosino de Investigacion Cientifica y Tecnologica, Av. V. Carranza 2025, San Luis Potosi (Mexico)

    2002-07-01

    We use a variation of the Rietveld refinement method to calculate the amorphous content of composites formed by a silica xerogel amorphous matrix and iron particles embedded into. In order to apply the Rietveld refinement to amorphous structures an initial crystalline model is assumed with the same composition as the material to be modelled. In this work we try to refine the structure of compounds using the program MAUD. It is shown how this program can be used to determine the amorphous and crystalline fractions in composites consisting of an amorphous matrix and incorporated iron oxide particles. The analysed compounds underwent different thermal treatments. (Author)

  9. Rietveld refinement and FTIR analysis of bulk ceramic Co3-xMnxO4 compositions

    Meena, P. L.; Kumar, Ravi; Sreenivas, K.

    2013-02-01

    Co3-xMnxO4 (x = 0.0, 0.6, 1.2) prepared by solid state reaction method and characterized by powder X-ray diffraction (XRD) and Fourier transform infrared (FTIR). Lattice parameters (a), oxygen parameter (u), and ionic radii of cations have been determined through Rietveld analysis. Both a and u parameters are related to expansion of octahedral site as Mn content in Co3O4. Analysis of XRD data show that Mn (x ≤ 1.2) is accommodated at the octahedral site, while retaining the cubic spinel structure. FTIR results also confirm the same and signify strong interactions due to overlapping of Co and Mn octahedra.

  10. Gerrit Rietveld. Casas después de la Schroeder

    Rafael García

    1997-07-01

    Full Text Available Las historias de la arquitectura moderna han incidido una y otra vez en un reducido número de obras que por su insistente atención, han llegado a convertirse en hitos imprescindibles. Entre estos edificios canónicos y prácticamente obligados, está la célebre casa Schröder-Schräder (1924' del arquitecto holandés Gerrit Rietveld. Ampliamente conocida por el público interesado, su gran popularidad ha tenido sin embargo, el efecto de dejar en segundo plano el resto de su obra arquitectónica. A ello se debe añadir además, el hecho de que su trayectoria está fundamentalmente asociada al movimiento neoplasticista, lo que ha tenido por resultado desviar la atención de una obra posterior, más difícilmente clasificable. Sin embargo, ello no significa que dicha obra sea en absoluto carente de atractivo.

  11. Magnesium substitution in carbonated hydroxyapatite: Structural and microstructural characterization by Rietveld's refinement

    Lala, S. [Materials Science Division, Department of Physics, The University of Burdwan, Golapbag, Burdwan 713104, West Bengal (India); Ghosh, M.; Das, P.K. [Department of Biological Chemistry, Indian Association for the Cultivation of Science, Jadavpur, Kolkata 700 032 (India); Das, D. [UGC-DAE Consortium for Scientific Research, Kolkata 700098 (India); Kar, T. [Department of Materials Science, Indian Association for the Cultivation of Science, Jadavpur, Kolkata 700032 (India); Pradhan, S.K., E-mail: skpradhan@phys.buruniv.ac.in [Materials Science Division, Department of Physics, The University of Burdwan, Golapbag, Burdwan 713104, West Bengal (India)

    2016-02-15

    Four stoichiometric compositions of nanocrystalline Mg doped carbonated hydroxyapatite (cHAp) powders are synthesized by mechanical alloying (ball milling) the powder mixtures of CaCO{sub 3}, CaHPO{sub 4}.2H{sub 2}O and MgO in open air at room temperature. FTIR analysis confirms the A-type carbonation in all milled HAp powder samples (A-cHAp). Microstructure characterization in terms of lattice imperfections and phase quantification of ball milled samples are made by analyzing XRD patterns employing Rietveld's structure refinement method. Transmission electron microscopy (TEM) study of 15 mol % Mg doped A-cHAp sample reveals microstructure similar to that obtained from XRD pattern analysis. Cumulative effect of Mg substitution and mechanical alloying results in amorphization of a major part of crystalline A-cHAp, analogous to native bone mineral. Rietveld analysis reveals that the Ca2 vacancy site is energetically more favorable for occupation of Mg substitution. MTT [3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide] assay test reveals sufficiently high percentage cell viability confirming the cytocompatibility of the sample. - Graphical abstract: Mg substitution for Ca2 site. - Highlights: • Single phase Mg doped A-cHAp synthesized by mechanical alloying (MA). • FTIR analysis confirms A-type carbonation in HAp. • Amorphization of a part of crystalline A-cHAp due to MA and Mg insertion. • Mg{sup 2+} ions substitute the Ca2 vacancy site. • High cell viability under MTT assay.

  12. Rietveld quantitative phase analysis of high surface area commercial alumina doped with niobia

    Gomes, L.B.; Pereira, A.S.; Pokorny, A.; Bergmann, C.P.

    2014-01-01

    The quantification of crystalline phases present in a given material can provide important information about the phenomena related to the diffusion of new elements in a ceramic matrix, as well as the formation and precipitation of minority phases and their microstructural evaluation. In this work, a high content of niobia (16 and 32 %w.t)was added to a high specific surface commercial alumina powder. The specimens were uniaxially pressed (200 MPa) and sintered in two stages: a first step at 1100°C for 3, 6 or 9 hours followed by a second step at 1350°C for 3 hours. The crystalline phases were analyzed by X-ray Diffraction (XRD) and quantified by the Rietveld method. The morphology of the samples was evaluated by Scanning Electron Microscopy (SEM). From the results obtained, some aluminum niobates phases expected for the Al_2O_3-Nb_2O_5 system could be identified as an intergranular phase and their relative fraction was quantified. (author)

  13. Method of semi-automatic high precision potentiometric titration for characterization of uranium compounds; Metodo de titulacao potenciometrica de alta precisao semi-automatizado para a caracterizacao de compostos de uranio

    Cristiano, Barbara Fernandes G.; Dias, Fabio C.; Barros, Pedro D. de; Araujo, Radier Mario S. de; Delgado, Jose Ubiratan; Silva, Jose Wanderley S. da, E-mail: barbara@ird.gov.b, E-mail: fabio@ird.gov.b, E-mail: pedrodio@ird.gov.b, E-mail: radier@ird.gov.b, E-mail: delgado@ird.gov.b, E-mail: wanderley@ird.gov.b [Instituto de Radioprotecao e Dosimetria (IRD/CNEN-RJ), Rio de Janeiro, RJ (Brazil); Lopes, Ricardo T., E-mail: ricardo@lin.ufrj.b [Universidade Federal do Rio de Janeiro (LIN/COPPE/UFRJ), RJ (Brazil). Coordenacao dos Programas de Pos-Graduacao de Engenharia. Lab. de Instrumentacao Nuclear

    2011-10-26

    The method of high precision potentiometric titration is widely used in the certification and characterization of uranium compounds. In order to reduce the analysis and diminish the influence if the annalist, a semi-automatic version of the method was developed at the safeguards laboratory of the CNEN-RJ, Brazil. The method was applied with traceability guaranteed by use of primary standard of potassium dichromate. The standard uncertainty combined in the determination of concentration of total uranium was of the order of 0.01%, which is better related to traditionally methods used by the nuclear installations which is of the order of 0.1%

  14. In-situ high-energy X-ray diffraction and batch Rietveld refinement of phase changes in titanium aluminides

    Whitfield, R.

    2007-01-01

    Full text: We have used the Rietveld refinement method for the analysis of high-energy X-ray power diffraction for quantitatve phase analysis. This method has the advantage of being able to model the multiple phases appearing in the diffraction pattern and tell us about the composition of the phases of a sample as we change the temperature. It has been applied to various TiAl compounds allowing us to follow in detail the phase transitions of the intermetallics when heated to around 1400 0 Cand subsequently cooled. Small amounts of additives like V, Cr and Gd as well as signatures from different production processes can be seen to have an effect on the phase transitions. With increasing temperature we can see the evolution of the unit cell due to thermal expansion, chemical segregation and the relative proportion of phase changes

  15. Combined PDF and Rietveld studies of ADORable zeolites and the disordered intermediate IPC-1P

    Morris, S. A.; Wheatley, P. S.; Položij, M.; Nachtigall, P.; Eliášová, Pavla; Čejka, Jiří; Lucas, T. C.; Hriljac, J. A.; Pinar, A. B.; Morris, R. E.

    2016-01-01

    Roč. 45, č. 36 (2016), s. 14124-14130 ISSN 1477-9226 R&D Projects: GA ČR GBP106/12/G015 Institutional support: RVO:61388955 Keywords : Distribution functions * Rietveld refinement * Zeolites Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 4.029, year: 2016

  16. National Nanotechnology Laboratory (LNNano) open facilities for scientific community: new methods for polymeric materials characterization; Instalacoes abertas a comunidade cientifica no Laboratorio Nacional de Nanotecnologia (LNNano): novos metodos de caracterizacao de materiais polimericos

    Silva, Cristiane A.; Santos, Ramon H.Z. dos; Bernardes, Juliana S.; Gouveia, Rubia F., E-mail: rubia.gouveia@lnnano.cnpem.br [Centro Nacional de Pesquisa em Energia e Materiais (LNNano/CNPEM), Campinas, SP (Brazil). Laboratorio Nacional de Nanotecnologia

    2015-07-01

    National Nanotechnology Laboratory (LNNano) at the National Center for Energy and Materials (CNPEM) presents open facilities for scientific public in some areas. In this work will be discussed the facilities for mainly the polymeric community, as well as new methods for the characterization. Low density polyethylene (LDPE) surfaces were characterized by X-ray microtomography and X-ray photoelectron spectroscopy (XPS). The results obtained by microtomography have shown that these surfaces present different contrasts when compared with the bulk. These differences are correlated with the formation of an oxidized layer at the polymer surface, which consequently have a greater X-ray attenuation. This hypothesis is confirmed by XPS, which shows LDPE surface layers are richer in carbonyl, carboxyl and vinyl groups than the bulk. This work presents that microtomography can be used as a new method for detection and characterization of polymer surface oxidation. (author)

  17. EL APARADOR DE RIETVELD DEL MUSEO NACIONAL DE ARTES DECORATIVAS (MADRID.

    María Villalba Salvador

    2012-01-01

    Full Text Available Este artículo trata de hacer una aproximación al estudio de una de las piezas más relevantes de la historia del diseño de mobiliario de vanguardia: el aparador de Rietveld, también conocido como Buffet Elling. Su diseño data de 1919, y responde a la estética propia del autor en aquellos años posteriores a la Primera Guerra Mundial, cuyas piezas son coincidentes con los planteamientos artísticos del grupo De Stijl. Es representativo de los principios básicos de la obra de Rietveld, uno de los pioneros del funcionalismo junto con J.J.P. Oud, en cuanto a la opción por el diseño y la arquitectura, y por la producción en masa y el diseño industrial accesible al conjunto de la sociedad. Merece destacar la colaboración de Gerard A. Van de Groenekan, asistente de Rietveld a lo largo de toda su trayectoria artística. Esta pieza nos ayuda a estudiar el pensamiento de Gerrit Th. Rietvel en relación con el diseño de vanguardia.This article tries to be an approach to the study of one of the most relevant pieces of furniture in the history of the design of avant-garde furniture: Rietveld´s dresser, also known as Elling Buffet. It was designed in 1919, and it shows the author´s aesthetics in the years that followed World War I, with pieces that are much related to the artistic orientation of the group De Stijl. It clearly shows the main characteristics of Rietveld´s work, one of the pioneers of functionalism, together with J.J.P. Oud, regarding design and architecture, mass production and industrial design accessible to society as a whole. It is worth mentioning the collaboration of Gerard A. Van de Groenekan, Rietveld´s assistant throughout his artistic trajectory. This piece of furniture helps us study Rietveld´s thinking regarding avant-garde design.

  18. Physical-mechanical characterization of hydroxyapatite-titanium oxide composites made by the polymeric sponge method; Caracterizacao fisico-mecanica de compositos porosos de hidroxiapatita-titania confeccionados pelo metodo da esponja polimerica

    Galdino, A.G.S.; Zavaglia, C.A.C. [Universidade Estadual de Campinas (FEM/UNICAMP), SP (Brazil)

    2011-07-01

    Bioceramics have been used as bone reconstruction materials since last decades, where hydroxyapatite is one of the most used for this purpose. However, hydroxyapatite's mechanical strength is not so high when compared to other bioceramics. This work aimed on characterizing physically and mechanically composites of HA-TiO{sub 2}. Samples were made by the polymeric sponge method with 70% - 30% wt., 60% - 40% wt. and 50% - 50% wt. of HA - TiO{sub 2}, calcined at 550 deg C for sponge burning and sintered at 1250 deg C, 1300 deg C and 1350 deg C. Samples were submitted to mechanical essays of compression and Hardness Vickers and to physical essays of water absorption, apparent density, burning linear retraction and apparent density. Results showed relatively better than those of pure hydroxyapatite and they are in accordance with the literature. (author)

  19. Development of methodology for characterization of cartridge filters from the IEA-R1 using the Monte Carlo method; Desenvolvimento de uma metodologia para caracterizacao do filtro cuno do reator IEA-R1 utilizando o Metodo Monte Carlo

    Costa, Priscila

    2014-07-01

    The Cuno filter is part of the water processing circuit of the IEA-R1 reactor and, when saturated, it is replaced and becomes a radioactive waste, which must be managed. In this work, the primary characterization of the Cuno filter of the IEA-R1 nuclear reactor at IPEN was carried out using gamma spectrometry associated with the Monte Carlo method. The gamma spectrometry was performed using a hyperpure germanium detector (HPGe). The germanium crystal represents the detection active volume of the HPGe detector, which has a region called dead layer or inactive layer. It has been reported in the literature a difference between the theoretical and experimental values when obtaining the efficiency curve of these detectors. In this study we used the MCNP-4C code to obtain the detector calibration efficiency for the geometry of the Cuno filter, and the influence of the dead layer and the effect of sum in cascade at the HPGe detector were studied. The correction of the dead layer values were made by varying the thickness and the radius of the germanium crystal. The detector has 75.83 cm{sup 3} of active volume of detection, according to information provided by the manufacturer. Nevertheless, the results showed that the actual value of active volume is less than the one specified, where the dead layer represents 16% of the total volume of the crystal. A Cuno filter analysis by gamma spectrometry has enabled identifying energy peaks. Using these peaks, three radionuclides were identified in the filter: {sup 108m}Ag, {sup 110m}Ag and {sup 60}Co. From the calibration efficiency obtained by the Monte Carlo method, the value of activity estimated for these radionuclides is in the order of MBq. (author)

  20. Study of ceramics from circular archaeological sites of Amazonic Basin by geochemical methods: dating and characterization; Estudo de ceramicas de sitios arqueologicos circulares da Bacia Amazonica por meio de metodos geoquimicos: datacao e caracterizacao

    Nicoli, Ieda Gomes

    2000-09-01

    The aim of this work is to examine by means of characterization and dating pottery recently discovery inside archaeological sites recognized with circular earth structure in Acre State - Brazil which may contribute to the research in the reconstruction of part of the pre-history of the Amazonic Basin. These sites are located mainly in the Hydrographic Basin of High Purus River. Three of them were strategic chosen which provide the ceramics: Lobao, in Sena Madureira County at north; Alto Alegre, in Rio Branco County at east and Xipamanu I, in Xapuri County at south. The X-ray diffraction mineral analysis made possible to identify two types of crystal structures of ceramic minerals: quartz and M-Kaolinite. Neutron activation analysis in conjunction with multivariate statistical methods were applied for the ceramic characterization and classification. An homogeneous group was established by all sherds collected from Alto Alegre and was distinct from all the other two groups analyzed. Some of the sherds collected from Xipamanu I appeared in Lobao's urns, probably because they had the same fabrication process. The Lobao's urns presented a homogeneous group. Geochronology of these materials was carried out by Thermoluminescence. The Xipamanu I was the oldest site and Lobao the youngest. The average age of Xipamanu I and Alto Alegre were 2600 and 2070 years respectively. The average age of of occupation was 400 years to Alto Alegre and 970 years to Xipamanu I. The most probably date for Lobao was 1880 years. (author)

  1. Study of ceramics from circular archaeological sites of Amazonic Basin by geochemical methods: dating and characterization; Estudo de ceramicas de sitios arqueologicos circulares da Bacia Amazonica por meio de metodos geoquimicos: datacao e caracterizacao

    Nicoli, Ieda Gomes

    2000-09-01

    The aim of this work is to examine by means of characterization and dating pottery recently discovery inside archaeological sites recognized with circular earth structure in Acre State - Brazil which may contribute to the research in the reconstruction of part of the pre-history of the Amazonic Basin. These sites are located mainly in the Hydrographic Basin of High Purus River. Three of them were strategic chosen which provide the ceramics: Lobao, in Sena Madureira County at north; Alto Alegre, in Rio Branco County at east and Xipamanu I, in Xapuri County at south. The X-ray diffraction mineral analysis made possible to identify two types of crystal structures of ceramic minerals: quartz and M-Kaolinite. Neutron activation analysis in conjunction with multivariate statistical methods were applied for the ceramic characterization and classification. An homogeneous group was established by all sherds collected from Alto Alegre and was distinct from all the other two groups analyzed. Some of the sherds collected from Xipamanu I appeared in Lobao's urns, probably because they had the same fabrication process. The Lobao's urns presented a homogeneous group. Geochronology of these materials was carried out by Thermoluminescence. The Xipamanu I was the oldest site and Lobao the youngest. The average age of Xipamanu I and Alto Alegre were 2600 and 2070 years respectively. The average age of of occupation was 400 years to Alto Alegre and 970 years to Xipamanu I. The most probably date for Lobao was 1880 years. (author)

  2. Micro-structural study and Rietveld analysis of fast reactor fuels: U–Mo fuels

    Chakraborty, S.; Choudhuri, G.; Banerjee, J.; Agarwal, Renu; Khan, K.B.; Kumar, Arun

    2015-01-01

    U–Mo alloys are the candidate fuels for both research reactors and fast breeder reactors. In-reactor performance of the fuel depends on the microstructural stability and thermal properties of the fuel. To improve the fuel performance, alloying elements viz. Zr, Mo, Nb, Ti and fissium are added in the fuel. The first reactor fuels are normally prepared by injection casting. The objective of this work is to compare microstructure, phase-fields and hardness of as-cast four different U–Mo alloy (2, 5, 10 and 33 at.% Mo) fuels with the equilibrium microstructure of the alloys. Scanning electron microscope with energy dispersive spectrometer and optical microscope have been used to characterize the morphology of the as-cast and annealed alloys. The monoclinic α'' phase in as-cast U-10 at.% Mo alloy has been characterized through Rietveld analysis. A comparison of metallographic and Rietveld analysis of as-cast (dendritic microstructure) and annealed U-33 at.% Mo alloy, corresponding to intermetallic compound, has been reported here for the first time. This study will provide in depth understanding of microstructural and phase evolution of U–Mo alloys as fast reactor fuel. - Highlights: • U–Mo alloys in as-cast as well as in annealed conditions have been studied using Optical Microscope, SEM, XRD. • The monoclinic α'' phase in as-cast U-10 at.% Mo alloy has been characterized through Rietveld analysis. • The dendritic microstructure of γ-(U,Mo) and B.C.C. ‘Mo’ phase of 33 at.% U–Mo alloy have been analysed. • Rietveld analysis has been done to optimize lattice parameters and calculate phase fractions in annealed alloys. • The Vickers microhardness of U_2Mo phase shows lower hardness than two phase microstructures in annealed alloys.

  3. Micro-structural study and Rietveld analysis of fast reactor fuels: U–Mo fuels

    Chakraborty, S., E-mail: sibasis@barc.gov.in [Radiometallurgy Division, Bhabha Atomic Research Centre, Mumbai, 400085 (India); Choudhuri, G. [Atomic Fuels Division, Bhabha Atomic Research Centre, Mumbai, 400085 (India); Banerjee, J. [Radiometallurgy Division, Bhabha Atomic Research Centre, Mumbai, 400085 (India); Agarwal, Renu [Product Development Division, Bhabha Atomic Research Centre, Mumbai, 400085 (India); Khan, K.B.; Kumar, Arun [Radiometallurgy Division, Bhabha Atomic Research Centre, Mumbai, 400085 (India)

    2015-12-15

    U–Mo alloys are the candidate fuels for both research reactors and fast breeder reactors. In-reactor performance of the fuel depends on the microstructural stability and thermal properties of the fuel. To improve the fuel performance, alloying elements viz. Zr, Mo, Nb, Ti and fissium are added in the fuel. The first reactor fuels are normally prepared by injection casting. The objective of this work is to compare microstructure, phase-fields and hardness of as-cast four different U–Mo alloy (2, 5, 10 and 33 at.% Mo) fuels with the equilibrium microstructure of the alloys. Scanning electron microscope with energy dispersive spectrometer and optical microscope have been used to characterize the morphology of the as-cast and annealed alloys. The monoclinic α'' phase in as-cast U-10 at.% Mo alloy has been characterized through Rietveld analysis. A comparison of metallographic and Rietveld analysis of as-cast (dendritic microstructure) and annealed U-33 at.% Mo alloy, corresponding to intermetallic compound, has been reported here for the first time. This study will provide in depth understanding of microstructural and phase evolution of U–Mo alloys as fast reactor fuel. - Highlights: • U–Mo alloys in as-cast as well as in annealed conditions have been studied using Optical Microscope, SEM, XRD. • The monoclinic α'' phase in as-cast U-10 at.% Mo alloy has been characterized through Rietveld analysis. • The dendritic microstructure of γ-(U,Mo) and B.C.C. ‘Mo’ phase of 33 at.% U–Mo alloy have been analysed. • Rietveld analysis has been done to optimize lattice parameters and calculate phase fractions in annealed alloys. • The Vickers microhardness of U{sub 2}Mo phase shows lower hardness than two phase microstructures in annealed alloys.

  4. Profex: a graphical user interface for the Rietveld refinement program BGMN

    Doebelin, Nicola; Kleeberg, Reinhard

    2015-01-01

    Profex is a graphical user interface for the Rietveld refinement program BGMN. Its interface focuses on preserving BGMN’s powerful and flexible scripting features by giving direct access to BGMN input files. Very efficient workflows for single or batch refinements are achieved by managing refinement control files and structure files, by providing dialogues and shortcuts for many operations, by performing operations in the background, and by providing import filters for CIF and XML crystal str...

  5. Modulation wave approach to the structural parameterization and Rietveld refinement of low carnegieite

    Withers, R.L.; Thompson, J.G.

    1993-01-01

    The crystal structure of low carnegieite, NaAlSiO 4 [M r =142.05, orthorhombic, Pb2 1 a, a=10.261(1), b=14.030(2), c=5.1566(6) A, D x =2.542 g cm -3 , Z=4, Cu Kα 1 , λ=1.5406 A, μ=77.52 cm -1 , F(000)=559.85], is determined via Rietveld refinement from powder data, R p =0.057, R wp =0.076, R Bragg =0.050. Given that there are far too many parameters to be determined via unconstrained Rietveld refinement, a group theoretical or modulation wave approach is used in order to parameterize the structural deviation of low carnegieite from its underlying C9 aristotype. Appropriate crystal chemical constraints are applied in order to provide two distinct plausible starting models for the structure of the aluminosilicate framework. The correct starting model for the aluminosilicate framework as well as the ordering and positions of the non-framework Na atoms are then determined via Rietveld refinement. At all stages, chemical plausibility is checked via the use of the bond-length-bond-valence formalism. The JCPDS file number for low carnegieite is 44-1496. (orig.)

  6. Dos artículos de Rietveld Comprensión. Nuevo Funcionalismo en la Arquitectura

    Editor Cuaderno de Notas

    1995-12-01

    Full Text Available Los siguientes dos artículos de Rietveld (1888-1964 fueron publicados por primera vez en la revista i10 en 1928 y en De Vrije Bladen en 1932 respectivamente. Esta es su primera traducción al castellano, para lo que se ha partido de sus correspondientes traducciones inglesas; "Inzicht" (comprensión, en el libro de Theodore M.. Brown, The Work of G. Rietveld architect, Utrecht 1958, y "Nieuwe zakelijkheid in de Nederlandsche architectuur" (Nueva objetividad en la arquitectura holandesa, en la monografía-catálogo, Gerrit Rietveld 1888-1964. The complet works, Central Museum, Utrecht, 1992. En cuanto al último, de bastante mayor extensión, contaba originariamente con ilustraciones de obras de JA.Brinkman y L.C. van der Vlugt, A. Bodón, J. Duiker, J.J.P. Oud y Le Corbusier como único arquitecto extranjero representado, aparte de las de sus propio trabajo.

  7. Study of selection and purification of Brazilian bentonite clay by elutriation: a XRF, SEM and Rietveld analysis

    Alves, J.L.; Zanini, A.E.; Souza, M.E. de; Nascimento, M.L.F., E-mail: jeff_eq@yahoo.com.br, E-mail: mlfn@ufba.br [Universidade Federal da Bahia (UFBA/PROTEC/PEI), Salvador, BA (Brazil). Departamento de Engenharia Quimica

    2016-01-15

    Clays obtained from nature have a lot of impurities. Therefore, for best using of these materials, it is necessary its selection and purification. Thus, the aim of this work is to separate and to purify the smectite fractions using water as a solvent at a low flux mixed with a bentonite clay extracted from a mine in Vitoria da Conquista - Bahia / Brazil. For this a separation method of fractions of expandable clays based on the Stokes' Law was applied - this process is called elutriation, in order to ensure and to expand possible industrial applications of this material. The samples were characterized by analysis of X-ray diffraction, X-ray fluorescence and scanning electron microscopy. The Rietveld method enabled the quantification of main phase minerals: montmorillonite, kaolinite, nontronite and quartz, reaching 85% in mass of montmorillonite phase at the end of the process. Results showed that the method used was efficient to remove almost all quartz, carbonates and organic matter from the sample. It was also observed a monomodal grain size distribution of elutriated materials with thinner grains, around (18.1 ± 1.8) μm at the end of the process. It has been concluded that the method developed and applied showed promising characters to be applied to elutriate kilograms of clays and could be used in industrial scale. (author)

  8. Study of selection and purification of Brazilian bentonite clay by elutriation: a XRF, SEM and Rietveld analysis

    J. L. Alves

    2016-03-01

    Full Text Available Abstract Clays obtained from nature have a lot of impurities. Therefore, for best using of these materials, it is necessary its selection and purification. Thus, the aim of this work is to separate and to purify the smectite fractions using water as a solvent at a low flux mixed with a bentonite clay extracted from a mine in Vitória da Conquista - Bahia / Brazil. For this a separation method of fractions of expandable clays based on the Stokes' Law was applied - this process is called elutriation, in order to ensure and to expand possible industrial applications of this material. The samples were characterized by analysis of X-ray diffraction, X-ray fluorescence and scanning electron microscopy. The Rietveld method enabled the quantification of main phase minerals: montmorillonite, kaolinite, nontronite and quartz, reaching 85% in mass of montmorillonite phase at the end of the process. Results showed that the method used was efficient to remove almost all quartz, carbonates and organic matter from the sample. It was also observed a monomodal grain size distribution of elutriated materials with thinner grains, around (18.1 ± 1.8 μm at the end of the process. It has been concluded that the method developed and applied showed promising characters to be applied to elutriate kilograms of clays and could be used in industrial scale.

  9. Study of selection and purification of Brazilian bentonite clay by elutriation: a XRF, SEM and Rietveld analysis

    Alves, J.L.; Zanini, A.E.; Souza, M.E. de; Nascimento, M.L.F.

    2016-01-01

    Clays obtained from nature have a lot of impurities. Therefore, for best using of these materials, it is necessary its selection and purification. Thus, the aim of this work is to separate and to purify the smectite fractions using water as a solvent at a low flux mixed with a bentonite clay extracted from a mine in Vitoria da Conquista - Bahia / Brazil. For this a separation method of fractions of expandable clays based on the Stokes' Law was applied - this process is called elutriation, in order to ensure and to expand possible industrial applications of this material. The samples were characterized by analysis of X-ray diffraction, X-ray fluorescence and scanning electron microscopy. The Rietveld method enabled the quantification of main phase minerals: montmorillonite, kaolinite, nontronite and quartz, reaching 85% in mass of montmorillonite phase at the end of the process. Results showed that the method used was efficient to remove almost all quartz, carbonates and organic matter from the sample. It was also observed a monomodal grain size distribution of elutriated materials with thinner grains, around (18.1 ± 1.8) μm at the end of the process. It has been concluded that the method developed and applied showed promising characters to be applied to elutriate kilograms of clays and could be used in industrial scale. (author)

  10. Micro-structural study and Rietveld analysis of fast reactor fuels: U-Mo fuels

    Chakraborty, S.; Choudhuri, G.; Banerjee, J.; Agarwal, Renu; Khan, K. B.; Kumar, Arun

    2015-12-01

    U-Mo alloys are the candidate fuels for both research reactors and fast breeder reactors. In-reactor performance of the fuel depends on the microstructural stability and thermal properties of the fuel. To improve the fuel performance, alloying elements viz. Zr, Mo, Nb, Ti and fissium are added in the fuel. The first reactor fuels are normally prepared by injection casting. The objective of this work is to compare microstructure, phase-fields and hardness of as-cast four different U-Mo alloy (2, 5, 10 and 33 at.% Mo) fuels with the equilibrium microstructure of the alloys. Scanning electron microscope with energy dispersive spectrometer and optical microscope have been used to characterize the morphology of the as-cast and annealed alloys. The monoclinic α'' phase in as-cast U-10 at.% Mo alloy has been characterized through Rietveld analysis. A comparison of metallographic and Rietveld analysis of as-cast (dendritic microstructure) and annealed U-33 at.% Mo alloy, corresponding to intermetallic compound, has been reported here for the first time. This study will provide in depth understanding of microstructural and phase evolution of U-Mo alloys as fast reactor fuel.

  11. Rietveld refinement of magnetic structures from pulsed-neutron-source powder-diffraction data

    Robinson, R.A.; Lawson, A.C.; Larson, A.C.; Von Dreele, R.B.; Goldstone, J.A.

    1994-01-01

    The General Structure Analysis System, GSAS, has recently been modified to include magnetic neutron- scattering cross-sections. Low-temperature diffraction data have been taken on the hexagonal noncollinear antiferromagnet UPdSn on both the HIPD and the NPD powder diffractometers ail LANSCE. The low-resolution data reveal that the magnetic structure has orthorhombic symmetry (magnetic space group P c m'c2 1 ) between 25K and 40K, and monoclinic symmetry (magnetic space group PC 1121 ) below 25K. The high-resolution data reveal that there are structural distortions with corresponding symmetry changes in each of these phases, to give chemical space groups Cmc2 1 and P2 1 , respectively, while the paramagnetic phase above 40K has space group P6 3 mc. Using GSAS, we have refined data sets from both diffractometers simultaneously, including both magnetic and structural cross-sections. Magnetoelastic coefficients for the distortions have been extracted and we have determined the sign of the coupling between the structural monoclinicity and the magnetic monoclinicity. The magnetic results from Rietveld refinement are in good agreement with model fitting to the integrated intensities of seven independent magnetic reflections and these, in turn, agree with measurements made on the same sample using the constant-wavelength reactor technique. Our results therefore validate, to some level, both the technique of using spallation sources for complicated magnetic structures and the specifics of the GSAS Rietveld code

  12. Rietveld refinement and electronic structure studies for the Sm2FeMnO6 new complex perovskite

    Landinez Tellez, D.A.; Munevar, J.A.; Arbey Rodriguez, J.M.; Fajardo, F.; Roa-Rojas, J.

    2008-01-01

    We report synthesis and crystalline structure study of the Sm 2 FeMnO 6 new complex perovskite, by X-ray diffraction experiments and through the application of Rietveld refinement. Results revealed the crystallization of system in a structure given by Pmn21 (no. 31) space group and lattice parameters a=7.621(1) A, b=5.675(3) A and c=5.378(3) A. Ab initio calculations of density of states (DOS) and electronic structure were carried out for this perovskite-like system by the density functional theory (DFT) and using the full-potential linearized augmented plane waves (FP-LAPW) method. All calculations were carried out using spin polarization. Material evidences a conductor-like character, predominantly due to d-xy Fe orbital of the spin down channel. Magnetic response of system has contributions of Fe and Mn spin up orientation. The calculated magnetic moment in cell was 34.48 μ B and the magnetic moment in interstitial was 1.54 μ B

  13. Determination of Cation Distributions in Mineral Structures by use of the Rietveld Full-Profile Refinement Technique

    Nord, A.G.

    1986-01-01

    Use of the Rietveld full-profile refinement technique with X-ray or neutron powder diffraction data for the determination of divalent-metal cation distributions in three mineral structure types (farringtonite, grafonite, sarcopside) is demonstrated. The accuracy of the conventional cation distribution coefficient Ksub(D) is about 5-10 percent with 24-46 parameters to be refined, and the averaged metal-oxygen distances are reliable and well correlated to the observed cation distribution pattern. In particular the usefulness of the Rietveld technique in combination with Moessbauer spectroscopy is stressed. Some concluding remarks are also given

  14. Analysis of the zirconia structure by `ab initio` and Rietveld methods; Analise da estrutura da zirconia por metodos `Ab initio` e de Rietveld

    Bechepeche, A.P.; Nasar, R.S.; Longo, E. [Sao Carlos Univ., SP (Brazil). Dept. de Quimica; Treu Junior, O.; Varela, J.A. [UNESP, Araraquara, SP (Brazil). Inst. de Quimica

    1995-12-31

    The zirconia was doped with 0,113 mol of Mg O e 0,005 mol of Ti O{sub 2}, and it was calcined in 1550{sup d}eg C and it was analyzed by XRD. The results shows that pure zirconia contains 96,19% of monoclinic phase and 3,18% of cubic. However, the doping magnesia stabilizes the zirconia in 17,24 of monoclinic; 29,63 of tetragonal and 53,13% of cubic phase. The addition of titanium in zirconia gives 25,85% of tetragonal phase and 37,66% of cubic, and this shows the no stabilizing action of this transition metal. By the other side, the results with ab-initio calculating shows the same tendency resulting in the next values of total energy: pure zirconia - monoclinic -11.316,86ua; tetragonal -8742,09 ua and cubic -8742,80 ua and Zr O{sub 2} Ti O{sub 2} system - monoclinic -9463,02 ua, tetragonal -9459,39 ua and cubic -9459,97 ua (author) 3 figs., 2 tabs.

  15. Profex: a graphical user interface for the Rietveld refinement program BGMN.

    Doebelin, Nicola; Kleeberg, Reinhard

    2015-10-01

    Profex is a graphical user interface for the Rietveld refinement program BGMN . Its interface focuses on preserving BGMN 's powerful and flexible scripting features by giving direct access to BGMN input files. Very efficient workflows for single or batch refinements are achieved by managing refinement control files and structure files, by providing dialogues and shortcuts for many operations, by performing operations in the background, and by providing import filters for CIF and XML crystal structure files. Refinement results can be easily exported for further processing. State-of-the-art graphical export of diffraction patterns to pixel and vector graphics formats allows the creation of publication-quality graphs with minimum effort. Profex reads and converts a variety of proprietary raw data formats and is thus largely instrument independent. Profex and BGMN are available under an open-source license for Windows, Linux and OS X operating systems.

  16. Rietveld refinement of Y2O3 using the pearson VII profile shape function

    Smrcok, L.

    1989-01-01

    Very good agreement between the observed and the calculated intensities was obtained using the Pearson VII profile shape function. The variable exponent m could be refined only in the damped iterations involving exclusively the profile parameters. Simultaneous refinement of the m with the positional and/or thermal parameters has led to large oscillations of the shifts of almost all parameters. Precision of the refined atomic coordinates is better than those from previously published Rietveld refinement and is comparable with single crystal results. The degree of serial correlation in residuals has been determined by the use of the Durbin-Watson d statistic. Normal probability plot based on δR i has been almost linear with the slope greater than one. The weighting scheme with w i = 1/y oi has proved to be good first approximation. (author)

  17. Application of low current intensity electrolytic treatment for the chlorides extraction in underwater archaeological objects of iron. Observation of the mineralogical phases evolution through XRD-Rietveld

    Bethencourt, M.; Gil, M. L. A.; Fernandez-Lorenzo, C.; Santos, A.

    2004-01-01

    With the purpose of optimising a suitable methodology for the conservation of an archaeological object of iron, a low current intensities electrolytic treatment has been applied, to a piece of cast iron, proving to be effective in the extraction of chloride ions from the structure of akaganeite, principal corrosion product of iron in the marine medium. The monitoring of the electrolytic treatment has been proven by applying the Rietveld method to the patterns XRD of samples extracted from the corroded surface before and after the treatment. This method has permitted the unequivocal determination of the akaganeite and its chemical composition. This identification has been corroborated by means of SEM and EDS. After the electrolytic treatment, akaganeite was not present in the sample. (Author) 9 refs

  18. Analysis of the zirconia structure by 'ab initio' and Rietveld methods

    Bechepeche, A.P.; Nasar, R.S.; Longo, E.; Treu Junior, O.; Varela, J.A.

    1995-01-01

    The zirconia was doped with 0,113 mol of Mg O e 0,005 mol of Ti O 2 , and it was calcined in 1550 d eg C and it was analyzed by XRD. The results shows that pure zirconia contains 96,19% of monoclinic phase and 3,18% of cubic. However, the doping magnesia stabilizes the zirconia in 17,24 of monoclinic; 29,63 of tetragonal and 53,13% of cubic phase. The addition of titanium in zirconia gives 25,85% of tetragonal phase and 37,66% of cubic, and this shows the no stabilizing action of this transition metal. By the other side, the results with ab-initio calculating shows the same tendency resulting in the next values of total energy: pure zirconia - monoclinic -11.316,86ua; tetragonal -8742,09 ua and cubic -8742,80 ua and Zr O 2 Ti O 2 system - monoclinic -9463,02 ua, tetragonal -9459,39 ua and cubic -9459,97 ua (author)

  19. Rietveld structure refinement and elastic properties of MgAlxCrxFe2-2xO4 spinel ferrites

    Thummer, K. P.; Tanna, Ashish R.; Joshi, Hiren H.

    2017-05-01

    MgAlxCrxFe2-2xO4 (x = 0.1, 03 & 0.6) ferrites are synthesized by solid state reaction method. The Rietveld refinement of X-ray diffraction (XRD) data confirms the cubic spinel structure with Fd3m space group. The Fourier Transform Infrared Transmission Spectroscopy (FTIR) is employed to study elastic properties of present systems at 300K. The force constants for tetrahedral (A) and octahedral (B) sites of the spinel lattice are determined by infrared spectral and X-ray diffraction analysis. The elastic constants like bulk modulus, rigidity modulus, Young's modulus, Poisson's ratio and Debye temperature are determined. The vibrational frequency of both the interstitial sites increases as Al-Cr content increases hence the force constant and elastic moduli for all the samples are found to increase for the present ferrite system.

  20. Analysis of Polymorphic Nanocrystals of TiO2 by X-Ray Rietveld Refinement and High-Resolution Transmission Electron Microscopy: Acetaldehyde Decomposition

    R. Carrera

    2008-01-01

    Full Text Available In this work, TiO2 nanocrystals were synthesized by the sol-gel method. These materials were annealed at 200 and 500∘C; and characterized by the XRD-Rietveld refinement; and by BET and TEM. As for the low-temperature-treated sample (200∘C, nanocrystals with small crystallite sizes (7 nm and high abundance of anatase, coexisting with the brookite phase, were obtained. Meanwhile, the sample annealed at 500∘C showed an increased crystallite size (22 nm and an important polymorphic increment. The sample annealed at 200∘C showed a high activity in the photocatalytic decomposition of acetaldehyde.

  1. Rietveld refinement, dielectric and magnetic properties of Nb modified Bi0.80Ba0.20FeO3 ceramic

    Jangra, Sandhaya; Sanghi, Sujata; Agarwal, Ashish; Rangi, Manisha

    2018-05-01

    Bi0.80Ba0.20Fe0.95Nb0.05O3 ceramic has been prepared via conventional solid state reaction method. Structure analysis was carried out by X-ray diffraction (XRD) technique at room temperature. XRD pattern confirmed the crystalline nature of prepared sample. Rietveld analysis used for further structural investigations and confirmed the existence of rhombohedral symmetry (R3c space group). The dielectric response shows dispersion at lower frequency range and becomes frequency independent at high frequency. The approximation of conduction mechanism is determined by the temperature dependent behavior of frequency exponent `s'. Fitting results suggests the applicability of small polaron conduction mechanism at lower temperatures and CBH model at higher temperature. Room temperature magnetic measurements give the evidence of significant enhancement in magnetic properties with remanent magnetization (Mr = 0.1218 emu/g) and coercive field (Hc = 3.5342 kOe).

  2. Rietveld refinement of the crystal structures of Rb2XSi5O12 (X = Ni, Mn

    Anthony M. T. Bell

    2016-02-01

    Full Text Available The synthetic leucite silicate framework mineral analogues Rb2XSi5O12 {X = Ni [dirubidium nickel(II pentasilicate] and Mn [dirubidium manganese(II pentasilicate]} have been prepared by high-temperature solid-state synthesis. The results of Rietveld refinements, using X-ray powder diffraction data collected using Cu Kα X-rays, show that the title compounds crystallize in the space group Pbca and adopt the cation-ordered structure of Cs2CdSi5O12 and other leucites. The structures consist of tetrahedral SiO4 and XO4 units sharing corners to form a partially substituted silicate framework. Extraframework Rb+ cations sit in channels in the framework. All atoms occupy the 8c general position for this space group. In these refined structures, silicon and X atoms are ordered onto separate tetrahedrally coordinated sites (T-sites. However, the Ni displacement parameter and the Ni—O bond lengths suggest that for the X = Ni sample, there may actually be some T-site cation disorder.

  3. Neutron irradiated uranium silicides studied by neutron diffraction and Rietveld analysis

    Birtcher, R.C.; Mueller, M.H.; Richardson, J.W. Jr.; Faber, J. Jr.

    1989-11-01

    Uranium silicides have been considered for use as reactor fuels in both high power and low enrichment applications. However, U 3 Si was found to become amorphous under irradiation and to become mechanically unstable to rapid growth by plastic flow. U 2 Si 2 appears to be stable against amorphization at low displacement rates, but the extent of this stability is uncertain. Although the mechanisms responsible for plastic flow in U 3 Si and other amorphous systems are unknown, as is the importance of crystal structure for amorphization, it may not be surprising that these materials amorphize, in light of the fact that many radioactive nuclide - containing minerals are known to metaminctize (lose crystallinity) under irradiation. The present experiment follows the detailed changes in the crystal structures of U 3 Si and U 3 Si 2 introduced by neutron bombardment and subsequent uranium fission at room temperature. U-Si seems the ideal system for a neutron diffraction investigation since the crystallographic and amorphous forms can be studied simultaneously by combining conventional Rietveld refinement of the crystallographic phases with Fourier-filtering of the non-crystalline scattering component

  4. The role of iron in tetrahedrite and tennantite determined by Rietveld refinement of neutron powder diffraction data

    Andreasen, Jens Wenzel; Makovicky, Emil; Lebech, Bente

    2008-01-01

    Rietveld refinement of neutron powder diffraction data on four samples of synthetic, iron-bearing tetrahedrite (Cu12-xFexSb4S13) with x = 0.28, 0.69, 0.91, 2.19 and four samples of synthetic tennantite (Cu12-xFexAs4S13) with x = 0.33, 0.38, 0.86, 1.5 indicate unambiguously that iron is incorporated...

  5. Rietveld refinement of the structures of 1.0 C-S-H and 1.5 C-S-H

    Battocchio, Francesco; Monteiro, Paulo J.M.; Wenk, Hans-Rudolf

    2012-01-01

    Low-Q region Rietveld analyses were performed on C-S-H synchrotron XRD patterns, using the software MAUD. Two different crystal structures of tobermorite 11 Å were used as a starting model: monoclinic ordered Merlino tobermorite, and orthorhombic

  6. Crystal structure refinement of Ba5Nb4O15 and Ba5Nb4O15-x by Rietveld analysis of neutron and X-ray diffraction data

    Pagola, S.; Leyva, G.; Casais, M.T.; Alonso, J.A.; Rasines, I.; Carbonio, R.E.

    1996-01-01

    Both X-ray and neutron diffraction data were analyzed by the Rietveld method, taking as starting structural model that of the Ba 5 Ta 4 O 15 structure. The results of such an analysis show that the progressive elimination of oxygen ions produce only small changes in the structure. A decrease in the unit-cell parameters as the number of oxygen vacancies increases has been observed, which can be correlated with a gradual loss of oxygen ions in the close-packed layers. No ordering of the oxygen vacancies was found even in the sample with the highest x value, x=0.56. (orig.)

  7. Effect of powder sample granularity on fluorescent intensity and on thermal parameters in x-ray diffraction Rietveld analysis

    Sparks, C.J.; Specht, E.D.; Ice, G.E.; Kumar, R.; Zschack, P.; Shiraishi, T.; Hisatsune, K.

    1991-01-01

    The effect of sample granularity on diffracted x-ray intensity was evaluated by measuring the 2θ dependence of x-ray fluorescence from various samples. Measurements were made in the symmetric geometry on samples ranging from single crystals to highly absorbing coarse powders. A characteristic shape for the absorption correction was observed. A demonstration of the sensitivity of Rietveld refined site occupation parameters is made on CuAu and Cu 50 Au 44 Ni 6 alloys refined with and without granularity corrections. These alloys provide a good example of the effect of granularity due to their large linear x-ray absorption coefficients. Sample granularity and refined thermal parameters obtained from the Rietveld analysis were found to be correlated. Without a granularity correction, the refined thermal parameters are too low and can actually become negative in an attempt to compensate for granularity. A general shape for granularity correction can be included in refinement procedures. If no granularity correction is included, data should be restricted to above 30 degrees 2θ, and thermal parameters should be ignored unless extreme precautions are taken to produce >5 μm particles and high packing densities

  8. Synthesis and structural characterisation using Rietveld and pair distribution function analysis of layered mixed titanium-zirconium phosphates

    Burnell, Victoria A.; Readman, Jennifer E.; Tang, Chiu C.; Parker, Julia E.; Thompson, Stephen P.; Hriljac, Joseph A.

    2010-01-01

    Crystalline metal (IV) phosphates with variable zirconium-to-titanium molar ratios of general formula (Ti 1-x Zr x )(HPO 4 ) 2 .H 2 O have been prepared by precipitation of soluble salts of the metals with phosphoric acid and heating the amorphous solids in 12 M H 3 PO 4 in an autoclave. The new materials are structurally characterised by Rietveld analysis of synchrotron X-ray powder diffraction data and pair distribution function (PDF) analysis of high energy synchrotron X-ray total scattering data. A broad range of zirconium-titanium phosphate solid solutions were formed showing isomorphous substitution of titanium by zirconium in the α-titanium phosphate lattice and vice versa for titanium substitution into the α-zirconium phosphate lattice. In both cases the solubility is partial with the coexistence of two substituted phases observed in samples with nominal compositions between the solubility limits. - Graphical abstract: Layered phosphates of general formula (Ti 1-x Zr x )(HPO 4 ).H 2 O have been prepared by the hydrothermal treatment of amorphous gels in phosphoric acid and characterised by Rietveld analysis of high resolution synchrotron X-ray powder diffraction data and pair distribution function analysis of high energy synchrotron X-ray total scattering data.

  9. Rietveld and impedance analysis of cold and hot rolled duplex and lean duplex steels for application in paper and pulp industry

    Esteves, Luiza; Lins, Vanessa de Freitas Cunha, E-mail: luizaeq@yahoo.com.br [Universidade Federal de Minas Gerais (UFMG), Belo Horizonte, MG (Brazil). Departamento de Engenharia Quimica; Paiva, Paulo Renato Perdigao [Centro Federal de Educacao Tecnologica de Minas Gerais (CEFET), Belo Horizonte, MG (Brazil); Viana, Adolfo Kalergis do Nascimento [APERAM South America, Timoteo, MG (Brazil)

    2017-01-15

    In this study, X-Ray Diffraction (XRD) and Rietveld Refinement were performed to identify and quantify the ferrite and austenite phase of cold and hot rolled duplex stainless steels (UNS S31803) and lean duplex stainless steels (UNS S32304). Electrochemical impedance spectroscopy (EIS) was applied to evaluate the chemical behavior of duplex and lean duplex stainless steels in white, green, and black liquors of paper and pulp industry. Rietveld analysis results showed a higher austenite content than the standard limit for duplex steels in the hot rolled condition. The hot rolling condition plays a major role in improving corrosion resistance in white liquor mainly for the lean duplex steel. (author)

  10. Rietveld and impedance analysis of cold and hot rolled duplex and lean duplex steels for application in paper and pulp industry

    Esteves, Luiza; Lins, Vanessa de Freitas Cunha; Viana, Adolfo Kalergis do Nascimento

    2017-01-01

    In this study, X-Ray Diffraction (XRD) and Rietveld Refinement were performed to identify and quantify the ferrite and austenite phase of cold and hot rolled duplex stainless steels (UNS S31803) and lean duplex stainless steels (UNS S32304). Electrochemical impedance spectroscopy (EIS) was applied to evaluate the chemical behavior of duplex and lean duplex stainless steels in white, green, and black liquors of paper and pulp industry. Rietveld analysis results showed a higher austenite content than the standard limit for duplex steels in the hot rolled condition. The hot rolling condition plays a major role in improving corrosion resistance in white liquor mainly for the lean duplex steel. (author)

  11. Synthesis and characterization of Al{sub 2}O{sub 3} obtained from the polymeric precursor method using glycerin as a poly alcohol; Sintese e caracterizacao de Al{sub 2}O{sub 3} obtida por meio do metodo dos precursores polimericos utilizando glicerina como polialcool

    Elicker, C.; Gaier, M.; Almeida, S.R.; Vieiraaa, B.M.; Ratmann, C.W.R.; Pereira, C.M.P. de; Cava, S.S. [Universidade Federal de Pelotas (UFPel), Pelotas, RS (Brazil); Egea, J.J. [Consejo Superior de Investigaciones Cientificas, Madrid (Spain)

    2014-07-01

    In this study, calcium aluminate was synthesized using glycerin to replace ethylene glycol in the polymeric precursor method. The resulting resin was pre-calcined in a muffle at 300 °C for 2 h and the resulting material was calcined at 900 °C for 2 h. The powders were analyzed by XRD, SEM and EDX, TEM, Micro-Raman and IR. The results demonstrated the possibility of using glycerin as an alternative to ethylene glycol in the polymeric precursor method. (author)

  12. In situ X-ray Rietveld analysis of Ni-YSZ solid oxide fuel cell anodes during NiO reduction in H2

    Reyes Rojas, A; Esparza-Ponce, H E; Fuentes, L; Lopez-Ortiz, A; Keer, A; Reyes-Gasga, J

    2005-01-01

    A synthesis and characterization of solid oxide fuel cell (SOFC) anodes of nickel with 8%mol yttrium stabilized zirconia (Ni-YSZ) is presented. Attention was focused on the kinetics and phase composition associated with the transformation of NiO-YSZ to Ni-YSZ. The anodes were prepared with an alternative synthesis method that includes the use of nickel acetylacetonate as an inorganic precursor to obtain a highly porous material after sintering at 1400 deg. C and oxide reduction (NiO-YSZ → Ni-YSZ) at 800 deg. C for 8 h in a tubular reactor furnace using 10% H 2 /N 2 . The obtained material was compressed by unidirectional axial pressing into 1 cm-diameter discs with 15-66 wt% Ni and calcinated from room temperature to 800 deg. C. A heating rate of 1 deg. C min -1 showed the best results to avoid any anode cracking. Their structural and chemical characterization during the isothermal reduction were carried out by in situ time-resolved X-ray diffraction, refined with the Rietveld method (which allowed knowing the kinetic process of the reduction), scanning electron microscopy and X-ray energy dispersive spectroscopy. The results showed the formation of tetragonal YSZ 8%mol in the presence of nickel, a decrement in the unit cell volume of Ni and an increment of Ni in the Ni-YSZ anodes during the temperature reduction. The analysis indicated that the Johnson-Mehl-Avrami equation is unable to provide a good fit to the kinetics of the phase transformation. Instead, an alternative equation is presented

  13. Clays as green catalysts in the cholesterol esterification: spectroscopic characterization and polymorphs identification by thermal analysis methods. An interdisciplinary laboratorial proposal for the undergraduate level; Argilas como catalisadores verdes na esterificacao do colesterol: caracterizacao espectroscopica e identificacao de polimorfos por metodos de analise termica. Uma proposta laboratorial interdisciplinar para o primeiro ciclo universitario

    Maria, Teresa M R.; Nunes, Rui M. D.; Pereira, Mariette M.; Eusebio, M. Ermelinda S. [Universidade de Coimbra, Coimbra (Portugal). Dept. de Quimica], e-mail: troseiro@ci.uc.pt

    2009-07-01

    A laboratory experiment that enables the professor to introduce the problematic of sustainable development in pharmaceutical chemistry to undergraduate students is proposed, using a simple synthetic procedure. Cholesteryl acetate is prepared by the esterification of cholesterol using Montmorillonite K10 as heterogeneous catalyst. Cholesterol and cholesteryl acetate are characterized by spectroscopic ({sup 1}H RMN, {sup 13}C RMN, FTIR) and thermal analysis techniques. The thermal methods are used to introduce the concepts of polymorphism and the nature of mesophases. (author)

  14. Structural and morphological characterization of TiO{sub 2}-ZrO{sub 2} powders obtained by the polymeric precursors method; Caracterizacao estrutural e morfologica de pos de TiO{sub 2}-ZrO{sub 2} obtidos pelo metodo dos precursores polimericos

    Ribeiro, M.A.; Gama, L.; Bispo, A.; Neiva, L.S., E-mail: m_aparecidaribeiro@yahoo.com.b [Universidade Federal de Campina Grande (DEMa/UFCG), PB (Brazil). Dept. de Engenharia de Materiais; Bernardi, M.I.B. [Universidade de Sao Paulo (IFSC/USP), Sao Carlos, SP (Brazil). Inst. de Fisica; Kiminami, R.H.G.A. [Universidade Federal de Sao Carlos (DEMa/UFSCar), SP (Brazil). Dept. de Engenharia de Materiais

    2010-07-01

    This work aims to characterize the structure and morphology of TiO{sub 2}-ZrO{sub 2} powders obtained by polymeric precursor method. For this we studied the following compositions: 0.25, 0.5 and 0.75 moles of Zr and calcined at 800 deg C for one hour. The powders obtained were characterized by XRD, SEM and nitrogen adsorption (BET). The analysis of X-ray diffraction showed that the powders had a phase of TiO{sub 2} in the anatase form and a tetragonal phase of ZrO{sub 2}. The crystallite size was between 8, 13 and 11 nm respectively. The analysis of scanning electron microscopy showed the growth of ZrO{sub 2} nanoparticles and that these comprise spherical agglomerates of less than 100 nm. Particle size determined by the BET ranging 28.1-29.5 nm, showing thereby the character of nanosized powders. (author)

  15. Hydrodynamic characterization of an alluvial soil for the Cajueiro Reservoir in Tuparetama-PE (Brazil), by using the internal drainage method; Caracterizacao hidrodinamica de um solo aluvial do Acude Cajueiro em Tuparetama-PE utilizando-se o metodo da drenagem interna

    Robalinho, Aviani Maria Bezerra

    2000-10-01

    The determination of the hydraulic properties of an alluvial soil in Cajueiro reservoir has been carried out in two experimental plots of 3.5 m x 3.5 m, installed in the opposite banks of the brook in which is located the dam, (Tuparetama Country, Pernambuco). For the determination of the hydraulic conductivity as a function of the soil water volumetric content K({theta}), the internal driainage method proposed by Hillel et al. (1972) has been applied. The soil-water retention curves h ({theta}) have been determined through the experimental data of volumetric water content and pressure obtained in field experiments. The h ({theta}) and K ({theta}) curves have been fitted to van Genuchten's closed - form equations (1980), using the Burdine's model, and Brooks and Corey's model, respectively. The volumetric water content, matric potential, and total water content estimates have been fitted to two analytical functions: one being composed by the addition of three exponentials terms the other composed and by representation the reverse of the power functions. The latter has been preferred due to its smoother representation between the fast and the slow its drainage phases. Considering the hydraulic behavior, three different layers have been identified in the soil profiles of the two experimental parcels A2 and B4 in the alluvial soil Cajueiro reservoir. The second layer of the soil profile in parcel A2 turned out the more pemeable than the other two layers. As to the soil profile in parcel B4, the first layer turned out more conductive than the other layers. However, the biggest volumetric water content variations were due to the differences found in the texture and structure of the soil profiles under study. The hydrodynamic characterization of the two soil profiles, A2 and B4, brings significant elements for the simulation of scenarios related to the soil of water transport processes. It is of particular importance the study of scenarios related to the

  16. Rietveld profile analysis of calcined AlPO/sub 4/-11 using pulsed neutron powder diffraction

    Richardson, J.W. Jr.; Pluth, J.J.; Smith, J.V.

    1988-08-01

    Aluminium phosphate, AlPO/sub 4/, M/sub r/=121.95, orthorhombic, Icmm (disordered Al, P), Icm2 (ordered Al, P), a=13.5333(8), b=18.4845(10), c=8.3703(4) A, V=2094 A/sup 3/, Z=20, D/sub x/=1.93 g cm/sup -3/, T approx. = 295 K, R/sub wp/=0.031, R/sub F//sup 2/=0.109 (Icmm) and R/sub wp/=0.027, R/sub F//sup 2/=0.058 (Icm2) for 1017 independent reflections. Sample calcined at 873 K and dehydrated at 573 K. Time-of-flight neutron powder diffraction data were taken on the GPPD diffractometer at the Argonne National Laboratory Intense Pulsed Neutron Source. The structure was refined by Rietveld profile analysis in the range d=0.86-3.91 A in two space groups: Icmm assuming no ordering of Al and P, and Icm2 assuming strict alternation of Al and P on tetrahedral nodes. (orig./BHo).

  17. Preparation and Crystal Structures of Some AIVB2IIO4 Compounds: Powder X-Ray Diffraction and Rietveld Analysis

    K. Jeyadheepan

    2014-01-01

    Full Text Available The AIVB2IIO4 compounds such as cadmium tin oxide (Cd2SnO4 or CTO and zinc tin oxide (Zn2SnO4 or ZTO are synthesized by solid state reaction of the subsequent binary oxides. The synthesized powders were analyzed through the powder X-ray diffraction (PXRD. Cell search done on the PXRD patterns shows that the Cd2SnO4 crystallizes in orthorhombic structure with space group Pbam and the cell parameters as a=5.568(2 Å, b=9.894(3 Å, and c=3.193(1 Å and the Zn2SnO4 crystallizes as cubic with the space group Fd3 -m and with the cell parameter a=8.660(2 Å. Rietveld refinement was done on the PXRD patterns to get the crystal structure of the Cd2SnO4 and Zn2SnO4 and to define the site deficiency of atoms which causes the electrical properties of the materials.

  18. A new approach to texture measurements: Orientation distribution function (ODF) determination by Rietveld refinement

    Vondreele, R.; Larson, A.; Lawson, A.; Sheldon, R.; Wright, S.

    1996-01-01

    The preferred orientation of crystal grains within a manufactured part is described most fully by its orientation distribution function (ODF), which is a mapping of the probability of each of the possible grain orientations with respect to the exterior dimensions. Traditionally, an ODF is determined from pole figures for a relatively small number of reflections. These pole figures are measured with x-rays or neutrons using short detector scans over the center of an individual diffraction peak for a large number of different sample orientations. This is efficient if the selected diffraction peaks are reasonably strong (relative to background) and well separated, such as in pure fcc and bcc metals. It is also appropriate for constant wavelength sources where collection of individual diffraction peak intensities is a reasonably efficient use of the source. However, the traditional method is not very efficient for neutron diffraction at a spallation source such as LANSCE where the entire diffraction pattern is accessible for each sample setting. Moreover, a different approach is necessary for complicated diffraction patterns, such as from composite materials, intermetallic compounds, high T c ceramics, polyphasic minerals and polymers where there is expected to be heavy overlap of adjacent diffraction peaks. In addition, the large number of settings normally collected for an individual pole figure may not be necessary, since the entire pattern is obtained at each setting. Thus, a new method of ODF analysis needs to be developed to handle the more complex diffraction patterns obtained from modern technological materials as well as take advantage of the particular characteristics of spallation neutron sources. This project sought to develop the experimental procedures and the mathematical treatment needed to produce an orientation distribution function (ODF) directly from full diffraction patterns from a sample in a limited number of orientations

  19. Crystal structures of iron bearing tetrahedrite and tennantite at 25 and 250 degrees C by means of Rietveld refinement of synchrotron data

    Friese, K.; Grzechnik, A.; Makovicky, E.

    2008-01-01

    Rietveld refinement of X-ray synchrotron data was performed for two synthetic tetrahedrite samples, with 0.61 and 1.83 Fe atoms, and two synthetic tennantite samples with 0.10 and 1.23 Fe atoms p.f.u. M-12(Sb,As)(4)S-13. Measurements were performed at 25 and 250 degrees C. For both the phases...

  20. Structural Rietveld refinement and vibrational study of MgCr{sub x}Fe{sub 2−x}O{sub 4} spinel ferrites

    Sabri, K. [Laboratoire des Sciences et technique de l’Environnement et de la Valorisation, département de Génie des Procédés, Université de Mostaganem, Mostaganem (Algeria); Rais, A., E-mail: amrais@yahoo.com [Laboratoire des Sciences et technique de l’Environnement et de la Valorisation, département de Génie des Procédés, Université de Mostaganem, Mostaganem (Algeria); Taibi, K. [Laboratoire de Science et Génie des Matériaux, USTHB, Alger, Algéria (Algeria); Moreau, M.; Ouddane, B. [Laboratory of LASIR Spectrochemistry, University of Science and Technology, 59650 Villeneuve d’Ascq (France); Addou, A. [Laboratoire des Sciences et technique de l’Environnement et de la Valorisation, département de Génie des Procédés, Université de Mostaganem, Mostaganem (Algeria)

    2016-11-15

    Spinel ferrites with the general formula MgCr{sub x}Fe{sub 2−x}O{sub 4} (0≤x≤1) were synthesized by the standard ceramic technique and characterized by X-ray diffraction. The XRD patterns confirmed that the mixed ferrite samples are in the cubic spinel structure which is further validated by Rietveld refinement in the space group Fd3m. The crystal structure and cell parameters were refined by Rietveld analysis. The vibrational study was achieved using Fourier Transform-InfraRed (FT-IR) and Raman spectroscopy. From FT-IR band frequencies, the force constants K{sub t} and K{sub o} , for tetrahedral (A) and octahedral (B) sites respectively, have been calculated and discussed with the trend of bond lengths obtained from Rietveld refinement. For all compositions, Raman spectra revealed the five active modes showing the vibration of O{sup 2−} ions at both the A-site and B-site ions. The frequencies trend with chromium content of both FT-IR and Raman spectra showed a shift toward higher values for all modes.

  1. Synthesis and characterization photocatalyst of titanium oxide obtained by the Pechini; Sintese e caracterizacao fotocatalitica do oxido de titanio obtido pelo Metodo Pechini

    Ribeiro, P.C.; Costa, A.C.F.M.; Lira, H.L. [Universidade Federal de Campina Grande (UFCG), PB (Brazil). Departamento de Engenharia de Materiais; Sasaki, J.M. [Universidade Federal do Ceara (UFC), Fortaleza, CE (Brazil). Departamento de Fisica; Santos, S.K., E-mail: pollyanacae@yahoo.com.br [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil). Departamento de Engenharia Quimica

    2011-07-01

    The photocatalysis using TiO{sub 2} semiconductor has shown great efficiency in the treatment of toxic pollutants and non-biodegradable materials, commonly present in air and domestic and industrial effluents. Thus, the aim of this work is to study the evaluation of photocatalytic activity of TiO{sub 2} samples synthesized by the Pechini method at a ratio of citric acid / metal cation of 2:1 and 4:1. The synthesized samples were characterized by X-ray diffraction, quantification of phases using the Rietveld method of refinement of the structure and after analyzed in photocatalytic bench tests using methyl red dye. The results showed that in a 2:1 ratio, the sample resulted in the formation of 100% of anatase phase, while in the 4:1 ratio sample showed 73.51% of anatase phase and 10.5% of rutile phase. The 4:1 sample showed the best performance discoloring over 70% of the dye for a period close to 24h. (author)

  2. Structural studies of TiC1−xOx solid solution by Rietveld refinement and first-principles calculations

    Jiang, Bo; Hou, Na; Huang, Shanyan; Zhou, Gege; Hou, Jungang; Cao, Zhanmin; Zhu, Hongmin

    2013-01-01

    The lattice parameters, structural stability and electronic structure of titanium oxycarbides (TiC 1−x O x , 0≤x≤1) solid solution were investigated by Rietveld refinement and first-principles calculations. Series of TiC 1−x O x were precisely synthesized by sintering process under the vacuum. Rietveld refinement results of XRD patterns show the properties of continuous solid solution in TiC 1−x O x over the whole composition range. The lattice parameters vary from 0.4324 nm to 0.4194 nm decreasing with increasing oxygen concentration. Results of first-principles calculations reveal that the disorder C/O structure is stable than the order C/O structure. Further investigations of the vacancy in Ti 1−Va (C 1−x O x ) 1−Va solid solution present that the structure of vacancy segregated in TiO-part is more stable than the disorder C/O structure, which can be ascribed to the Ti–Ti bond across O-vacancy and the charge redistributed around Ti-vacancy via the analysis of the electron density difference plots and PDOS. - Graphical abstract: XRD of series of titanium oxycarbides (TiC 1−x O x , 0≤x≤1) solid solution prepared by adjusting the proportion of TiO in the starting material. Highlights: • Titanium oxycarbides were obtained by sintering TiO and TiC under carefully controlled conditions. • Rietveld refinement results show continuous solid solution with FCC structure in TiC 1−x O x . • The disorder C/O structure is stable than the order C/O structure. • Introduction of vacancy segregated in TiO-part is more stable than disorder C/O structure. • Ti–Ti bond across O-vacancy and the charge redistributed around Ti-vacancy enhance structural stability

  3. Rietveld refinement and dielectric relaxation of a new rare earth based double perovskite oxide: BaPrCoNbO{sub 6}

    Bharti, Chandrahas, E-mail: bharti.chandrahas@gmail.com [Sensor and Actuator Division, CSIR-Central Glass and Ceramic Research Institute, 196, Raja SC Mullick Road, Kolkata 700032 (India); Das, Mrinmoy K.; Sen, A. [Sensor and Actuator Division, CSIR-Central Glass and Ceramic Research Institute, 196, Raja SC Mullick Road, Kolkata 700032 (India); Chanda, Sadhan; Sinha, T.P. [Department of Physics, Bose Institute, 93/1, Acharya Prafulla Chandra Road, Kolkata-700009 (India)

    2014-02-15

    A new rare earth based double perovskite oxide barium praseodymium cobalt niobate, BaPrCoNbO{sub 6} (BPCN) is synthesized by solid-state reaction technique. Rietveld analysis of X-ray diffraction (XRD) data shows that the compound crystallizes in a perovskite like tetragonal structure which belongs to the I4/mmm space group with lattice parameters a=b=5.6828(9) Å, c=8.063(2) Å. Structural analysis reveals 1:1 ordered arrangement for the Co{sup 2+} and Nb{sup 5+} cations over the six-coordinate B-sites of BPCN. The superlattice line (1 0 1) at 2θ=19.10° arising from the alternate ordering of Co{sup 2+} and Nb{sup 5+} sites is observed in the XRD pattern which confirms the presence of cation ordering in BPCN. Fourier transform infrared spectrum shows two phonon modes of the sample due to the antisymmetric NbO{sub 6} stretching vibration. The relaxation dynamics of the conductive process in BPCN is investigated in the temperature range 303 to 503 K and in the frequency range 100 Hz to 1 MHz using impedance spectroscopy. The relaxation mechanism of the sample in the framework of electric modulus formalism is modeled by Davidson–Cole model (DCM). The values of α (distribution of relaxation time) for the DCM varies from 0.1 to 0.3 which suggests the asymmetric distribution of relaxation time for BPCN. The activation energy of the sample, calculated from both conductivity and modulus spectra, are found to be almost the same ∼0.4 eV, which indicates that the conduction mechanism for BPCN is polaron hopping. The scaling behaviour of the imaginary part of electric modulus suggests that the relaxation follows the same mechanism at various temperatures. - Graphical abstract: Rietveld refinement plot for BPCN. Inset shows the schematic presentation of the BPCN tetragonal unit cell. The Co{sup 2+} atoms are located at the centers of the CoO{sub 6} (blue) octahedra. The Nb{sup 5+} atoms are located at the centers of the NbO{sub 6} (green) octahedra. Display Omitted

  4. Characterization of an ecological binder for mortars obtained from recycling of ladle furnace slag; Caracterizacao de aglomerante ecologico para argamassas obtido a partir da reciclagem de escoria de forno panela

    Marinho, A.B.; Santos, C.M.; Fontes, W.C.; Matias, A.C.P.; Brigolini, G.J.; Peixoto, R.A.F. [Universidade Federal de Ouro Preto (UFOP), MG (Brazil). Departamento de Engenhaira Civil; Carvalho, J.F., E-mail: josemaria.carvalho@ufv.br [Universidade Federal de Vicosa (UFV), MG (Brazil). Departamento de Engenharia Civil

    2016-07-01

    A sustainable binder obtained from recycling of a ladle furnace slag from Piracicaba, Sao Paulo, was produced in Laboratory of Construction Materials of Federal University of Ouro Preto (UFOP). A characterization work was performed and the results are presented. The physical, chemical and mineralogical properties was obtained using, among others, the following techniques: X-ray fluorescence (XRF), X-ray diffraction (XRD) with Rietveld refining method, optical microscopy and Scanning electronic microscopy (SEM) with energy dispersive spectroscopy (EDS). The chemical analysis showed predominance of CaO and SiO{sub 3}; the mineralogical analysis pointed the predominant presence of calcium-olivine, merwinite and pyroxene and; the images showed predominance of angulous and elongated grains. According to results, the material was classified as a hydraulic binder, with characteristics comparable to hydraulic limes. (author)

  5. Rietveld refinement and dielectric studies of Bi{sub 0.8}Ba{sub 0.2}FeO{sub 3} ceramic

    Kaswan, Kavita, E-mail: kaswan.kavita@gmail.com; Agarwal, Ashish; Sanghi, Sujata; Rangi, Manisha; Jangra, Sandhaya; Singh, Ompal [Department of Applied Physics, Guru Jambheshwar University of Science and Technology, Hisar 125001, Haryana (India)

    2016-05-23

    Polycrystalline Bi{sub 0.8}Ba{sub 0.2}FeO{sub 3} ceramic has been synthesized via conventional solid state reaction technique. The Rietveld refinement of x-ray powder diffraction revealed that the sample has a rhombohedral crystal structure (space group R3c). With increase in temperature, the values of dielectric constant (ϵ′) and dielectric loss (tan δ) are found to be increase at different frequencies which may be the result of increase in the number of charge carriers and their mobilities due to the thermal activation. Further the ac conductivity data is analyzed by using Jonscher’s universal power law. The values of frequency exponent ‘s’ lies in the range 0.2 ≤ s ≤ 0.7 and decreases with increase in temperature which can be explained on the basis of CBH (Correlated Barrier Height) model.

  6. Aplicación de tratamiento electroquímico a baja intensidad de corriente para la extracción de cloruros en objetos arqueológicos de hierro de procedencia subacuática. Observación de la evolución de fases mineralógicas mediante XRD-Rietveld

    Bethencourt, M.

    2004-12-01

    Full Text Available With the purpose of optimising a suitable methodology for the conservation of an archaeological object of iron, a low current intensities electrolytic treatment has been applied, to a piece of cast iron, proving to be effective in the extraction of chloride ions from the structure of akaganeite, principal corrosion product of iron in the marine medium. The monitoring of the electrolytic treatment has been proven by applying the "Rietveld" method to the patterns XRD of samples extracted from the corroded surface before and after the treatment. This method has permitted the unequivocal determination of the akaganeite and its chemical composition. This identification has been corroborated by means of SEM and EDS. After the electrolytic treatment, akaganeite was not present in the sample.

    Con objeto de optimizar una metodología adecuada para la conservación de una pieza de hierro arqueológico de fundición, se ha aplicado un tratamiento electrolítico a bajas intensidades de corriente, demostrando su efectividad en la extracción de iones cloruro de la estructura de akaganeita, principal producto de corrosión del hierro en medio marino. La monitorización del proceso se ha comprobado aplicando el método Rietveld a los patrones XRD de muestras extraídas de la superficie corroída antes y después del tratamiento. Este método ha permitido la determinación inequívoca de la akaganeita y la composición química de este oxihidróxido de hierro no estequiométrico. Dicha identificación se corrobora mediante SEM y EDS. Después del tratamiento electrolítico la akaganeita no está presente en la muestra.

  7. ESTUDIO DE LAS FASES MINERALÓGICAS DEL CLÍNKER EN UNA CEMENTERA ESPAÑOLA, UTILIZANDO EL MÉTODO DE RIETVELD

    ANA M. CASTAÑÓN

    2012-01-01

    Full Text Available Con el objetivo de implantar un método de control de calidad de forma continua en una fábrica de cementos española, para mejorar las características del producto final, se están desarrollando nuevas metodologías de caracterización. El método de Rietveld [1] se ha utilizado con éxito para analizar la composición de las fases principales del clínker. Utilizando esta metodología, se ha llevado a cabo un estudio para cuantificar adecuadamente la fase minoritaria de Cal Libre, de gran importancia en la calidad del clínker. El método ha permitido obtener unos resultados satisfactorios en muestras cuyos contenidos superan el 3% de CaO. Estos resultados son posibles combinando adecuadamente las técnicas de difracción y fluorescencia de rayos-X, así como los resultados del análisis por vía química.

  8. Rietveld refinement of the structures of 1.0 C-S-H and 1.5 C-S-H

    Battocchio, Francesco

    2012-11-01

    Low-Q region Rietveld analyses were performed on C-S-H synchrotron XRD patterns, using the software MAUD. Two different crystal structures of tobermorite 11 Å were used as a starting model: monoclinic ordered Merlino tobermorite, and orthorhombic disordered Hamid tobermorite. Structural modifications were required to adapt the structures to the chemical composition and the different interlayer spacing of the C-S-H samples. Refinement of atomic positions was done by using special constraints called fragments that maintain interatomic distances and orientations within atomic polyhedra. Anisotropic crystallite size refinement showed that C-S-H has a nanocrystalline disordered structure with a preferred direction of elongation of the nanocrystallites in the plane of the Ca interlayer. The quality of the fit showed that the monoclinic structure gives a more adequate representation of C-S-H, whereas the disordered orthorhombic structure can be considered a more realistic model if the lack of long-range order of the silica chain along the c-direction is assumed. © 2012 Elsevier Ltd. All rights reserved.

  9. Rietveld refinement of the crystal structure of perovskite solar cells using CH3NH3PbI3 and other compounds

    Ando, Yuji; Ohishi, Yuya; Suzuki, Kohei; Suzuki, Atsushi; Oku, Takeo

    2018-01-01

    The crystal structures of perovskite thin films including CH3NH3PbI3, CH3NH3Pb1-xSbxI3, and CH3NH3PbI3-yCly in the solar cell configuration were studied by using Rietveld refinement. For the CH3NH3PbI3 and CH3NH3Pb1-xSbxI3 samples, satisfactory agreement with the measured profiles was obtained with a weighted profile R-factor (Rwp) of as low as 3%. It was shown that the site occupancy of methylammonium (MA) was decreased in the antimonized cell due to the compensation effect of an increased positive charge brought about by replacing Pb2+ with Sb3+. Photovoltaic measurements showed that the power conversion efficiency was enhanced by adding a small amount of Sb to the CH3NH3PbI3 cell, but it was monotonically decreased as the mole fraction of Sb exceeded 0.03. This variation of the conversion efficiency was considered as a result of suppressed crystallization of PbI2 and carrier recombination via MA vacancies in the antimonized cells. In the case of CH3NH3PbI2.88Cl0.12 sample, the agreement with the measured profile with an Rwp of as high as 7% suggested the co-existence of cubic and tetragonal phases in the chlorinated cell.

  10. Application of powder X-ray diffraction and the Rietveld method to the analysis of oxidation processes and products in sulphidic mine tailings

    Balic Zunic, Tonci; Katerinopoulou, Anna; Edsberg, Anders

    2011-01-01

    silica were applied as proper models. The procedures developed on test mixtures result in estimated errors of determination typically lower than 2 wt%. The approach was applied to the analysis of the complex problem of estimating mass balance in oxidized mine tailings from the Nanisivik Mine, Nunavut......, Canada revealing an oxidized proportion of 9 % of total pyrite content in the well drained tailings during a period of 8 years and a negligible oxidation in the water-covered tailings....

  11. Structure of the new Tl(Ba sub 1.0 Sr sub 1.0) PrCu sub 2 O sub 7-x by Rietveld analysis

    Yang, P.; Fun, H. K.; Lee, T.J.; Ku, H.C.; Lai, C.C.

    1994-01-01

    The crystalline structure of Tl(Ba sub 1.0 Sr sub 1.0)PrCu sub 2 O sub 7-x was obtained at room temperature from x-ray powder diffraction with CuK sub α radiation using Rietveld analysis. Tl(Ba sub 1.0 Sr sub 1.0)PrCu sub 2 O sub 7-x isomorphous at both room temperature (300 K) and low temperature (100 K) with TlBa sub 2 ca Cu sub 2 O sub 7-x type (1212) structure, crystallized with space group P4/mmm and one formula in the unit cell. At 300 K, cell parameters a=3.8892(2) A, c=12.3099(6) A, the structure was refined with 25 parameters to R sub WP = 6.30%, R sub P = 4.38% for 3551 step intensities and R sub b = 5.01%, R sub f = 4.20% for 156 reflections. The goodness of fitting S=3.18. At 100K, cell parameters a=3.8866(4) A, c= 12.289(1) A, the structure was refined with 26 parameters to R sub WP = 8.42%, R sub P = 6.21% for 2676 step intensities and R sub b = 6.72%, R sub f = 5.28% for 120 reflections. The goodness of fitting S=2.32. Reasonable anisotropic thermal parameters were obtained. The compositions of Ba and Sr atoms were refined to about Ba sub 1.1 Sr sub 0.9 compared with the stoichiometric Ba sub 1.0 Sr sub 1.0

  12. Characterization and concentration of manganese ore waste; Caracterizacao e concentracao de rejeito de minerio de manganes

    Lima, Rosa Malena Fernandes; Pereira, Eder Esper; Reis, Erica Linhares; Silva, Glaucia Regina da [Universidade Federal de Ouro Preto (UFOP), MG (Brazil)

    2010-07-01

    In this work is presented the tests results of characterization and concentration by gravity and flotation methods carried out with a manganese sample waste. By optical microscopy, SEM/EDS and X-ray diffractometry were identified the Mn minerals spessartite (20%), tephroite (15%), rhodonite (5%), rhodochrosite and carbonates minerals (29%), opaque minerals and others (16%), micaceus minerals (6%) and quartz (4%). It was obtained Mn metallurgical recovery of 58% with Mn concentrate contents varying from 30 to 32.5%. The concentrates SiO{sub 2} contents of flotation were until 1.5% smaller than those contents of gravity method concentrates. (author)

  13. Characterization of hydroxyapatite substituted with silicon; Caracterizacao de hiroxiapatita substituida com silicio

    Silva, H.M. da; Soares, G.A., E-mail: helena@metalmat.ufrj.b [Universidade Federal do Rio de Janeiro (COPPE/UFRJ), RJ (Brazil). Coordenacao dos Programas de Pos-graduacao em Engenharia. Lab. de Biomateriais para Engenharia Ossea; Mateescu, M.; Anselme, K. [Universite de Haute-Alsace (UHA/IS2M), Mulhouse (France). Inst. de Science des Materiaux; Palard, M.; Champion, E. [Universite de Limoges (France). Fac. des Sciences et Techniques

    2009-07-01

    Incorporation of silicon (Si) ions into hydroxyapatite structure (HA) influences on physical, chemical and physiological properties. Some studies reported the improved bioactivity Si substitution, and it also accelerates the biomineralization process. The main objective of this work is to characterize stoichiometric hydroxyapatite and hydroxyapatite substituted with 1.13% in weight of Si (SiHA) using a wet precipitation method followed by a heat treatment. SEM/EDS, AFM, DRX and FTIR analyses were used to characterize the samples. EDS and FTIR results confirmed the presence of Si. Silicon induces small changes on crystal structure of HA, not detected on X-ray diffraction patterns of sintered tablets of SiHA and HA. No secondary phases were observed, that indicates the Si had entered the HA lattice. (author)

  14. Naphthenic acid characterization and distribution in crude oils; Caracterizacao e distribuicao de acidos naftenicos em petroleos

    Guimaraes, Regina C.L.; Gomes, Alexandre de O. [PETROBRAS S.A., Rio de Janeiro, RJ (Brazil)

    2008-07-01

    Naphthenic acid corrosion was observed for the first time during the distillation process of some kind of crude oils in 1920. Recent reports about naphthenic acid corrosion have been found in China, India, Venezuela, Eastern Europe, Russia and the USA. In Brazil, heavy and acid crude oil processing is rising. Some brazilian crude oils have TAN around 3,0 mg KOH/g. The presence of relatively high levels of naphthenic acids in crude oils is a bane of petroleum refiners; and more recently, of producers as well, who have reported problems during production with calcium and sodium naphthenate . Essentially, these acids which are found to greater or lesser extent in virtually all crude oils are corrosive and tend to cause equipment failures, lead to high maintenance costs and may pose environmental disposal problems. In order to give these information to PETROBRAS, The Research and Development Center of PETROBRAS (CENPES) has been working in house and with brazilian universities developing analytical technicians to know better molecular structures and distribution of these acids compounds in crude oils. This work presents the actual methods and some results from these developments. (author)

  15. The formation and structure of mechano-synthesized nanocrystalline Sr{sub 3}Fe{sub 2}O{sub 6.4}: XRD Rietveld, Mössabuer and XPS analyses

    Al-Rawas, A.D., E-mail: arawas@squ.edu.om [Department of Physics, Sultan Qaboos University, P.O. Box 36, 123 Al-Khoud, Muscat (Oman); Widatallah, H.M.; Al-Harthi, S.H. [Department of Physics, Sultan Qaboos University, P.O. Box 36, 123 Al-Khoud, Muscat (Oman); Johnson, C. [Chemistry Department, Open University, Walton Hall, Milton Keynes MK7 6AA (United Kingdom); Gismelseed, A.M.; Elzain, M.E.; Yousif, A.A. [Department of Physics, Sultan Qaboos University, P.O. Box 36, 123 Al-Khoud, Muscat (Oman)

    2015-05-15

    Highlights: • The formation of mechano-synthesized nanocrystalline Sr{sub 3}Fe{sub 2}O{sub 7−δ} is investigated. • Pre-milling the reactants substantially lowers the formation temperature. • The core and surface structures were studied. • XRD and {sup 57}Fe Mössbauer spectroscopic analyses indicate the δ-value to be 0.60. • XPS shows a complex surface structure for the mechanosynthesized Sr{sub 3}Fe{sub 2}O{sub 7−δ} nanoparticles. - Abstract: The influence of ball milling and subsequent sintering of a 3:1 molar mixture of SrCO{sub 3} and α-Fe{sub 2}O{sub 3} on the formation of Sr{sub 3}Fe{sub 2}O{sub 7−δ} double perovskite is investigated with different analytical techniques. Milling the mixture for 110 h leads to the formation of SrCO{sub 3}-α-Fe{sub 2}O{sub 3} nanocomposites and the structural deformation of α-Fe{sub 2}O{sub 3} via the incorporation of Sr{sup 2+} ions. Subsequent sintering of the pre-milled reactants’ mixture has led to the partial formation of an SrFeO{sub 3} perovskite-related phase in the temperature range 400–600 °C. This was followed by the progressive development of an Sr{sub 3}Fe{sub 2}O{sub 7−δ} phase that continued to increase with increasing sintering temperature until a single-phased nanocrystalline Sr{sub 3}Fe{sub 2}O{sub 7−δ} phase was attained at 950 °C (12 h). This temperature is ∼350 °C lower than the temperature at which the material is prepared conventionally using the ceramic method. The evolution of different structural phases during the reaction process is discussed. Rietveld refinement of the X-ray diffraction data shows a value of 0.60 for the oxygen deficiency δ, in consistency with the Fe{sup 3+}/Fe{sup 4+} ratio derived from the {sup 57}Fe Mössbauer data recorded at both 300 K and 78 K. The Mössbauer data suggests that the Sr{sub 3}Fe{sub 2}O{sub 6.4} nanoparticles are superparamagnetic with blocking temperatures below 78 K. The surfaces of the Sr{sub 3}Fe{sub 2}O{sub 6

  16. Rietveld refinement of the orthorhombic Pbca structures of Rb2CdSi5O12, Cs2MnSiO5O12, Cs2CoSi5O12 and Cs2NiSi5O12 leucites by synchrotron X-ray powder diffraction

    Bell, A.M.T.; Henderson, C.M.B.

    1996-01-01

    Analysis of high-resolution synchrotron X-ray powder diffraction patterns for hydrothermally synthesized Rb 2 CdSi 5 O 12 and Cs 2 MnSi 5 O 12 leucite analogues, and dry-synthesized Cs 2 CoSi 5 O 12 and Cs 2 NiSi 5 O 12 leucite analogues showed that they have an orthorhombic Pbca structure. The structures have been refined by the Rietveld method, showing that the tetrahedrally coordinated atoms (Si, Cd, Mn, Co and Ni) are ordered on separate sites. The Cs 2 MnSi 5 O 12 , Cs 2 CoSi 5 O 12 and Cs 2 NiSi 5 O 12 leucite samples are unusual in containing SiO 4 tetrahedra which are more distorted, on average, than the larger MnO 4 , CoO 4 and NiO 4 tetrahedra. The JCPDS file numbers for Rb 2 CdSi 5 O 12 , Cs 2 MnSi 5 O 12 and Cs 2 CoSi 5 O 12 are 46-1491, 46-1492 and 46-1493, respectively. (orig.)

  17. Rietveld refinement and dielectric properties of (Na{sub 0.5}Bi{sub 0.5}TiO{sub 3})-(Bi{sub 0.8}Ba{sub 0.2}FeO{sub 3}) ceramics

    Kaswan, Kavita, E-mail: kaswan.kavita@gmail.com; Agarwal, Ashish; Sanghi, Sujata; Singh, Ompal [Department of Applied Physics, Guru Jambheshwar University of Science and Technology, Hisar-125001 (India)

    2015-06-24

    (1-x)(Na{sub 0.5}Bi{sub 0.5}TiO{sub 3})-x(Bi{sub 0.8}Ba{sub 0.2}FeO{sub 3}) lead free ceramics (NBT, NBT-BBFO; x = 0.0, 0.1 respectively) have been synthesized by conventional solid state reaction method. Crystalline phase of sintered ceramics was investigated at room temperature using X-ray diffraction. Rietveld refinement of XRD data performed by FullProf revealed that both the samples exhibited rhombohedral structure with R3c space group. Dielectric properties of these ceramics were studied at different temperatures in a wide frequency range using impedance analyzer. Dielectric constant and dielectric loss were found to be increase with increase of BBFO content. The prepared ceramics exhibit a broad maximum in dielectric permittivity at 593K and dispersive permittivity at high temperatures. The NBT-BBFO sample shows a relaxor ferroelectric behavior at different frequencies.

  18. The new insight into the structure-activity relation of Pd/CeO2-ZrO2-Nd2O3 catalysts by Raman, in situ DRIFTS and XRD Rietveld analysis.

    Yang, X; Yang, L; Lin, J; Zhou, R

    2016-01-28

    Pd/CeO2-ZrO2-Nd2O3 (CZN) catalysts with different CeO2/ZrO2 molar ratios were synthesized and have been characterized by multiple techniques, e.g. XRD in combination with Rietveld refinement, UV-Raman, XPS and in situ DRIFTS. The XRD pattern of CZN with CeO2/ZrO2 molar ratios ≥1/2 can be indexed satisfactorily to the fluorite structure with a space group Fm3̄m, while the XRD patterns of CZ12 only display diffraction peaks of the tetragonal phase (S.G. P42/nmc). Nd addition can effectively stabilize the cubic structure of the CZN support and increase the enrichment of defect sites on the surface, which may be related to the better catalytic activity of Pd/CZN12 catalysts compared with Pd/CZ12. The presence of moderate ZrO2 can increase the concentration of O* active species, leading to accelerate the formation of nitrate species and thus enhance the catalytic activity of NOx and HC elimination. The Pd-dispersion decreases with the increasing Zr content, leading to the decreased CO catalytic activity, especially for the aged catalysts. The change regularity of the OSC value is almost the same with the in situ dynamic operational window, demonstrating that the in situ dynamic operational window is basically affected by the OSC value.

  19. Study and characterization of the hexa ferrite Ba{sub 2}Co{sub 2}Fe{sub 12}O{sub 22} (Co{sub 2}-Y); Sintese e caracterizacao da hexaferrita Ba{sub 2}Co{sub 2}Fe{sub 12}O{sub 22} (Co{sub 2}-Y)

    Pires Junior, G.F.M.; Rodrigues, H.O. [Universidade Federal do Ceara (DETI/UFC), Fortaleza, CE (Brazil). Dept. de Teleinformatica; Sales, J.C [Universidade Estadual Vale do Acarau (UVA), Fortaleza, CE (Brazil). Dept. de Engenharia; Sancho, E.O. [Universidade Federal do Ceara (UFC), Fortaleza, CE (Brazil). Dept. de Engenharia de Materiais; Sombra, A.S.B. [Universidade Federal do Ceara (LOCEM/UFC), Fortaleza, CE (Brazil). Dept. de Fisica. Lab. de Telecomunicacoes e Ciencias e Engenharia de Materiais

    2009-07-01

    The objective of this work is to synthesize and to characterize the Hexaferrita Ba2Co{sub 2}Fe{sub 12}O{sub 22} (Co{sub 2}Y). The Y-type Hexaferrita (Co{sub 2}Y) was prepared by the ceramic conventional method. The mixed powder by 1 h was calcined at 1050 deg C for 3 h. After of the calcination the powders were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD) using a diffractometer DMAXB of the Rigaku (Japan), CuK{sub {alpha}} radiation ({lambda}=1.5405 angstrom) in a tax of 0.5 deg /min and linear band (20 deg at 80 deg) in 2{theta}. The characterization more detailed by XRD was made using the DBWS9807a program that uses the method of Rietveld for refinement of crystalline structures and confirmed the isolated attainment of the phase (Co{sub 2}Y) with hexagonal crystalline structure (a = b = 5,8560 angstrom and c = 43,4977 angstrom; {alpha} = {beta} = 90 deg and {gamma} = 120 deg) with density and volume of the unit cell calculated of 5.45 g/cm{sup 3} and 1292,3 angstrom respectively. (author)

  20. Presence of a monoclinic (Pm) phase in the morphotropic phase boundary region of multiferroic (1 − x)Bi(Ni{sub 1/2}Ti{sub 1/2})O{sub 3}-xPbTiO{sub 3} solid solution: A Rietveld study

    Pandey, Rishikesh, E-mail: akhilesh-bhu@yahoo.com, E-mail: aksingh.mst@itbhu.ac.in; Singh, Akhilesh Kumar, E-mail: akhilesh-bhu@yahoo.com, E-mail: aksingh.mst@itbhu.ac.in [School of Materials Science and Technology, Indian Institute of Technology (Banaras Hindu University), Varanasi 221005 (India)

    2014-07-28

    We present here the results of structural studies on multiferroic (1 − x)Bi(Ni{sub 1/2}Ti{sub 1/2})O{sub 3}-xPbTiO{sub 3} solid solution using Rietveld analysis on powder x-ray diffraction data in the composition range 0.35 ≤ x ≤ 0.55. The stability region of various crystallographic phases at room temperature for (1 − x)Bi(Ni{sub 1/2}Ti{sub 1/2})O{sub 3}-xPbTiO{sub 3} is determined precisely. Structural transformation from pseudo-cubic (x ≤ 0.40) to tetragonal (x ≥ 0.50) phase is observed via phase coexistence region demarcating the morphotropic phase boundary. The morphotropic phase boundary region consists of coexisting tetragonal and monoclinic structures with space group P4mm and Pm, respectively, stable in composition range 0.41 ≤ x ≤ 0.49 as confirmed by Rietveld analysis. The results of Rietveld analysis completely rule out the coexistence of rhombohedral and tetragonal phases in the morphotropic phase boundary region reported by earlier workers. A comparison between the bond lengths for “B-site cations-oxygen anions” obtained after Rietveld refinement, with the bond length calculated using Shannon-Prewitt ionic radii, reveals the ionic nature of B-O (Ni/Ti-O) bonds for the cubic phase and partial covalent character for the other crystallographic phases.

  1. Characterization of poly pyrrole/montmorillonite electro polymerised onto Pt; Caracterizacao de filmes PPy/montmorilonita eletropolimerizados sobre Pt

    Castagno, K.R.L., E-mail: katiarlc@pelotas.ifsul.edu.b [Instituto Federal Sul-rio-grandense (IFSul), RS (Brazil). Dept. de Quimica; Azambuja, D.S.; Dalmoro, V.; Mauller, R.S. [Universidade Federal do Rio Grande do Sul (UFRGS), Pelotas, RS (Brazil). Inst. de Quimica

    2010-07-01

    In this study films of polypyrrole/montmorillonite (PPy/MT) were electropolymerized on platinum in order to evaluate the performance of this technique in the preparation of nanocomposite materials and to determine the thermal properties and conductivity of the composites. The films were synthesized from a solution containing pyrrole, dodecylbenzene sulfonate, acid and two types of clays: montmorillonite-Na + (MT-Na) and montmorillonite-30B (MT-M). The characterization of the films we have used FT-IR, TEM, XRD, TGA, DSC and resistivity measurement by the four-point van der Pauw method. The study showed that the adopted method of exfoliation and the electropolymerization method used, allows obtaining nanocomposite materials. Analyses of FT-IR, TEM and XRD show that the clays are exfoliated in the polymer matrix. Thermal analysis of the films indicates that the addition of clay reflects an enhancement in the thermal properties of the matrix of PPy, but decreases the conductivity of the same. (author)

  2. Preparation, characterization and certification of uranium isotope reference materials; Preparacao, Caracterizacao e certificacao de materiais de referencia isotopicos de uranio

    Oliveira Junior, Olivio Pereira de

    2006-07-01

    This work describes the preparation, characterization and certification of a set of uranium isotope reference materials ranging from 0.5 to 20.0 % of {sup 235}U in mass. The most important concepts of metrology in chemical measurements were applied so that the certified quantities in these materials could be directly traceable to the International System of Units (SI). As a consequence of this approach, these materials can be used in the instruments calibration, estimation of measurement uncertainty, method validation, assessment of performance of analysts, quality control routines and interlaboratory comparison programmes. The most advanced methods and techniques in mass spectrometry, that is, gas source mass spectrometry (GSMS), thermal ionisation mass spectrometry (TIMS) and inductively coupled plasma mass spectrometry (ICPMS) were investigated to identify which are the dominant components in the uncertainty and to quantify its contribution to the final value of the measurement uncertainty of the isotopic ratio. The results obtained were then compared to verify which are the methods and techniques associated to the lowest measurement uncertainty values. The isotope amount ratio n({sup 235}U)/n({sup 238}U) was certified in the materials produced to expanded uncertainties ranging from 0.02 to 0.10 % and the ratios n({sup 234}U)/n({sup 238}U) and n({sup 236}U)/n({sup 238}U), to uncertainties ranging from 0.03 to 2.20 %. These values fully comply to the requirements of the isotopic characterization of nuclear fuel as well as the analysis of environmental samples for nuclear safeguards. (author)

  3. Chemistry characterization and samples beryllium process impurity determination; Caracterizacao quimica e determinacao de impurezas de amostras de processo de berilio

    Carvalho, Leonel Mathry de

    1992-12-01

    Brazil is the greatest world producer of beryl (3 Be O.Al{sub 2}O{sub 3}.6SiO{sub 2}) and has recently begun to produce beryllium compounds by means of a pilot plant constructed at Governador Valadares city (Minas Gerais - Brazil). The aim of this work was the determination of trace level impurities and macro constituents in the tenth % range to support analytical control process of plant production and characterization of beryllium compounds. The impurities separations and purification process was developed by two steps procedure. The first one using EDTA complexation has separated and reduced some impurities to less than 1 {mu}g/ml level. In the second one it was used a chelating resin (Chelex 100) and the separation efficiency was about 75 to 97 % related with the element tested. High pure berylium oxide standard was obtained from purification of Be(OH)2. The R X fluorescence presented only traces of Cu and Si < 1 % Fe and Mn, Zn, Ca, Al, Na and S were completely removed. The beryllium content was determined by direct atomic emission spectroscopy in argon plasma (Dcp) and compared with classic gravimetric method as Be O. The results were in agreement (49,2+/-0,2 % and 48,3+/-0,1 % respectively) between 95 % of confidence. A low temperature gravimetric method for beryllium determination was also studied using Oxine with microwave furnace. A total of 24 elements including macro and trace level were determined by Dcp and/or spectrophotometric methods. The Be/B separation was studied using anionic resin in poly alcohols medium. A more detailed study of equilibrium conditions is necessary. This work was realized at Laboratorio de Analise Mineral (LAM) of Comissao Nacional de Energia Nuclear - Rio de Janeiro (CNEN). (author)

  4. Synthesis and characterization of tungsten or calcium doped PZT ceramics; Sintese e caracterizacao do PZT dopado com W ou Ca

    Santos, D.M.; Caracas, L.B.; Noronha, R.G.; Santos, M.M.T. dos [Universidade Federal do Maranhao (UFMA), Sao Luis, MA (Brazil). Dept. de Desenho e Tecnologia. Curso de Desenho Industrial; Paiva-Santos, C.O., E-mail: denilson@ufma.b [Universidade Estadual Paulista (IQ/UNESP), Araraquara, SP (Brazil). Inst. de Quimica

    2009-07-01

    Pure and doped (tungsten or calcium) PZT ceramics were prepared by association of the polymeric precursor and partial oxalate method. The phase formation was investigated by thermal analysis (TG/DSC) and X-ray diffraction (XRD). The affect of W or Ca doping PZT and their electrical properties was evaluated. Substitution of W by Ti and Ca by Pb leads to an increase of Curie temperature and broadening of dielectric constant. A typical hysteresis loop was observed at room temperature and the remnant polarization was increased with the content of W and Ca. (author)

  5. Poly(vinylpyrrolidone)/silver nanoparticles: preparation and characterization; Nanoparticulas de prata/poli(vinilpirrolidona): obtencao e caracterizacao

    Andrade, P.F.; Goncalves, M.C. [Instituto de Quimica - UNICAMP, Campinas, SP (Brazil)], e-mail: patandrade@iqm.unicamp.br

    2010-07-01

    In this work silver nanoparticles were prepared by chemical reduction method using PVP as dispersant agent. The formation of silver nanoparticles was investigated by UV-vis optical spectroscopy and X-ray diffraction. FT-IR spectroscopy confirmed the formation of Ag/PVP complex. The transmission electron microscopy images indicated that the concentration of Ag{sup +} precursor influenced the nanoparticles dispersion and size distribution significantly. The results indicated that dispersed nanoparticles with uniform size distribution can be prepared by this methodology to obtain polymeric nano composites. (author)

  6. Development and characterization of the lead iodide semiconductor detector; Desenvolvimento e caracterizacao do detector semicondutor de iodeto de chumbo

    Oliveira, Icimone Braga de

    2001-07-01

    A methodology for purification and growth of PbI{sub 2} crystal as well as for its characterization as a room temperature radiation detector was developed in this work. Commercial salts were purified using the zone refining method and, for the purified material growth, the Bridgman method was used. To calculate the purification efficiency, studies of the decrease impurities concentrations were made in the salts and in three sections of the materials purified, using the neutron activation analysis technique. The results showed that the impurities segregate preferentially in the ingot final section. A significant decrease of the impurities concentration in function of the purification pass number was observed. The grown crystals presented good crystalline quality according to the results of the X-ray diffraction analysis. To evaluate the crystal as a semiconductor detector, measurements of dark leakage current, resistivity and the response of ({sup 241}Am) alpha particle and ({sup 241}Am, {sup 57}Co, {sup 133}Ba and {sup 137}Cs) gamma rays were carried out. The radiation response is strongly dependent on the crystals purity. The crystals purified with 500 passes exhibited energy resolution of 10% for {sup 241} Am alpha particle and the gamma rays resolution was compatible with the literature. The photosensibility of the PbI{sub 2} crystal found in the wavelength from 400 to 600 nm range suggests an another application at this crystal as a photodetector to be coupled to scintillators. (author)

  7. Characterization of application of acu sandstone in ceramic mass; Caracterizacao da aplicacao do arenito acu na massa ceramica

    Nobrega, L.F.P.M.; Souza, M.M.; Gomes, Y.S.; Fernandes, D.L., E-mail: junior.luiz09@hotmail.com [Universidade Federal do Rio Grande do Norte (DIAREN/UFRN), Natal, RN (Brazil). Laboratorio de Processamento Mineral e Residuo

    2016-07-01

    The sandstone is a sedimentary rock formed mainly by quartz grains. In Rio Grande do Norte, there is the Potiguar Basin with the Jandaira and Acu Formations. The latter consists of thick layers of whitish-colored sandstones. It stands out as a water storage facility in the state, but it is also used for building aggregates. This article aimed at the use of the sandstone of this formation in the ceramic mass for coating. Initially, the material was sampled. It went through the comminution process to achieve the required granulometry. After this, three formulations were made to incorporate this new material into the traditional ones. The methods were performed according to ISO 13816. After sintering at 1200 °C, the specimens were subjected to the physical tests. A positive result was obtained for the use of the Acu sandstone in low concentrations. It is clear, therefore, its use in ceramics for coating.

  8. Synthesis and characterization of hydroxyapatite-doped silver nanoparticles; Sintese e caracterizacao de hidroxiapatita dopada com nanoparticulas de prata

    Andrade, Flavio Augusto Cavadas da Silva; Rollo, Joao Manuel Domingos de Almeida, E-mail: flavio.andrade@usp.br [Universidade de Sao Paulo (EESC/FMRP/IQSC/USP), Sao Carlos, SP (Brazil). Programa de Pos-Graduacao Interunidades Bioengenharia; Rigo, Eliana Cristina da Silva; Vercik, Andres; Vercik, Luci Cristina de Oliveira; Valencia, German Ayala; Ferreira, Leticcia Gaviao [Universidade de Sao Paulo (USP), Pirassununga, SP (Brazil). Faculdade de Zootecnia e Engenharia de Alimentos. Departamento de Ciencias Basicas

    2012-07-01

    Hydroxyapatite-doped silver nanoparticles was obtained by immersing the powder in increasing dilutions of a solution containing AGNPS which were synthesized in different times and were characterized by UV-vis spectroscopy. The X-ray diffraction (XRD)studies demonstrate no change in the major phase of HA. Scanning Electron Microscopy (SEM) revealed morphological characteristics of powders after doping and the presence of silver was confirmed by energy dispersive X-ray (EDAX) analysis.The antibacterial effect of the doped powders was evaluated using strain of Staphylococcus aureus by disc-diffusion test. The zone of inhibition was found to vary with the amount of silver nanoparticle in the doped powder even for low concentrations of AgNPs. These results indicate that the method of immersion hydroxyapatite in solutions containing AgNPs is promising to obtain bioactive materials with low cytotoxicity and antibacterial effects. (author)

  9. Preparation and characterization of the fish reference material; Preparacao e caracterizacao de um material de referencia de peixe

    Ulrich, Joao Cristiano

    2011-07-01

    The certified reference materials (CRMs) play an important role in obtaining measurement results traceable to the International System of Units, through an unbroken chain of comparisons. Thus, the demand for new certified reference materials (CRMs) increases every day in all areas of knowledge. The availability of reference materials, mainly in Brazil is still incipient, given that the demand far exceeds the available variety of these materials. The amount of certified reference materials available in the country is insufficient to meet the need of the scientific community and demands for development of new methodologies. Among the many areas in need of reference materials, we highlight the importance for the food trade balance for these products within the country. The certification of food products, intended both for export and for domestic consumption, requires analysis methods that provide precise and accurate results to ensure product quality. This paper describes the preparation and certification of a reference material in the fish matrix in mercury and methylmercury. The study brings together since the stage of material selection, preparation, development of homogeneity and stability studies and characterization. The certification was performed by means of measurements using two analytical techniques, flow injection analysis - cold vapor atomic absorption spectrometry (FIA-CV-AAS) and isotope dilution applied to mass spectrometry (IDMS), which is a primary method. In this work the standards of the ISO 30 (ABNT 30-34) and ISO Guide 35 was used as the basis for the preparation and characterization of the material. For the calculation of uncertainties was used the GUM and Eurachem guide. As a result, was produced and certified a lot of material in relation to the concentration of mercury (Hg = 0.271 {+-} 0.057 mg g{sup -1}) and methylmercury (MeHg = 0.245 {+-} 0.038 mg g{sup -1}), and informational values of lead and arsenic. (author)

  10. Study and characterization of the BBT (BaBi{sub 4}Ti{sub 4}O{sub 15}) ceramic added with 1 wt. % Nb{sub 2}O{sub 5}; Estudo e caracterizacao da ceramica BBT (BaBi{sub 4}Ti{sub 4}O{sub 15}) dopada com 1% de Nb{sub 2}O{sub 5}

    Silva, P.M.O.; Sales, A.J.M.; Freitas, D.B.; Oliveira, R.G.M.; Sombra, A.S.B., E-mail: paulo2003@gmail.com [Universidade Federal do Ceara (UFC), Fortaleza, CE (Brazil); Sales, J.C. [Universidade Estadual Vale do Acarau (UVA), Fortaleza, CE (Brazil)

    2012-07-01

    This study aims to synthesize and characterize the ceramic BBT (BaBi{sub 4}TI{sub 4}O{sub 15}) doped with 1% by mass of the densification Nb2O5 to improve the products. The phase of the BBT has been found by solid state reaction. The mixed oxides starting processed by high-energy milling in planetary mill reactor polymer and spheres of zirconia and calcined at 850°C/3h. Later, 'bulks' prepared with the calcined powder were sintered at 950°C/3h. The calcined powder was characterized by X-ray diffraction data and refined by the beta 3.2 DBWSTools program using the Rietveld method. The grain morphology and distribution of pores on the surface of the 'bulks' were analyzed by Scanning Electron Microscopy. The result confirmed the refined to obtain the single phase with tetragonal structure BaBi{sub 4}TI{sub 4}O{sub 15} density of 5.088 g/cm3 calculated in the unit cell. SEM analysis by SEM showed improved densification of the doped. (author)

  11. Characterization of beta radiation fields using radiochromic films; Caracterizacao de campos de radiacao beta utilizando filmes radiocromicos

    Benavente, Jhonny A.; Silva, Teogenes A. da, E-mail: jabc@cdtn.b [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil). Programa de Pos-Graduacao em Ciencia e Tecnologia das Radiacoes, Minerais e Materiais; Meira-Belo, Luiz C.; Reynaldo, Sibele R. [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil)

    2011-07-01

    The objective of this work was to study the response of radiochromic films for beta radiation fields in terms of absorbed dose. The reliability of the EBT model Gafchromic radiochromic film was studied. A 9800 XL model Microtek, transmission scanner, a 369 model X-Rite optical densitometer and a Mini 1240 Shimadzu UV spectrophotometer were used for measurement comparisons. Calibration of the three systems was done with irradiated samples of radiochromic films with 0.1; 0.3; 0.5; 0.8; 1.0; 1.5; 2.0; 2.5; 3.0; 3.5; 4.5 e 5.0 Gy in beta radiation field from a Sr-90/Y-90 source. Calibration was performed by establishing a correlation between the absorbed dose values and the corresponding radiochromic responses. Results showed significant differences in the absorbed dose values obtained with the three methods. Absorbed dose values showed errors from 0.6 to 4.4%, 0.3 to 31.8% and 0.2 to 47.3% for the Microtek scanner, the X-Rite Densitometer and the Shimadzu spectrophotometer, respectively. Due to the easy acquisition and use for absorbed dose measurements, the densitometer and the spectrophotometer showed to be suitable techniques to evaluate radiation dose in relatively homogeneous fields. In the case of inhomogeneous fields or for a two dimension mapping of radiation fields to identify anisotropies, the scanner technique is the most recommended. (author)

  12. Rietveld refinement, impedance spectroscopy and magnetic properties of Bi{sub 0.8}Sr{sub 0.2}FeO{sub 3} substituted Na{sub 0.5}Bi{sub 0.5}TiO{sub 3} ceramics

    Kumari, Rekha [Department of Applied Physics, Guru Jambheshwar University of Science & Technology, Hisar 125001, Haryana (India); Ahlawat, Neetu, E-mail: neetugju@yahoo.co.in [Department of Applied Physics, Guru Jambheshwar University of Science & Technology, Hisar 125001, Haryana (India); Agarwal, Ashish; Sanghi, Sujata [Department of Applied Physics, Guru Jambheshwar University of Science & Technology, Hisar 125001, Haryana (India); Sindhu, Monica [Department of Physics, MKJK College, Rohtak 124001, Haryana (India); Ahlawat, Navneet [Matu Ram Institute of Engineering and Management, Rohtak 124001, Haryana (India)

    2016-09-15

    We herein presented the investigation on the structural, electrical and magnetic properties of (1−x)(Na{sub 0.5}Bi{sub 0.5}TiO{sub 3})–x(Bi{sub 0.8}Sr{sub 0.2}FeO{sub 3}) polycrystalline ceramic samples, with x=0.1, 0.3, 0.5 and 0.7. These samples were prepared by conventional solid state reaction method and the crystalline phase of prepared ceramics was identified with the help of X-ray diffraction pattern. Rietveld analysis of the obtained XRD data confirmed that all the synthesized samples adopt the rhombohedral crystal structure with R3c space group. Impedance spectroscopic measurements were performed on all the compositions in the frequency range 10 Hz–5 MHz to probe the electrical microstructure of polycrystalline (1−x)(Na{sub 0.5}Bi{sub 0.5}TiO{sub 3})–x(Bi{sub 0.8}Sr{sub 0.2}FeO{sub 3}) ceramics, which changes significantly as a function of x (content of BSFO). A significant increase in dielectric constant has been observed with increase in BSFO concentration, which was attributed to enhancement of oxygen vacancies. Detailed study of impedance complex plane plots revealed the presence of non-Debye type relaxation for all the prepared systems and enabled us to separate the contribution from grains and grain boundaries. Equivalent circuit model (R{sub g}CPE{sub g})(R{sub gb}CPE{sub gb})(R{sub e}CPE{sub e}) was employed to explain the impedance data for all the prepared samples. The activation energies obtained from electric modulus as well as dc conductivity increase with increase in BSFO content, which approaches the value 1 eV and indicates an Arrehenius type thermally activated process. Remnant magnetization (M{sub r}) and coercive field (H{sub c}) are found to be increase with BSFO concentration. - Highlights: • (1−x)NBT–xBSFO (x=0.1, 0.3, 0.5, 0.7) ceramics were prepared. • There is no change in crystal structure. • These can be used as data storage materials.

  13. Method

    Ling Fiona W.M.

    2017-01-01

    Full Text Available Rapid prototyping of microchannel gain lots of attention from researchers along with the rapid development of microfluidic technology. The conventional methods carried few disadvantages such as high cost, time consuming, required high operating pressure and temperature and involve expertise in operating the equipment. In this work, new method adapting xurography method is introduced to replace the conventional method of fabrication of microchannels. The novelty in this study is replacing the adhesion film with clear plastic film which was used to cut the design of the microchannel as the material is more suitable for fabricating more complex microchannel design. The microchannel was then mold using polymethyldisiloxane (PDMS and bonded with a clean glass to produce a close microchannel. The microchannel produced had a clean edge indicating good master mold was produced using the cutting plotter and the bonding between the PDMS and glass was good where no leakage was observed. The materials used in this method is cheap and the total time consumed is less than 5 hours where this method is suitable for rapid prototyping of microchannel.

  14. method

    L. M. Kimball

    2002-01-01

    Full Text Available This paper presents an interior point algorithm to solve the multiperiod hydrothermal economic dispatch (HTED. The multiperiod HTED is a large scale nonlinear programming problem. Various optimization methods have been applied to the multiperiod HTED, but most neglect important network characteristics or require decomposition into thermal and hydro subproblems. The algorithm described here exploits the special bordered block diagonal structure and sparsity of the Newton system for the first order necessary conditions to result in a fast efficient algorithm that can account for all network aspects. Applying this new algorithm challenges a conventional method for the use of available hydro resources known as the peak shaving heuristic.

  15. Nano sized La2Co2O6 double perovskite synthesized by sol gel method

    Solanki, Neha; Lodhi, Pavitra Devi; Choudhary, K. K.; Kaurav, Netram

    2018-05-01

    We report here the synthesis of double perovskite La2Co2O6 (LCO) compound by a sol gel route method. The double perovskite structure of LCO system was confirmed via X-ray diffraction (XRD) analysis. Further, the lattice parameter, unit cell volume and bond length were refined by means of rietveld analysis using the full proof software. Debye Scherer formula was used to determine the particle size. The compound crystallized in triclinic structure with space group P-1 in ambient condition. We also obtained Raman modes from XRD spectra of poly-crystalline LCO sample. These results were interpreted for the observation of phonon excitations in this compound.

  16. Resveratrol-loaded poly({epsilon}-caprolactone) microparticles: preparation and characterization; Microparticulas de poli({epsilon}-caprolactona) contendo resveratrol: preparacao e caracterizacao

    NONE

    2011-07-01

    Resveratrol-loaded poly({epsilon}-caprolactone) (PCL) microparticles were obtained by simple emulsion/solvent evaporation method. Three drug-loaded formulations were prepared with the aim of investigating the influence of composition on the encapsulation efficiency. Morphological and spectroscopic methods were performed for these materials. The microparticles revealed residual moisture close to 1.5% and encapsulation efficiency above 80%. Spherical shape and smooth surface were observed by SEM. No pores were either verified. Resveratrol-loaded microparticles showed an average particle size of around 50 {mu}m. X-ray diffraction analysis demonstrated that the microencapsulation reduced the drug crystallinity. The FTIR results suggest that no chemical bond was formed between polymer and drug. (author)

  17. Marble waste characterization as a desulfurizing slag component for steel; Caracterizacao do residuo de marmore como componente de escorias dessulfurantes para aco

    Coleti, J.L.; Grillo, F.F.; Tenorio, J.A.S. [Universidade de Sao Paulo (USP), SP (Brazil); De Oliveira, J.R. [Instituto Federal do Espirito Santo (IFES), ES (Brazil)

    2014-07-01

    The current steel market requires from steel plants better quality of its products. As a result, steel plants need to search for improvements and costs reduction in its process. Hence, the residue of marble containing significant quantities of calcium and magnesium carbonates, raw materials of steel refining slag, was characterized in order to replace the conventional lime used. Therefore, it will be possible to reduce the cost and volume of waste produced by the ornamental rock industry. The following methods were applied to test the waste potential: SEM with EDS, x-ray diffraction, x-ray fluorescence (EDX), Thermogravimetry (TG) and analysis of surface area and particle size by the BET method using dispersion leisure. The results indicated the feasibility of waste as raw material in the composition of desulfurizing slags. (author)

  18. Characterization of contaminated oil with tritium, from of production of gas tripolar scintillators; Caracterizacao de oleo contaminado com tritio, proveniente da producao de centelhadores tripolares a gas

    Potiens Junior, Ademar J.; Marumo, Julio T.; Goes, Marcos M.; Isiki, Vera L.K. [Instituto de Pesquisas Energeticas e Nucleares (IPEN), Sao Paulo, SP (Brazil)

    2001-07-01

    The objective of this work was to develop a methodology to estimate the activity level present in radioactive oil samples. This oil is derived from vacuum pumps used to produce tension protector of electronic equipment in telecommunication area. The method consisted in obtain a calibration curve in counts per minute versus tritium activity. After the equipment calibration it was analyzed 3 batches of radioactive oil samples. (author)

  19. Physico-chemical characterization of biodiesel from pests attacked corn oil; Caracterizacao fisico-quimica do biodiesel de oleo de milho danificado por pragas

    Carvalho, Fabia M.; Correa, Paulo C.; Martins, Marcio A.; Santos, Silmara B.; Damian, Amanda D. [Universidade Federal de Vicosa (UFV), MG (Brazil)], Emails: copace@ufv.br, aredes@ufv.br, syllmara@vicosa.ufv.br

    2009-07-01

    The biodiesel is a renewable energy source alternative to fossil fuels. The biodiesel synthesis can be made by many types of triglycerides transesterification, it is possible to use this biofuel in vehicles if it has the quality required from Agencia Nacional de Petroleo, Gas Natural e Biocombustiveis (ANP). Searching an application for pests attacked corn, there is feasibility technical for the biodiesel production from this corn oil. The biodiesel synthesis was made through ethyl transesterification process with alkaline catalyst using ethanol. The biodiesel physical-chemical characterization was performed using ANP methods. (author)

  20. Characterization and improvement gas diffusion layer of low temperature fuel cell; Caracterizacao e aprimoramento da camada difusora de celulas a combustivel de funcionamento a baixa temperatura

    Ramos, C.Z.; Dantas, R.; Oliveira, I.S. de; Azevedo, C.M.N.; Pires, M. [Pontificia Univ. Catolica do Rio Grande do Sul (PUC-RS), Porto Alegre, RS (Brazil). Faculdade de Quimica; Canalli, V. [Pontificia Univ. Catolica do Rio Grande do Sul (PUC-RS), Porto Alegre, RS (Brazil). Faculdade de Engenharia

    2006-07-01

    In low temperature fuel cells the main part is the membrane electrode assembly (MEA). The gas diffusion layer is a component of the MEA, being a composite material constituted by carbon powder and polytetrafluoroethylene, used to increases hydrofobicity, fundamental characteristic in water transport into system. In this work methods were adapted with the aim to a better characterization of the diffusion layer by the measuring the following parameter: contact angle and hysteresis; morphology, thickness and porosity. From these characterization results optimized MEAS will be produced to better fuel cell performance. (author)

  1. Synthesis and characterization of semi-IPNs based on PVP and PLLA; Sintese e caracterizacao de semi-IPNs envolvendo os homopolimeros PVP e PLLA

    Camilo, A.P.R.; Mano, V., E-mail: mano@ufsj.edu.b [Universidade Federal de Sao Joao del Rei (UFSJ), MG (Brazil). Dept. de Ciencias Naturais; Felisberti, M.I. [Universidade Estadual de Campinas (IQ/UNICAMP), SP (Brazil). Inst. de Quimica

    2010-07-01

    The specific interest in the synthesis of semi-IPNs based on PLLA and PVP homopolymers due to the fact these are biodegradable and biocompatible, which allows us to infer applications in the medical field as sutures, implants, matrices for controlled release of drugs etc. The objective was to prepare a multicomponent material amphiphile in the form of semi-interpenetrating polymer networks, based on poly (L-lactide), PLLA, hydrophobic homopolymer, and poly (vinylpyrrolidone), PVP, hydrophilic component. The preparation of semi-IPN combined the polymerization and crosslinking of N-vinylpyrrolidone in the presence of poly (L-lactide). The products were characterized by spectroscopic and thermal methods. (author)

  2. Electrical characterization of zirconia-niobium and zirconia-titanium composites; Caracterizacao eletrica dos compositos zirconia-niobio e zirconia-titanio

    Reis, S.T. dos

    1994-12-31

    Zirconia-niobium and zirconia-titanium composites were made by powder mixing, cold pressing, and vacuum sintering at 1600{sup 0} C. The metallic particles were added in the proportion of 0-50% by volume. Electrical resistivity measurements were performed by the two probes and the four probes d.c. method as a function of metallic particle concentration. Electrical resistivity of these composites decreased sharply in the region of 30-40 vol% Nb or Ti, in agreement with the percolation theory. Tests in an induction furnace were performed to check the self-heating response of these composites. (author). 33 refs, 40 figs, 11 tabs.

  3. Synthesis and characterization of nanocomposite powders of calcium phosphate/silica-gel; Sintese e caracterizacao de pos nanoestruturados de fosfato de calcio/silica-gel

    Muller, D.T.; Delima, S.A. [Universidade do Estado de Santa Catarina (UDESC), Joinville, SC (Brazil). Dept. de Engenharia Mecanica; Santos, R.B.M.; Camargo, N.H.A., E-mail: dem2nhac@joinville.udesc.b [Universidade do Estado de Santa Catarina (UDESC), Joinville, SC (Brazil). Programa de Pos Graduacao em Ciencia e Engenharia de Materiais

    2009-07-01

    In the recent years ceramics of calcium phosphate are pointed out as an outstanding material in substitution and regeneration in defects from osseous tissue, in reason of their similar mineralogical characteristics of apatite of bone structure. However, the challenge with phosphate calcium ceramics find out about the mechanical properties and the development of biomaterials similar of the bone structure, what sometimes is not so easy, about fragile materials. The aim of this work focused in synthesis and characterization nanocomposites powders of calcium phosphate/silica-gel with percentages 1, 2, 3 e 5% of nanometric silica. The method synthesis used for the compositions elaboration was dissolution-precipitation. The presented results are related with the optimization to method elaboration of nanostructured powders, the mineralogical characterization with X-ray diffraction, thermal behavior with thermal differential analysis, differential scanning calorimetry here is ADT and dilatometer. The scanning electronic microscopy was used to help of morphological characterization the nanostructured powders and the surfaces from body test recovered from the mechanical test. (author)

  4. Characterization, analysis and dating of archaeological ceramics from the Amazon basin through nuclear techniques; Caracterizacao, analise e datacao de ceramicas arqueologicas da Bacia Amazonica atraves de tecnicas nucleares

    Latini, Rose Mary

    1998-07-01

    The aim of this work is to contribute to the research in the reconstruction of part of the pre-history of the Amazon Basin by means of an analytical methods combined with multivariate analysis, given a analytic basis that can be continued by the archaeological work, through the identification, classification, provenance and dating the ceramics found in different archaeological sites of the Hydro graphic Basin of the Purus river. Neutron activation analysis in conjunction multivariate statistical methods were used for the identification and classification and thermoluminescence was used for the dating. Chemical composition results were in better agreement with archaeological classification for the archaeologically define Iquiri, Quinan and Xapuri phases and less characteristics the Iaco and Jacuru archaeological phase were not well characterized. An homogeneous group was established by most of the samples collected from the Los Angeles Archaeological Site (LA) and was distinct from all the other groups analysed. The provenance studies made with ceramics collected at this site shows that they were made with clay from nearby river (Rio Ina). From the LA ceramics dating the average date of site occupation was 1660 years. The ceramic dating results from the external wall of a circular earth wall construction confirm the relation with the local pre-history. Beyond the Acre material two urns were dated from the Archaeological Site Morro Grande and Sao Jose at Araruama, Rio de Janeiro. (author)

  5. Validation of the method of quantitative phase analysis by X-ray diffraction in API: case of Tibolone

    Silva, R P; Ambrósio, M F S; Epprecht, E K; Avillez, R R; Achete, C A; Kuznetsov, A; Visentin, L C

    2016-01-01

    In this study, different structural and microstructural models applied to X-ray analysis of powder diffraction data of polymorphic mixtures of known concentrations of Tibolone were investigated. The X-ray data obtained in different diffraction instruments were analysed via Rietveld method using the same analytical models. The results of quantitative phase analysis show that regardless of the instrument used, the values of the calculated concentrations follow the same systematics with respect to the final errors. The strategy to select a specific analytical model that leads to lower measurement errors is here presented. (paper)

  6. Characterization of composite metal-ceramic of nickel-oxide cerium doped gadolinium; Caracterizacao de compositos ceramica-metal de niquel e oxido de cerio dopado com gadolinio

    Silva, M.L.A. da, E-mail: maria.andrade@pro.unifacs.br [Universidade Salvador (UNIFACS), BA (Brazil). Escola de Engenharia, Arquitetura e TI; Universidade Federal da Bahia (UFBA), BA (Brazil); Varela, M.C.R.S. [Universidade Federal da Bahia (UFBA), BA (Brazil)

    2016-07-01

    Composite nickel doped cerium oxide are used in SOFC anode materials. In this study we evaluated the effect of the presence of gadolinium on the properties of composite nickel and ceria and. The supports were synthesized by sol-gel method. The impregnation with nickel nitrate was taken sequentially, followed by calcination. The materials were characterized by X-ray diffraction, measurement of specific surface area, temperature programmed reduction, Raman spectroscopy. The presence of gadolinium retained the fluorite structure of ceria by forming a solid solution, also not influencing significantly on the specific surface area of the support. On the other hand, there was a decrease in the area catalysts, which can be attributed to sintering of nickel. Furthermore, addition of gadolinium favored the formation of intrinsic and extrinsic vacancies in cerium oxide, which leads to an increase in the ionic conductivity of the solid, desirable property for an SOFC anode catalyst. (author)

  7. Processing and characterisation of magnesia composites with graffiti and alumina addition; Processamento e caracterizacao de compositos magnesianos com adicao de grafite e alumina

    Carregosa, J.D.C.; Diniz, W.A.; Oliveira, R.M.P.B., E-mail: jdcovello@hotmail.com [Universidade Federal de Sergipe (UFS), Sao Cristovao, SE (Brazil)

    2016-07-01

    The use of refractory materials is of great importance for industries that use high temperature kilns, most of the internal components of the ovens do not support high temperatures and refractory blocks have the function to support, physically and chemically, direct contact with molten materials and also function as a thermal insulator. In this work were prepared 5 different formulations of Aluminum Magnesium Oxide refractory with added graphite. In a first step the characterization of the raw materials through the techniques of Particle Size analysis, X - ray fluorescence and X - ray diffraction, was also developed a method for formulating a binding system. Then the specimens were sintered at 1250 °C in stagnant atmosphere. The proposed refractories were assessed by determining the compressive strength, microstructural characterization by X - ray diffraction and Scanning Electron Microscopy. (author)

  8. Synthesis, characterization and electrical properties of solid electrolyte for solid oxide fuel cell; Preparacao, caracterizacao e propriedades eletricas de eletrolito solido para celula a combustivel de oxido solido

    Berton, Marco Antonio Coelho; Garcia, Carlos Mario; Matos, Jeferson Hrenechen [Instituto de Tecnologia para o Desenvolvimento (LACTEC), Curitiba, PR (Brazil)], Emails: felsky@latec.org.br, garcia@latec.org.br, jeferson.h@latec.org.br

    2010-04-15

    Solid electrolytes of BaCe{sub 08}Gd{sub O29} were prepared by the polymeric precursor method. X-ray diffraction data shows a single phase with orthorhombic crystalline structure. The densification process was followed by scanning electronic microscopy and apparent density measurements. The apparent density was developed for different temperatures of sintering, reaching > 96% for sintered temperature of 1550 {sup 0}C deg . The electrochemical impedance analysis was development in the temperature of 400-700 deg C, in air atmosphere at 700 deg C a value of 30,6 mS.cm{sup -1} was obtained. The results of conductivity have confirmed the gadolinium doped barium cerate has a great potential for use as solid electrolyte for intermediate temperature solid oxide fuel cell, at experimental controlled conditions. (author)

  9. Preparation and characterization of bentonite clays mixture destined to the removal of heavy metals; Preparacao e caracterizacao da mistura de argilas bentoniticas destinadas a remocao de metais pesados

    Almeida Neto, A.F. de; Silva, M.G.C. da, E-mail: ambrosio@feq.unicamp.b [Universidade Estadual de Campinas (UNICAMP), SP (Brazil). Fac. de Engenharia Quimica. Dept. de Termofluidodinamica

    2009-07-01

    In this work a mixture was prepared with 50% wt. of the Bofe and Verde-lodo clays. The characterization methods used they were: thermal analyses (TG and DTG), X-ray diffraction, fisissorption of N{sub 2}, scanning electron microscopy and X-ray energy dispersive spectroscopy. The rehearsals of adsorption we accomplished in system of finite bath using as adsorbent the mixture loamy in natura or it mixes calcined. Starting from TG and DTG a thermal treatment was accomplished to 500 deg C of the loamy mixture. Through the results of the copper adsorption, it was verified that mixes loamy it provokes chemical precipitation of the copper while the calcined sample presents amount metal adsorbed around 7.31 mg of copper/g of adsorbent. The value of removal percentage obtained by the calcined sample it was of 63.02%. (author)

  10. Characteristics of the radiochromic film Gafchromictm EBT3 model for use in brachytherapy; Caracterizacao do filme radiocromico Gafchromictm modelo EBT3 para uso em braquiterapia

    Luvizotto, Jessica

    2015-07-01

    Brachytherapy is a radiotherapy treatment modality using radioactive sealed sources within walking distance of the tumor, reducing the risk of applying an unwanted dose to adjacent healthy tissues. For brachytherapy is reliable, it is necessary to establish a dosimetric practices program aimed at determining the optimal dose of radiation for this radiotherapy practice. This paper presents the application of two methodologies for the dosimetry using radiochromic films. Experimental measurements were performed with EBT3 films in phantoms consisting of homogeneous and heterogeneous material (lung, bone and soft tissue) built especially for dose measurements in brachytherapy. The processing and analysis of the resulting images of the experimental procedure were performed with ImageJ software and MATLAB. The results were evaluated from comparisons dose of experimental measurements and simulations obtained by the Monte Carlo method. (author)

  11. Superficial characterization of titanium league when submitted to abrasive blasting; Caracterizacao superficial de titanio liga ao ser submetido a tratamento de jateamento

    Suzuki, L.Y.; Leite, I.V.; Szesz, E.M.; Siqueira, C.J.M., E-mail: lsuzuki@neoortho.com.b [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil)

    2010-07-01

    Commercially pure titanium and some of its alloys exhibit a good biocompatibility. These characteristics are frequently used in the manufacture of orthopedic and dental implants. It is possible to modify its surface making it the bioactive using various methods, such as deposition of hydroxyapatite by plasma spray and increasing the roughness of the surface by abrasive blasting. This work is to modify the surface of titanium alloy Ti6Al4V ELI (ASTM F136: 02a) for abrasive blasting and study the morphology, crystallographic phases and the mechanical characteristics of the surface obtained. For such purpose, SEM images, diffraction of X-rays and tests of risk produced by nanoindenter. The sandblasting was done using alumina powder and blasting time of 6s. The morphology of the surfaces of Ti6Al4V ELI changed after sandblasting with increased roughness. It is possible to conclude that after sandblasting the titanium surface do not have a ductile behavior. (author)

  12. Application of artificial neural networks on the characterization of radioactive waste drums; Aplicacao de redes neurais artificiais na caracterizacao de tambores de rejeito radioativo

    Potiens Junior, Ademar Jose; Hiromoto, Goro, E-mail: apotiens@ipen.b, E-mail: hiromoto@ipen.b [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2011-10-26

    The methodology consist of system simulation of drum-detector by Monte Carlo for obtention of counting efficiency. The obtained data were treated and a neural artificial network (RNA) were constructed for evaluation of total activity of drum. For method evaluation measurements were performed in ten position parallel to the drum axis and the results submitted to the RNA. The developed methodology showed to be effective for isotopic characterization of gamma emitter radioactive wastes distributed in a heterogeneous way in a 200 litters drum. The objective of this work as to develop a methodology of analyse for quantification and localization of radionuclides not homogeneous distributed in a 200 liters drum based on the mathematical techniques

  13. Characterization of two clays - attapulgite and sepiolite - before and after acid activation; Caracterizacao de duas argilas - atapulgita e sepiolita - antes e apos ativacao acida com HCl

    Oliveira, R.N.; Soares, G.A., E-mail: renataoliveira@poli.ufrj.b [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil). Centro de Tecnologia; Barreto, L.S. [Universidade Federal de Sergipe (UFS), Sao Cristovao, SE (Brazil)

    2009-07-01

    Among the special clays, two of them are distinguished by their large surface area: attapulgite and sepiolite. Although, being natural clays, when they are removed from the formation sites, their structural channels may be filled of impurities. The process done to clean these channels is called acid activation. The present work aim to treated samples from both clays by using 3M and 5M HCl solution under ultrasonic waves for 1 hour. The characterization of the clays before and after activation was carried out by SEM/EDS, XRD and surface area measure by method BET. The acid treatments employed were too aggressive, in special that with 5M HCl solution, which results in partial lixiviation of these clays. (author)

  14. Physicochemical characterization of ceramics from Sao Paulo II archaeological site; Caracterizacao fisico-quimica da ceramica do sitio arqueologico Sao Paulo II

    Ribeiro, Rogerio Baria

    2013-08-01

    Archaeometry is a consolidated field with a wide application of nuclear analytical techniques for the characterization, protection, and restoration of archaeological pieces. This project aimed at studying the elementary chemical composition of 70 ceramic fragments samples from Sao Paulo II archaeological site, located along the Solimoes River channel, next to Coari city, in Brazilian Amazon. The characterization of samples was performed by neutron activation analysis (NAA). By the determination of 24 elements in the ceramic fragments ( Ce, Co, Cr, Cs, Eu, Fe, Hf, K, La, Lu, Na, Nd, Sb, Sm. Rb, Se, Ta, Tb, Th, U, Yb and Zn), it was possible to define groups of samples regarding the similarity/dissimilarity in elementary chemical composition. For such a task, the multivariate statistical methods employed were cluster analysis (C A), principal component analysis (PCA) and discriminant analysis (DA). Afterwards, seven ceramic fragments were selected based on the groups previously established, for the characterization of the site temporal horizon. Those ceramic fragments were analyzed by thermoluminescence (TL) and EPR for dating purposes. The firing temperatures were determined by electron paramagnetic resonance (EPR) technique, in order to infer about some aspects of the ceramic manufacture employed by the ancient peoples that lived in Sao Paulo 11. By the results obtained in this study, it was possible to identify the quantity of clay sources employed by the ceramists and the age of the ceramic pieces. Therefore, the results of this research may contribute to the study on the occupation dynamics in the pre-colonial Brazilian Amazon. (author)

  15. Esterification and characterization of lignin aiming the synthesis of polymeric composite; Esterificacao e caracterizacao da lignina visando a sintese de compositos polimericos

    Victor, Priscilla A.; Machado, Fabricio, E-mail: fmachado@unb.br [Universidade de Brasilia (UnB), DF (Brazil). Instituto de Quimica; Goncalves, Silvia B., E-mail: silvia.belem@embrapa.br [Embrapa Agroenergia, Parque Estacao Biologica (PqEB), Brasilia, DF (Brazil)

    2015-07-01

    Lignin is a natural polymer derived from lignocellulosic materials with high availability, presenting a huge potential for production of new materials. Due to its complex macromolecular structure, and its low compatibility with styrene, eucalyptus wood-extracted lignin method was esterified with methacrylic anhydride - exhibiting a yield of 64% - in order to ensure homogeneity in the organic phase into the reaction medium. The evaluation of both the natural and esterified lignin through infrared (IR) spectroscopy showed a decrease of the hydroxyl band, characteristic of natural lignin (3200-3400 cm{sup -1}) and an increase of the characteristic ester band (1720 to 1740 cm{sup -1}). According to nuclear magnetic resonance ({sup 1}H NMR) analysis on esterified lignin, intense peaks were observed in the range from 1.7 to 2.05 ppm (-CH{sub 3}) and 5.4 ppm to 6.2 ppm (=CH{sub 2}), related to methacrylic anhydride. According to the thermogravimetric analysis (TGA), the esterified lignin showed a decrease in its thermal stability when compared to natural lignin, exhibiting two main weight losses between 200 °C and 300 °C and in the interval from 550 °C to 800 °C. Comparatively, the esterified lignin also displayed an increase in its glass transition temperature (Tg = 98 °C) for, when compared to natural lignin, whose Tg value was determined to be equal to 91 °C. (author)

  16. Morphologic characterization and quantitative analysis on in vitro bacteria by nuclear techniques of measurement; Caracterizacao morfologica e analise quantitativa de bacterias in vitro por tecnicas nucleares de medidas

    Lopes, Joana D' Arc Ramos

    2001-10-01

    The great difficulty to identify microorganisms (bacteria) from infectious processes is related to the necessary time to obtain a reliable result, about 72 hours. The purpose of this work is to establish a faster method to characterize bacterial morphologies through the use of neutron radiography, which can take about 5 hours. The samples containing the microorganisms, bacteria with different morphologies, after the appropriate microbiologic procedures were incubated with B{sup 10} for 30 minutes and soon after deposited in a plate of a solid detector of nuclear tracks (SSNTD), denominated CR-39. To obtain the images relative to bacteria, the detector was submitted to the flow of thermal neutrons of the order of 2.2 x 10{sup 5} n/cm{sup 2}.s from the J-9 channel of the Reactor Argonauta (IEN/CNEN). To observe the images from bacteria in each sample under an optical microscope, the sheets were chemically developed. The analysis of the images revealed morphologic differences among the genera (Gram positive from Gram-negative and coccus from bacillus), in samples containing either isolated or mixed bacteria. We thus verified the viability of the technique to achieve morphological characterization of different microorganisms. A quantitative approach seemed also to be feasible with the technique. The whole process took about 2 hours. (author)

  17. Fishing activity characterization in areas under influence of seismic activity; Caracterizacao da atividade pesqueira em areas sob influencia da atividade sismica

    Fuse, Izabel Yukimi; Zanella, Joao Francisco Illa Font; Eliseire Junior, Dirceu; Pereira, Edisio [Hidrosfera Oceanografia e Meio Ambiente, Rio de Janeiro, RJ (Brazil); Souza, Sergio Augusto Coelho de; Ferraz, Alexandre; Costa, Leandro Soares da; Vidal, Leonardo; Duppre, Mauricio [Okeanos Consultoria e Meio Ambiente Ltda. (Brazil); Uller, George [CGG do Brasil, Rio de Janeiro, RJ (Brazil)

    2004-07-01

    Seismic surveys are an important method in prospecting for oil and gas reservoirs in the marine environment. The ELPN/IBAMA has required that companies develop an adequate social programme in parallel with the seismic surveys to establish a better interaction with the communities influenced by these operations and reduce possible negative effects. Between January and October 2003, CGG Brazil studied coastal communities in the following areas. BM-CE-1 e BM -CE-2, Ceara; Fragata, BM-ES-5 e BM-ES-6, Espirito Santo; BM BAR-1 e BM BAR-3, Maranhao and BM-C-25 and BM-C-16 off Campos basin. Communities and groups that could potentially be influenced by the surveys were visited to mitigate direct and indirect impacts. Preliminary results show that fisheries were the main group to be monitored. A standard questionnaire was used to characterize the local fisheries and interviews were held with fishermen, boat owners and members of the fishery industries (n=422). In Ceara the fishery is typically handmade and occurs in water depths up to 200 meters. The main boat propulsion is sail and the 'Cacoeira' is the most popular gear used. Off Espirito Santo, small and medium motored boats are usually used and line is the main gear among the fishermen. At Barreirinhas (Maranhao), boats are usually up to 14 meters long, and operate in water depths of up to 120 metres. Again the 'cacoeira' is the proffered gear. We concluded that Programs carried out by CGG reached their purpose. This is confirmed by low incident rate between seismic ships and the fisheries fleet. (author)

  18. Structural analysis and magmatism characterization of the Major Gercino shear zone, Santa Catarina State, Brazil; Analise estrutural e caracterizacao do magmatismo da zona de cisalhamento Major Gercino, SC

    Passarelli, Claudia Regina

    1996-12-31

    This work describes the geometric and kinematic characteristics of the Major Gercino Shear Zone (MGSZ) in the Canelinha-Garcia area. This shear zone is one of the major lineaments that affect all southern Brazilian precambrian terrains. In Santa Catarina State, it separates, along its whole extension, the supracrustal rocks of the Brusque belt (northern part) from the Granitoid belt (southern). This zone is characterized by a regional NE trend and a dextral sense of movement where ductile-brittle structures predominate. The MGSZ is composed of two mylonitic belts separated by granitoid rocks probably associated to the development of the shear zone. Both shear zones show cataclastic to ultra mylonitic rocks, but mylonites and protomylonites conditions at high strain rate. The calc-alkaline granitoids present in the area can be grouped in two granitoid associations with meta to peraluminous affinities. The Rolador Granitoid Association is characterized by grayish porphyritic biotite-monzogranites and the Fernandes Granitoid Association by coarsed-grained to porphyritic pinkish amphibole-syenogranites. The U-Pb and Rb-Sr ages range from 670 to 590 Ma with the Sr{sup 87} / Sr{sup 86} initial ratios suggesting a crustal contribution in the generation of these rocks. The importance of the pure shear component is also emphasized by the results of the Fry method. Many z axes of the strain ellipses are at high angle to the shear foliation. Symmetric porphyroclasts also corroborate this hypothesis. The micaceous minerals formed during the shear development indicate K-Ar ages around 555 {+-} 15 Ma. Brittle reactivations of the shear zone have been placed by K-Ar in fine-fraction materials at Triassic time (215 {+-} 15 Ma.) 220 refs., 107 figs., 18 tabs., 4 maps

  19. Synthesis of zeolites from boiler fly ash: physical, chemical and mineralogical characterization; Sintese de zeolitas a partir de cinza volante de caldeiras: caracterizacao fisica, quimica e mineralogica

    Rocha Junior, C.A.F.; Santos, S.C.A.; Souza, C.A.G., E-mail: augustorocha2@gmail.com [Programa de Pos Graduacao em Engenharia Quimica (PPEQ-UFPA), Belem, PA (Brazil); Angelica, R.S.; Neves, R.F. [Programa de Pos-Graduacao em Geologia e Geoquimica, Instituto de Geociencias (PPGG-IG-UFPA), Ananindeua, PA (Brazil)

    2012-01-15

    Along the years, worldwide industrial development has causing a growing generation of residues, bringing potentials environmental problems. A study of the characteristics of these wastes, as well as the development of techniques for their use in new processes becomes indispensable for the environment preservation. The main purpose of this work is to evaluate the possible use of two important industrial residues from the Amazon region for zeolite synthesis: (a) the fly ash (particle size < 100 {mu}m) that comes from burning of mineral coal in boiler; and (b) the micro silica, a by-product of the reaction between quartz and coal in the production of metallic silicon and alloys iron-silicon.The following chemical, physical and mineralogical characterization methods were carried out: X-ray diffractometry, X-ray fluorescence, scanning electron microscopy, granulometric analysis, differential thermal and thermogravimetric analysis (DTA-TG). The analyses were carried out at the following conditions: 60, 100, 150 and 190 deg C, Na{sub 2}O/Al{sub 2}O{sub 3} molar ratio of 5 and Si/Al molar ratio ranging from 2.12 to 15, and reaction time of 24 h. The results of the fly characterization demonstrate its enormous potential as raw material for the zeolite synthesis. SiO{sub 2} and Al{sub 2}O{sub 3} represent more than 50% of its composition, mineralogical phases defined, low humidity content, low particle size (d{sub 90} < 10 {mu}m), among others. Mineralogical analyses of the synthesized products showed the formation of some zeolite types, as follow: analcime, phillipsite, sodalite, zeolite P and tobermorite. The results show that the mixture fly ash-micro silica in these reaction conditions point to a promising material for zeolite synthesis (author)

  20. Chemical and radiological characterization of meals served by the COSEAS (USP-SP); Caracterizacao quimica e radiologica de refeicoes servidas pelo COSEAS/USP-SP

    Favaro, Deborah Ines Teixeira [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), SP (Brazil). Centro do Reator de Pesquisas. Lab. de Analise por Ativacao Neutronica], e-mail: defavaro@ipen.br; Chioccola, Gabriella Saitta; Bortoli, Maritsa; Cozzolino, Silvia Maria Franciscato [Universidade de Sao Paulo (USP), SP (Brazil). Faculdade de Ciencias Farmaceuticas. Lab. de Alimentos e Nutricao Experimental; Taddei, Maria Helena [Comissao Nacional de Energia Nuclear (CNEN), Pocos de Caldas, MG (Brazil). Coordenacao do Laboratrio de Pocos de Caldas (COLAB); Mazzilli, Barbara Paci [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), SP (Brazil). Div. de Radiometria Ambiental

    2009-01-15

    This study presents the results obtained for the chemical and radiological analyses of lunch meals served in the cafeteria at the University of Sao Paulo-USP (COSEAS restaurant) in Brazil, on 5 non-consecutive days. On each of the five days, the meals were collected in triplicate and then freeze-dried for analysis totalizing 15 samples. The determination of the proximate composition complied with the AOAC standardized methodologies. The content of Ca, Fe, K, Na, Se, and Zn was determined by instrumental neutron activation analysis and the method validation was performed by certified reference materials analyses. Based on the concentration data, the daily intake of each mineral was calculated (corresponding to 40% of the total daily intake) and compared to the new recommendations set by the National Research Council (USA) considering the 19-30 year-old women range group. Comparing the average values obtained in this study with the recommended values, it was possible to verify that for macronutrients and the micronutrients Fe, Se, and Zn the recommendations were followed; for Ca and K they were deficient and exceeded the recommendation value for Na. The radionuclides {sup 40}K, {sup 60}Co, {sup 137}Cs, and {sup 131}I were determined by gamma spectrometry; {sup 90}Sr by liquid scintillation and {sup 210}Po, {sup 234}U, {sup 232}Th, {sup 238}U, {sup 235}U, {sup 228}Th, {sup 230}Th, and {sup 232}Th by alpha spectrometry. All radionuclides are present in concentrations below the limits set by the Food and Agriculture Organization (FAO). (author)

  1. Nanostructured synthetic hydroxyapatite and dental enamel heated and irradiated by ER,CR:YSGG: characterized by FTIR and XRD; Hidroxiapatita sintetica nanoestruturada e esmalte dental aquecidos e irradiados por laser de Er,Cr:YSGG: caracterizacao por FTIR e por DRX

    Rabelo Neto, Jose da Silva

    2009-07-01

    The study evaluate the physical changes and/or chemical that occurs in synthetic hydroxyapatite (HAP) and in enamel under action of thermal heating in oven or laser irradiation of Er,Cr:YSGG that may cause changes in its structure to make them more resistant to demineralization aiming the formation of dental caries. The synthetic HAP was produced by reaction of solutions of Ca(NO{sub 3}) and (NH{sub 4}){sub 2}HPO{sub 4} with controlled temperature and pH. The enamel powder was collected from the bovine teeth. Samples of powder enamel and synthetic HAP were subjected to thermal heating in oven at temperatures of 200 deg C, 400 deg C, 600 deg C, 800 deg C and 1000 deg C. For the laser irradiation of materials, were made with 5,79 J/cm{sup 2} of irradiation, 7,65 J/cm{sup 2}, 10,55 J/cm{sup 2} and 13,84 J/cm{sup 2} for synthetic HAP and 7,53 J/cm{sup 2}, 10,95 J/cm{sup 2}, and 13,74 J/cm{sup 2} for the enamel. The samples were evaluated by X-ray diffraction (XRD) for analysis of crystallographic phases and analysis by the Rietveld method, to determine their respective proportions in the material, as well as results of changes of the lattice unit cell parameters (axis-a, axis-c and volume), crystallites sizes and the occupation rate of sites of Ca and P atoms. The samples were analyzed by Fourier transform infrared spectroscopy (FTIR), which should compositional changes due to treatment related to carbonate, phosphate, adsorbed water and hydroxyl radicals content. The infrared was used to measure the surface temperature generated by the laser beam in the solid samples of enamel. Besides the major hydroxyapatite crystallographic phases, there was formations of octa calcium phosphate (OCP) and phase {beta} of tricalcium phosphate ({beta}-TCP ) in enamel heated at 800 deg C. There was reduction of the axis-a, volume and size of crystallites to the temperatures between 400 degree C and 600 deg C and also on laser irradiated samples. Above the temperature of 600 degree C it

  2. Method for fitting crystal field parameters and the energy level fitting for Yb3+ in crystal SC2O3

    Qing-Li, Zhang; Kai-Jie, Ning; Jin, Xiao; Li-Hua, Ding; Wen-Long, Zhou; Wen-Peng, Liu; Shao-Tang, Yin; Hai-He, Jiang

    2010-01-01

    A method to compute the numerical derivative of eigenvalues of parameterized crystal field Hamiltonian matrix is given, based on the numerical derivatives the general iteration methods such as Levenberg–Marquardt, Newton method, and so on, can be used to solve crystal field parameters by fitting to experimental energy levels. With the numerical eigenvalue derivative, a detailed iteration algorithm to compute crystal field parameters by fitting experimental energy levels has also been described. This method is used to compute the crystal parameters of Yb 3+ in Sc 2 O 3 crystal, which is prepared by a co-precipitation method and whose structure was refined by Rietveld method. By fitting on the parameters of a simple overlap model of crystal field, the results show that the new method can fit the crystal field energy splitting with fast convergence and good stability. (condensed matter: electronic structure, electrical, magnetic, and optical properties)

  3. Rietveld analysis, dielectric and impedance behaviour of Mn /Fe ion ...

    Figure 1 compares X-ray diffraction patterns of pow- ders calcined at temperature .... ground, absorption coefficient, atomic positions, two theta zero error, thermal ... attributed to segregation of Mn and Fe at grain boundaries. (Dai et al 1995).

  4. Electronic structure and magnetic properties of FeWO{sub 4} nanocrystals synthesized by the microwave-hydrothermal method

    Almeida, M.A.P. [INCTMN-DQ-Universidade Federal de Sao Carlos, Sao Carlos, P.O. Box 676, 13565-905, SP (Brazil); Cavalcante, L.S., E-mail: laeciosc@bol.com.br [INCTMN-Universidade Estadual, Paulista, P.O. Box 355, 14801-907, Araraquara, SP (Brazil); Morilla-Santos, C.; Filho, P.N. Lisboa [MAv-Universidade Estadual, Paulista, P.O. Box 473, 17033-360, Bauru, SP (Brazil); Beltran, A.; Andres, J.; Gracia, L. [Department de Quimica Fisica i Analitica, Universitat Jaume I, E-12071 Castello (Spain); Longo, E. [INCTMN-DQ-Universidade Federal de Sao Carlos, Sao Carlos, P.O. Box 676, 13565-905, SP (Brazil); INCTMN-Universidade Estadual, Paulista, P.O. Box 355, 14801-907, Araraquara, SP (Brazil)

    2012-11-15

    This communication reports that FeWO{sub 4} nanocrystals were successfully synthesized by the microwave-hydrothermal method at 443 K for 1 h. The structure and shape of these nanocrystals were characterized by X-ray diffraction, Rietveld refinement, and transmission electron microscopy. The experimental results and first principles calculations were combined to explain the electronic structure and magnetic properties. Experimental data were obtained by magnetization measurements for different applied magnetic fields. Theoretical calculations revealed that magnetic properties of FeWO{sub 4} nanocrystals can be assigned to two magnetic orderings with parallel or antiparallel spins in adjacent chains. These factors are crucial to understanding of competition between ferro- and antiferromagnetic behavior. Highlights: Black-Right-Pointing-Pointer Monophasic FeWO{sub 4} nanocrystals were synthesized by the microwave-hydrothermal method. Black-Right-Pointing-Pointer Rietveld refinement and clusters model for monoclinic structure Black-Right-Pointing-Pointer Magnetic properties of FeWO{sub 4} nanocrystals at different temperatures.

  5. Synthesis and characterization of Fe{sub 3}O{sub 4} nanoparticles stabilized by polyvinylpyrrolidone / polyethylene glycol with variable mass ratios; Sintese e caracterizacao de nanoparticulas de Fe{sub 3}O{sub 4} estabilizadas pelo sistema polivinilpirrolidona/polietilenoglicol em proporcoes massicas variaveis

    Silva, F.A.S. da; Campos, M.F. de; Rojas, E. E.G., E-mail: fernandasampaio@id.uff.br [Universidade Federal Fluminense (EEIMVR/UFF), Volta Redonda, RJ (Brazil)

    2014-07-01

    Magnetic nanoparticles are devices able to optimize cancer treatments. In particular, magnetite nanoparticles are very effective in producing heat to cause lysis of tumor cells. However, in order that nanoparticles are internalized without causing damage to body they must be coated by biocompatible material. In this work, Fe{sub 3}O{sub 4} nanoparticles were coated by a polymer blend: polyethylene glycol / polyvinylpyrrolidone. Some variations in mass ratio of polymer mixture were made. The effect of varying mass ratio in polymers was investigated. Samples were characterized by X-ray diffraction and Rietveld analysis. Moreover, hysteresis curves were analyzed. The results indicate good agreement between mass proportions used and physical and magnetic properties of nanocomposite. (author)

  6. A new method of Debye-Scherrer pattern integration on two-dimensional detectors, demonstrated for the new structure powder diffractometer (SPODI) at the FRM-II in Garching

    Elf, F; Artus, G R J; Roth, S

    2002-01-01

    The expected diffraction patterns of the new powder diffractometer SPODI, currently under construction at the FRM-II in Garching, will be smeared Debye-Scherrer rings as depicted by Monte Carlo (MC) simulations. To overcome this disadvantage, a concept based on the combination of MC simulations and empirical approximation methods is developed to reverse the smearing by deconvolution and then summing up along the rings, including corrections for different arc lengths, resulting in conventional one-dimensional diffraction patterns suitable for Rietveld-refinement programs without further processing. (orig.)

  7. Solution combustion method for synthesis of nanostructured hydroxyapatite, fluorapatite and chlorapatite

    Zhao, Junjie; Dong, Xiaochen; Bian, Mengmeng; Zhao, Junfeng; Zhang, Yao; Sun, Yue; Chen, JianHua; Wang, XuHong

    2014-09-01

    Hydroxyapatite (HAP), fluorapatite (Fap) and chlorapatite (Clap) were prepared by solution combustion method with further annealing at 800 °C. The characterization and structural features of the synthesized powders were evaluated by the powder X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FT-IR), scanning electron microscope (SEM) and transmission electron microscopy (TEM) techniques. Characterization results from XRD and Rietveld analysis revealed that OH- in the HAP lattice were gradually substituted with the increase of F- and Cl- content and totally substituted at the molar concentration of 0.28 and 0.6, respectively. The results from FI-IR have also confirmed the incorporation of substituted anions in the apatite structure.

  8. Microstructural study of Ce1-xGdxO2-δ (x = 0.1 and 0.2) nano crystallized powders synthesized by the polymeric precursor method

    Cela, B.; Macedo, D.A.; Souza, G.L.; Paskocimas, C.A.; Martinelli, A.E.; Nascimento, R.M.

    2009-01-01

    Gadolinia-doped ceria powders (Ce 1-x Gd x O 2-δ ) were prepared with substitution of 10 and 20% of the dopant element by the polymeric precursor method. This method makes possible the attainment of homogeny powder in molecular level, ideal to application in Solid Oxide Fuel Cell (SOFC) component. In this work, the particulated materials were calcinated in a range from 500 °C to 900 °C and structurally characterized by X-Ray Diffraction (XRD). The sintering behaviors of the compact samples were determined by dilatometric analyses. The results showed the method efficiency to attain monophasic nanopowder with cubic crystalline structure starting at 700 °C. The crystallite average size and crystalline parameter were determined by the Rietveld refinement method. (author)

  9. Quantitative firing transformations of a triaxial ceramic by X-ray diffraction methods

    Conconi, M.S.; Gauna, M.R.; Serra, M.F.; Suarez, G.; Aglietti, E.F.; Rendtorff, N.M.

    2014-01-01

    The firing transformations of traditional (clay based) ceramics are of technological and archaeological interest, and are usually reported qualitatively or semi quantitatively. These kinds of systems present an important complexity, especially for X-ray diffraction techniques, due to the presence of fully crystalline, low crystalline and amorphous phases. In this article we present the results of a qualitative and quantitative X-ray diffraction Rietveld analysis of the fully crystalline (kaolinite, quartz, cristobalite, feldspars and/or mullite), the low crystalline (metakaolinite and/or spinel type pre-mullite) and glassy phases evolution of a triaxial (clay-quartz-feldspar) ceramic fired in a wide temperature range between 900 and 1300 deg C. The employed methodology to determine low crystalline and glassy phase abundances is based in a combination of the internal standard method and the use of a nanocrystalline model where the long-range order is lost, respectively. A preliminary sintering characterization was carried out by contraction, density and porosity evolution with the firing temperature. Simultaneous thermo-gravimetric and differential thermal analysis was carried out to elucidate the actual temperature at which the chemical changes occur. Finally, the quantitative analysis based on the Rietveld refinement of the X-ray diffraction patterns was performed. The kaolinite decomposition into metakaolinite was determined quantitatively; the intermediate (980 deg C) spinel type alumino-silicate formation was also quantified; the incongruent fusion of the potash feldspar was observed and quantified together with the final mullitization and the amorphous (glassy) phase formation.The methodology used to analyze the X-ray diffraction patterns proved to be suitable to evaluate quantitatively the thermal transformations that occur in a complex system like the triaxial ceramics. The evaluated phases can be easily correlated with the processing variables and materials

  10. Quantitative firing transformations of a triaxial ceramic by X-ray diffraction methods

    Conconi, M.S.; Gauna, M.R.; Serra, M.F. [Centro de Tecnologia de Recursos Minerales y Ceramica (CETMIC), Buenos Aires (Argentina); Suarez, G.; Aglietti, E.F.; Rendtorff, N.M., E-mail: rendtorff@cetmic.unlp.edu.ar [Universidad Nacional de La Plata (UNLP), Buenos Aires (Argentina). Fac. de Ciencias Exactas. Dept. de Quimica

    2014-10-15

    The firing transformations of traditional (clay based) ceramics are of technological and archaeological interest, and are usually reported qualitatively or semi quantitatively. These kinds of systems present an important complexity, especially for X-ray diffraction techniques, due to the presence of fully crystalline, low crystalline and amorphous phases. In this article we present the results of a qualitative and quantitative X-ray diffraction Rietveld analysis of the fully crystalline (kaolinite, quartz, cristobalite, feldspars and/or mullite), the low crystalline (metakaolinite and/or spinel type pre-mullite) and glassy phases evolution of a triaxial (clay-quartz-feldspar) ceramic fired in a wide temperature range between 900 and 1300 deg C. The employed methodology to determine low crystalline and glassy phase abundances is based in a combination of the internal standard method and the use of a nanocrystalline model where the long-range order is lost, respectively. A preliminary sintering characterization was carried out by contraction, density and porosity evolution with the firing temperature. Simultaneous thermo-gravimetric and differential thermal analysis was carried out to elucidate the actual temperature at which the chemical changes occur. Finally, the quantitative analysis based on the Rietveld refinement of the X-ray diffraction patterns was performed. The kaolinite decomposition into metakaolinite was determined quantitatively; the intermediate (980 deg C) spinel type alumino-silicate formation was also quantified; the incongruent fusion of the potash feldspar was observed and quantified together with the final mullitization and the amorphous (glassy) phase formation.The methodology used to analyze the X-ray diffraction patterns proved to be suitable to evaluate quantitatively the thermal transformations that occur in a complex system like the triaxial ceramics. The evaluated phases can be easily correlated with the processing variables and materials

  11. Quantitative firing transformations of a triaxial ceramic by X-ray diffraction methods

    M. S. Conconi

    2014-12-01

    Full Text Available The firing transformations of traditional (clay based ceramics are of technological and archeological interest, and are usually reported qualitatively or semiquantitatively. These kinds of systems present an important complexity, especially for X-ray diffraction techniques, due to the presence of fully crystalline, low crystalline and amorphous phases. In this article we present the results of a qualitative and quantitative X-ray diffraction Rietveld analysis of the fully crystalline (kaolinite, quartz, cristobalite, feldspars and/or mullite, the low crystalline (metakaolinite and/or spinel type pre-mullite and glassy phases evolution of a triaxial (clay-quartz-feldspar ceramic fired in a wide temperature range between 900 and 1300 ºC. The employed methodology to determine low crystalline and glassy phase abundances is based in a combination of the internal standard method and the use of a nanocrystalline model where the long-range order is lost, respectively. A preliminary sintering characterization was carried out by contraction, density and porosity evolution with the firing temperature. Simultaneous thermo-gravimetric and differential thermal analysis was carried out to elucidate the actual temperature at which the chemical changes occur. Finally, the quantitative analysis based on the Rietveld refinement of the X-ray diffraction patterns was performed. The kaolinite decomposition into metakaolinite was determined quantitatively; the intermediate (980 ºC spinel type alumino-silicate formation was also quantified; the incongruent fusion of the potash feldspar was observed and quantified together with the final mullitization and the amorphous (glassy phase formation.The methodology used to analyze the X-ray diffraction patterns proved to be suitable to evaluate quantitatively the thermal transformations that occur in a complex system like the triaxial ceramics. The evaluated phases can be easily correlated with the processing variables and

  12. Structure and physical properties of the LaBiFe2O6 Perovskite produced by the modified Pechini method

    Palacio, Johny Andrés Jaramillo; Bello, Elixir William Barrera; Landínez-Téllez, David A.; Roa-Rojas, Jairo; Cagigas, Julián Andrés Munévar; Arnache, Oscar

    2017-01-01

    In this paper the synthesis of the LaBiFe 2 O 6 material by the modified Pechini method is reported. Structural, morphologic, magnetic and optic experimental studies were performed. Rietveld refinement of x-ray diffraction patterns revealed that LaBiFe 2 O 6 crystallizes in an orthorhombic perovskite structure (space group Pnma, ⧣ 62). Scanning electron microscopy images showed the nanometric feature of grains. X-ray dispersive spectroscopy permitted to infer the obtaining of the LaBiFe 2 O 6 expected stoichiometry. Results of magnetic susceptibility as a function of temperature and field magnetization evidenced mixed ferromagnetism and superparamagnetism behavior at T=300 K. Mössbauer spectroscopy supported the superparamagnetic and ferromagnetic responses as a result of the nanogranular morphology and anisotropy effects. Spectrum of diffuse reflectance suggest that this material behaves as a semiconductor with energy gap E g =2.13 eV. (author)

  13. Characterization of clay and mass used in red ceramic industry in Cariri region - Ceara; Caracterizacao de argilas e massas utilizadas na industria G. Matos de ceramica vermelha na regiao do Cariri - Ceara

    Neta, I.A.B.; Cartaxo, A.S.; Esmeraldo, A.D.; Gomes, F.F.; Silva, F.C.; Ribeiro, S.B.N.; Neiva, L.S.; Brasileiro, M.I. [Universidade Federal do Cariri (UFCA), Juazeiro do Norte, CE (Brazil)

    2016-07-01

    The study of the characteristics of raw materials used in the production of red ceramic industry articles, such as bricks and tiles, has a key role in determining the quality of the final product. This study aims to evaluate the chemical and physical properties of clays and pasta from pottery G. Matos, Crato, Ceara. Three samples were collected, processed and submitted to the characterization DRX. They were also analyzed for plasticity by the methods of Atterberg and Pfefferkorn. In the method Atterberg, samples and Fat Mass Ready clay are within the plasticity index range for red ceramics, Pferfferkorn method, pasta and ready Fat also had plasticity, but with different results of the above method. In both ostestes, the red mass showed no moldability. XRD, the samples show quartz peaks, which were in the greatest amount in the sample that did not develop plasticity, addition, montmorillonite obtained peaks kaolinite. (author)

  14. ETBP (Extended True Boiling Point) curve extension of extra heavy crudes; Extensao da curva PEV (Ponto de Ebulicao Verdadeiro) de petroleos extrapesados por destilacao molecular e ampliacao da caracterizacao

    Rocha, Rodrigo S.; Batistella, Cesar B.; Maciel, Maria Regina W.; Maciel Filho, Rubens [Universidade Estadual de Campinas (UNICAMP), SP (Brazil). Faculdade de Engenharia Quimica; Medina, Lilian C. [PETROBRAS S.A., Rio de Janeiro, RJ (Brazil). Centro de Pesquisas (CENPES)

    2008-07-01

    For the determination of the TBP (True Boiling Point) Curve, which defines the yield of petroleum products, the ASTM D2892 method for petroleum distillation and ASTM D5236 method for vacuum distillation of heavy hydrocarbons were applied. Furthermore, from these distillations, cuts that are submitted to several analyses to determine its physical-chemical properties are obtained, and all this information generates the evaluation of petroleum. For heavy petroleum, these conventional methods have been limited, since the total distilled percentage determined for temperatures up to 565 deg C (maximum reached with ASTM D5236 method) is lower for these oils, reducing the points of the curve, limiting its information. To improve this data set for heavy oils, a methodology for the extension of TBP curve through molecular distillation was established. It was possible to reach values up to 700 deg C, representing a considerable progress for the extension of TBP curve. The objective of this work is to present the results of Extended TBP curve for a heavy petroleum and characterization carried out through the cuts and residues obtained in molecular distillation of the residue 'Zeta' 400 deg C+ (fancy name), made by ASTM D2892 method. (author)

  15. Synthesis and characterization of Tin / Titanium mixed oxide nanoparticles doped with lanthanide for biomarking; Sintese e caracterizacao de nanoparticulas de oxido misto de estanho/titanio dopadas com lantanideos para marcacao biologica

    Paganini, Paula Pinheiro

    2012-07-01

    This work presents the synthesis, characterization and photo luminescent study of tin and titanium mixed oxide nanoparticles doped with europium, terbium and neodymium to be used with luminescent markers on biological systems. The syntheses were done by co-precipitation, protein sol-gel and Pechini methods and the nanoparticles were characterized by infrared spectroscopy, thermogravimetric analysis, scanning electron microscopy, X-ray diffraction and X-ray absorption spectroscopy. The photo luminescent properties studies were conducted for luminophores doped with europium, terbium and neodymium synthesized by coprecipitation method. For luminophore doped with europium it was possible to calculate the intensity parameters and quantum yield and it showed satisfactory results. In the case of biological system marking it was necessary the functionalization of these particles to allow them to bind to the biological part to be studied. So the nanoparticles were functionalized by microwave and Stoeber methods and characterized by infrared spectroscopy, scanning electron microscopy, energy dispersive X-ray spectroscopy and X-ray diffraction obtaining qualitative response of functionalization efficacy. The ninhydrin spectroscopic method was used for quantification of luminophores functionalization. The photo luminescent studies of functionalized particles demonstrate the potential applying of these luminophores as luminescent markers. (author)

  16. Synthesis and characterization of strontium molybdate doped with copper, cobalt and zinc for purposes photocatalytic; Sintese e caracterizacao do molibdato de estroncio dopado com cobre, cobalto e zinco para fins fotocataliticos

    Dutra, F.B.; Silva, M.M.S.; Moriyama, A.L.L.; Souza, C.P., E-mail: faby_qui@hotmail.com [Universidade Federal do Rio Grande do Norte (LAMNRC/UFRN), Natal, RN (Brazil). Lab. de Materiais Nanoestruturados e Reatores Catalicos

    2016-07-01

    The broad concerns of contemporary society with environmental problems requires legislation and more effective techniques for wastewater treatment. In recent years, ceramic materials that have properties such as high melting points and high stability have been receiving great emphasis in several studies in particular heterogeneous photocatalysis, rapid and efficient method for the complete mineralization of contaminants. In this context, the present work deals with the synthesis and characterization of molybdate Strontium (SrMoO4) doped with copper, cobalt and zinc for the purpose of photocatalytic studies. The compounds were synthesized by complexation method EDTA / Citrate basic medium. The powders were characterized by Thermogravimetric Analysis (TG), X-Ray Diffraction (XRD), Particle size distribution by laser diffraction, Spectroscopy in the UV-Visible region, Energy Dispersive Spectroscopy (EDS) and Scanning Electron Microscopy (SEM), showing promising results as the crystalline phase of development and potential uses for the purpose of heterogeneous photocatalysis. (author)

  17. Physical, chemical and mineralogical characterization of water treatment plant waste for use in soil-cement brick; Caracterizacao fisica, quimica e mineralogica de residuo de estacao de tratamento de aguas para aproveitamento em tijolo solo-cimento

    Pessin, L.R.; Destefani, A.Z.; Holanda, J.N.F., E-mail: larapessin@hotmail.com [Universidade Estadual do Norte Fluminense Darcy Ribeiro (CCT/PPGECM/UENF), Campos dos Goytacazes, RJ (Brazil)

    2011-07-01

    The water treatment plants (WTP) for human consumption generate huge amounts of waste in the form of sludge (sludge) that have been over the years mostly inadequately prepared in water resources and the environment. Moreover, traditional methods of disposal of waste water treatment plants commonly used are generally costly activities. An alternative method for disposal of this waste abundant is its incorporation in ceramic products. This work is focused on the physical-chemical and mineralogical composition of a sample of waste water treatment plants from the region of Campos dos Goytacazes-RJ to their use in the manufacture of soil-cement brick. Several characterization techniques were used including X-ray diffraction, X-ray fluorescence, scanning electron microscopy, picnometry, particle size analysis and plasticity. The experimental results indicate that the waste water treatment plants have the potential to be used in the manufacture of ecologic soil-cement bricks. (author)

  18. Active film of poly(vinyl chloride)/silver: synthesis, characterization and evaluation as antimicrobial active packaging; Filme ativo de poli(cloreto de vinila)/prata: sintese, caracterizacao e avaliacao como embalagem ativa antimicrobiana

    Braga, Lilian R.; Rangel, Ellen T.; Machado, Fabricio, E-mail: lilianrodribraga@gmail.com [Universidade de Brasilia (UnB), Brasilia, DF, (Brazil)

    2015-07-01

    The antimicrobial films based on poly(vinyl chloride) (PVC) mediated silver (1, 2, 4 and 8 wt%) were evaluated as antimicrobial active packaging using the casting method. The structure of the active films was characterized by SEM, EDX-XRF, XRD, FTIR and TG. FTIR spectra confirmed the PVC-Ag interaction due to the presence of new bands at 1745 cm{sup -1} and 1165 cm{sup -1} bands, which are absent in the PVC control. The FRX-EDX spectrum confirmed the presence of silver ions in all the films. TG and SEM results showed that the increased concentration of silver provided an improved thermal stability and presence of pores in the active films, respectively. Antimicrobial activity was evaluated by disk diffusion method for Bacillus subtilis, Fusarium solani and Apergillus niger, which proved the efficiency of the films active. (author)

  19. Synthesis and characterization of SnO2 doped with fluorine by the technique of polymeric precursors; Sintese e caracterizacao de SnO2 dopado com fluor pela tecnica dos precursores polimericos

    Pereira, Gilberto J.; Lopes, Rafael Ialago, E-mail: gilbertop@fei.edu.br [Centro Universitario FEI, Sao Bernardo do Campo, SP (Brazil). Departamento de Engenharia de Materiais

    2016-07-01

    The present work deals with the synthesis of tin dioxide powders doped with fluorine and chlorine anions to evaluate the influence of these on the physico-chemical properties of SnO2, as well as to verify if the dopant does not make a solid solution with the material and its possible use as sintering additive. The samples were synthesized by Pechini method (polymer precursors) with tin oxalate as a source not contaminated with chlorine of this metal. Specific surface area characterization (BET method) and X-ray diffractometry (XRD) show that doping reduces the particle size of SnO2, being more effective at lower dopant levels. The dilatometry of the doped powders shows a reduction in the beginning and end temperatures of the sintering of the tin dioxide when compared with values in the literature.

  20. Preparation and characterization of sugar cane bagasse fiber modified with nanoparticles of zirconium oxide; Preparacao e caracterizacao de fibras de bagaco de cana modificadas com nanoparticulas de oxido de zirconio

    Carvalho, K.C.C. de; Mulinari, D.R.; Voorwald, H.C.J.; Cioffi, M.O.H., E-mail: kcccarvalho@hotmail.com.b [UNESP, Guaratingueta, SP (Brazil). Fac. de Engenharia. Dept. de Materiais e Tecnologia(FEG)

    2010-07-01

    The sugar cane bagasse fiber are renewable materials and have great application potential when used as reinforcement in a polymer matrix to give rise to composite materials and as supports for adsorption of heavy metals. This paper therefore describes the preparation and characterization of bleached and hydrated zirconium oxide modified sugar cane bagasse fiber by conventional precipitation method. Through the technique of electron microscopy we observed the presence of oxide nanoparticles on the fiber surface, proving the efficiency of the conventional precipitation method. With the X-ray diffraction analysis it was determined a decrease of 6.2% in the crystallinity index of modified fibers when compared to the bleached fibers showing the deposition of amorphous zirconium oxide on the fiber surface. (author)

  1. Preparation and characterization of nickel catalysts supported on cerium for obtaining hydrogen from steam reforming of ethanol; Preparacao e caracterizacao de catalisadores de niquel suportados em ceria para obtencao de hidrogenio a partir da reforma a vapor do etanol

    Urbaninho, A.B.; Bergamaschi, V.S.; Ferreira, J.C., E-mail: jcferrei@ipen.br [Instituto de Pesquisas Energéticas e Nucleares (IPEN/CNEN-SP), São Paulo, SP (Brazil). Centro de Células à Combustível e Hidrogênio

    2016-07-01

    The Ni/Ce catalysts for were prepared by co- precipitation method with a view to their use in steam reforming of ethanol to produce a hydrogen-rich gas mixture. The catalysts were characterized by scanning electron microscopy; x-ray dispersive Spectroscopy and surface area BET method. This paper proposes to prepare, characterize and test nickel catalyst supported on cerium in order to obtain a material with higher activity and selectivity of the catalyst using the steam reforming reaction of ethanol, by varying the reaction temperature, molar ratio water/ethanol and uptime. The catalytic tests were monitored by chemical analysis of syngas from steam reforming of ethanol using an analysis online by gas Chromatograph in the reactor. (author)

  2. Synthesis and characterization of ZSM-12 type zeolytic catalysts by using different aluminium sources in the petroleum industry; Sintese e caracterizacao de catalisadores zeoliticos do tipo ZSM-12 utilizando diferentes fontes de aluminio na industria do petroleo

    Moraes, Marilia R.F.S.; Jesus, Daniela B.; Souza, Marcelo J.B. [Universidade Federal de Sergipe (UFS), Sao Cristovao, SE (Brazil). Dept. de Engenharia Quimica; Santos, Consuelo D.; Machado, Sanny W.M.; Pedrosa, Anne M. Garrido [Universidade Federal de Sergipe (UFS), Sao Cristovao, SE (Brazil). Dept. de Quimica

    2010-12-15

    The main objective was to synthesize and characterize ZSM-12 zeolites from different sources of aluminium, using hydrothermal method and characterize the catalysts synthesized by X-ray diffractions, thermal analysis and infrared absorption spectroscopy. The X-ray diffractogram showed the formation of zeolites of the family pantasil crystalline. Thermogravimetric curves and FTIR spectra were utilized by monitoring the removal of template and by monitoring the maintenance of zeolite structure. (author)

  3. Structural and morphological characterization of TiO{sub 2} powders prepared using Pechini and combustion reaction; Caracterizacao estrutural e morfologica de nanopos de TiO{sub 2} preparados pelo metodo Pechini e por reacao de combustao

    Ribeiro, P.C.; Almeida, E.P.; Costa, A.C.F.M. da; Lira, H.L., E-mail: pollyanacae@yahoo.com.b [Universidade Federal de Campina Grande (UFCG), PB (Brazil). Dept. de Engenharia de Materiais; Kiminami, R.H.G.A. [Universidade Federal de Sao Carlos (UFSCar), SP (Brazil). Dept. de Engenharia de Materiais

    2010-07-01

    TiO{sub 2} is a semiconductor oxide and polymorphic and can exist in three crystallographic forms: anatase, rutile and broquita, and forms anatase and rutile are the major interests in scientific research. Thus, this study aims to synthesize TiO{sub 2} by Pechini methods and combustion reaction and to evaluate the influence of synthesis methods in structural and morphological characteristics of the samples. The nanopowders were characterized by X-ray diffraction, nitrogen adsorption, and particle size distribution and scanning electron microscopy. The results of X-ray diffraction showed that the samples obtained by the Pechini method showed the single phase anatase with crystallite size of 20 nm and surface area of 49.44 m{sup 2}/g, whereas the samples synthesized by combustion reaction using glycine as fuel showed the rutile phase as major phase and traces of anatase phase, with crystallite size of 65 nm and surface area 4.34 m{sup 2}/g. (author)

  4. Structural, magnetic and optical characterization of Ni{sub 0.8}Zn{sub 0.2}Fe{sub 2}O{sub 4} nano particles prepared by co-precipitation method

    Kannan, Y.B., E-mail: ybkans@gmail.com [Department of Physics, Arumugam Pillai Seethai Ammal College, Tiruppattur 630211 (India); Saravanan, R. [Research Centre & PG Department of Physics, The Madura College, Madurai 625011 (India); Srinivasan, N. [Research Centre & PG Department of Physics, Thiagarajar College, Madurai 625009 (India); Praveena, K. [School of Physics, Univeristy of Hyderabad, Hyderabad 500046 (India); Sadhana, K. [Material Research Center, Indian Institute of Science, Bangalore 560012 (India)

    2016-12-01

    Bond strength values, between tetrahedral sites and octahedral sites atoms in the unit cell, are evaluated using maximum entropy method (MEM) for the Ni{sub 0.8}Zn{sub 0.2}Fe{sub 2}O{sub 4} nano ferrite particles, prepared by co-precipitation method and sintered at 900 °C. The spinel structure is confirmed from the XRD analysis done using the Rietveld method. Substitution of zinc ion causes increase in lattice parameter value. Thermal behavior, morphology, magnetic properties and optical band gap energy values of the sample are determined by using thermogravimetric analysis and differential thermal analysis, scanning electron microscope, vibrating sample magnetometer and UV–VIS–NIR techniques respectively. Low value of saturation magnetization is attributed to the disorder in cation distribution.

  5. Microstructural characterization of industrial foams by gamma ray transmission and X-ray microtomography; Caracterizacao microestrutural de espumas industriais por transmissao de raios gama e microtomografia de raios X

    Rodrigues, Luiz Eduardo

    2004-07-01

    This work presents the total porosity measurements of the aluminum and silicon carbide (SiC) foams samples. For porosity determination the gamma ray transmission and X-ray microtomography with conic beam techniques were used. These methods have more advantage than conventional ones, because they are non destructive and provide more details of the analyzed material porous structure. The aluminum foam samples with 10, 20, 30, 40 and 45 ppi (pores per inch) and SiC ceramic foam samples with 20, 30, 45, 60, 75, 80 and 90 ppi were analysed by gamma transmission. The SiC 60, 75 and 90 ppi samples were also analyzed by X-ray microtomography. For the gamma ray transmission measurements it was used an {sup 241} Am source (59.53 keV), a NaI(Tl) scintillation detector, collimators, a XYZ micrometric table and standard gamma spectrometry electronics connected to a multichannel analyzer, at the LFNA/UEL. For the X-ray microtomographic measurements, the Fein Focus X-ray system of the Nuclear Instrumentation Laboratory of the COPPE, located at the Universidade Federal do Rio de Janeiro, Rio de Janeiro, RJ, was used. This equipment provide us images with micrometric resolution (53.48 {mu}m) using a conic X-ray beam and bidimensional detection. The microtomographic images were pre-processed and analyzed by the Imago software, developed at Porous Media and Materials Thermophysical Properties Laboratory (LMPT) of the Mechanical Engineering Department, located at Universidade Federal de Santa Catarina, Florianopolis, SC. Employing the The Imago software it was calculated the total porosity, pore size distribution and autocorrelation function C(u) of the binarized microtomographic images of the each sample. The microtomographic 3-D image of each sample was compared with 3-D image reconstructed by the Gaussian truncated method. This method generates a periodic 3-D porous structure by using of the autocorrelation function of one 2-D cross sectional image of the sample. (author)

  6. Impregnation of 12-tungstophosphoric acid on silica - part I: determination of impregnation parameters, characterization and evaluation of catalytic activity; Impregnacao do acido 12-fosfotungstico em silica - parte I: determinacao de parametros de impregnacao, caracterizacao e avaliacao da atividade catalitica

    Scroccaro, Karine Isabel; Tanobe, Valcineide Oliveira de Andrade; Cocco, Lilian Cristina; Yamamoto, Carlos Itsuo, E-mail: karineisabel@yahoo.com.br [Universidade Federal do Parana, Curitiba, PR (Brazil). Centro Politecnico. Dept. de Engenharia Quimica; Wypych, Fernando [Universidade Federal do Parana, Curitiba, PR (Brazil). Centro Politecnico. Dept. de Quimica

    2012-07-01

    Catalyst based on Kegging-type heteropolyacids (H{sub 3}PW{sub 12}O{sub 40} - HPA), supported on SiO{sub 2} (H{sub 3}PW), were prepared by the impregnation method under different thermal treatment conditions. The materials were characterized by different instrumental techniques and used as catalysts in the methyl esterification reactions of stearic acid. Using the catalyst with 15% of HPA, conversions higher than 60% were obtained after 2 h of reaction at 65 deg C. Recovery studies using hot-filtration with ethanol at 75 deg C showed satisfactory activity for two additional reaction cycles. (author)

  7. Thermal activation and characterization of chocolate clay for using as adsorbent in nickel removal; Ativacao termica e caracterizacao da argila chocolate visando sua aplicacao como adsorvente na remocao de niquel

    Villar, W.C.T.; Brito, A.L.F.; Laborde, H.M.; Rodrigues, M.G.F., E-mail: meiry@deq.ufcg.edu.br [Universidade Federal de Campina Grande (UFCG), PB (Brazil). Unidade Academica de Engenharia Quimica; Ferreira, H.S. [Universidade Federal de Campina Grande (UFCG), PB (Brazil). Programa de Ciencias e Engenharia de Materiais

    2009-07-01

    Clays present interesting properties as adsorbing material for the removal of heavy metals from effluents. This property is clearly modified by thermal activation. In this work, the characterization of chocolate clay before and after thermal activation (from 300 to 500 deg C) is realized by X-ray diffraction (XRD), differential thermal analysis and thermogravimetric analysis (DTA/TG), infrared spectroscopy (IR), scanning electron microscopy (SEM) and cation exchange capacity (CEC). The main differences between the activated and natural clays are structural modifications of the clay, as shown by XRD and DTA/TG, but also a modification of its cation exchange capacity as shown by the methylene blue method. (author)

  8. Thermal activation and characterization of clay aiming their use as sorbent in fixed bed columns to remove cadmium; Ativacao termica e caracterizacao da argila visando sua utilizacao como adsorvente em colunas de leito fixo para a remocao de cadmio

    Silva, M.M. da; Rodrigues, M.G.F. [Universidade Federal de Campina Grande (UFCG), PB (Brazil); Silva, M.L.P. [Universidade Federal Rural do Semi-Arido (UFERSA), RN (Brazil); Kleinübing, S.J.; Silva, M.G.C., E-mail: marciliomaximo@yahoo.com.br [Universidade Estadual de Campinas (UNICAMP), SP (Brazil)

    2011-07-01

    In this work we studied the removal of cadmium in a synthetic wastewater using clay of Pernambuco - Brazil, in systems of fixed bed column. Clay was thermally activated at 500 °C. The materials were characterized using X-ray Fluorescence (XRF), X-ray Diffraction (XRD) and nitrogen adsorption (BET method). For tests in fixed bed column, we applied a factorial design 2{sup 2} and found that increasing the flow adversely affects the process of removing cadmium concentration while acting positively. The studies showed these materials as promising for the removal of Cd{sup 2+} ions in synthetic wastewater containing low levels of this metal. (author)

  9. Characterization of PHB, zinc oxide and organophilic clay nanocomposites with low field; Caracterizacao de nanocompositos de PHB com oxido de zinco e argila organofilica por RMN de baixo campo

    Silva, Mariana B.R.; Tavares, Maria Ines B.; Junior, Alberto W.M.; Neto, Roberto P.C. [Universidade Federal do Rio de Janeiro (UFRJ), Rio de Janeiro, RJ (Brazil)

    2015-07-01

    Nanoparticles of zinc oxide and organophilic clay (Viscogel B8) were added to PHB matrix in some different proportions. The nanocomposites containing both nanoparticles were obtained from solution casting method using chloroform as solvent. The films obtained were analyzed with X-ray diffraction and low field nuclear magnetic resonance to obtain answers about the interactions, dispersion and homogeneity of nanoparticles in the polymer matrix, just like the synergistic effects and the influence of them over some characteristics of the polymer. The synergistic effect achieved from the addition of both nanoparticles was also observed through hydrogen nuclear relaxation time values. (author)

  10. Obtention and characterization of TiO{sub 2}/TiN multilayers coatings; Obtencao e caracterizacao de revestitimentos compostos de multicamadas TiO{sub 2}/TiN

    Goncalves, Andre

    2010-07-01

    Nano science has emerged in recent years as one of the most important areas for future technological developments, especially in the area of electronic devices. Nanotechnology has an interdisciplinary character which includes knowledge from physics, chemistry, engineering, and biology. This technology is being used in the manufacture of microprocessors, pumps for dose of medicine, and coating materials, among others. The MOCVD technique has been used recently to obtain nanocrystalline coatings, and provide films of better quality than those obtained by conventional CVD or physical methods. Furthermore, the MOCVD technique presents itself as a competitive alternative because it is relatively inexpensive and easy to deploy compared to physical deposition methods. In this work multilayer coatings of TiO{sub 2}/TiN were produced. During the experiment, the opening and closing of the valves of gases admission, requires from the operator manual ability to trigger the valve and controlling the deposition time, which creates the possibility of errors, leading directly into the thickness of each layer. Thus, the need of reducing the influence of the operator, and the possibility of using time intervals of less than a minute in the growths, created the opportunity to develop a computer program to manage the whole system. The software was developed using the 'State machine' concept for the process control and Hardware in the loop simulation. (author)

  11. Obtention of graft copolymers by ionizing radiation, characterization and study of hemo-compatible properties; Obtencao de copolimeros de enxerto via radiacao ionizante, caracterizacao e estudo de suas propriedades hemocompativeis

    Queiroz, A A.A. de

    1994-12-31

    The present work had as objectives the obtention and characterization of grafting copolymers by radiation induced polymerization and the study of its hemo compatible properties. The relationship between grafting conditions and anti-trombogenicity was examined for the purpose of clearing the necessity of controlling grafting conditions to enhance the copolymers blood compatibility. Two methods were chosen to accomplish the irradiation: mutual and pre-irradiation (peroxidation) of the films in {sup 6O} Co source and electron beam accelerator. Primarily grafting parameters were studied in the systems of the monomers N, N-dimethyl acrylamide (DMAA) and acrylic acid (AA) with the polymeric films: poly (tetrafluoroethylene) (PTFE), poly (ethylene-co-tetrafluoroethylene) (PETFE), low density polyethylene (LDPE) and poly (vinyl chloride) (PVC). The simultaneous irradiation was effective in the polymerization of all the substrates above mentioned, although the peroxidation method has given better results for PETFE-DMAA, LDPE-g-DMAA, LDPE-g-AA and PVC-g-AA. In the system AA/LDPE and AA/PVC the homo polymerization was controlled by the addition of the comonomer N, N-dimethyl acrylic acid (DMA). As for the grafting parameters, low dose rate and low irradiation dose, showed to be very effective for the graftability of DMAA and AA on the substrates. (author). 129 refs, 51 figs, 7 tabs.

  12. Intrinsic dependence of the magnetic properties of CoFe{sub 2}O{sub 4} nanoparticles prepared via chemical methods with addition of chelating agents

    Mendonça, E.C. [Núcleo de Pós-Graduação em Física, Campus Prof. José Aluísio de Campos, UFS, 49100-000 São Cristóvão, SE (Brazil); Tenório, Mayara A. [Departamento de Física, Campus Prof. Alberto Carvalho, UFS, 49500-000 Itabaiana, SE (Brazil); Mecena, S.G.; Zucolotto, B.; Silva, L.S. [Núcleo de Pós-Graduação em Física, Campus Prof. José Aluísio de Campos, UFS, 49100-000 São Cristóvão, SE (Brazil); Jesus, C.B.R. [Instituto de Física Gleb Wataghin, UNICAMP, C. P. 6165, 13083-970 Campinas, SP (Brazil); Meneses, C.T. [Núcleo de Pós-Graduação em Física, Campus Prof. José Aluísio de Campos, UFS, 49100-000 São Cristóvão, SE (Brazil); and others

    2015-12-01

    In this work, the effect of addition of different chelating agents on the magnetic properties of cobalt ferrite nanoparticles produced by the combining of both co-precipitation and hydrothermal methods is reported. The Rietveld analyses of X-ray diffraction patterns reveal that our samples are single phase (space group: Fd-3m) with small average sizes. The weight losses observed in the thermogravimetric measurements together with the M×H curves show that the organic contamination coming from chelating agent decomposition can give rise to misinterpretation of the magnetization measurements. Besides, analyses of the zero-field-cooled (ZFC) and field-cooled (FC) magnetization measurements and the M×H curves measured at room temperature allows us to state that both the average blocking temperature and particles size distribution are sensitive to the kind of chelating agent. - Highlights: Superparamagnetism. Chelating agents. Organic contamination.

  13. Investigation of microstructural and optical properties of La0.8Ca0.2FeO3 nanostructure synthesized via gel combustion method

    Naseem, Swaleha; Ali, S. Asad; Khan, Wasi; Khan, Shakeel

    2018-05-01

    Ca substituted LaFeO3 orthoferrite nanostructure perovskite has been synthesized by gel combustion method using citric acid as a fuel. The structural and optical properties were investigated by various tools. The structural analysis through Rietveld refinement of the XRD data revealed single phase of orthorhombic structure in R-3c space group of the sample without presence of any other impurity phase. Scanning electron microscopy (SEM) image exhibits non-uniform distribution of the nanoparticles in agglomerated form. The purity of the sample and stoichiometric ratio of the elements were established through energy dispersive x-ray spectroscopy (EDS). FTIR spectroscopy measurement predicts the presence of various band relation of the chemical species of Ca with LaFeO3. Optical properties were explored through UV-visible absorption spectroscopy that showed absorption edge at 347 nm and energy band gap was estimated as 3.47eV using Tauc's relation.

  14. Synthesis of LiNi0.8Co0.1Mn0.1O2 cathode material by chloride co-precipitation method

    李灵均; 李新海; 王志兴; 伍凌; 郑俊超; 李金辉

    2010-01-01

    LiNi0.8Co0.1Mn0.1O2 was prepared by a chloride co-precipitation method and characterized by thermogravimetric analysis, X-ray diffractometry with Rietveld refinement,electron scanning microscopy and electrochemical measurements.Effects of lithium ion content and sintering temperature on physical and electrochemical performance of LiNi0.8Co0.1Mn0.1O2 were also investigated. The results show that the sample synthesized at 750℃with 105%lithium content has fine particle sizes around 200 nm and homogenous sizes distribution.The initial discharge capacity for the powder is 184 mA·h/g between 2.7 and 4.3 V at 0.1C and room temperature.

  15. Chemometrics application in fuel's MTR type chemical characterization by X-ray fluorescence; Aplicacao da quimiometria para caracterizacao quimica de combustiveis tipo MTR por fluorescencia de raios-X

    Silva, Clayton Pereira da

    2012-07-01

    treatments (dissolving, digesting, and others). To corrections like effects of spectral and matrix were applied and evaluated the fundamental parameter method, univariate calibration curve and multivariate calibration. The results were compared by means of statistical tests in accordance with ISO 17025 in MRCs (123 (1-7) and 124 (1-7)) MCRs of U{sub 3}O{sub 8} from New Brunswick Laboratory (NBL) and 16 U{sub 3}Si{sub 2} samples provided by CC of IPEN/CNEN-SP. The chemometrics is a promising method to determination of minor and major constituents on the U3Si2 and U3O8 basis nuclear fuel, because the precision and accuracy are statistically equal volumetric analysis, gravimetric and ICPOES methods. (author)

  16. Synthesis and characterization of LDH/Ppi composite and its application as adsorbent of 2,4-dichlorophenoxyacetic (herbicide); Sintese e caracterizacao do composito HDL/Ppi e sua aplicacao como adsorvente do 2,4-diclorofenoxiacetico (herbicida)

    Pacheco, I.S.; Oliveira, R.S.; Girotto, L.G.; Freitas, L.L. de; Amaral, F.A. do; Canobre, S.C., E-mail: ingrid_1194@hotmail.com [Universidade Federal de Uberlandia (UFU), MG (Brazil). Instituto de Quimica

    2016-07-01

    This work had as main objective the synthesis and characterization of LDH [Co-Al-Cl] method by hydrolysis of urea and then its synthesized polypyrrole coating by chemically targeting the application as adsorbent dichlorophenoxyacetic acid (2,4-D). The x-ray diffractogram of well defined showed diffraction peaks corresponding to the planes 003, 006, 009 and 110 which allow them to rhombohedral indexes and lamellar structure. The composite LDH / Ppi had a percentage of 49% herbicide retention in aqueous solution. From the investigated adsorption isotherm models that more fit the experimental data was the Freundlich, so it could be inferred that the interaction between the LDH / Ppi and the herbicide was physical, ie an rapid, reversible adsorption and does not specify. (author)

  17. Preparation and characterization of high density polyethylene and residual fibre of Attalea funifera Mart (piacava) composites; Preparacao e caracterizacao de compositos de polietileno de alta densidade com residuos de fibras de piacava da especie Attalea funifera Mart

    Agrela, Sara P.; Guimaraes, Danilo H.; Jose, Nadia M., E-mail: saraagrela@hotmail.co [Universidade Federal da Bahia (GECIM/IQ/UFBA), Salvador, BA (Brazil). Inst. de Quimica. Grupo de Energia e Ciencias dos Materiais; Carvalho, Gleidson G.P. [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Escola de Medicina Veterinaria. Dept. de Producao Animal; Carvalho, Ricardo F. [Universidade Federal da Bahia (EP/UFBA), Salvador, BA (Brazil). Escola Politecnica. Curso de Mestrado em Engenharia Ambiental Urbana

    2009-07-01

    The use of natural fiber reinforcement thermoplastic polymer is continuously increasing. This fact is manly due to its advantages as low cost, availability, recyclability, low energy demand and then environmental appeal if compared to synthetics fibers. The composites were prepared in different fiber volume ratios (5%, 10% and 20%) mixed with high density polyethylene (HDPE) and heated at 190 deg C. Thermogravimetric analysis and differential scanning calorimetry were used to investigate thermal stability. The composites structure was characterized by Fourier Transform Infrared spectroscopy, X-ray diffractometry. Fiber and residue of piassava (Attalea funifera Mart) chemical composition were determined by Van Soest Method. The results indicate that thermo stability of the composites of HDPE prepared with fiber volume ratios up to 20% is only slightly lowered. (author)

  18. Synthesis and characterization of Pt-Sn-Ni alloys to application as catalysts for direct ethanol fuel cells; Sintese e caracterizacao de ligas de Pt-Sn-Ni para aplicacao como caztalisadores em celulas a combustivel do tipo DEFC

    Silva, E.L. da; Correa, P.S.; Oliveira, E.L. de; Takimi, A.S.; Malfatti, C.F., E-mail: celia.malfatti@ufrgs.b [Universidade Federal do Rio Grande do Sul (LAPEC/UFRGS), Porto Alegre, RS (Brazil). Programa de Pos-Graduacao em Engenharia Mecanica. Lab. de Pesquisa em Corrosao; Radtke, C. [Universidade Federal do Rio Grande do Sul (IQ/UFRGS), Porto Alegre, RS (Brazil). Inst. de Quimica

    2010-07-01

    Direct ethanol fuel cells (DEFCs) have been the focus of recent research due its application in mobile energy sources. In order to obtain the maximum efficiency from these systems, it is necessary the total ethanol oxidation, which implies in C-C bond break. Different catalysts described in literature are employed with this intent. This work consists in studying PtSnNi catalysts supported on carbon Vulcan XC72R, to application in DEFCs. Thus, it was used the impregnation/reduction method, varying the atomic proportion among Pt, Sn and Ni. The alloys were characterized by X-Ray Diffraction, Cyclic Voltammetry and Transmission Microscopy. Preliminary results show that predominant structure on the catalysts is the face centered cubic platinum and the densities currents are dependent on the platinum amount. (author)

  19. Characterization by X ray diffraction of deleterious phases precipitated in a super duplex stainless steel; Caracterizacao por difracao de raios X de fases deleterias precipitadas em aco inoxidavel superduplex

    Pardal, Juan M.; Tavares, Sergio S. Maior; Fonseca, Maria P. Cindra; Montenegro, Talles Ribeiro, E-mail: juanpardal@vm.uff.b [Universidade Federal Fluminense (PGEMEC/UFF), Niteroi, RJ (Brazil). Programa de Pos-graduacao em Engenharia Mecanica; Dias, Antonio Jose N.; Almeida, Sergio L. de [Instituto Nacional de Tecnologia (INT), Rio de Janeiro, RJ (Brazil). Div. de Materiais Ceramicos e Metalicos. Lab. de Tecnologia de Materiais

    2010-07-01

    In this work the identification and quantification of deleterious phases in two super duplex stainless steels grade UNS S32750, with quite different grain sizes, was performed by X-ray diffraction. The materials were isothermally aged in the 800 . 950 deg C range. Direct comparison method was used to quantify the ferrite phase in each sample. The amount of deleterious phases ({sigma}, {chi} and {gamma}2) formed was calculated by the difference of the amount of ferrite phase measured in each specimen to the amount of ferrite initially measured in the un-aged steel. The results obtained give an useful contribution to the understanding of kinetics of deleterious phases precipitation in super duplex steels. (author)

  20. {sup 1}H-NMR characterization of cellulose acetate obtained from sugarcane bagasse; Caracterizacao de acetato de celulose obtido a partir do bagaco de cana-de-acucar por {sup 1}H-RMN

    Cerqueira, Daniel A., E-mail: daniel.cerqueira@ufba.b [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Inst. de Ciencias Ambientais e Desenvolvimento Sustentavel; Rodrigues Filho, Guimes [Universidade Federal de Uberlandia (UFU), MG (Brazil). Inst. de Quimica; Carvalho, Rui de A. [Universidade de Coimbra (Portugal). Dept. de Bioquimica; Valente, Artur J.M. [Universidade de Coimbra (Portugal). Dept. de Quimica

    2010-07-01

    Cellulose from sugarcane bagasse was used for synthesizing cellulose acetate with different degrees of substitution, which were characterized by {sup 1}H-NMR through the relationship between the peak areas of the hydrogen atoms of the acetate groups (-(C=O)OCH{sub 3}) and the peaks of the hydrogen bonded to the carbon atoms of the glycosidic rings. Suppression of some signals was carried out in order to remove the residual water resonance in the materials and those related to impurities in cellulose triacetate as well. A deconvolution method for the computation of the degree of substitution of acetylation is proposed. The degrees of substitution for the cellulose samples were 2.94 and 2.60, in good agreement with those obtained by chemical determination through an acid-base titration. (author)

  1. Mechanical characterization of cemented carbide WC-6Co (%wt) manufactured by SPS (Spark Plasma Sintering; Caracterizacao mecanica de metal duro WC-6Co (%massa) sinterizado via SPS (Spark Plasma Sintering)

    Boidi, G.; Tertuliano, A.J.; Machado, I.F., E-mail: guido.boidi@usp.br [Universidade de Sao Paulo (USP), SP (Brazil). Departamento de Engenharia Mecatronica e Sistemas Mecanicos; Rodrigues, D. [BRATS- Filtros Sinterizados e Pos Metalicos, Cajamar, SP (Brazil)

    2016-07-01

    This work aimed to manufacture cemented carbide (WC-6%wtCo) obtained by SPS (Spark Plasma Sintering) process and to carry out the mechanical characterization by hardness and fracture toughness. The material was consolidated at 1100 deg C for different holding times (1 min, 5 min, 10 min), in order to evaluate the densification. A reference sample was also used to be compared to SPS. Optical and scanning electron microscopy were carried out to characterize the microstructural features of the samples and mechanical properties were obtained by hardness measurements (micro and macro) and instrumented indentation. The fracture toughness was calculated with the method of Palmqvist. Best results were found in the material sintered by SPS for 10 minutes of holding time, in which 97% of relative density and about 1600 HV{sub 10} was reached. (author)

  2. Characterization, treatment and utilization of rice husk ash in production processes of the industrial branch; Caracterizacao, tratamento e aproveitamento das cinzas da casca do arroz em processos produtivos do ramo industrial

    Stracke, Marcelo Paulo; Schmidt, Julia Isabel; Steffen, Ana Cristina; Sokolovicz, Boris; Kieckow, Flavio, E-mail: stracke@santoangelo.uri.br [Universidade Regional Integrada do Alto Uruguai e das Missoes (URI), Santo Angelo, RS (Brazil)

    2016-07-01

    The rice husk ash (CCA) is a black powder rich in silica (contents above 90%) with many industrial applications. The ash was obtained from a rice processing industry in the state of Rio Grande do Sul. In this work the purpose is to characterize the rice husk ash and eliminate the residual carbon by methods such as acid leaching. The white ash is obtained by a chemical process followed by heating between 600 and 800 °C. The results were analyzed in DR-X, TGA and DSC. The DR-X analysis showed that the samples present high levels of silica in the crystalline form of quartz, cristobalite and tridymite. The white ash was obtained with high purity and presented a good result in the manufacture of paints. (author)

  3. Synthesis and characterization of particles derived of poly(vinyl alcohol) (PVA) for treatment of embolization and chemoembolization;Sintese e caracterizacao de particulas derivadas de poli(alcool vinilico) (PVA) para embolizacao e quimioembolizacao

    Semenzim, Vinicius L.; Basso, Glaucia G.; Passos, Rodrigo A.; Nery, Jose G. [UNESP, Sao Jose do Rio Preto, SP (Brazil); Agreli, Guilherme; Oliveira, Ana P.M.L.; Kawasaki-Oyama, Rosa S.; Braile, Domingo M., E-mail: nery@ibilce.unesp.b [Braile Biomedica Industria e Comercio Representacoes S.A., Sao Jose do Rio Preto, SP (Brazil)

    2009-07-01

    The most effective way to treat cancerous tumors is by surgically removing them. However in some types of cancer, such as liver and uterine cancer, more than two-thirds of patients have no indication for surgery due to the size and location of the tumor, such as into the blood vessels. Doctors and researchers have invested in alternative and less invasive methods such as chemoembolization. The objectives of this research project are the synthesis and characterization of poly(vinyl alcohol) (PVA) particles for use in cancer treatment. PVA particles will be combined with chemotherapeutic agent Doxorubicin, drug commonly used in the treatment of cancers and carcinomas. The particles, obtained by controlled polymerization reaction followed by saponification, were characterized by SEM, XRD and NMR-CP/MAS. The functionalization of the particles with the drug is the next step of this study. (author)

  4. Cement for oil well developed from ordinary cement: characterization physical, chemical and mineralogical; Cimento para poco de petroleo desenvolvido a partir de cimento comum: caracterizacao fisica, quimica e mineralogica

    Oliveira, D.N.S.; Neves, G. de A.; Chaves, A.C.; Mendonca, A.M.G.D.; Lima, M.S. de [Universidade Federal de Campina Grande (UFCG), PB (Brazil); Bezerra, U.T., E-mail: daninascimento.eng@gmail.com [Instituto Federal de Educacao, Ciencia e Tecnologia da Paraiba (IFPB), Campina Grande, PB (Brazil)

    2012-07-01

    This work aims to characterize a new type of cement produced from the mixture of ordinary Portland cement, which can be used as an option in the cementing of oil wells. To enable this work we used the method of lineal programming for the new cement composition, then conducted tests to characterize through particle size analysis by laser diffraction, chemical analysis by EDX, TGA, X-ray diffraction, time grip, resistance to compression. The overall result showed that the new cement had made low-C3A, takes more time to the CPP, thermal stability up to 500 ° C, the kinetics of hydration and low levels of major components consistent with the specifications of ABNT. (author)

  5. Characterization and study of the behavior of wire Ti-Ni with shape memory effect enables manufacture of actuators; Estudo da caracterizacao e do comportamento de fios de Ti-Ni com efeito memoria de forma viabilizando fabricacao de atuadores

    Pina, E.A.C.; Araujo Filho, O.O. de; Urtiga Filho, S.L.; Gonzalez, C.H., E-mail: kikipina@hotmail.co [Universidade Federal de Pernambuco (DEM/CTG/UFPE), Recife, PE (Brazil). Centro de Tecnologia e Geociencias. Dept. de Engenharia Mecanica

    2010-07-01

    This work aims to characterize the wire commercial Ti-Ni of 1.27 mm in diameter with shape memory effect for the development of helical springs with the function of sensor / actuator. After heat treatment, the transformation temperatures, the presence of precipitates, the degree of damping, maximum stress of rupture, modulus of elasticity, the presence of phase R, the behavior of the alloy under tension, will be analyzed and compared in each situation. For characterization we used several methods including: heat treatment, Differential Scanning Calorimetry (DSC), tensile, dynamic mechanical analysis (DMA), X-ray diffraction, thermomechanical cycling. The wires were cut into pieces and heat-treated at 400 deg C with variation of time in muffle furnaces and quenching in water at 25 deg C. (author)

  6. Combustion synthesis by reaction and characterization of nano ferrites: study of fuel aniline, citric and its mixture; Sintese por reacao de combustao e caracterizacao de nanoferritas Ni-Zn: estudo dos combustiveis anilina, acido citrico e sua mistura

    Silva, M.C. da; Coutinho, J.P.; Costa, A.C.F.M., E-mail: normanda@ufcg.edu.br [Universidade Federal de Campina Grande (UFCG), PB (Brazil). Unidade Academica de Engenharia de Materiais; Kiminami, R.H.G.A. [Universidade Federal de Sao Carlos (UFSCar), SP (Brazil). Departamento de Engenharia de Materiais; Freitas, N.L. de [Universidade Federal de Campina Grande (UFCG), PB (Brazil). Unidade Academica de Tecnologia do Desenvolvimento

    2012-07-01

    The present study aims to evaluate the influence of aniline and citric acid used alone and combined in a ratio of 50% each in the characterization of NiZn ferrite synthesized by combustion reaction method in a muffle furnace. Measurements were made of temperature and reaction time. The nano-powders were characterized by XRD, EDX, textural analysis and SEM. The highest temperature was achieved by the reaction using the mixture of fuel and increased reaction time using citric acid. The nano ferrites using different fuels, and the mixture changed phases, the crystallite size and decreased surface area of the samples with aniline, citric acid and a mixture of both, respectively. The powder morphology ranged from presenting the formation of irregular blocks for the use of citric agglomerated in the form of skeins with aniline and a mixture to agglomerate larger particles. (author)

  7. Co-coagulation of the NBR latex and clay aqueous suspension: preparation and characterization;Co-coagulacao de latex de NBR e suspensao aquosa de argila: preparacao e caracterizacao

    Reis, Raquel S.; Brum, Elisson; Silva, Vanessa M. [Nitriflex S/A Industria e Comercio, Rio de Janeiro, RJ (Brazil); Souza, Diego H.S.; Gomes, Ailton de S.; Nunes, Regina C.R., E-mail: rcnunes@ima.ufrj.b [Universidade Federal do Rio de Janeiro (IMA/UFRJ), RJ (Brazil). Inst. de Macromoleculas Profa. Eloisa Mano

    2009-07-01

    Blends of nitrile rubber (NBR) and sodium montmorillonite (MMT-Na) were prepared by co-coagulation of the NBR latex with aqueous suspension of clay. The content of MMT was varied from 0 to 7 phr and different mixtures were analyzed by X-ray diffraction, light scattering, gel content, thermogravimetric analysis and the oscillating disk rheometer. The different methods used indicated that there was formation of a structure interspersed in the mixtures studied, and that increasing the content MMT-Na enhances the values obtained. Rheological measurements on compositions with NBR showed the influence of clay on increasing the time of healing in terms of its content, as is the gel content and the thermal resistance. All results were compared to composition of NBR without MMT. (author)

  8. Characterization of gadolinia-doped ceria with manganese addition synthesized by the cation complexation technique; Caracterizacao de ceria-gadolinia e ceria-gadolinia-manganes sintetizados pelo metodo de complexacao de cations

    Yang, J.D.; Muccillo, R.; Muccillo, E.N.S., E-mail: enavarro@usp.b [Instituto de Pesquisas Energeticas e Nucleares (CCTM/IPEN/CNEN-SP), Sao Paulo, SP (Brazil). Centro de Ciencia e Tecnologia de Materiais; Rocha, R.A. [Universidade Federal do ABC (CEMCSA/UFABC), Santo Andre, SP (Brazil). Centro de Engenharia, Modelagem e Ciencias Sociais Aplicadas

    2010-07-01

    Ceria-based compounds may be used for several technological applications like catalysts, grinding media and materials for electrolyte and electrodes in solid oxide fuel cells. For most of these applications fine powders are required. In this work, nanostructured ceria powders containing 20 mol % gadolinia with and without manganese addition were synthesized by the cation complexation technique. The prepared powders were calcined at 600 deg C for thermal decomposition of the metal citrate precursors. Results of X-ray diffraction, scanning electron microscopy and specific surface area evidenced the role of manganese on physical characteristics of the nanostructured materials. The cation complexation technique revealed to be a promising method for obtaining nanostructured powders with high yield and suitable physical properties for several technological applications. (author)

  9. Chemometrics application in fuel's MTR type chemical characterization by X-ray fluorescence; Aplicacao da quimiometria para caracterizacao quimica de combustiveis tipo MTR por fluorescencia de raios-X

    Silva, Clayton Pereira da

    2012-07-01

    chemical treatments (dissolving, digesting, and others). To corrections like effects of spectral and matrix were applied and evaluated the fundamental parameter method, univariate calibration curve and multivariate calibration. The results were compared by means of statistical tests in accordance with ISO 17025 in MRCs (123 (1-7) and 124 (1-7)) MCRs of U{sub 3}O{sub 8} from New Brunswick Laboratory (NBL) and 16 U{sub 3}Si{sub 2} samples provided by CC of IPEN/CNEN-SP. The chemometrics is a promising method to determination of minor and major constituents on the U3Si2 and U3O8 basis nuclear fuel, because the precision and accuracy are statistically equal volumetric analysis, gravimetric and ICPOES methods. (author)

  10. Iron insertion and hematite segregation on Fe-doped TiO2 nanoparticles obtained from sol-gel and hydrothermal methods.

    Santos, Reginaldo da S; Faria, Guilherme A; Giles, Carlos; Leite, Carlos A P; Barbosa, Herbert de S; Arruda, Marco A Z; Longo, Claudia

    2012-10-24

    Iron-doped TiO(2) (Fe:TiO(2)) nanoparticles were synthesized by the sol-gel method (with Fe/Ti molar ratio corresponding to 1, 3, and 5%), followed by hydrothermal treatment, drying, and annealing. A similar methodology was used to synthesize TiO(2) and α-Fe(2)O(3) nanoparticles. For comparison, a mixture hematite/titania, with Fe/Ti = 4% was also investigated. Characterization of the samples using Rietveld refinement of X-ray diffraction data revealed that TiO(2) consisted of 82% anatase and 18% brookite; for Fe:TiO(2), brookite increased to 30% and hematite was also identified (0.5, 1.0, and 1.2 wt % for samples prepared with 1, 3, and 5% of Fe/Ti). For hematite/titania mixture, Fe/Ti was estimated as 4.4%, indicating the Rietveld method reliability for estimation of phase composition. Because the band gap energy, estimated as 3.2 eV for TiO(2), gradually ranged from 3.0 to 2.7 eV with increasing Fe content at Fe:TiO(2), it can be assumed that a Fe fraction was also inserted as dopant in the TiO(2) lattice. Extended X-ray absorption fine structure spectra obtained for the Ti K-edge and Fe K-edge indicated that absorbing Fe occupied a Ti site in the TiO(2) lattice, but hematite features were not observed. Hematite particles also could not be identified in the images obtained by transmission electron microscopy, in spite of iron identification by elemental mapping, suggesting that hematite can be segregated at the grain boundaries of Fe:TiO(2).

  11. Synthesis and characterization of pigments of hematite, obtained through a by-product of the siderurgy industry; Sintese e caracterizacao de pigmento de hematita, obtido atraves de um subproduto da industria siderurgica

    Prim, S.R.; Folgueiras, M.V.; Lima, M.A. de, E-mail: dem6srp@joinville.udesc.b [Universidade Estadual de Santa Catarina (PGCEM/UDESC), Joinville, SC (Brazil). Programa de Pos-Graduacao em Ciencia e Engenharia de Materiais

    2009-07-01

    In the ceramic industry of tooting, whose selection is strongly influenced by the visual aspect of the decorated surface, the color becomes one of the most important characteristic for the too tings. With the purpose of seeking new pigments that replace or optimize the already known, news method to synthesis are being researched, such as new pigments system and also the incorporation of new raw materials. In this form, in the present work search to study the possibility of use of a by-product deriving from of the siderurgical industry, that introduces high grades of the Fe{sub 2}O{sub 3}. For that different contests of the residue were added in one matrix of silica in the hape of quartz, and homogenized using conventional milling and high energy milling. The material obtained after heating treatment in temperature that varied between 1050 and 1300 deg C was characterization by x-ray diffractometry, differential thermal analysis and scanning electron microscopy. The results shown the feasibility of the process depend of the control of the variables temperature and condition of milling in the quality of material obtained. (author)

  12. Poly(phenylsesquioxane) base silicon resins: synthesis, characterization and structural study by SAXS; Resinas de silicona a base de poli(fenilsilsesquioxano): sintese, caracterizacao e estudo estrutural por SAXS

    Prado, Luis Antonio Sanchez de Almeida; Yoshida, Inez Valeria Pagotto [Universidade Estadual de Campinas (UNICAMP), SP (Brazil). Inst. de Quimica], e-mail: valeria@iqm.unicamp.br

    2000-07-01

    T{sup Ph}, T{sup Ph}D{sup L} and T{sup Ph}D{sup C} silicone resins were prepared by sol-gel method, using phenyltriethoxysilane as a source of T{sup Ph} repeating units, and poly(dimethylsiloxane), D{sup L}, or tetramethyldiethoxydissiloxane, D{sup C}, as sources of D segments. The molecular structure of these resins were characterized by FT-IR and {sup 29}Si MAS NMR spectra. SAXS traces of T{sup Ph}D{sup L} resins presented a halo associated to a high concentration of scattering units with spatial correlation. The behavior of the SAXS traces for T{sup Ph}D{sup C} were an indication of a random distribution of scattering centers. The nano structure of these materials cannot be described as a system of isolated scattering centers. The electron density contrast was attributed to the presence of regions richer in T{sup Ph} repeating units. TGA curves evidenced good thermal stability for all resins obtained. (author)

  13. E-waste: development of recycling process and chemical characterization of circuit printed - motherboard; Lixo eletronico: desenvolvimento de processo de reciclagem e caracterizacao quimica de placa de circuito impresso - motherboard

    Junior, O.L.F.; Vargas, R.A.; Andreoli, M.; Martinelli, J.R.; Seo, E.S.M., E-mail: olfjunior@usp.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN-CNEN/SP), Sao Paulo, SP (Brazil)

    2011-07-01

    The electro-electronic industry has been regulated by the National Politic of Solid Residues Act (PNRS) and Bill no. 7.404, concerning the actions, procedures, and method to collect, recycle and promotion of environmentally acceptable final destination of residues. The present work contributes to develop recycling process of printed circuit used in microcomputers and in its chemical characterization. The experimental procedure consisted of grinding, classification, magnetic and electrostatic separation, and separation based on density difference, followed by chemical characterization of the metallic and non metallic materials in the motherboard. It was determined that the amounts of Ag, Al, Ba, Cl, Cr, Cu, Fe, Mn, Pb, and Zn in the residue are above the toxicity allowable levels, and they are in the samples of the decanted material. Among the samples of the floating material, Al, Ba, Br, Ca, Cu, Fe, Pb (in less quantity), Si (in more quantity), and Sn, Ti and Zn were detected. Those materials can be useful in the preparation of red ceramics. (author)

  14. Synthesis and characterization of pillared bentonite with Al, AL/Fe and impregnated with Pd; Sintese e caracterizacao de bentonitas pilarizadas com Al, AL/Fe e impregnadas com Pd

    Silva, Marcus Vinicius Costa; Pizarro, Alejandro Herrero; Molina, Carmen Belen, E-mail: marcus.ufpa@yahoo.com.br [Universidade Federal do Para (UFPA), Belem, PA (Brazil). Instituto de Tecnologia. Faculdade de Engenharia Quimica; Seccion de Ingenieria Quimica, Facultad de Ciencias, Universidad Autonoma de Madri (Spain)

    2017-10-01

    In this work, a north american bentonite was pillared with Al and Al/Fe, creating the Al-PILC and Al-Fe-PILC, respectively. Then the Pd was impregnated in the materials, generating Pd-Al-PILC and Pd-Al-Fe-PILC, respectively. The samples were characterized by X-ray diffraction, differential thermal analysis and thermogravimetric and N{sub 2} adsorption at 77 K to determine the specific surface area by BET method (Brunauer - Emmett - Teller). There was an increase in the basal spacing of bentonite from 12.4Å in the original sample to 17.81Å in the Al-Fe-PILC, 17.20Å in Pd-Al-PILC and 17.05Å in the Pd-Al-Fe-PILC. The specific surface area increased from 19.05m{sup 2}/g in the original sample to 173.49m{sup 2}/g in Al-Fe-PILC, 101.31m{sup 2}/g to Pd-Al-PILC and 92m{sup 2}/g in Pd-Al-Fe-PILC. The pillaring process was successful and the synthesized materials have great potential for use as catalysts. (author)

  15. Microstructural characterization of composite cobaltite and lanthanum-based ceria for use as fuel cell cathodes; Caracterizacao microestrutural de compositos a base de cobaltita de lantanio e ceria para aplicacao como catodos de celulas a combustivel

    Rodrigues, E.R.T.; Nascimento, R.M.; Miranda, A.C. de; Lima, A.M. de, E-mail: erickssonrtr@gmail.com [Universidade Federal do Rio Grande do Norte (UFRN), RN (Brazil); Macedo, D.A. [Universidade Federal da Paraiba (UFPB), PB (brazil)

    2016-07-01

    Fuel cells are devices that convert chemical energy into electricity via redox reactions. In this work, the lanthanum cobaltite doped with strontium and iron (La{sub 0,6}Sr{sub 0,4}Co{sub 0,2}Fe{sub 0,8}O{sub 3} - LSCF) a traditional cathodes material of the fuel cell was mixed with an electrolyte material (composite) to the base ceria doped with gadolinia and a eutectic mixture of lithium carbonates and sodium (CGO-NLC). The powders of LSCF and CGO-NLC were obtained by the citrate method and mixed to obtain a composite cathode. Samples obtained by uniaxial pressure between 5 and 10 MPa were sintered at 1100°C and investigated by X-ray diffraction, scanning electron microscopy and micro hardness test. A symmetric cell cathode / electrolyte / cathode, obtained by co-pressing and co-sintering was investigated by electron microscopy. The results indicated that the composite is chemically stable up to the sintering temperature used. The hardness ranged between 51 and 227 HV. (author)

  16. Microstructural development and characterization of lanthanum chromite-based ceramics to application in solid oxide fuel cells; Desenvolvimento microestrutural e caracterizacao de ceramicas a base de cromita de lantanio para aplicacao em celulas a combustivel de oxido solido

    Oliveira, R.N.; Furtado, J.G. de M.; Soares, C.M.; Serra, E.T. [Centro de Pesquisas de Energia Eletrica (CEPEL), Rio de Janeiro, RJ (Brazil)], e-mail: rnunes@cepel.br

    2006-07-01

    This work has for objective to investigate and to characterize the microstructural development of lanthanum chromite-based ceramics (LaCrO{sub 3}) doped with earth alkaline metals, correlating the microstructural parameters (mainly the densification level) and processing parameters with the electrothermal properties reached. Lanthanum chromite-based ceramic systems doped with earth-alkaline metals (Ca, Mg and Sr) had been produced from respective metallic nitrates by solid state reactions process. The phase compositions were evaluated by X-ray diffraction and the densification level by Archimedes method. The microstructural characterization was effected by scanning electron microscopy, energy dispersive X-ray spectroscopy and thermal analysis techniques. Electrical tests were used to evaluate the electrical conductivity of the studied ceramics. The obtained results corroborate the literature comments concerning the difficulty of lanthanum chromite-based ceramics with high densification level and evidence the great influence of the nature of the dopants on the sintering mechanism and the microstructural and electric characteristics of the produced ceramics. The best ones results, in terms of densification and electrical conductivity, had been gotten through multiple doping with calcium and strontium, and in sintering temperature conditions lower that the normally considered to pure or monodoped lanthanum chromite-based ceramics. (author)

  17. Technological characterization of a mineral deposit. A case study: the niobium of Catalao I, Goias State, Brazil; Caracterizacao tecnologica de um deposito mineral. Um estudo de caso: o niobio de Catalao I, Goias

    Sant` Agostino, Lilia Mascarenhas

    1997-12-31

    This thesis presents a contribution to the subject of ore technological characterization integrated to orebody context, regarding sample, ore characteristics, ore types definition and distribution through the mineral occurrence, and ore reserves modeling using technological parameters. A professional experience in this specialization based a conceptual discussion of the matter, supported by a practical approach. The initial approach is the subject definition, and it`s importance for technological and economical feasibility studies, in all phases of mining research and development, as a tool for beneficiation alternatives definition. The multidisciplinary aspect of the knowledge involved for ore characterization is remarked, considering that is an interface segment to be conduced interactively with others. It is an applied mineralogy, that needs some geological and some ore dressing imputes. After the general considerations about importance and applicability, it follows a methodological approach of laboratory procedures and analytical techniques, as a result of practical experience acquired in the study of several ores. The main points discussed are related with criterion to organized laboratory preparation scheme and to select appropriated analytical techniques, without detailing them, for what some specialized bibliography is indicated. Finalizing the theoretical explanation, there is a concise description about computers resources for 3D orebody modeling, and integrated software applied for geology and mining. For illustration, it is exposed a complex ore case study: niobium mineralization associated with the alkaline-carbonatitic occurrence of Catalao I, located in Goias State, Brazil. Besides the explanation of laboratory procedures and methods applied, results treatment and interpretation are emphasized, under both characterization and economic point of view. (author) 135 refs., 57 figs., 38 tabs.

  18. Synthesis and characterization of rare earth molybdates nanoparticles for detection of specific prostatic cancer (PSA); Preparacao e caracterizacao de nanoparticulas de molibdatos de terras raras para deteccao do antigeno especifico da prostata (PSA)

    Dias, Clarissa Lombardi

    2013-07-01

    The interest in using rare earths to investigate the properties and functions of biochemical systems as well as to determinate biological substances has increased in several fields, including biomarkers in immunology (fluoro immunoassays). Nowadays the use of lanthanides in the diagnosis of various diseases have become more important through the development of commercial diagnostic kits. As main feature, these rare earths can show a long lifetime, photo stability and emission bands of atomic like behavior and well defined, in the visible region, demonstrating unique advantages when compared to other luminescent species. The present work had as its goal to synthesize rare earth molybdates by the co-precipitation method as well as to characterize these materials by X-ray diffraction, near infrared spectroscopy, thermogravimetric analysis, scanning electronic microscopy, transmission electronic microscopy and luminescent studies. In this work, three different studied were developed: the influence of the vortex speed variation during co-precipitation in the structure of the final product, morphology and luminescence properties; the influence of the annealing temperature also in the structure, morphology and luminescence properties; and the influence of concentration of the doping in the luminescence properties. Another important step of this work was the functionalization of nanoparticles using an organosilane (APTES) to coat and establish points for binding the particles to biological species. It was proved that this process was very efficient by the characterization results and the silica incorporation was well succeeded. Specific prostatic cancer (PSA) was then linked to the functionalized nanoparticles to diagnostic prostatic cancer by fluoroimmunoassay and levels for detection were established. (author)

  19. Preparation and characterization of electrocatalysts based on palladium for electro-oxidation of alcohols in alkaline medium; Preparacao e caracterizacao de eletrocatalisadores a base de paladio para oxidacao eletroquimica de alcoois em meio alcalino

    Brandalise, Michele

    2012-07-01

    In this study Pd/C, Au/C, PdAu/C, PdAuPt/C, PdAuBi/C and PdAuIr/C electrocatalysts were prepared by the sodium borohydride reduction method for the electrochemical oxidation of methanol, ethanol and ethylene glycol. This methodology consists in mix an alkaline solution of sodium borohydride to a mixture containing water/isopropyl alcohol, metallic precursors and the Vulcan XC 72 carbon support. The electrocatalysts were characterized by energy dispersive X-ray (EDX), X-ray diffraction (XRD), transmission electron microscopy (TEM) and cyclic voltammetry. The electrochemical oxidation of the alcohols was studied by chronoamperometry using a thin porous coating technique. The mechanism of ethanol electro-oxidation was studied by Fourier Transformed Infrared (FTIR) in situ. The most effective electrocatalysts were tested in alkaline single cells directly fed with methanol, ethanol or ethylene glycol. Preliminary studies showed that the most suitable atomic composition for preparing the ternary catalysts is 50:45:05. Electrochemical data in alkaline medium show that the electrocatalysts PdAuPt/C (50:45:05) showed the better activity for methanol electro oxidation, while PdAuIr/C was the most active for ethanol oxidation and PdAuBi/C (50:45:05) was the most effective for ethylene glycol oxidation in alkaline medium. These results show that the addition of gold in the composition of electrocatalysts increases their catalytic activities. The spectroelectrochemical FTIR in situ data permitted to conclude that C-C bond is not broken and the acetate is formed. (author)

  20. Preparation and characterization of sulfated zirconia acid catalysts for application in the esterification of cottonseed oil; Preparacao e caracterizacao de catalisadores acidos de zirconia sulfatada para aplicacao na esterificacao do oleo de algodao

    Silva, F. N.; Moura, T. F. B.; Silva, A.S.; Costa, A.C.F.M., E-mail: fnilson.s@hotmail.com [Universidade Federal de Campina Grande (UFCG), PB (Brazil). Pos-graduacao em Engenharia de Materiais; Pallone, E.M.J.A. [Universidade de Sao Paulo (USP), Pirassununga, SP (Brazil). Dept. de Ciencias Basicas

    2017-07-15

    This work aimed to produce zirconia by combustion synthesis, to analyze the structure and morphology comparatively with a commercial monoclinic ZrO{sub 2} , as well as, to investigate the sulfation, aiming to obtain acid catalysts for its use in the esterification of cotton oil for biodiesel. The samples were characterized by X-ray diffraction, scanning electron microscopy (SEM), specific surface area by BET method, infrared spectroscopy (FTIR), thermal analysis (TG/DrTG/DTA), granulometric distribution, pH and chromatography. The synthesized sample evidenced the formation of the monoclinic phase with traces of the orthorhombic phase, while in the commercial sample only the monoclinic phase was observed. In the sulfation process, traces of the tetragonal phase, typical of sulfated zirconia, were observed with the presence of the monoclinic phase in the two samples. With the impregnation of the sulfate ion on the surface of the samples, an increase in the particle size was observed, as seen in the characterization of BET, granulometric distribution and SEM, which also indicated a homogeneous morphology consisting of fine particles of approximately spherical shape for both samples. The chromatography indicated conversion of 65.5 and 91.8% in methyl esters to the synthesized and commercial SO{sub 4} {sup 2-}/ZrO{sub 2} , respectively. The results indicated that the sulfation increased the acidity, which was evidenced by the decrease in the pH, ranging from 5.12 to 2.65, which contributed significantly to the increase of the conversion, indicating that the SO{sub 4} {sup 2-}/ZrO{sub 2} is a promising catalyst in the esterification. (author)

  1. Technological characterization of a mineral deposit. A case study: the niobium of Catalao I, Goias State, Brazil; Caracterizacao tecnologica de um deposito mineral. Um estudo de caso: o niobio de Catalao I, Goias

    Sant`Agostino, Lilia Mascarenhas

    1996-12-31

    This thesis presents a contribution to the subject of ore technological characterization integrated to orebody context, regarding sample, ore characteristics, ore types definition and distribution through the mineral occurrence, and ore reserves modeling using technological parameters. A professional experience in this specialization based a conceptual discussion of the matter, supported by a practical approach. The initial approach is the subject definition, and it`s importance for technological and economical feasibility studies, in all phases of mining research and development, as a tool for beneficiation alternatives definition. The multidisciplinary aspect of the knowledge involved for ore characterization is remarked, considering that is an interface segment to be conduced interactively with others. It is an applied mineralogy, that needs some geological and some ore dressing imputes. After the general considerations about importance and applicability, it follows a methodological approach of laboratory procedures and analytical techniques, as a result of practical experience acquired in the study of several ores. The main points discussed are related with criterion to organized laboratory preparation scheme and to select appropriated analytical techniques, without detailing them, for what some specialized bibliography is indicated. Finalizing the theoretical explanation, there is a concise description about computers resources for 3D orebody modeling, and integrated software applied for geology and mining. For illustration, it is exposed a complex ore case study: niobium mineralization associated with the alkaline-carbonatitic occurrence of Catalao I, located in Goias State, Brazil. Besides the explanation of laboratory procedures and methods applied, results treatment and interpretation are emphasized, under both characterization and economic point of view. (author) 135 refs., 57 figs., 38 tabs.

  2. Proposal of a methodology to be applied for the characterization of external exposure risk of employees in nuclear medicine services; Proposta de uma metodologia para caracterizacao de risco de exposicao externa de funcionarios de servicos de medicina nuclear

    Simoes, Rafael Figueiredo Pohlmann

    2010-07-01

    Nuclear medicine procedure requires the administration of radioactive material by injection, ingestion or inhalation. After incorporation, the patient becomes a mobile source of radiation and, after their examination; they can irradiate everyone on their way out of the Nuclear Medicine Service (NMS). A group of workers in this path is considered a critical group, but there are no conviction on this classification, because there are not measurements available. Thus, workers claiming for occupationally exposed individual's (OEI) rights are common. Employers are always in a complex situation, because if they decided to undertake the individual external monitoring of the critical working groups, the Court considers all as OEI and employers are taxed. On the other hand, if they do not provide monitoring, it is impossible to prove that these workers were not exposed to effective doses higher than individual annual public's limit and they lose the actions, too. This work proposes a methodology to evaluate, using TLD environmental monitors, air kerma rate at critical staff points in a NMS. This method provides relevant information about critical groups' exposure. From these results, the clinic or hospital may prove technically, without individual monitoring of employees, the classification of areas and can estimate the maximum flow of patients in the free areas which guarantees exposures below the public individual dose limit. This methodology has been applied successfully to a private clinic in Rio de Janeiro, which operates a NMS. The only critical group that received exposure statistically different from clinic background radiation was that on the antechamber of the NMS. This is a site that should be characterized as a supervised area and the group of workers in this environment as OEI, as the estimated extrapolated annual effective dose in this position was 1.2 +- 0.7 mSv/year, above the public annual limit (1,0 mSv/year). Normalizing by the number of

  3. Characterization of the wind behavior in Botucatu-SP region (Brazil) by Weibull distributing; Caracterizacao do comportamento eolico da regiao de Botucatu-SP atraves da distribuicao de Weibull

    Gabriel Filho, Luis Roberto Almeida [Universidade Estadual Paulista (CE/UNESP), Tupa, SP (Brazil). Coordenacao de Estagio; Cremasco, Camila Pires [Faculdade de Tecnologia de Presidente Prudente, SP (Brazil); Seraphim, Odivaldo Jose [Universidade Estadual Paulista (FCA/UNESP), Botucatu, SP (Brazil). Fac. de Ciencias Agronomicas; Cagnon, Jose Angelo [Universidade Estadual Paulista (FEB/UNESP), Bauru, SP (Brazil). Faculdade de Engenharia

    2008-07-01

    The wind behavior of a region can be described by frequency distribution that provide information and characteristics needed for a possible deployment of wind energy harvesting in the region. These characteristics, such as the annual average speed, the variance and shunting line standard of the registered speeds and the density of aeolian power average hourly, can be gotten by the frequency of occurrence of determined speed, that in turn must be studied through analytical expressions. The more adjusted analytical function for aeolian distributions is the function of density of Weibull, that can be determined by numerical methods and linear regressions. Once you have determined this function, all wind characteristics mentioned above may be determined accurately. The objective of this work is to characterize the aeolian behavior in the region of Botucatu-SP and to determine the energy potential for implementation of aeolian turbines. For the development of the present research, was used an Monitorial Young Wind anemometer of Campbell company installed a 10 meters of height. The experiment was developed in the Nucleus of Alternative Energies and Renewed - NEAR of the Laboratory of Agricultural Energize of the Department of Agricultural Engineering of the UNESP, Agronomy Sciences Faculty, Lageado Experimental Farm, located in the city of Botucatu - SP. The geographic localization is defined by the coordinates 22 deg 51' South latitude (S) and 48 deg 26' Longitude West (W) and average altitude of 786 meters above sea level. The analysis was carried through using registers of speed of the wind during the period of September of 2004 the September of 2005. After determined the distribution of frequencies of the hourly average speed of the wind, it was determined function of associated Weibull, thus making possible the determination of the annual average speed of the wind (2,77 m/s), of the shunting line standard of the registered speeds (0,55 m/s), of the

  4. Crystal structure and ionic conduction path of solid electrolytic materials by high temperature neutron diffraction method

    Yashima, Masatomo; Nomura, Katsuhiro

    2005-01-01

    Research of the distribution of oxide ions and the ionic conduction path of bismuth oxide (Bi 2 O 3 ), cerium oxide (CeO 2 ) and lanthanum gallate ((La 0.8 Sr 0.2 )(Ga 0.8 Mg 0.15 Co 0.05 )O 3-δ ) is stated. The high temperature neutron diffraction method, analytical method such as Rietveld method, crystal structure analysis of ionic conductor and MEM (Maximum- Entropy Method) are explained. The nuclear density distribution of oxide ions in bismuth oxide showed so larger distribution in the direction of and than Bi ions that the oxide ions conducted these direction in the crystal. The nuclear density distribution of oxide ions of cerium oxide indicated larger distribution in the direction of than Ce ions and its tendency was remarkable at high temperature. Accordingly, the oxide ions conducted in the direction of and . The oxide ions distribution in lanthanum gallate compound was larger and complicated than positive ions. The oxide ions conducted to by describing an arc between the two stable positions. The nuclear density on the conduction path increased with increasing temperature. This above result corresponded to increase of oxide ion conductivity in the area. (S.Y.)

  5. Characterization of working iron Fischer-Tropsch catalysts using quantitative diffraction methods

    Mansker, Linda Denise

    This study presents the results of the ex-situ characterization of working iron Fischer-Tropsch synthesis (F-TS) catalysts, reacted hundreds of hours at elevated pressures, using a new quantitative x-ray diffraction analytical methodology. Compositions, iron phase structures, and phase particle morphologies were determined and correlated with the observed reaction kinetics. Conclusions were drawn about the character of each catalyst in its most and least active state. The identity of the active phase(s) in the Fe F-TS catalyst has been vigorously debated for more than 45 years. The highly-reduced catalyst, used to convert coal-derived syngas to hydrocarbon products, is thought to form a mixture of oxides, metal, and carbides upon pretreatment and reaction. Commonly, Soxhlet extraction is used to effect catalyst-product slurry separation; however, the extraction process could be producing irreversible changes in the catalyst, contributing to the conflicting results in the literature. X-ray diffraction doesn't require analyte-matrix separation before analysis, and can detect trace phases down to 300 ppm/2 nm; thus, working catalyst slurries could be characterized as-sampled. Data were quantitatively interpreted employing first principles methods, including the Rietveld polycrystalline structure method. Pretreated catalysts and pure phases were examined experimentally and modeled to explore specific behavior under x-rays. Then, the working catalyst slurries were quantitatively characterized. Empirical quantitation factors were calculated from experimental data or single crystal parameters, then validated using the Rietveld method results. In the most active form, after pretreatment in H 2 or in CO at Pambient, well-preserved working catalysts contained significant amounts of Fe7C3 with trace alpha-Fe, once reaction had commenced at elevated pressure. Amounts of Fe3O 4 were constant and small, with carbide dpavg 65 wt%, regardless of pretreatment gas and pressure, with

  6. Biopolymer chitin: extraction and characterization; Biopolimero quitina: extracao e caracterizacao

    NONE

    2011-07-01

    The biopolymers are materials made from renewable sources such as soybean, corn, cane sugar, cellulose and chitin. Chitin is the most abundant biopolymer found in nature, after cellulose. The chemical structure of chitin is distinguished by the hydroxyl group, of structure from cellulose, located at position C-2, which in the chitin is replaced by acetamine group. The objective of this study was to develop the chitin from exoskeletons of Litopenaeus vannamei shrimp, which are discarded as waste, causing pollutions, environmental problems and thus obtain better utilization of these raw materials. It also, show the extraction process and deacetylation of chitosan. The extraction of chitin followed steps of demineralization, desproteinization and deodorization. Chitin and chitosan were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD) and the thermals properties were analyzed by thermogravimetry (TG/DTG). (author)

  7. Characterization of cellulose nanowhiskers; Caracterizacao do nanowhiskers de celulose

    Nascimento, Nayra R.; Pinheiro, Ivanei F.; Morales, Ana R.; Ravagnani, Sergio P.; Mei, Lucia, E-mail: 25nareis@gmail.com [Universidade Estadual de Campinas (UNICAMP), SP (Brazil)

    2015-07-01

    Cellulose is the most abundant polymer earth. The cellulose nanowhiskers can be extracted from the cellulose. These have attracted attention for its use in nanostructured materials for various applications, such as nanocomposites, because they have peculiar characteristics, among them, high aspect ratio, biodegradability and excellent mechanical properties. This work aims to characterize cellulose nanowhiskers from microcrystalline cellulose. Therefore, these materials were characterized by X-ray diffraction (XRD) to assess the degree of crystallinity, infrared spectroscopy (FT-IR), transmission electron microscopy (TEM) to the morphology of nanowhiskers and thermal stability was evaluated by Thermogravimetric Analysis (TGA). (author)

  8. Obtention and characterization of biodiesel; Obtencao e caracterizacao do biodiesel

    Santos, Leonidas B.O. dos; Caitano, Moises; Aranda, Donato A.G.; Mothe, Cheila G. [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil)

    2004-07-01

    Biodiesel is an ester resulting from the transesterification reaction of an alcohol and an oil obtained from biomass. The products of the transesterification are an ester and the glycerol. The biodiesel and the petroleum commercial diesel have similar properties, and they can be mixed and used in diesel motors. The use of biodiesel will allow a better exploration of the energetic potential of our cultures. The biodiesel has some advantages compared to others combustibles, such as adaptability to usual diesel motors and non-generation of NO{sub x} and SO{sub x} compounds. Many experiments with biodiesel have been made in Brazil since the 70's. This work made samples of biodiesel by transesterification batch reactions to many blends of soybean oil and residual fry oil, at room temperature, using mechanical mixture or magnetic agitation by a magnetic stirrer, using as catalysts sodium methoxide and potassium hydroxide. For each obtained sample tests to determine the Acidity Index (ABNT-MB-74), Saponification Index (ABNT-MB-75), Iodine Wijz Index (ABNT-MB- 77), thermal analysis by DTA and TG (TA Instruments SDT 2960, 30 to 800 deg C, 10 deg C/min at nitrogen atmosphere) and rheological test (Haake RS 150 Rheo Stress rheometer) were done. (author)

  9. Energetic characterization of Amazonian biomass; Caracterizacao energetica de biomassas amazonicas

    Feitosa Netto, Genesio Batista; Oliveira, Antonio Geraldo de Paula; Coutinho, Hebert Willian Martins; Nogueira, Manoel Fernandes Martins; Rendeiro, Goncalo [Universidade Federal do Para (UFPA), Belem, PA (Brazil). Dept. de Engenharia Mecanica

    2006-07-01

    In order to asses the potentiality of Amazon biomasses to generate power, either to supply electric energy to the grid or as fuel to plants supplying power for off-grid location, data for their proximate analysis must be available. A literature review on the subject indicated a lack of information and data concerning typical Amazon rain forest species. This work aimed to characterize (proximate analysis) 43 Amazon species in order to evaluate the energy resource from woody biomass wastes in Amazon region. Higher heating value, carbon, volatile and ash contents were measured in a dry basis. The measurements were performed obeying the following Brazilian standards, NBR 6923, NBR 8112, NBR 8633, NBR 6922. (author)

  10. Synthesis and characterization of Ni{sub 0.7}Zn{sub 0.3}Fe{sub 2}O{sub 4} ferrospinel: performance evaluation for methyl and ethyl esterification; Sintese e caracterizacao do ferroespinelio Ni{sub 0,7}Zn{sub 0,3}Fe{sub 2}O{sub 4}: avaliacao de desempenho na esterificacao metilica e etilica

    Mapossa, A.B., E-mail: mapossabenjox@gmail.com [Curso de Quimica, Dept. de Ciencias Naturais, Universidade Pedagogica de Mocambique, Delegacao de Manica, Chimoio (Mozambique); Dantas, J.; Diniz, V.C.S.; Costa, A.C.F.M. [Universidade Federal de Campina Grande (UFCG), PB (Brazil). Programa de Pos-Graduacao em Ciencia e Engenharia de Materiais; Silva, M.R. [Universidade Federal de Itajuba (UNIFEI), MG (Brazil). Dept. de Fisica; Kiminami, R.H.G.A. [Universidade Federal de Sao Carlos (UFSCar), SP (Brazil). Departamento de Engenharia de Materiais

    2017-04-15

    Ni{sub 0.7}Zn{sub 0.3}Fe{sub 2}O{sub 4} ferrospinel was synthesized by combustion and its catalytic performance in methyl and ethyl esterification of the soybean oil was investigated. The samples were characterized by X-ray diffraction, Rietveld refinement analysis, energy dispersive X-ray fluorescence spectroscopy, Fourier transform infrared spectroscopy, textural analysis, scanning electron microscopy, density by picnometry, particle size analysis, thermogravimetric analysis, magnetic measurements, and catalytic tests. The synthesis was efficient resulting in a ferrospinel with single phase Ni{sub 0.7}Zn{sub 0.3}Fe{sub 2}O{sub 4} with crystallite size of 20 nm, high surface area (86 m{sup 2}/g) and saturation magnetization of 18 emu/g. The ferrospinel had promising catalytic activity in both reaction conditions studied, being more active in the conversion of soybean oil to biodiesel in methyl esterification with an average conversion of 93.9±2.8%. (author)

  11. Solution combustion method for synthesis of nanostructured hydroxyapatite, fluorapatite and chlorapatite

    Zhao, Junjie; Dong, Xiaochen; Bian, Mengmeng [School of Chemistry and Materials Engineering, Changshu Institute of Technology, Changshu (China); Zhao, Junfeng, E-mail: daidai02304@163.com [School of Chemistry and Materials Engineering, Changshu Institute of Technology, Changshu (China); Jiangsu Laboratory of Advanced Functional Materials, Changshu Institute of Technology, Changshu (China); Zhang, Yao; Sun, Yue [School of Chemistry and Materials Engineering, Changshu Institute of Technology, Changshu (China); Chen, JianHua; Wang, XuHong [School of Chemistry and Materials Engineering, Changshu Institute of Technology, Changshu (China); Jiangsu Laboratory of Advanced Functional Materials, Changshu Institute of Technology, Changshu (China)

    2014-09-30

    Highlights: • We report a synthesis of HA, Fap and Clap vio a modified solution combustion method. The nucleation of β-TCP was inhibited in the abundant-calcium system (Ca/P = 2.3>>1.67) in this study. F{sup −} brushed into the structure of HA and replace the position of OH{sup −} is easier than that of Cl{sup −}. - Abstract: Hydroxyapatite (HAP), fluorapatite (Fap) and chlorapatite (Clap) were prepared by solution combustion method with further annealing at 800 °C. The characterization and structural features of the synthesized powders were evaluated by the powder X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FT-IR), scanning electron microscope (SEM) and transmission electron microscopy (TEM) techniques. Characterization results from XRD and Rietveld analysis revealed that OH{sup −} in the HAP lattice were gradually substituted with the increase of F{sup −} and Cl{sup −} content and totally substituted at the molar concentration of 0.28 and 0.6, respectively. The results from FI-IR have also confirmed the incorporation of substituted anions in the apatite structure.

  12. A simple dissolved metals mixing method to produce high-purity MgTiO3 nanocrystals

    Pratapa, Suminar; Baqiya, Malik A.; Istianah,; Lestari, Rina; Angela, Riyan

    2014-01-01

    A simple dissolved metals mixing method has been effectively used to produce high-purity MgTiO 3 (MT) nanocrystals. The method involves the mixing of independently dissolved magnesium and titanium metal powders in hydrochloric acid followed by calcination. The phase purity and nanocrystallinity were determined by making use of laboratory x-ray diffraction data, to which Rietveld-based analyses were performed. Results showed that the method yielded only one type magnesium titanate powders, i.e. MgTiO 3 , with no Mg 2 TiO 4 or MgTi 2 O 5 phases. The presence of residual rutile or periclase was controlled by adding excessive Mg up to 5% (mol) in the stoichiometric mixing. The method also resulted in MT nanocrystals with estimated average crystallite size of 76±2 nm after calcination at 600°C and 150±4 nm (at 800°C). A transmission electron micrograph confirmed the formation of the nanocrystallites

  13. Development and applications of the reverse neutron time-of-flight method with Fourier-type beam chopper

    Antson, O.

    1991-09-01

    The neutron powder diffraction method has been applied to the crystal structure analysis of high-temperature superconductors such as La 0 .8Sr 0 .2CuO 4 - y , YBa 2 Cu 3 O 7 - y and Bi 2 Sr 2 CaCu 2 O 8 + y optically active yttriumformate Y(HCOO) 3 , and β phase of deuterated acetonitrile, CD 3 CN. The structural information, containing symmetry, positional and thermal parameters, occupation factors and the order parameter, was obtained by measuring the coherent elastic scattering cross-section. The Rietveld profile refinement method was used for the extraction of structural parameters from experimental data. The diffraction spectra were obtained by measuring the time-of-flight distribution of neutrons with a Fourier-type beam chopper. The neutron diffraction spectrum is created by the on-line synthesis of the cross-correlation function between the beam modulation function and the detector intensity. Such an operational mode, called the reverse time-of-flight method, has many unique properties. The possibility of filtering out a low-frequency part of a diffraction spectrum, eg. incoherent background, by a properly selected band-pass filter has been studied. One of the practical applications of the reverse time-of-flight method, the Mini-Sfinks facility, is described with technical details, and its operational characteristics are compared with other high-resolution instruments

  14. Effect of synthesis methods with different annealing temperatures on micro structure, cations distribution and magnetic properties of nano-nickel ferrite

    El-Sayed, Karimat [XRD Lab, Physics Department, Faculty of Science, Ain-Shams University, Cairo (Egypt); Mohamed, Mohamed Bakr, E-mail: mbm1977@yahoo.com [XRD Lab, Physics Department, Faculty of Science, Ain-Shams University, Cairo (Egypt); Hamdy, Sh.; Ata-Allah, S.S. [Reactor Physics Department, NRC, Atomic Energy Authority, P.O. Box 13759, Cairo (Egypt)

    2017-02-01

    Nano-crystalline NiFe{sub 2}O{sub 4} was synthesized by citrate and sol–gel methods at different annealing temperatures and the results were compared with a bulk sample prepared by ceramic method. The effect of methods of preparation and different annealing temperatures on the crystallize size, strain, bond lengths, bond angles, cations distribution and degree of inversions were investigated by X-ray powder diffraction, high resolution transmission electron microscope, Mössbauer effect spectrometer and vibrating sample magnetometer. The cations distributions were determined at both octahedral and tetrahedral sites using both Mössbauer effect spectroscopy and a modified Bertaut method using Rietveld method. The Mössbauer effect spectra showed a regular decrease in the hyperfine field with decreasing particle size. Saturation magnetization and coercivity are found to be affected by the particle size and the cations distribution. - Highlights: • Annealed nano NiFe{sub 2}O{sub 4} was prepared by different methods. • The crystallite sizes are critical. • Mössbauer spectra show superparamagnetic doublet. • Cations distributions by MÓ§ssbauer and Bertaut method are constituents. • Cations distribution are significantly affects the magnetic properties.

  15. Nanocystalline ZnO films prepared via polymeric precursor method (Pechini)

    Sanchez, C.; Doria, J.; Paucar, C.; Hernandez, M. [Laboratorio de Materiales Ceramicos y Vitreos, Universidad Nacional de Colombia, Sede Medellin, A.A. 568, Medellin (Colombia); Mosquera, A.; Rodriguez, J.E. [Grupo CYTEMAC, Universidad del Cauca, Calle 5 No 4-70, Popayan (Colombia); Gomez, A. [Departamento de Ingenieria de Materiales, Universidad Nacional de Colombia, sede Medellin, A.A. 568, Medellin (Colombia); Baca, E. [Grupo de Ingenieria de Nuevos Materiales, Universidad del Valle, A.A. 25360 Cali (Colombia); Moran, O., E-mail: omoranc@unal.edu.c [Laboratorio de Materiales Ceramicos y Vitreos, Universidad Nacional de Colombia, Sede Medellin, A.A. 568, Medellin (Colombia)

    2010-09-01

    The polymeric precursor method (Pechini) was employed to prepare high-quality nanocrystalline zinc oxide (ZnO) films. Briefly, the process started off with the preparation of a coating solution by the Pechini process followed by a coating of the glass substrates by a dip-coating technique and subsequent heat-treatment of the as-deposited films up to 550 {sup o}C for 30 min. The Rietveld profile analysis of the X-ray diffraction (XRD) spectra revealed the wuerzite structure as expected for ZnO with a P6{sub 3}mc symmetry. No additional peaks were observed that would correspond to any secondary crystalline phase. The average crystallites size was 20 nm as calculated by Sherrer's equation. UV-vis spectroscopy showed sharp ultraviolet absorption edges at {approx}380 nm. The absorption edge analysis yielded optical band gap energy of 3.24 eV with electronic transition of the direct transition type. The Fourier transform infrared (FTIR) analysis showed asymmetric and symmetric stretching modes of the carboxyl group (C=O). Scanning electron microscope (SEM) analysis revealed a crack-free surface morphology indicating that coating of the amorphous glass substrates was homogeneous on large surface areas. The temperature dependent conductivity featured a typical semiconducting-like behavior with resistivity approaching 3x10{sup -1} {Omega} cm at 220 K.

  16. Synthesis and characterization of Cr2O3 nanoparticles through sol-gel proteic method

    Medeiros, Angela Maria de Lemos

    2007-01-01

    In the last years, nanoparticles have becoming important to several researchers. This research reside in the fact that new and uncommon physical and chemical properties, absent in the same material in macro and microscopic size, are observed in this new scale. The subject of this study is obtaining chromium oxide nanoparticles (Cr 2 O 3 ) by sol–gel proteic process using gelatin as an organic precursor. This process appears as a new alternative for the synthesis of oxides for great applications with high efficiency and low cost. The interest in that material is due to the several applications such as green pigments, coverings of materials for thermal protection and mainly as catalyst of countless products originating from of the industry of the petroleum, among others. This new route, using chromium salt as chromium source, produces nanoparticles with average particle size between 20 and 60nm. These values were obtained for different crystallographic direction by means of X-Ray Diffraction (XRD) technique and the structure refinement by Rietveld method were applied in several samples prepared at different temperatures. Other techniques have been used in order to complement the XRD results. (author)

  17. Enhancement of magnetic properties of Co{sub 2}MnSi Heusler alloy prepared by mechanical alloying method

    Rabie, Naeemeh; Gordani, Gholam Reza; Ghasemi, Ali, E-mail: ali13912001@yahoo.com

    2017-07-15

    Highlights: • Ferromagnetic Heusler alloys of Co{sub 2}MnSi were synthesized at low temperature. • There is an at least 30% reduction in the phase formation temperature. • Saturation magnetization of alloy was increased significantly after annealing. - Abstract: Ferromagnetic Heusler alloys of Co{sub 2}MnSi were synthesized by mechanical alloying method at low temperature. The effect of milling time and annealing process on structural and magnetic properties of ferromagnetic alloy samples were studied by X-ray diffraction, scanning electron microscopy and vibration sample magnetometer methods, respectively. Structural characteristics such as crystallite size, phase percentage, and lattice parameter determined using the Rietveld method. The values of these parameters were obtained 362.9 nm, 5.699 Å and 98.7%, respectively for annealed sample. Magnetization studies show that the Co2MnSi phase is formed at 15 h of milling and is optimized after 20 h of milling. VSM results showed that saturation magnetization (M{sub s}) of milled samples reduces from 112 to 75 (emu/g) with increasing milling time and then increased gradually to 95 emu/g. The effect of post-annealing on the structural and magnetic properties of milled samples was also investigated. The saturation magnetization of annealed sample (120 emu/g) is higher than the optimum milled sample (95 emu/g) due to increasing preferential ordered L2{sub 1} structure.

  18. Synthesis and characterization of La(Cr,Fe,Mn)O{sub 3} nanoparticles obtained by co-precipitation method

    Fabian, F.A., E-mail: fernandafabianro@gmail.com [Universidade Federal de Sergipe, Campus Prof. Aluísio Campos, Departamento de Física, 49100-000 São Cristóvão, SE (Brazil); Pedra, P.P.; Filho, J.L.S. [Universidade Federal de Sergipe, Campus Prof. Aluísio Campos, Departamento de Física, 49100-000 São Cristóvão, SE (Brazil); Duque, J.G.S.; Meneses, C.T. [Universidade Federal de Sergipe, Campus Prof. Alberto Carvalho, Departamento de Física, 49500-000 Itabaiana, SE (Brazil)

    2015-04-01

    Magnetic and structural properties have been investigated in La(Cr,Fe,Mn)O{sub 3} nanoparticles obtained by co-precipitation method. The X-ray diffraction measurements allied to Rietveld method confirm the formation of LaCrO{sub 3}, LaFeO{sub 3} and LaMnO{sub 3} nanoparticles with crystal structure orthorhombic (Pbnm), orthorhombic (Pnma) and rhombohedral (R-3c), respectively. We also verified an decreasing in the average crystallite size from 73 to 26 nm, depending of the transition metal. The magnetic measurements reveal an antiferromagnetic behavior for the LaCrO{sub 3} sample with T{sub N}~289 K, and a weak ferromagnetic ordering for the LaMnO{sub 3} sample with T{sub c}~200 K. - Highlights: • La(Cr,Fe,Mn)O{sub 3} nanoparticles were synthesized by coprecipitation method. • XRD results confirm the formation single phase in the compounds studied. • Magnetic property in the La(Fe,Cr,Mn)O{sub 3} nanoparticles dependent on the TM. • La(Cr,Fe)O{sub 3} nanoparticles presented behavior antiferromagnetic and LaMnO{sub 3} ferromagnetic.

  19. Enhancement of magnetic properties of Co2MnSi Heusler alloy prepared by mechanical alloying method

    Rabie, Naeemeh; Gordani, Gholam Reza; Ghasemi, Ali

    2017-01-01

    Highlights: • Ferromagnetic Heusler alloys of Co 2 MnSi were synthesized at low temperature. • There is an at least 30% reduction in the phase formation temperature. • Saturation magnetization of alloy was increased significantly after annealing. - Abstract: Ferromagnetic Heusler alloys of Co 2 MnSi were synthesized by mechanical alloying method at low temperature. The effect of milling time and annealing process on structural and magnetic properties of ferromagnetic alloy samples were studied by X-ray diffraction, scanning electron microscopy and vibration sample magnetometer methods, respectively. Structural characteristics such as crystallite size, phase percentage, and lattice parameter determined using the Rietveld method. The values of these parameters were obtained 362.9 nm, 5.699 Å and 98.7%, respectively for annealed sample. Magnetization studies show that the Co2MnSi phase is formed at 15 h of milling and is optimized after 20 h of milling. VSM results showed that saturation magnetization (M s ) of milled samples reduces from 112 to 75 (emu/g) with increasing milling time and then increased gradually to 95 emu/g. The effect of post-annealing on the structural and magnetic properties of milled samples was also investigated. The saturation magnetization of annealed sample (120 emu/g) is higher than the optimum milled sample (95 emu/g) due to increasing preferential ordered L2 1 structure.

  20. Quantitative Mineralogical Analysis of Mars Analogues Using CHEMIN Data and Rietveld Refinement

    Bish, D. L.; Sarrazin, P.; Chipera, S. J.; Vaniman, D. T.; Blake, D.

    2004-01-01

    Mineralogical analysis is a critical component of planetary surface exploration. Chemical data alone leave serious gaps in our understanding of the surfaces of planets where complex minerals may form in combination with H, S, and halogens. On such planets (e.g., Mars) a single chemical composition may represent a range of mineral assemblages. For example, Viking chemical analyses of excavated duricrust indicate that Mg and S are correlated and 10% MgSO4 (anhydrous weight) is a likely cementing agent. Pathfinder chemical data support a similar abundance of MgSO4 in the most altered materials. However, there are many possible Mg-sulfates with widely varying hydration states (including dehydrated and 1-, 2-, 3-, 4-, 5-, 6-, and 7-hydrates). In addition, other sulfate minerals such as gypsum (CaSO4 .2H2O) and other salts containing Cl may also exist. X-ray diffraction (XRD) has the ability to decipher mixtures of these phases that would be difficult, if not impossible to unravel using only chemical or spectral data.

  1. Rietveld refinement of KLaTiO4 from X-ray powder data

    Bai-Chuan Zhu

    2011-04-01

    Full Text Available Potassium lanthanum titanate(IV, KLaTiO4, has been synthesized by conventional solid-state reaction. It crystallizes isotypically with the NaLnTiO4 (Ln = La, Pr, Nd, Sm, Eu, Gd, Y and Lu family. Five of the six atoms in the asymmetric unit (one K, one La, one Ti and two O atoms are situated on sites with 4mm symmetry, whereas one O atom has 2mm. site symmetry. The crystal structure can be described as being composed of single layers of distorted corner-sharing TiO6 octahedra extending parallel to (001. The layers are alternately separated by K+ and La3+ cations along [001]. The coordination number of both K+ and La3+ cations is nine, resulting in distorted KO9 and LaO9 polyhedra.

  2. Rietveld analysis of phase separation in annealed and leach tested Cm-doped perovskite

    White, T.J.

    1995-01-01

    A quantitative powder X-ray diffraction study was made of actinide doped perovskite of bulk composition Ca 0.98919 An 0.98919 Al 0.01081 O 3 where An corresponded to approximately equimolar proportions of Cm-244 and Pu-240. Sections of this sample accumulated irradiation doses up to 7.51 x 10 17 alpha decay events per gram (α/g). The damaged samples were treated in two ways. First, to establish the critical temperature for structural recovery under the reducing conditions of geological repositories, isochronal annealing was carried out at 600, 800, 1,000 and 1,100 C for 12 hours in graphite crucibles. Two groups of perovskites that had previously sustained doses of 4.5 x 10 17 and 7.4 x 10 17 α/g were tested in this way. For the former group, these conditions resulted in up to 9 weight percent (wt%) of available actinide separating as a fluorite-type dioxide near the perovskite surface. In the latter group, calcium was reduced to the metal which vaporized, leaving an excess of refractory titanium that crystallized as rutile. Second, material which has sustained doses of 1.6--4.0 x 10 17 alpha decays per gram was subjected to an MCC-1 leach test for two months at 90 C using a pH ∼ 2 solution. Under these conditions surficial perovskite dissolved congruently to release calcium into solution while the titanium reprecipitated as anatase. The implications of these results for the ultimate disposal of perovskite-bearing polyphase nuclear waste ceramics are considered

  3. Perturbation methods

    Nayfeh, Ali H

    2008-01-01

    1. Introduction 1 2. Straightforward Expansions and Sources of Nonuniformity 23 3. The Method of Strained Coordinates 56 4. The Methods of Matched and Composite Asymptotic Expansions 110 5. Variation of Parameters and Methods of Averaging 159 6. The Method of Multiple Scales 228 7. Asymptotic Solutions of Linear Equations 308 References and Author Index 387 Subject Index 417

  4. Distillation methods

    Konecny, C.

    1975-01-01

    Two main methods of separation using the distillation method are given and evaluated, namely evaporation and distillation in carrier gas flow. Two basic apparatus are described for illustrating the methods used. The use of the distillation method in radiochemistry is documented by a number of examples of the separation of elements in elemental state, volatile halogenides and oxides. Tables give a survey of distillation methods used for the separation of the individual elements and give conditions under which this separation takes place. The suitability of the use of distillation methods in radiochemistry is discussed with regard to other separation methods. (L.K.)

  5. Application of a dynamic-nanoindentation method to analyze the local structure of an Fe-18 at.% Gd cast alloy

    Choi, Yong; Baik, Youl [Dept. of Materials Science and Technology, Dankook University, Cheonan(Korea, Republic of); Moon, Byung M. [Liquid Processing and Casting Technology R and D Group, KITECH, Incheon (Korea, Republic of); Sohn, Dong Seong [Nuclear Engineering Department, UNIST, Ulsan (Korea, Republic of)

    2017-04-15

    A dynamic nanoindentation method was applied to study an Fe-18 at.% Gd alloy as a neutron-absorbing material prepared by vacuum arc-melting and cast in a mold. The Fe-18 at.% Gd cast alloy had a microstructure with matrix phases and an Fe-rich primary dendrite of Fe9Gd. Rietveld refinement of the X-ray spectra showed that the Fe-18 at.% Gd cast alloy consisted of 35.84 at.% Fe3Gd, 6.58 at.% Fe5Gd, 16.22 at.% Fe9Gd, 1.87 at.% Fe2Gd, and 39.49 at.% β-Fe17Gd2. The average nanohardness of the primary dendrite phase and the matrix phases were 8.7 GPa and 9.3 GPa, respectively. The fatigue limit of the matrix phase was approximately 37% higher than that of the primary dendrite phase. The dynamic nanoindentation method is useful for identifying local phases and for analyzing local mechanical properties.

  6. Ferrimagnetism and spin excitation in a Ni–Mn partially inverted spinel prepared using a modified polymeric precursor method

    Ferreira, Rafael A. [Programa de Pos-Graduação em Ciência e Tecnologia de Materiais (POSMAT), Universidade Estadual Paulista, Faculdade de Ciências, Caixa Postal 473, 17033-360 Bauru, São Paulo (Brazil); Institut des Sciences Chimiques de Rennes – UMR 6226, Université de Rennes 1, F-35042 Rennes (France); Tedesco, Julio C.G.; Birk, Jonas O. [The Niels Bohr Institute, University of Copenhagen, DK-2100 Copenhagen (Denmark); Kalceff, Walter, E-mail: wkalceff@uts.edu.au [School of Physics and Advanced Materials, University of Technology Sydney (UTS), P.O. Box 123, Broadway, NSW 2007 (Australia); Yokaichiya, Fabiano [Laboratório Nacional de Luz Síncrotron (LNLS), Caixa Postal 6192, CEP 13083-970 Campinas, São Paulo (Brazil); Comissao Nacional de Energia Nuclear (CNEN), Instituto de Pesquisas Energeticas e Nucleares (IPEN), Reactor Multiproposito Brasileiro - RMB, Avenida Lineo Prestes 2242, Bloco A, Cidade Universitaria Armando Salles de Oliveira, Sao Paulo (Brazil); Rasmussen, Nina [The Niels Bohr Institute, University of Copenhagen, DK-2100 Copenhagen (Denmark); Peña, Octavio [Institut des Sciences Chimiques de Rennes – UMR 6226, Université de Rennes 1, F-35042 Rennes (France); Henry, Paul F. [European Spallation Source ESS AB, Box 176, 22100 Lund (Sweden); Simeoni, Giovanna G. [Heinz Maier-Leibnitz Zentrum (MLZ) and Physics Department, Technische Universität München, Lichtenbergstr. 1, 85748 Garching (Germany); Bordallo, Heloisa N. [The Niels Bohr Institute, University of Copenhagen, DK-2100 Copenhagen (Denmark); European Spallation Source ESS AB, Box 176, 22100 Lund (Sweden); and others

    2014-07-01

    We demonstrate that a Ni–Mn oxide partially inverted spinel (Ni{sub 1−ν}Mn{sub ν})[Ni{sub ν}Mn{sub 2−ν}]O{sub 4} having inversion degree ν ≈ 0.8 and produced by a modified polymeric precursor method exhibits behaviour previously reported only in monophased samples. The structure of the specimen was determined using Rietveld analysis of X-ray and neutron powder diffraction data, showing that at room temperature the material crystallizes in the Fd3{sup ¯}m space group with a lattice constant a = 8.392 Å. Combining magnetization measurements with neutron powder diffraction, we show that the magnetic structure of this spinel is associated with the interplay between the ferromagnetic and antiferromagnetic lattices which coexist due to the cations' presence on both tetrahedral and octahedral sites. Our analysis of the neutron diffraction data confirms the postulated magnetic structure involving a star-like moment arrangement, arising from competition for the B (octahedral) spinel sites by the Ni and Mn cations. Finally, we show that strong magnetic fluctuations are observed in the inelastic neutron scattering data. - Highlights: • Ni–Mn oxide partially-inverted spinel made by modified polymeric precursor method. • Magnetic measurements showed a ferrimagnetic and a parasitic magnetic transition. • NPD revealed a magnetic structure consistent with a star-like moment arrangement. • INS measurements indicated four distinct temperature-dependent magnetic regimes.

  7. galerkin's methods

    user

    The assumed deflection shapes used in the approximate methods such as in the Galerkin's method were normally ... to direct compressive forces Nx, was derived by Navier. [3]. ..... tend to give higher frequency and stiffness, as well as.

  8. Low-temperature synthesis and characterization of anatase TiO2 nanoparticles by an acid assisted sol–gel method

    Leyva-Porras, C.; Toxqui-Teran, A.; Vega-Becerra, O.; Miki-Yoshida, M.; Rojas-Villalobos, M.; García-Guaderrama, M.

    2015-01-01

    The synthesis of anatase TiO 2 nanoparticles by an acid-assisted sol–gel method at 25 and 80 °C is described. Specifically, acetic acid (AA) was used and the evolution of the anatase phase with the amount of AA was observed. The results of X-ray diffraction (XRD) and transmission electron microscopy (TEM) both showed that a pure anatase phase was obtained with particle size smaller than 5 nm. Structural refinements and quantitative determination of phase composition was achieved by using the Rietveld method. The particle size distribution became slightly narrower as the amount of AA was increased. Raman spectroscopy showed that when the amount of AA was increased a small amount of brookite was present at the contamination level. The anatase phase was studied by differential thermal analysis (DTA), providing phase stability up to 600 °C. These and other results were discussed in terms of particle size and structure. Likewise, the formation of the anatase phase under these synthesis conditions was explained. - Highlights: • Synthesis of anatase TiO 2 nanoparticles by an acid assisted sol–gel method at mild conditions. • Microstructure characterization by XRD, TEM and Raman spectroscopy. • Observation of the formation and evolution of the anatase phase as acetic acid was increased. • Anatase thermal stability up to 600 °C and band gap range between 3.2 and 3.5 eV. • A simplified method which can be considered as a green chemistry process

  9. Zeta potential study of Sb2S3 nanoparticles synthesized by a facile polyol method in various surfactants

    Saxena, Monika; Okram, Gunadhor Singh

    2018-05-01

    In the present work, we report the successful synthesis of stibnite Sb2S3 nanoparticles (NPs) by a facile polyol method using various surfactant. The structural and optical properties were investigated by X-ray diffraction (XRD), Raman spectroscopy and Zeta potential. Rietveld refinement of XRD data confirms the single phase orthorhombic crystal structure of stibnite Sb2S3. Presence of six obvious Raman modes further confirmed their stoichiometric formation. Effect of different surfactants on the surface charge of Sb2S3 NPs was studied using Zeta potential measurement in deionized water at different pH values. They reveal that these NPs are more stable when it was synthesized in presence of EDTA than that of CTAB or without surfactant samples with high zeta potential. The isoelectronic point was found at pH = 6.4 for pure sample, 3.5 and 7.2 for CTAB and not found for EDTA Sb2S3 samples. This information can be useful for many industrial applications like pharmaceuticals, ceramics, waste water treatment and medicines.

  10. Mg doped Li2FeSiO4/C nanocomposites synthesized by the solvothermal method for lithium ion batteries.

    Kumar, Ajay; Jayakumar, O D; Jagannath; Bashiri, Parisa; Nazri, G A; Naik, Vaman M; Naik, Ratna

    2017-10-14

    A series of porous Li 2 Fe 1-x Mg x SiO 4 /C (x = 0, 0.01, 0.02, 0.04) nanocomposites (LFS/C, 1Mg-LFS/C, 2Mg-LFS and 4Mg-LFS/C) have been synthesized via a solvo-thermal method using the Pluronic P123 polymer as an in situ carbon source. Rietveld refinement of the X-ray diffraction data of Li 2 Fe 1-x Mg x SiO 4 /C composites confirms the formation of the monoclinic P2 1 structure of Li 2 FeSiO 4 . The addition of Mg facilitates the growth of impurity-free Li 2 FeSiO 4 with increased crystallinity and particle size. Despite having the same percentage of carbon content (∼15 wt%) in all the samples, the 1Mg-LFS/C nanocomposite delivered the highest initial discharge capacity of 278 mA h g -1 (∼84% of the theoretical capacity) at the C/30 rate and also exhibited the best rate capability and cycle stability (94% retention after 100 charge-discharge cycles at 1C). This is attributed to its large surface area with a narrow pore size distribution and a lower charge transfer resistance with enhanced Li-ion diffusion coefficient compared to other nanocomposites.

  11. Zeta potential and Raman studies of PVP capped Bi2S3 nanoparticles synthesized by polyol method

    Tarachand, Sathe, Vasant G.; Okram, Gunadhor S.

    2018-05-01

    Here we report the synthesis and characterisation of polyvinylpyrrolidone (PVP) capped Bi2S3 nanoparticles via one step catalyst-free polyol method. Raman spectroscopy, dynamic light scattering and zeta potential analysis were performed on it. Rietveld refinement of powder XRD of PVP capped samples confirmed the formation of single phase orthorhombic Bi2S3 for all PVP capped samples. The presence of eight obvious Raman modes further confirmed the formation of stoichiometric Bi2S3. Dynamic light scattering (DLS) studies show a clear increase in hydrodynamic diameter for samples made with increasing PVP concentration. Particle size obtained from DLS and XRD (using Scherrer's formula) combine with change in full width half maxima of Raman modes collectively suggest overall improvement in crystallinity and quality of product on introducing PVP. In zeta potential (ζ) measurement, steric hindrance of carbon chains plays very crucial role and a systematic reduction of ζ value is observed for samples made with decreasing PVP concentration. An isoelectric point is obtained for sample made with low PVP (1g). Present results are likely to open a window for its medical and catalytic applications.

  12. Structural and optical study of CaF{sub 2} nanoparticles produced by a microwave-assisted hydrothermal method

    Bezerra, Claudiane dos S., E-mail: cdsantos20@gmail.com; Valerio, Mário E.G.

    2016-11-15

    CaF{sub 2} nanoparticles were synthesized by the microwave-assisted hydrothermal method. With the addition of the ethylenediamine (EDA) as chelating agent, the size of the particles was reduced. The CaF{sub 2} exhibit single phase identified for X-ray diffraction (XRD) and confirmed by Rietveld refinement. Scanning electron microscopy (SEM) images showed nanoparticles with non-uniform morphology and statistical analysis of collections of particles reviewed that the EDA decreases both the average particle size and average aspect ratio of the particles. The chemical composition of the surface of the particles was investigated by X-ray Photoelectron Spectroscopy (XPS) and the results indicated the presence of reasonable amounts of hydroxyl groups and oxygen ions in the samples produced with EDA. Radioluminescence (RL) measurements showed that both types of nanoparticles presented intrinsic scintillation emission formed by two main bands and that the CaF{sub 2} samples produced without EDA presented higher emission intensity. The broad RL band centered at approximately 293 nm is related to self-trapped exciton (STE) emission of calcium fluoride, while the band at 428 nm can be due to the presence of F centers. The STE excitation and optical band gap were measured through photoluminescent excitation spectra in the VUV range.

  13. Mining Method

    Kim, Young Shik; Lee, Kyung Woon; Kim, Oak Hwan; Kim, Dae Kyung [Korea Institute of Geology Mining and Materials, Taejon (Korea, Republic of)

    1996-12-01

    The reducing coal market has been enforcing the coal industry to make exceptional rationalization and restructuring efforts since the end of the eighties. To the competition from crude oil and natural gas has been added the growing pressure from rising wages and rising production cost as the workings get deeper. To improve the competitive position of the coal mines against oil and gas through cost reduction, studies to improve mining system have been carried out. To find fields requiring improvements most, the technologies using in Tae Bak Colliery which was selected one of long running mines were investigated and analyzed. The mining method appeared the field needing improvements most to reduce the production cost. The present method, so-called inseam roadway caving method presently is using to extract the steep and thick seam. However, this method has several drawbacks. To solve the problems, two mining methods are suggested for a long term and short term method respectively. Inseam roadway caving method with long-hole blasting method is a variety of the present inseam roadway caving method modified by replacing timber sets with steel arch sets and the shovel loaders with chain conveyors. And long hole blasting is introduced to promote caving. And pillar caving method with chock supports method uses chock supports setting in the cross-cut from the hanging wall to the footwall. Two single chain conveyors are needed. One is installed in front of chock supports to clear coal from the cutting face. The other is installed behind the supports to transport caved coal from behind. This method is superior to the previous one in terms of safety from water-inrushes, production rate and productivity. The only drawback is that it needs more investment. (author). 14 tabs., 34 figs.

  14. Projection Methods

    Wagner, Falko Jens; Poulsen, Mikael Zebbelin

    1999-01-01

    When trying to solve a DAE problem of high index with more traditional methods, it often causes instability in some of the variables, and finally leads to breakdown of convergence and integration of the solution. This is nicely shown in [ESF98, p. 152 ff.].This chapter will introduce projection...... methods as a way of handling these special problems. It is assumed that we have methods for solving normal ODE systems and index-1 systems....

  15. Discipline methods

    Maria Kikila; Ioannis Koutelekos

    2012-01-01

    Child discipline is one of the most important elements of successful parenting. As discipline is defined the process that help children to learn appropriate behaviors and make good choices. Aim: The aim of the present study was to review the literature about the discipline methods. The method οf this study included bibliography research from both the review and the research literature, mainly in the pubmed data base which referred to the discipline methods. Results: In the literature it is ci...

  16. Maintenance methods

    Sanchis, H.; Aucher, P.

    1990-01-01

    The maintenance method applied at the Hague is summarized. The method was developed in order to solve problems relating to: the different specialist fields, the need for homogeneity in the maintenance work, the equipment diversity, the increase of the materials used at the Hague's new facilities. The aim of the method is to create a knowhow formalism, to facilitate maintenance, to ensure the running of the operations and to improve the estimation of the maintenance cost. One of the method's difficulties is the demonstration of the profitability of the maintenance operations [fr

  17. Spectroscopic methods

    Ivanovich, M.; Murray, A.

    1992-01-01

    The principles involved in the interaction of nuclear radiation with matter are described, as are the principles behind methods of radiation detection. Different types of radiation detectors are described and methods of detection such as alpha, beta and gamma spectroscopy, neutron activation analysis are presented. Details are given of measurements of uranium-series disequilibria. (UK)

  18. Method Mixins

    Ernst, Erik

    2002-01-01

    . Method mixins use shared name spaces to transfer information between caller and callee, as opposed to traditional invocation which uses parameters and returned results. This relieves a caller from dependencies on the callee, and it allows direct transfer of information further down the call stack, e......The procedure call mechanism has conquered the world of programming, with object-oriented method invocation being a procedure call in context of an object. This paper presents an alternative, method mixin invocations, that is optimized for flexible creation of composite behavior, where traditional...

  19. Method Mixins

    Ernst, Erik

    2002-01-01

    invocation is optimized for as-is reuse of existing behavior. Tight coupling reduces flexibility, and traditional invocation tightly couples transfer of information and transfer of control. Method mixins decouple these two kinds of transfer, thereby opening the doors for new kinds of abstraction and reuse......The procedure call mechanism has conquered the world of programming, with object-oriented method invocation being a procedure call in context of an object. This paper presents an alternative, method mixin invocations, that is optimized for flexible creation of composite behavior, where traditional....... Method mixins use shared name spaces to transfer information between caller and callee, as opposed to traditional invocation which uses parameters and returned results. This relieves a caller from dependencies on the callee, and it allows direct transfer of information further down the call stack, e...

  20. Dosimetry methods

    McLaughlin, W.L.; Miller, A.; Kovacs, A.

    2003-01-01

    Chemical and physical radiation dosimetry methods, used for the measurement of absorbed dose mainly during the practical use of ionizing radiation, are discussed with respect to their characteristics and fields of application....

  1. Method Mixins

    Ernst, Erik

    2005-01-01

    The world of programming has been conquered by the procedure call mechanism, including object-oriented method invocation which is a procedure call in context of an object. This paper presents an alternative, method mixin invocations, that is optimized for flexible creation of composite behavior, ...... the call stack, e.g., to a callee's callee. The mechanism has been implemented in the programming language gbeta. Variants of the mechanism could be added to almost any imperative programming language.......The world of programming has been conquered by the procedure call mechanism, including object-oriented method invocation which is a procedure call in context of an object. This paper presents an alternative, method mixin invocations, that is optimized for flexible creation of composite behavior...

  2. Characteristics of Nanosize Spinel NixFe3-xO4 Prepared by Sol-Gel Method Using Egg White as Emulsifying Agent

    Rudy Situmeang

    2015-07-01

    Full Text Available In this study, sol-gel method using egg white as emulsifying agent was applied to prepare nano size spinel NixFe3-xO4 (with x = 0.2–1. Sample preparation was carried out by mixing the solution of Fe(NO33.9 H2O and Ni(NO33.6 H2O with egg white, and then the sample was stirred thoroughly using magnetic stirrer. After freeze–drying process, the sample was subjected to calcination treatment and subsequently characterized. The phase composition was evaluated using the X-ray diffraction (XRD technique, followed by quantitative analysis using Rietveld and Debye-Scherrer Methods. The functionality of the sample was identified using Fourier Transform Infrared (FTIR spectroscopy, and surface morphology and elemental composition were analyzed using scanning electron microscopycoupled with electron dispersive spectroscopy (SEM/EDS. The results of XRD characterization indicated that materials consist of various crystalline phases, with NiFe2O4 as a major phase. FTIR Analysis revealed the existence of both Lewis and Brønsted–Lowry acid sites, with Lewis acid as the prominent site. The sample was found to display relatively homogeneous surface morphology, having the crystallite size in the range of 33 to 61 nm according to the Debye-Scherrer equation. The EDS data indicated that the ratio of Fe/Ni is in agreement with the composition of the raw materials used.

  3. Structural and magnetic study of CoCr{sub 2}O{sub 4} thin films obtained by employing the sol-gel method

    Del Toro, A.D.; Garcia, R.P.; Davila, Y.G.; Gomes, J.L.; Goncalves, L.P.; Hernandez, E.P. [Universidade Federal de Pernambuco (UFPE), PE (Brazil)

    2016-07-01

    Full text: In this work we made a study about the structural and magnetic properties of cobalt chromite. We obtained samples in a film format and also in chromite nanopowder. Both, the powder and films were fabricated by the sol-gel chemical method, the film were deposited by the spin coating technique followed by an appropriate heat treatment at 500 °C. The used substrate was glass based on silica and we studied the rotating speed parameter during deposition. The initial aim of the work was the study of the influence of rotating speed on the quality of cromite films. The crystallinity of samples was confirmed by diffraction X-ray (XRD). The lattice parameters were determined using the Rietveld method from which we calculate grain size of 8.6 nm. The scanning electron microscopy (SEM) showed granular films with good homogeneity and we observed the dependence of the rotating speed on the quality of the deposited films. The magnetic properties were measured using a vibrating sample magnetometer (VSM). For powder samples we obtained Curie temperature of 94 K, which is a phase transition from ferrimagnetic to paramagnetic. The applied magnetic field during in the characterization of the film was oriented parallel to the plane of the substrate and we observed a high coercivity. The Curie temperature value for the films was 93 K, similar to the powder samples. (author)

  4. Ensemble Methods

    Re, Matteo; Valentini, Giorgio

    2012-03-01

    Ensemble methods are statistical and computational learning procedures reminiscent of the human social learning behavior of seeking several opinions before making any crucial decision. The idea of combining the opinions of different "experts" to obtain an overall “ensemble” decision is rooted in our culture at least from the classical age of ancient Greece, and it has been formalized during the Enlightenment with the Condorcet Jury Theorem[45]), which proved that the judgment of a committee is superior to those of individuals, provided the individuals have reasonable competence. Ensembles are sets of learning machines that combine in some way their decisions, or their learning algorithms, or different views of data, or other specific characteristics to obtain more reliable and more accurate predictions in supervised and unsupervised learning problems [48,116]. A simple example is represented by the majority vote ensemble, by which the decisions of different learning machines are combined, and the class that receives the majority of “votes” (i.e., the class predicted by the majority of the learning machines) is the class predicted by the overall ensemble [158]. In the literature, a plethora of terms other than ensembles has been used, such as fusion, combination, aggregation, and committee, to indicate sets of learning machines that work together to solve a machine learning problem [19,40,56,66,99,108,123], but in this chapter we maintain the term ensemble in its widest meaning, in order to include the whole range of combination methods. Nowadays, ensemble methods represent one of the main current research lines in machine learning [48,116], and the interest of the research community on ensemble methods is witnessed by conferences and workshops specifically devoted to ensembles, first of all the multiple classifier systems (MCS) conference organized by Roli, Kittler, Windeatt, and other researchers of this area [14,62,85,149,173]. Several theories have been

  5. Method Mixins

    Ernst, Erik

    2005-01-01

    The world of programming has been conquered by the procedure call mechanism, including object-oriented method invocation which is a procedure call in context of an object. This paper presents an alternative, method mixin invocations, that is optimized for flexible creation of composite behavior...... of abstraction and reuse. Method mixins use shared name spaces to transfer information between caller and callee, as opposed to traditional invocation which uses parameters and returned results. This relieves the caller from dependencies on the callee, and it allows direct transfer of information further down...... the call stack, e.g., to a callee's callee. The mechanism has been implemented in the programming language gbeta. Variants of the mechanism could be added to almost any imperative programming language....

  6. Statistical methods

    Szulc, Stefan

    1965-01-01

    Statistical Methods provides a discussion of the principles of the organization and technique of research, with emphasis on its application to the problems in social statistics. This book discusses branch statistics, which aims to develop practical ways of collecting and processing numerical data and to adapt general statistical methods to the objectives in a given field.Organized into five parts encompassing 22 chapters, this book begins with an overview of how to organize the collection of such information on individual units, primarily as accomplished by government agencies. This text then

  7. Sieve methods

    Halberstam, Heine

    2011-01-01

    Derived from the techniques of analytic number theory, sieve theory employs methods from mathematical analysis to solve number-theoretical problems. This text by a noted pair of experts is regarded as the definitive work on the subject. It formulates the general sieve problem, explores the theoretical background, and illustrates significant applications.""For years to come, Sieve Methods will be vital to those seeking to work in the subject, and also to those seeking to make applications,"" noted prominent mathematician Hugh Montgomery in his review of this volume for the Bulletin of the Ameri

  8. Characterization methods

    Glass, J.T. [North Carolina State Univ., Raleigh (United States)

    1993-01-01

    Methods discussed in this compilation of notes and diagrams are Raman spectroscopy, scanning electron microscopy, transmission electron microscopy, and other surface analysis techniques (auger electron spectroscopy, x-ray photoelectron spectroscopy, electron energy loss spectroscopy, and scanning tunnelling microscopy). A comparative evaluation of different techniques is performed. In-vacuo and in-situ analyses are described.

  9. Digital Methods

    Rogers, R.

    2013-01-01

    In Digital Methods, Richard Rogers proposes a methodological outlook for social and cultural scholarly research on the Web that seeks to move Internet research beyond the study of online culture. It is not a toolkit for Internet research, or operating instructions for a software package; it deals

  10. Chromatographic methods

    Marhol, M.; Stary, J.

    1975-01-01

    The characteristics are given of chromatographic separation and the methods are listed. Methods and data on materials used in partition, adsorption, precipitation and ion exchange chromatography are listed and conditions are described under which ion partition takes place. Special attention is devoted to ion exchange chromatography where tables are given to show the course of values of the partition coefficients of different ions in dependence on the concentration of agents and the course of equilibrium sorptions on different materials in dependence on the solution pH. A theoretical analysis is given and the properties of the most widely used ion exchangers are listed. Experimental conditions and apparatus used for each type of chromatography are listed. (L.K.)

  11. Numerical methods

    Dahlquist, Germund

    1974-01-01

    ""Substantial, detailed and rigorous . . . readers for whom the book is intended are admirably served."" - MathSciNet (Mathematical Reviews on the Web), American Mathematical Society.Practical text strikes fine balance between students' requirements for theoretical treatment and needs of practitioners, with best methods for large- and small-scale computing. Prerequisites are minimal (calculus, linear algebra, and preferably some acquaintance with computer programming). Text includes many worked examples, problems, and an extensive bibliography.

  12. Sampling methods

    Loughran, R.J.; Wallbrink, P.J.; Walling, D.E.; Appleby, P.G.

    2002-01-01

    Methods for the collection of soil samples to determine levels of 137 Cs and other fallout radionuclides, such as excess 210 Pb and 7 Be, will depend on the purposes (aims) of the project, site and soil characteristics, analytical capacity, the total number of samples that can be analysed and the sample mass required. The latter two will depend partly on detector type and capabilities. A variety of field methods have been developed for different field conditions and circumstances over the past twenty years, many of them inherited or adapted from soil science and sedimentology. The use of them inherited or adapted from soil science and sedimentology. The use of 137 Cs in erosion studies has been widely developed, while the application of fallout 210 Pb and 7 Be is still developing. Although it is possible to measure these nuclides simultaneously, it is common for experiments to designed around the use of 137 Cs along. Caesium studies typically involve comparison of the inventories found at eroded or sedimentation sites with that of a 'reference' site. An accurate characterization of the depth distribution of these fallout nuclides is often required in order to apply and/or calibrate the conversion models. However, depending on the tracer involved, the depth distribution, and thus the sampling resolution required to define it, differs. For example, a depth resolution of 1 cm is often adequate when using 137 Cs. However, fallout 210 Pb and 7 Be commonly has very strong surface maxima that decrease exponentially with depth, and fine depth increments are required at or close to the soil surface. Consequently, different depth incremental sampling methods are required when using different fallout radionuclides. Geomorphic investigations also frequently require determination of the depth-distribution of fallout nuclides on slopes and depositional sites as well as their total inventories

  13. Structure and physical properties of the LaBiFe{sub 2}O{sub 6} Perovskite produced by the modified Pechini method

    Palacio, Johny Andrés Jaramillo; Bello, Elixir William Barrera; Landínez-Téllez, David A.; Roa-Rojas, Jairo, E-mail: jroar@unal.edu.com [Grupo de Física de Nuevos Materiales, Universidad Nacional de Colombia, Bogotá DC (Colombia); Cagigas, Julián Andrés Munévar [Laboratory for Muon Spin Spectroscopy, Paul Scherrer Institut (Switzerland); Arnache, Oscar [Grupo de Estado Sólido, Universidad de Antioquia, Medellín (Colombia)

    2017-10-15

    In this paper the synthesis of the LaBiFe{sub 2}O{sub 6} material by the modified Pechini method is reported. Structural, morphologic, magnetic and optic experimental studies were performed. Rietveld refinement of x-ray diffraction patterns revealed that LaBiFe{sub 2}O{sub 6} crystallizes in an orthorhombic perovskite structure (space group Pnma, ⧣ 62). Scanning electron microscopy images showed the nanometric feature of grains. X-ray dispersive spectroscopy permitted to infer the obtaining of the LaBiFe{sub 2}O{sub 6} expected stoichiometry. Results of magnetic susceptibility as a function of temperature and field magnetization evidenced mixed ferromagnetism and superparamagnetism behavior at T=300 K. Mössbauer spectroscopy supported the superparamagnetic and ferromagnetic responses as a result of the nanogranular morphology and anisotropy effects. Spectrum of diffuse reflectance suggest that this material behaves as a semiconductor with energy gap E{sub g} =2.13 eV. (author)

  14. Synthesis of Bi{sub 25}FeO{sub 39} by molten salts method and its Mössbauer spectrum

    Flores Morales, Shirley Saraí; León Flores, Jesús A.; Pérez Mazariego, José Luis, E-mail: mazariego@ciencias.unam.mx; Marquina Fábrega, Vivianne; Gómez González, Raúl W.

    2017-01-01

    A sample of Bi{sub 25}FeO{sub 39} was synthesized by the molten salts method in 2 h at 750 °C with KCl-KBr as reaction media. The sample was characterized with X-ray powder diffraction and Mössbauer spectroscopy. The Rietveld refinement of the X-ray diffraction confirms that a sillenite type structure with a cell parameter a=10.190(4) Å was achieved, with only small traces of Bi{sub 2}O{sub 3}. In order to get a Mössbauer spectrum with a good signal to noise ratio, the synthesis was made using 95% enriched α–{sup 57}Fe{sub 2}O{sub 3}. To our knowledge, this is the first time that a Mössbauer spectrum for the Bi{sub 25}FeO{sub 39} has been recorded. The nonappearance of a magnetic sextet confirms its paramagnetic behavior. The measured Mössbauer parameters (IS=0.20±0.004 mm/s and QS=0.2±0.07 mm/s) correspond to Fe{sup +3} in very symmetric surroundings, and rule out some interpretations given to the doublet observed in some Mössbauer spectra of BiFeO{sub 3}.

  15. Effect of Preparation Method on Phase Formation Process and Structural and Magnetic Properties of Mn2.5Ge Samples

    R. Sobhani

    2016-12-01

    Full Text Available In this paper, the phase formation process of Mn2.5Ge samples, prepared by mechanical alloying of Mn and Ge metal powders and annealing, has been studied. Results showed that in the milled samples the stable phase is Mn11Ge8 compound with orthorhombic structure and Pnam space group. The value of saturation magnetization increases by increasing milling time from 0.2 up to 1.95 (Am2Kg-1. The remanece of the samples increases by increasing the milling time while the coercivity decreases. Annealing of 15-hour milled sample results in disappearance of Mn and Ge and the formation of new phases of Mn3Ge, Mn5Ge2, Mn5Ge3 and Mn2.3Ge. Mn3Ge is the main phase with Do22 tetragonal structure and I4/mmm space group which is stable and dominant. The enhancement of saturation magnetization in the annealed sample is related to the formation of three new magnetic phases and the increase of coercivity is due to the presence of Mn3Ge compound with tetragonal structure. Studies were replicated on samples made by arc melting method to compare the results and to investigate the effect of the preparation method on phase formation and structural and magnetic properties of the materials. In these samples the saturation value was in range of 0.2 up to 1.95 (Am2Kg-1 depending on preparation methods. Rietveld refinement shows that Mn2.3Ge sample prepared from arc melted under 620oC anealing is single phase. Magnetic analysis of this sample show a saturation magnetization of 5.252(Am2Kg-1 and 0.005 T coercive field.

  16. Effect of lanthanide on the microstructure and structure of LnMn0.5Fe0.5O3 nanoparticles with Ln=La, Pr, Nd, Sm and Gd prepared by the polymer precursor method

    Romero, Mariano; Faccio, Ricardo; Martínez, Javier; Pardo, Helena; Montenegro, Benjamín; Plá Cid, Cristiani Campos; Pasa, André A.

    2015-01-01

    The synthesis of LnMn 0.5 Fe 0.5 O 3 perovskite nanoparticles by the polymer precursor method showed a strong intrinsic dependence with different lanthanides (Ln=La, Pr, Nd, Sm and Gd). The polymerization level reached in the polymer precursor was proportional to the atomic number of lanthanide with exception of samarium, which showed the formation of a different precursor based in a citrate chelate with ethyleneglycol bonded as adduct. The increasing level of polymerization of the polymer precursors showed the formation of large-size perovskite nanoparticles after its calcination. SAXS and TEM analyses suggested that nanoparticles obtained, using this method, have a squared-like microstructure in connection with the polymer precursor microstructure. Structural analysis showed an orthorhombic structure with a slight decline in the Jahn–Teller distortion when the atomic number of lanthanide increases. Mössbauer spectroscopy showed the presence of a majority site in agreement with the Pbnm orthorhombic structure best fitted with Rietveld refinements and in some cases, a more distorted site attributed to local inhomogeneities and oxygen vacancies. - Highlights: • Precursor polymerization level is lower in the presence of lighter lanthanides. • Lighter lanthanide perovskite nanoparticles after calcination are lower-sized. • Nanoparticles obtained by this method have lamellae microstructure. • Jahn–Teller distortion declines for heavier lanthanide perovskites. • Oxygen vacancy phase was observed in lighter lanthanide perovskites

  17. Decontaminating method

    Furukawa, Toshiharu; Shibuya, Kiichiro.

    1985-01-01

    Purpose: To provide a method of eliminating radioactive contaminations capable of ease treatment for decontaminated liquid wastes and grinding materials. Method: Those organic grinding materials such as fine wall nuts shell pieces cause no secondary contaminations since they are softer as compared with inorganic grinding materials, less pulverizable upon collision against the surface to be treated, being capable of reusing and producing no fine scattering powder. In addition, they can be treated by burning. The organic grinding material and water are sprayed by a nozzle to the surface to be treated, and decontaminated liquid wastes are separated into solid components mainly composed of organic grinding materials and liquid components mainly composed of water by filtering. The thus separated solid components are recovered in a storage tank for reuse as the grinding material and, after repeating use, subjected to burning treatment. While on the other hand, water is recovered into a storage tank and, after repeating use, purified by passing through an ion exchange resin-packed column and decontaminated to discharge. (Horiuchi, T.)

  18. The structure of denisovite, a fibrous nanocrystalline polytypic disordered `very complex' silicate, studied by a synergistic multi-disciplinary approach employing methods of electron crystallography and X-ray powder diffraction

    Ira V. Rozhdestvenskaya

    2017-05-01

    Full Text Available Denisovite is a rare mineral occurring as aggregates of fibres typically 200–500 nm diameter. It was confirmed as a new mineral in 1984, but important facts about its chemical formula, lattice parameters, symmetry and structure have remained incompletely known since then. Recently obtained results from studies using microprobe analysis, X-ray powder diffraction (XRPD, electron crystallography, modelling and Rietveld refinement will be reported. The electron crystallography methods include transmission electron microscopy (TEM, selected-area electron diffraction (SAED, high-angle annular dark-field imaging (HAADF, high-resolution transmission electron microscopy (HRTEM, precession electron diffraction (PED and electron diffraction tomography (EDT. A structural model of denisovite was developed from HAADF images and later completed on the basis of quasi-kinematic EDT data by ab initio structure solution using direct methods and least-squares refinement. The model was confirmed by Rietveld refinement. The lattice parameters are a = 31.024 (1, b = 19.554 (1 and c = 7.1441 (5 Å, β = 95.99 (3°, V = 4310.1 (5 Å3 and space group P12/a1. The structure consists of three topologically distinct dreier silicate chains, viz. two xonotlite-like dreier double chains, [Si6O17]10−, and a tubular loop-branched dreier triple chain, [Si12O30]12−. The silicate chains occur between three walls of edge-sharing (Ca,Na octahedra. The chains of silicate tetrahedra and the octahedra walls extend parallel to the z axis and form a layer parallel to (100. Water molecules and K+ cations are located at the centre of the tubular silicate chain. The latter also occupy positions close to the centres of eight-membered rings in the silicate chains. The silicate chains are geometrically constrained by neighbouring octahedra walls and present an ambiguity with respect to their z position along these walls, with displacements between neighbouring layers being

  19. WELDING METHOD

    Cornell, A.A.; Dunbar, J.V.; Ruffner, J.H.

    1959-09-29

    A semi-automatic method is described for the weld joining of pipes and fittings which utilizes the inert gasshielded consumable electrode electric arc welding technique, comprising laying down the root pass at a first peripheral velocity and thereafter laying down the filler passes over the root pass necessary to complete the weld by revolving the pipes and fittings at a second peripheral velocity different from the first peripheral velocity, maintaining the welding head in a fixed position as to the specific direction of revolution, while the longitudinal axis of the welding head is disposed angularly in the direction of revolution at amounts between twenty minutas and about four degrees from the first position.

  20. Casting methods

    Marsden, Kenneth C.; Meyer, Mitchell K.; Grover, Blair K.; Fielding, Randall S.; Wolfensberger, Billy W.

    2012-12-18

    A casting device includes a covered crucible having a top opening and a bottom orifice, a lid covering the top opening, a stopper rod sealing the bottom orifice, and a reusable mold having at least one chamber, a top end of the chamber being open to and positioned below the bottom orifice and a vacuum tap into the chamber being below the top end of the chamber. A casting method includes charging a crucible with a solid material and covering the crucible, heating the crucible, melting the material, evacuating a chamber of a mold to less than 1 atm absolute through a vacuum tap into the chamber, draining the melted material into the evacuated chamber, solidifying the material in the chamber, and removing the solidified material from the chamber without damaging the chamber.

  1. Radiochemical methods

    Geary, W.J.

    1986-01-01

    This little volume is one of an extended series of basic textbooks on analytical chemistry produced by the Analytical Chemistry by Open Learning project in the UK. Prefatory sections explain its mission, and how to use the Open Learning format. Seventeen specific sections organized into five chaptrs begin with a general discussion of nuclear properties, types, and laws of nuclear decay and proceeds to specific discussions of three published papers (reproduced in their entirety) giving examples of radiochemical methods which were discussed in the previous chapter. Each section begins with an overview, contains one or more practical problems (called self-assessment questions or SAQ's), and concludes with a summary and a list of objectives for the student. Following the main body are answers to the SAQ's, and several tables of physical constants, SI prefixes, etc. A periodic table graces the inside back cover

  2. Moment methods and Lanczos methods

    Whitehead, R.R.

    1980-01-01

    In contrast to many of the speakers at this conference I am less interested in average properties of nuclei than in detailed spectroscopy. I will try to show, however, that the two are very closely connected and that shell-model calculations may be used to give a great deal of information not normally associated with the shell-model. It has been demonstrated clearly to us that the level spacing fluctuations in nuclear spectra convey very little physical information. This is true when the fluctuations are averaged over the entire spectrum but not if one's interest is in the lowest few states, whose spacings are relatively large. If one wishes to calculate a ground state (say) accurately, that is with an error much smaller than the excitation energy of the first excited state, very high moments, μ/sub n/, n approx. 200, are needed. As I shall show, we use such moments as a matter of course, albeit without actually calculating them; in fact I will try to show that, if at all possible, the actual calculations of moments is to be avoided like the plague. At the heart of the new shell-model methods embodied in the Glasgow shell-model program and one or two similar ones is the so-called Lanczos method and this, it turns out, has many deep and subtle connections with the mathematical theory of moments. It is these connections that I will explore here

  3. Morphological and structural characterization of the Zn{sub 0,9}Mn{sub 0,1}O powder synthesized by combustion reaction and Pechini; Caracterizacao estrutural e morfologica de pos de Zn{sub 0,9}Mn{sub 0,1}O sintetizados por reacao de combustao e metodo Pechini

    Ribeiro, M A; Torquato, R; Simoes, A N; Costa, A C.F.M.; Gama, L [Universidade Federal de Campina Grande (DEMA/UFCG), PB (Brazil). Dept. de Engenharia dos Materiais; Kiminami, R H.G.A. [Universidade Federal de Sao Carlos (DEMA/UFSCar), SP (Brazil). Dept. de Engenharia de Materiais

    2009-07-01

    Zinc oxide, due to the piezoelectric and electro-optical characteristics, is used in application such as, chemical sensor, varistor, transparent conductive thin film and DMS. The aim of this work is to evaluate and compare structural and morphological characteristics of nanometric powders of Zn{sub 0,9}Mn{sub 0,1}O prepared by chemical synthesis of combustion reaction and Pechini method. The powders were characterized by XRD, SEM and BET. The XRD data shown to both studied method the presence of ZnO phase with hexagonal structure and without second phase. The powder prepared by combustion reaction presented 9% of reduction in crystallinity and 42% of increase in surface area in comparison with the powder prepared by Pechini method. The morphological analysis of the powder showed that both method produce powders with soft agglomerates constituted by nano size particles. (author)

  4. On method

    Frederik Kortlandt

    2018-01-01

    Full Text Available The basis of linguistic reconstruction is the comparative method, which starts from the assumption that there is “a stronger affinity, both in the roots of verbs and in the forms of grammar, than could possibly have been produced by accident”, implying the existence of a common source (thus Sir William Jones in 1786. It follows that there must be a possible sequence of developments from the reconstructed system to the attested data. These developments must have been either phonetically regular or analogical. The latter type of change requires a model and a motivation. A theory which does not account for the data in terms of sound laws and well-motivated analogical changes is not a linguistic reconstruction but philosophical speculation.The pre-laryngealist idea that any Proto-Indo-European long vowel became acute in Balto-Slavic is a typical example of philosophical speculation contradicted by the comparative evidence. Other examples are spontaneous glottalization (Jasanoff’s “acute assignment”, unattested anywhere in the world, Jasanoff’s trimoraic long vowels, Eichner’s law, Osthoff’s law, and Szemerényi’s law, which is an instance of circular reasoning. The Balto-Slavic acute continues the Proto-Indo-European laryngeals and the glottalic feature of the traditional Proto-Indo-European “unaspirated voiced” obstruents (Winter’s law. My reconstruction of Proto-Indo-European glottalic obstruents is based on direct evidence from Indo-Iranian, Armenian, Baltic and Germanic and indirect evidence from Indo-Iranian, Greek, Latin and Slavic.

  5. New methods for removal of pollutants from exhaust gases

    Braestrup, F.

    2009-06-15

    with the electrode materials during sintering and formed different oxides. In-situ high temperature neutron diffraction was performed on ZnFe{sub 2}O{sub 4} in order to determine the cation distribution and to understand the electronic resistivity as well as the dilatometry measurement of the material. Data were analyzed with the Rietveld refinement method and results showed that cations start to rearrange at around 600 deg. C which, to some extend, confirm the behaviour of the resistivity data and the dilatometry measurement. X-ray adsorption spectroscopy was performed on MgFe{sub 2}O{sub 4}, NiFe{sub 2}O{sub 4}, NiCr{sub 2}O{sub 4}, ZnFe{sub 2}O{sub 4} and NiCrFeO{sub 4}. This was done in order to investigate possible changes in oxidation states of the transition elements. In the case of ZnFe{sub 2}O{sub 4} the cation distribution was tried analyzed in order to compare the results with Rietveld refinements on high temperature neutron diffraction. Results show that it was difficult to obtain a good quality refinement without violating the bond distances with respect to reported values found by neutron diffraction and literature. MgFe{sub 2}O{sub 4} and NiFe{sub 2}O{sub 4} were also analyzed in different gases at 400 deg. C and results show that NO and NO{sub 2} adsorb very strongly on MgFe{sub 2}O{sub 4} and decreases the X-ray signal significantly. A change in oxidation state of Ni was observed in atmospheres containing NO{sub 2}. (author)

  6. Low-temperature synthesis and characterization of anatase TiO{sub 2} nanoparticles by an acid assisted sol–gel method

    Leyva-Porras, C. [Centro de Investigación en Materiales DIP-CUCEI, Universidad de Guadalajara, Av. Revolución # 1500, Col. Olímpica, C.P. 44430, Guadalajara (Mexico); Centro de Investigación en Materiales Avanzados, S.C. (CIMAV), Alianza Norte No. 202, Parque de Investigación e Innovación Tecnológica (PIIT), Carretera Aeropuerto km. 10, C.P. 66600, Apodaca, N.L. (Mexico); Toxqui-Teran, A.; Vega-Becerra, O. [Centro de Investigación en Materiales Avanzados, S.C. (CIMAV), Alianza Norte No. 202, Parque de Investigación e Innovación Tecnológica (PIIT), Carretera Aeropuerto km. 10, C.P. 66600, Apodaca, N.L. (Mexico); Miki-Yoshida, M. [Centro de Investigación en Materiales Avanzados, S.C. (CIMAV), Miguel de Cervantes No. 120, Parque Industrial Chihuahua, C.P. 31109, Chihuahua (Mexico); Rojas-Villalobos, M.; García-Guaderrama, M. [Centro de Investigación en Materiales DIP-CUCEI, Universidad de Guadalajara, Av. Revolución # 1500, Col. Olímpica, C.P. 44430, Guadalajara (Mexico); and others

    2015-10-25

    The synthesis of anatase TiO{sub 2} nanoparticles by an acid-assisted sol–gel method at 25 and 80 °C is described. Specifically, acetic acid (AA) was used and the evolution of the anatase phase with the amount of AA was observed. The results of X-ray diffraction (XRD) and transmission electron microscopy (TEM) both showed that a pure anatase phase was obtained with particle size smaller than 5 nm. Structural refinements and quantitative determination of phase composition was achieved by using the Rietveld method. The particle size distribution became slightly narrower as the amount of AA was increased. Raman spectroscopy showed that when the amount of AA was increased a small amount of brookite was present at the contamination level. The anatase phase was studied by differential thermal analysis (DTA), providing phase stability up to 600 °C. These and other results were discussed in terms of particle size and structure. Likewise, the formation of the anatase phase under these synthesis conditions was explained. - Highlights: • Synthesis of anatase TiO{sub 2} nanoparticles by an acid assisted sol–gel method at mild conditions. • Microstructure characterization by XRD, TEM and Raman spectroscopy. • Observation of the formation and evolution of the anatase phase as acetic acid was increased. • Anatase thermal stability up to 600 °C and band gap range between 3.2 and 3.5 eV. • A simplified method which can be considered as a green chemistry process.

  7. Structural and physicochemical properties of nickel manganite NiMn{sub 2}O{sub 4-δ}synthesized by sol-gel and ultra sound assisted methods

    Alburquenque, D. [Materials Chemistry Department, USACH, Ave L.B.O' Higgins 3363, Santiago 9170022 (Chile); Metallurgy Department, USACH, Ave Ecuador 3469, Santiago 9170124 (Chile); Troncoso, L.; Denardin, J.C. [Physics Department, USACH, Ave. Ecuador 3493, Santiago 9170124 (Chile); Butera, A. [Atomic Center, CNEA, Ito. Balseiro, Bariloche Rio Negro 84000 (Argentina); Padmasree, K.D. [Cinvestav, U.Saltillo, Monterrey Km 13.5, Saltillo CP 25900 (Mexico); Ortiz, J.; Herrera, F. [Materials Chemistry Department, USACH, Ave L.B.O' Higgins 3363, Santiago 9170022 (Chile); Marco, J.F. [Institute of Physical Chemistry “Rocasolano”, CSIC, Serrano 119, Madrid 28006 (Spain); Gautier, J.L., E-mail: juan.gautier@usach.cl [Materials Chemistry Department, USACH, Ave L.B.O' Higgins 3363, Santiago 9170022 (Chile)

    2016-07-05

    In this work we present the structural, magnetic and surface characterization of the ceramic nickel manganite oxide NiMn{sub 2}O{sub 4-δ} synthesized by two methods: sol-gel and ultrasound-assisted sol-gel using nitrate salts as precursors. We have characterized the non-stoichiometric samples NiMn{sub 2}O{sub 4-δ} using different physicochemical analyses. X-ray diffraction and Rietveld refinement of the X-ray data indicated that the samples crystallize in the Fd3m space group characteristic of cubic spinel-related oxides. The specific surface area of the oxides was 1.3 m{sup 2}/g (SG) and 16.3 m{sup 2}/g (UASG). SEM results showed particle agglomerates of 1.05 μm (SG) and 0.85 μm (UASG). Temperature dependence magnetization measurements were performed and a ferrimagnetic transition was identified at 103 K and 105 K depending on the preparation method (SG and UASG, respectively). The observed Curie constant was found to vary from 7.4 to 7.7 cm{sup 3} K mol{sup −1} and hysteretic magnetization vs. applied field curves at different temperatures were obtained. XPS studies of these oxides reveal the presence of Ni{sup 2+}, Mn{sup 2+}, Mn{sup 3+} and Mn{sup 4+} ions at the surface. A probable ionic distribution as a function of the synthesis method is proposed. - Highlights: • Nickel manganite was synthesized by sol gel synthesis and a novel ultrasound-assisted sol gel method. . • Bulk and surface cation distributions are proposed. • Physicochemical properties, including magnetic and surface area measurements, were studied for both types of samples.

  8. Preparation and characterization of phase-pure anatase and rutile TiO{sub 2} powder by new chemistry route; Preparacao e caracterizacao de nanoparticulas de TiO{sub 2} nas fases anatase e rutila por uma nova rota quimica

    Pereira, E. A.; Montanhera, M.A.; Paula, F.R., E-mail: sevlarede2@yahoo.com.br [Universidade Estadual Paulista Julio de Mesquista Filho (UNESP), Ilha Soltiera, SP (Brazil). Faculdade de Engenharia. Departameinto de Fisica e Quimica; Spada, E.R. [Universidade de Sao Paulo (USP), Sao Carlos, SP (Brazil). Institutlo de Fisica

    2014-07-01

    Titanium dioxide (TiO{sub 2}) is used in a wire range applications such as photocatalysis and sensor device. In this work is shown a new and effective method for the preparation of TiO{sub 2} nanocrystalline in the crystallographic forms, anatase and rutile. The method involves dissolving the TiOSO{sub 4} powder in H{sub 2}O{sub 2} solution and thermal treatment of amorphous precipitate. The technique of X-ray diffraction was used to follow the structure evolution of amorphous precipitate. Pure anatase structure and rutile are obtained at 600 deg C and 1000 deg C with a grain size estimated 24 and 55 nm respectively. TiO{sub 2} nanoparticles is a promising alternative of the low cost whose potential for solar cells deserve a careful evaluation, especially in hybrid solar cells that employs TiO{sub 2} as electron acceptor and as transport channels. (author)

  9. Obtainment and characterization of Al{sub 2}O{sub 3} ceramic membranes applied to the produced water treatment in petroleum wells; Obtencao, caracterizacao de membranas ceramicas de Al{sub 2}O{sub 3} aplicadas para o tratamento de agua de producao em pocos petroliferos

    Santos, J.J.M. dos; Cela, B.; Melo, G.N.; Timoteo Junior, J.F. [Universidade Federal do Rio Grande do Norte (PPGCEM/UFRN), Natal, RN (Brazil). Programa de Pos-Graduacao em Ciencia e Engenharia de Materiais; Paskocimas, C.A.; Floreoto, N.T. [Universidade Federal do Rio Grande do Norte (DEM/UFRN), Natal, RN (Brazil). Dept. de Engenharia de Materiais

    2008-07-01

    The use of filter membranes is widely disseminated in industry and in sanitation companies to the high quality process and use of membrane systems to treat and reuse wastewater. This work aimed the obtaining and characterization of conventional alumina membranes produced through the Slip Casting process, calcined at the temperature of 1000 deg C, heating rate used was 2 deg C/min., then the samples with starch were sintered at 1200 deg C and the ones without starch at 1300 deg C and 1400 deg C with the same heating rate used at the calcination step. The techniques used for the membranes material characterization were scanning electron microscopy (SEM), the method of Archimedes. The efficiency of the membranes was examined by the spectrophotometry methods, suspended solids and the oil concentration of the produced water samples previously treated by the oil industry. (author)

  10. Development of an optimized algorithm for the characterization of microflow using speckle patterns present in optical coherence tomography signal; Desenvolvimento de um algoritimo otimizado para caracterizacao de fluxos microfluidicos utilizando padroes de speckle presentes no sinal de tomografia por coerencia optica

    Pretto, Lucas Ramos de

    2015-07-01

    This work discusses the Optical Coherence Tomography system (OCT) and its application to the microfluidics area. To this end, physical characterization of microfluidic circuits were performed using 3D (three-dimensional) models constructed from OCT images of such circuits. The technique was thus evaluated as a potential tool to aid in the inspection of microchannels. Going further, this work paper studies and develops analytical techniques for microfluidic flow, in particular techniques based on speckle pattern. In the first instance, existing methods were studied and improved, such as Speckle Variance - OCT, where a gain of 31% was obtained in processing time. Other methods, such as LASCA (Laser Speckle Contrast Analysis), based on speckle autocorrelation, are adapted to OCT images. Derived from LASCA, the developed analysis technique based on intensity autocorrelation motivated the development of a custom OCT system as well as an optimized acquisition software, with a sampling rate of 8 kHz. The proposed method was, then, able to distinguish different flow rates, and limits of detection were tested, proving its feasibility for implementation on Brownian motion analysis and flow rates below 10 μl/min. (author)

  11. Synthesis of LiFePO4/C composites based on natural iron stone using a sol gel method

    Angela, Riyan; Islam, Humaatul; Sari, Vamellia; Latif, Chaironi; Zainuri, Mochamad; Pratapa, Suminar

    2017-01-01

    Synthesis of LiFePO4/C composites has been carried out using a sol gel method. The Fe precursor was made from a natural iron stone of Tanah Laut, South Kalimantan, while the other raw materials were commercial Li2CO3 powder and NH4H2PO4 powder with HCl and water as solvents. Citric acid was used as the carbon source in the synthesis. This study used a molar ratio of 1:1:2 for Li:Fe:P with variation of added citric acid of 1.5 and 2.5 g. The solutions were dried in air at 100°C. The dried powders were characterized using DSC-TGA and then calcined at 600 and 700°C under argon environment for 10 hours. The calcined powders were characterized by X-ray diffractometry (XRD), scanning electron microscopy-energy dispersive x-ray (SEM-EDX), and LCR meter. It was found that the samples contained LiFePO4 as the dominant phase and LiFeP2O7 and Fe2O3 as secondary phases. The analysis showed that the addition of citric acid influenced the electronic conductivity of the composites. A Rietveld relative weight fraction of up to 94.7% was achieved in the synthesis at temperature 600°C. The LFP/C sample exhibited electronic conductivity of 4.56×10-3 Scm-1 which was six times of that of the pure LFP.

  12. Synthesis and characterization of nanostructured powders of hydroxyapatite and of three-calcium {beta} phosphate: elaboration of two phase compositions for application in the orthopedics and traumatology; Sintese e caracterizacao de pos nanoestruturados de hidroxiapatita e de fosfato tricalcico {beta}: elaboracao de composicoes bifasicas para aplicacoes na ortopedia e traumatologia

    Dalmonico, G.M.L.; Pinheiro, D.M.; Camargo, N.H.A.; Orzechowki, L.G.; Goncalves, A.F.; Melnik, V.; Jesus, J.; Gemelli, E. [Universidade do Estado de Santa Catarina (UDESC), Joinville, SC (Brazil). Centro de Ciencias Tecnologicas], e-mail: gidalmonico@gmail.com

    2010-07-01

    This paper synthesized nano structured hydroxyapatite and three calcium {beta} phosphate, for elaboration of two phase compositions of HA/TCP in the concentration in volume of 80% HA/20% TCP-{beta}, 60% HA/40% TCP-{beta} and 50% HA/50% TCP-{beta}. For phase mixing realization, the method of mechanical fragmentation by attritor mill were used. The material recovered from the process of mechanical fragmentation was dried in rotate evaporator, supplying the two phase compositions. The preliminary studies shown the obtention of nano metric powders and a good phase dispersions inside the two phase compositions. (author)

  13. Synthesis and characterization of inorganic ion exchangers based on mixed oxide tin-titanium to be used in recovery of cadmium and nickel and photoluminescent studies; Sintese e caracterizacao de trocadores ionicos inorganicos a base de oxidos mistos estanho-titanio para utilizacao na recuperacao de cadmio e niquel e estudos fotoluminescentes

    Paganini, Paula Pinheiro

    2007-07-01

    This work presents the synthesis, characterization and adsorption studies of inorganic ion exchangers based on mixed tin-titanium oxide for recovery of cadmium and nickel metals from aqueous effluents, discarded in the environment mainly through Ni-Cd battery. The exchangers were synthesized by sol-gel modified method using a mixture of tin(IV) chloride and titanium(III) chloride and ammonium hydroxide, as precursors reagents. The materials obtained: SnO{sub 2}/TiO{sub 2} and SnO{sub 2}/TiO{sub 2}:Eu{sup 3+} were characterized by infrared spectroscopy, thermal analysis, scattering electronic microscopy (SEM), X-ray powder diffraction (XRD) (powder method) and electronic spectroscopy (excitation and emission) for the europium doped exchanger. The same materials also were synthesized in polymeric matrix too and can be used in column, because the synthesized materials showed crystals size in nano metric scale. It was determined by the distribution ratios for metals taking as parameters the influence of pH, the concentration of metals (by adsorption isotherms) and the contact time (by adsorption kinetic). The inorganic ion exchanger presented high exchange capacity with adsorption percent above 90 por cent for the studied conditions, quickly kinetic, heterogeneous exchange surfaces, physic adsorption and spontaneous process of exchange. To the doped exchanger spectroscopy properties were studied and also it was calculated the intensity parameters and it was found a satisfactory quantum yield. (author)

  14. Characterization of cathode materials SrCoO3 and La0,2Sr0,8CoO3 for use in solid oxide fuel cells (SOFC); Caracterizacao de materiais catodicos SrCoO3 e La0,2Sr0,8CoO3 para aplicacao em celulas a combustivel de oxido solido (SOFC)

    Galvao, G.O.; Aquino, F.M; Silva, R.M.; Medeiros, I.D.M. de, E-mail: gabriela.galvao@cear.ufpb.br [Universidade Federal da Paraiba (UFPB), Joao Pessoa, PB (Brazil)

    2016-07-01

    Mixed oxide ceramics with chemical structure of ABO{sub 3} type are promising candidates for cathodes of solid oxide fuel cells (SOFC) for performing well on the electrical conductivity and thermal stability. Various methods of preparation have been studied and used for the synthesis of these materials. In this study, SrCoO{sub 3} and La{sub 0,2}Sr{sub 0,8}CoO{sub 3} perovskites were synthesized using gelatin as directing agent with the purpose of producing homogeneous and porous particles. The powders obtained at 350 ° C / 2 h were calcined at 600, 800 and 1000 ° C for 4 hours and characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results showed that gelatin is a good polymerizing agent for metal ions as the material showed characteristic peaks of perovskite, with good porosity and uniformity. Furthermore, the method of synthesis employed has advantages related to cost and toxicity, which are very low. (author)

  15. Metallogenetic characterization of granitoid rocks through geochemical prospection: the Lagoa Real example related to uranium mineralization in Bahia state, Brazil; Caracterizacao metalogenetica de corpos gratinoides atraves de prospeccao geoquimica: o exemplo da suite intrusiva Lagoa Real relacionada a mineralizacoes de uranio no Estado da Bahia

    Oliveira, J.E., E-mail: cprmsa@bahianet.com.br [Servico Geologico do Brasil (GEREMI/SUREG/SA/CPRM), Salvador, BA (Brazil)

    2011-07-01

    Within a broad metallogenetic evaluation program carried out by CPRM - Geological Survey of Brazil in covenant with the CBPM - Companhia Baiana de Pesquisa Mineral in the central part of the Sao Francisco Craton, the Lagoa Real granitoid rocks was one of the selected targets. The work included geochemical exploration supplemented by follow-in survey and integrated 1:200.000 scale geochemical cartography. The Lagoa Real granitoid was recognized with composition ranging from monzogranitic to alcaligranitic type. The geochemical surveying led to the definition of the metallogenetic specialization of the granitoid rock, with characteristic geochemical and mineralogic associations. These associations are related to uranium mineralization. The genetic model using stream sediment and pan concentrate data, show similarity with the metallogenetic model of zonal partitioning proposed by Routhier (1963), for plutonogenic lode deposits with potential for Sn, W, Nb, Be, REE, Au, and U. In this work emphasis is given to the importance of the integrated use of different prospective methods toward the evaluation of granitoid systems, particularly the combination of geochemical surveying methods with results for a better understanding of the geologic and metallogenetic settings. (author)

  16. Characterization and study of dielectric and electrical properties of CaBi4Ti4O{sub 15} (CBT) added with Bi{sub 2}O{sub 3}; Caracterizacao e estudo das propriedades eletricas e dieletricas do CaBi{sub 4}Ti{sub 4}O{sub 15} (CBT) adicionado com Bi{sub 2}O{sub 3}

    Freitas, D.B.; Campos Filho, M.C.; Sales, J.C.; Silva, P.M.O.; Sombra, A.S. [Universidade Federal do Ceara (UFC), Fortaleza, CE (Brazil)

    2011-07-01

    The ceramic perovskite CaBi{sub 4}Ti{sub 4}O{sub 15} (CBT) of space group A21am, Aurivillius family with deficiency A{sub 5}B{sub 4}O{sub 15} cation has been prepared by solid state method in a planetary ball mill of high energy. The reagents samples were ground and calcined and then added with Bi{sub 2}O{sub 3} (2% wt.) This work aims to characterize by X-ray diffraction to study the electrical properties and dielectric properties of (CBT). The x-ray diffraction revealed the formation of single orthorhombic phase. As for the dielectric properties (dielectric constant and dielectric loss) were measured at 30 deg C to 450 deg C, through which can be verified the presence of thermally activated processes. This phase has properties very relevant for possible use in capacitive devices, miniaturized filters, dielectric resonators antennas and oscillators. (author)

  17. Synthesis and characterization of Ce{sub 1-x}SmXO{sub 2-(x/2)} as solid electrolyte for application in IT-SOFCs; Sintese e caracterizacao de Ce{sub 1-x}SmXO{sub 2-(x/2)} como eletrolito solido para aplicacao em IT-SOFCs

    Nicodemo, J.P.; Martinelli, A.E.; Nascimento, R.M. [Universidade Federal do Rio Grande do Norte (DECM/UFRN), Natal, RN (Brazil). Dept. de Engenharia de Materiais], e-mail: juli_pivotto@yahoo.com.br; Melo, D.M.A. [Universidade Federal do Rio Grande do Norte (DQ/UFRN), Natal, RN (Brazil). Dept. de Quimica; Cela, B. [Universidade Federal do Rio Grande do Norte (PPGCEM/UFRN), Natal, RN (Brazil). Programa de Pos-Graduacao em Ciencia e Engenharia de Materiais; Macedo, D.A. [Universidade Federal do Rio Grande do Norte (PPGEM/UFRN), Natal, RN (Brazil). Programa de Pos-Graduacao em Engenharia Mecanica

    2008-07-01

    Mixed rare earth doped CeO{sub 2} oxide-based have been extensively studied for use in solid electrolytes for fuel cells. Ceramics-based CeO{sub 2} have high ionic conductivity and enable the operation of solid oxide fuel cells (SOFCs) in intermediate temperatures, in the range of 500 to 750 deg C. In this work, was investigated the Sm{sub 2}O{sub 3} doped CeO{sub 2} by Pechini method to obtain Ce{sub 0,9}Sm{sub 0,1}O{sub 1,95}. The resulting powders were characterized by the chemical composition (EDS) and crystallographic (XRD), thermal analysis (TG/ATD and DTG), and particles morphology (SEM). After calcinations of 500 and 700 deg C for 2 hours were obtained nanosized powders with crystalline structure of cubic phase type fluorite fully formed. (author)

  18. Rietveld refinement of the mixed boracite Fe1.59Zn1.41B7O13Br

    Sandra Ulloa-Godínez

    2009-11-01

    Full Text Available The structural characterization of the new iron–zinc heptaborate bromide with composition Fe1.59Zn1.41B7O13Br, prepared by chemical transport is reported. A rigid-body model with constrained generalized coordinates was defined in order to hold the positions of the B atoms at reasonable interatomic distances that typically would reach unacceptable values because of the weak scattering power of boron. There are three independent sites for the B atoms of which two are tetrahedrally coordinated. The bond-valence sum around the third B atom, located on a threefold rotation axis, was calculated considering two cases of coordination of boron with oxygens: trigonal-planar and tetrahedral. The contribution of the fourth O atom to the bond-valence sum was found to be only 0.06 v.u., indicating the presence of a very weak bond in the right position to have a distorted tetrahedral coordination in favour of the trigonal-planar coordination for the third B atom. X-ray fluorescence (XRF was used to determinate the Fe/Zn ratio.

  19. Rietveld refinement of the mixed boracite Fe(1.59)Zn(1.41)B(7)O(13)Br.

    Ulloa-Godínez, Sandra; Rosales, Ivonne; Bucio, Lauro; Farías, Mario H; Campa-Molina, Jorge

    2009-10-31

    The structural characterization of the new iron-zinc hepta-borate bromide with composition Fe(1.59)Zn(1.41)B(7)O(13)Br, prepared by chemical transport is reported. A rigid-body model with constrained generalized coordinates was defined in order to hold the positions of the B atoms at reasonable inter-atomic distances that typically would reach unacceptable values because of the weak scattering power of boron. There are three independent sites for the B atoms of which two are tetra-hedrally coordinated. The bond-valence sum around the third B atom, located on a threefold rotation axis, was calculated considering two cases of coordination of boron with oxygens: trigonal-planar and tetrahedral. The contribution of the fourth O atom to the bond-valence sum was found to be only 0.06 v.u., indicating the presence of a very weak bond in the right position to have a distorted tetra-hedral coordination in favour of the trigonal-planar coordination for the third B atom. X-ray fluorescence (XRF) was used to determinate the Fe/Zn ratio.

  20. Quantitative study of Portland cement hydration by X-Ray diffraction/Rietveld analysis and geochemical modeling

    Coutelot, F.; Seaman, J. C.; Simner, S.

    2017-12-01

    In this study the hydration of Portland cements containing blast-furnace slag and type V fly ash were investigated during cement curing using X-ray diffraction, with geochemical modeling used to calculate the total volume of hydrates. The goal was to evaluate the relationship between the starting component levels and the hydrate assemblages that develop during the curing process. Blast furnace-slag levels of 60, 45 and 30 wt.% were studied in blends containing fly ash and Portland cement. Geochemical modelling described the dissolution of the clinker, and predicted quantitatively the amount of hydrates. In all cases the experiments showed the presence of C-S-H, portlandite and ettringite. The quantities of ettringite, portlandite and the amorphous phases as determined by XRD agreed well with the calculated amounts of these phases after different periods of time. These findings show that changes in the bulk composition of hydrating cements can be described by geochemical models. Such a comparison between experimental and modelled data helps to understand in more detail the active processes occurring during cement hydration.

  1. Strain and stress tensors of rolled uranium plate by Rietveld refinement of TOF neutron-diffraction data

    Balzar, D.; Popa, N.C.; Vogel, S.

    2010-01-01

    We report the complete macroscopic average strain and stress tensors for a cold-rolled uranium plate, based on the neutron TOF measurements. Both tensors were determined by the least-squares refinement of the interplanar spacings of 19 Bragg reflections. Based on the pole figures, as determined by GSAS, a triclinic sample symmetry of the uranium plate was assumed. Strain and stress are tensile in both the transverse and rolling directions and very small in the normal direction (through the thickness of the plate). Shear strain and stress components are compressive and of significant magnitude.

  2. Characterization of array scintillation detector for follicle thyroid 2D imaging acquisition using Monte Carlo simulation; Caracterizacao de uma matriz detectora cintiladora para aquisicao de imagem 2D da regiao folicular da glandula tireoide por emissao radioativa usando simulacao Monte Carlo

    Silva, Carlos Borges da

    2007-05-15

    The image acquisition methods applied to nuclear medicine and radiobiology are a valuable research study for determination of thyroid anatomy to seek disorders associated to follicular cells. The Monte Carlo (MC) simulation has also been used in problems related to radiation detection in order to map medical images since the improvement of data processing compatible with personnel computers (PC). This work presents an innovative study to find out the adequate scintillation inorganic detector array that could be coupled to a specific light photo sensor, a charge coupled device (CCD) through a fiber optic plate in order to map the follicles of thyroid gland. The goal is to choose the type of detector that fits the application suggested here with spatial resolution of 10 {mu}m and good detector efficiency. The methodology results are useful to map a follicle image using gamma radiation emission. A source - detector simulation is performed by using a MCNP4B (Monte Carlo for Neutron Photon transport) general code considering different source energies, detector materials and geometries including pixel sizes and reflector types. The results demonstrate that by using MCNP4B code is possible to searching for useful parameters related to the systems used in nuclear medicine, specifically in radiobiology applied to endocrine physiology studies to acquiring thyroid follicles images. (author)

  3. Development and characterization of AlCrN coated Si{sub 3}N{sub 4} ceramic cutting tool; Desenvolvimento e caracterizacao de ferramentas ceramicas de Si{sub 3}N{sub 4} revestidas com AlCrN

    Souza, J.V.C.; Nono, M.C.A.; Machado, J.P.B., E-mail: vitor@las.inpe.b [Instituto Nacional de Pesquisas Espaciais (INPE), Sao Jose dos Campos, SP (Brazil); Silva, O.M.M. [Centro Tecnico de Aeronautica (CTA-IAE/AMR), Sao Jose dos Campos, SP (Brazil). Inst. de Aeronautica e Espaco. Div. de Materiais; Pimenta, M. [Balzers, Jundiai, SP (Brazil); Sa, F.C.L. [Centro Universitario de Volta Redonda (UNIFOA), RJ (Brazil)

    2010-07-01

    Ceramic cutting tools are showing a growing market perspective in terms of application on machining operations due to their high hardness, wear resistance, and machining without a cutting fluid, therefore are good candidates for cast iron and Nickel superalloys machining. The objective of the present paper was the development of Si{sub 3}N{sub 4} based ceramic cutting insert, characterization of its physical and mechanical properties, and subsequent coating with AlCrN using a PVD method. The characterization of the coating was made using an optical profiler, XRD, AFM and microhardness tester. The results showed that the tool presented a fracture toughness of 6,43 MPa.m{sup 1/2} and hardness of 16 GPa. The hardness reached 31 GPa after coating. The machining tests showed an improvement on work piece roughness when machining with coated insert, in comparison with the uncoated cutting tool. Probably this fact is related to hardness, roughness and topography of AlCrN. (author)

  4. Synthesis and characterization of CeO{sub 2} - TiO{sub 2} system for use in heterogeneous photocatalysis in photodegradation of methylene blue dye; Sintese e caracterizacao do sistema CeO{sub 2} - TiO{sub 2} para aplicacao em fotocatalise heterogenea na fotodegradacao do corante azul de metileno

    Bragatto, Julia

    2016-07-01

    This study has as its goal the synthesis of a mixed oxide system type CeO{sub 2} - TiO{sub 2}, through the polymeric precursor method, to be used in heterogeneous photocatalysis. The synthesized materials were characterized by Thermogravimetry (TG), Derivative Thermogravimetry (DTG), Differential Thermal Analysis (DTA) and X-Ray Diffraction (XRD). The results of the thermal analysis showed in what temperature ranges certain events occur such as the formation of cerium oxide between 600 and 800 ° C, which refers to the crystallization of the material. Regarding the formation of titanium oxide, events between 600 and 800 ° C are perceived, which suggests the transformation of anatase to rutile phase. The XRD analysis showed no occurrence of the same phase for all materials, meaning that there is a variation in the formation of phases according to concentration of precursor for each sample. Noteworthy are the formation of CeO{sub 2} for Ce75-Ti25 and Ce50-Ti50 concentrations, with cubic crystal structure of the fluorite type. In Ce75-Ti25 and Ce25-Ti75 it is present the TiO{sub 2} in the anatase and rutile phase, with crystal structure of the tetragonal and tetrahedron type, respectively, as well as the formation of CeTi{sub 2}O{sub 6} in Ce50-Ti50 and Ce25-Ti75, with structure monoclinic. From these analyses, it is possible to see which samples, and in which temperatures of calcination the material has increased crystallinity, making the choice for their application in heterogeneous photocatalysis, aiming the degradation of methylene blue dye. Among the tested materials for methylene blue, the sample that stood out was the Ce50-Ti50, with calcination temperature of 800 °C, with values close to 50% degradation, because it was the sample that showed higher dye adsorption capacity, which is the step that precedes photodegradation. (author)

  5. Thermal-annealing effects on the structural and magnetic properties of 10% Fe-doped SnO{sub 2} nanoparticles synthetized by a polymer precursor method

    Aragón, F.H., E-mail: fermin964@hotmail.com [Núcleo de Física Aplicada, Instituto de Física, Universidade de Brasília, Brasília DF 70910-900 (Brazil); Instituto de Ciências Biológicas, Pós-graduação em Nanociência e Nanobiotecnologia, Universidade de Brasília, Brasilia DF 70919-970 (Brazil); Coaquira, J.A.H. [Núcleo de Física Aplicada, Instituto de Física, Universidade de Brasília, Brasília DF 70910-900 (Brazil); Nagamine, L.C.C.M.; Cohen, R. [Instituto de Física, Universidade de São Paulo, São Paulo SP 05508-090 (Brazil); Silva, S.W. da [Núcleo de Física Aplicada, Instituto de Física, Universidade de Brasília, Brasília DF 70910-900 (Brazil); Instituto de Ciências Biológicas, Pós-graduação em Nanociência e Nanobiotecnologia, Universidade de Brasília, Brasilia DF 70919-970 (Brazil); and others

    2015-02-01

    In this work, we present the experimental results of Sn{sub 0.9}Fe{sub 0.1}O{sub 2} nanoparticles synthesized by a polymer precursor method. Studies were performed in the as-prepared (AP) and thermally-annealed (TA) samples. The X-ray diffraction (XRD) data analysis carried out using the Rietveld refinement method shows the formation of only the rutile-type structure in the AP sample and this phase remains stable for the TA sample. Additionally, the mean crystallite size shows an increase from ∼4 nm to ∼17 nm after the annealing and a clear reduction of the residual strain has also been determined. Micro-Raman spectroscopy measurements show the formation of an iron oxide phase (likely α-Fe{sub 2}O{sub 3}) after the thermal treatment. Magnetic measurements show a paramagnetic behavior for the AP sample and the coexistence of a weak ferromagnetism and paramagnetism for the TA sample. The magnetically-ordered contribution of the TA sample has been assigned to the formation of the hematite phase. DC and AC magnetic features of the TA sample are consistent with a cluster-glass behavior which seems to be related to the magnetic disorder of spins located at the particle surface. Those spins clusters seem to be formed due to the diffusion of iron ions from the core of the particle to the surface caused by the annealing process. - Highlights: • Thermal annealing effects in the 10% Fe-doped SnO{sub 2} nanoparticles have been studied. • XRD data analysis shows the formation of the rutile-type structure. • Raman measurements show the formation of small amount of α-Fe{sub 2}O{sub 3} after the annealing. • Paramagnetic and magnetically ordered phases were determined after the annealing. • Spin clusters likely at the particle surface have been formed after the annealing.

  6. Catalytic oxidation of n-hexane promoted by Ce1−xCuxO2 catalysts prepared by one-step polymeric precursor method

    Araújo, Vinícius D.; Lima, Maurício M. de; Cantarero, Andrés; Bernardi, Maria I.B.; Bellido, Jorge D.A.; Assaf, Elisabete M.; Balzer, Rosana; Probst, Luiz F.D.; Fajardo, Humberto V.

    2013-01-01

    Ceria-supported copper catalysts (Ce 1−x Cu x O 2 , with x (mol) = 0, 0.01, 0.03, 0.05 and 0.10) were prepared in one step through the polymeric precursor method. The textural properties of the catalysts were investigated by X-ray diffraction (XRD), Rietveld refinement, N 2 -physisorption (BET surface area), electron paramagnetic resonance (EPR), UV–visible diffuse reflectance and photoluminescence spectroscopies and temperature-programmed reduction (TPR). In a previous study ceria-supported copper catalysts were found to be efficient in the preferential oxidation of CO. In this study, we extended the catalytic application of Ce 1−x Cu x O 2 systems to n-hexane oxidation and it was verified that the catalysts were highly efficient in the proposed reaction. The best performance (up to 95% conversion) was observed for the catalysts with low copper loads (Ce 0.97 Cu 0.03 O 2 and Ce 0.99 Cu 0.01 O 2 , respectively). The physicochemical characterizations revealed that these behaviors could be attributed to the copper species present in the catalysts and the interaction between CuO and CeO 2 , which vary according to the copper content. - Highlights: • Synthesis of CuO/CeO2 catalysts by the one-step polymeric precursor method. • 95% n-hexane conversion on Ce0.97Cu0.03O2 catalyst. • Redox properties play a key role in the catalytic performance

  7. Study of structural and optical properties of CaMoO{sub 4} nanoparticles synthesized by the microwave-assisted solvothermal method

    Botelho, G., E-mail: gleice.lorena@gmail.com [INCTMN-UFSCar, Universidade Federal de São Carlos, P.O. Box 676, 13565-905, São Carlos, SP (Brazil); Nogueira, I.C. [Instituto Federal do Maranhão, PPG em Engenharia de Materiais, 65030-005, São Luís, MA (Brazil); Moraes, E. [INCTMN-UFSCar, Universidade Federal de São Carlos, P.O. Box 676, 13565-905, São Carlos, SP (Brazil); Longo, E. [INCTMN-UNESP, Universidade Estadual Paulista, P.O. Box 355, CEP, 14801-907, Araraquara, SP (Brazil)

    2016-11-01

    Calcium molybdate (CaMoO{sub 4}) nanoparticles were synthesized by using a rapid assisted-microwave solvothermal method. X-ray diffraction measurements, Fourier transform Raman and Fourier transform infrared spectroscopies, revealed that the samples all have a scheelite-type tetragonal structure. In addition, the data obtained from the Rietveld refinements revealed distortions of the [Ca−O] and [Mo−O] bonds that led, in turn, to distortions of the [CaO{sub 8}] and [MoO{sub 4}] clusters. The presence of irregular spherical-like CaMoO{sub 4} nanoparticles and the corresponding crystallographic arrangement were confirmed and determined via transmission electron microscopy and high resolution transmission electron microscopy, respectively. First-principles quantum mechanical calculations based on the density functional theory at the B3LYP level were employed in order to understand the band structure and density of states of CaMoO{sub 4} in the excited singlet and triplet states. Furthermore, the optical properties were investigated by performing ultraviolet–visible spectroscopy and photoluminescence (PL) measurements. Maximum PL emission of CaMoO{sub 4} powders was detected in the green-region wavelength of the electromagnetic spectrum; this emission was attributed to the distorted [MoO{sub 4}] clusters. - Highlights: • Effect of propane-1,3-diol in the synthesis of nanoparticles by a rapid method. • Utilization of first-principles quantum mechanical calculations. • Investigation of photoluminescent properties of CaMoO{sub 4} nanoparticles.

  8. Optical and structural characterization of the pure and doped BaY{sub 2}F{sub 8} with rare earths for application in radiation detectors and scintillators; Caracterizacao optica e estrutural do BaY{sub 2}F{sub 8} puro e dopado com terras raras visando aplicacao em detectores de radiacao e cintiladores

    Mello, Ana Carolina Santana de

    2008-07-01

    In this work Barium Yttrium Fluoride (BaY{sub 2}F{sub 8} -BaYF) doped with different concentrations of ions Tb{sup 3+}, Er{sup 3+}, Tm{sup 3+} e Nd{sup 3+} were characterized, aiming the application in radiation detection devices that use the scintillating properties. Two types of samples were produced in the CLA-IPEN-SP, polycrystalline samples, obtained via solid state reaction of BaF{sub 2} and YF{sub 3} under HF atmosphere, and single crystals, obtained via the zone melting method also in a HF atmosphere. The samples were characterized using the following experimental techniques: X-ray powder diffraction, Radioluminescence (RL), Optical Absorption and Dispersive X-ray Absorption Spectroscopy (DXAS). The X-ray diffraction pattern showed the presence of the phase BaY{sub 2}F{sub 8} and a small amount of the phase Ba{sub 4}Y{sub 3}F{sub 17} in the polycrystalline pure and Tb{sup 3+}doped samples. The other samples showed only the desired BaY{sub 2}F{sub 8} phase. The radioluminescence measurements of the doped BaYF, when irradiated with X-rays, showed emission peaks in energies that are characteristics of the 4f-4f transitions of rare earths. The RL of the samples with 2 mol por cent and 3 mold of Tb{sup 3+}showed quite intense peaks with a maximum emission peak at 545 nm. The Tm{sup 3+}doped BYF showed that the scintillation efficiency is not directly proportional to the doping level, and the highest RL emission were obtained for the polycrystalline samples doped with 1 mol por cent, showing a maximum peak intensity at 456 nm (the blue region of the visible spectrum). All samples showed a phosphorescent decay time of the order of seconds. Single crystals of BaYF doped with 2 mol por cent of Er{sup 3+}, in addition to one of the highest phosphorescence time, presents a quite strong Rl in the green region of the spectra. The radiation damage was evaluated by the optical absorption techniques and the results showed that the formation of the absorption bands can be

  9. Electromagnetic attenuation analysis of Ni{sub 0.4}Zn{sub 0.6}Fe{sub 2O4} obtained by citrate precursor method; Analise da atenuacao de radiacao eletromagnetica de Ni{sub 0.4}Zn{sub 0.6}Fe{sub 2O4} obtido pelo metodo de citrato precursor

    Hwang, K. [Centro Tecnico Aeroespacial (CTA-IAE), Sao Jose dos Campos, SP (Brazil). Inst. de Atividades Espaciais. Div. Materiais; Moura, A.E.G.; Nasar, R.S.; Nasar, M.C. [Universidade Federal do Rio Grande do Norte (UFRN), Natal (Brazil). Dept. de Quimica; Pereira, J.J. [Universidade de Taubate, SP (Brazil)

    2010-07-01

    In this work, two types of synthesized Ni{sub 0,4}Zn{sub 0,6}Fe{sub 2}O{sub 4} by citrate precursor method. The first type was calcined at 350 deg C for 3.5 h, and the second, after calcination, it was subjected to heat treatment at 600 deg C for 2h in argon atmosphere. Both types were analyzed by X-ray diffraction (XRD) and equipment waveguide. The data were investigated by Rietveld refinement method and showed the NiZn ferrite phase with crystallite size of 12.2 +- 0.1 nm (350 deg C) and 166.7 +- 3.6 nm (600 deg C). The heat treatment also influenced the values of electric permittivity and magnetic permeability, and attenuation of electromagnetic radiation in the frequency range in microwave (8-12 GHz). The sample treated attenuates more and allows its application with thinner, making it attractive its use as absorber material in this frequency range. (author)

  10. Production and characterization of compounds based on MgB{sub 4}O{sub 7} for application in dosimetry; Producao e caracterizacao de compostos a base de MgB{sub 4}O{sub 7} para aplicacao em dosimetria

    Souza, Luiza Freire de

    2016-07-01

    B{sub 4}O{sub 7}:Nd and MgB{sub 4}O{sub 7}:Nd,Li RL were not observed emission from the ultraviolet to infrared. With the results obtained from the TL characterization, it were also discussed aspects such as: effect of sintering and dopant concentrations in emissions, influence of doping and codoping with Li in MgB{sub 4}O{sub 7} matrix, thermal treatment reuse, TL signal reproducibility, dose response curve , relative sensitivity and it were analyzed the kinetic parameters of the TL emission curves. The OSL analyses of MgB{sub 4}O{sub 7}:Dy,Li,MgB{sub 4}O{sub 7}:Ce,Li and MgB{sub 4}O{sub 7}:Nd,Li indicated that the compounds have high cross section for photoionization to the wavelength emitted by blue LEDs, and from three compounds analyzed the MgB{sub 4}O{sub 7}: Ce,Li showed greater intensity. The partial preheating and partial cleaning methods allowed to elucidate the OSL phenomenology in compounds. (author)

  11. The analysis of powder diffraction data

    David, W.I.F.; Harrison, W.T.A.

    1986-01-01

    The paper reviews neutron powder diffraction data analysis, with emphasis on the structural aspects of powder diffraction and the future possibilities afforded by the latest generation of very high resolution neutron and x-ray powder diffractometers. Traditional x-ray powder diffraction techniques are outlined. Structural studies by powder diffraction are discussed with respect to the Rietveld method, and a case study in the Rietveld refinement method and developments of the Rietveld method are described. Finally studies using high resolution powder diffraction at the Spallation Neutron Source, ISIS at the Rutherford Appleton Laboratory are summarized. (U.K.)

  12. Microstructural studies on variation of defect parameters in Zr–Sn

    ... modified Rietveld method and Warren–Averbach method taking silicon as standard. ... This analysis confirms that the growth fault, , is totally absent or negligibly ... faulting tendency abruptly drops to a level of negligible presence or zero.

  13. Investigation of structural and magnetic properties of Ni0.5Zn0.5Fe2O4 nano powders prepared by self combustion method

    Sudheesh, V.D.; Nehra, J.; Vinesh, A.; Sebastian, V.; Lakshmi, N.; Dutta, Dimple P.; Reddy, V.R.; Venugopalan, K.; Gupta, Ajay

    2013-01-01

    Graphical abstract: Display Omitted Highlights: ► Ni 0.5 Zn 0.5 Fe 2 O 4 prepared by self combustion with uniform/nonuniform heating. ► Characterized using TEM, XRD, in-field Mössbauer and DC magnetometry. ► Leads to bimodal (S1) and very narrow size distribution (S2) type nano samples. ► S1 has magnetic properties of bulk Ni 0.5 Zn 0.5 Fe 2 O 4 . ► Although very even sized, S2 large magnetic anisotropy distribution. -- Abstract: Nano powders of Ni 0.5 Zn 0.5 Fe 2 O 4 have been synthesized by the self-combustion method at a relatively low temperature of 473 K under conditions of non-uniform and uniform heating. Rietveld fitting of X-ray diffractograms confirm the formation of the pure spinel phase in both samples. Transmission electron microscopy indicates that the sample prepared under non-uniform heating has a bimodal particle size distribution (average values 16 nm and 6 nm) while the one prepared under uniform heating has a very narrow particle size distribution (average size 4 nm). Low temperature, in-field Mössbauer spectroscopic studies clearly show surface spin contributions. The hyperfine fields and Curie temperature of the non-uniformly heated sample are in good agreement with those reported for the corresponding bulk samples. Despite having a very narrow particle size distribution, the uniformly heated sample has a large anisotropy distribution which is evident in the broad transition visible in the temperature dependent magnetization curve. It is also corroborated by the fact that the experimental magnetization curve at room temperature requires two Langevin functions for satisfactory reproduction.

  14. Hydrogeological characterization of Itataia mine, Ceara, Brazil; Caracterizacao hidrogeologica da jazida de Itataia, CE

    Silva, Jose Roberto de Alcantara e

    2003-07-01

    This work analyzes the geological-geotechnical-geophysical behavior, aiming to define the characteristics of a karstic-fissural aquifer in the mid-northern region of the State of Ceara, named as Itataia Phosphor-Uranium Deposit. This area is constituted of marbles and gneisses from Itataia Group, which are morphologically located at a higher point to the south and at a lower point to the north, related to Paleoproterozoic Era. Fracture system led to the implantation of two karstic marble phases, being the oldest from Cambrian Period and the most recent from Tertiary/Quaternary Period. Porosity is secondary to fractures, fissures and crushed zones which act as hydraulic channels for groundwater flow. Major geophysics defined conducting lines are controlled by normal fractures and faults in both N70 deg E and N80 deg W directions, and secondarily in both N10 deg E and N30 deg W directions, dipping 70 deg -85 deg into the northern quadrant of the main axes. Fault characteristics are typical of graben and horst patterns. Rocks in the area are distributed into three classes of geotechnical massif: healthy rock, moderately altered and fractured rock, and strongly altered and fractured rock. The latter occurs predominantly in the center of the area, from the soil surface to an average depth of 150 meters. Groundwater flow is characterized by fractures which enlarged by the karstic phenomenon dissolution, and then become closer as deeper they are. This flow may be slower or even discontinue in light of silty-argillaceous alteration material that fill the open fracture gaps. Water level is not lower than 5 m or higher than 90 m, averaging by 30 m ali over the area. The synoptic piezometry map shows a general south-north direction; however in the southwestern portion - the recharge zone - it takes the south direction, while in the southeastern portion it takes the southeast direction. (author)

  15. Synthesis and characterization of biomorphic ceramics; Sintese e caracterizacao de ceramicas biomorficas

    Rambo, Carlos Renato

    2001-07-01

    Biotemplating represents a recently developed technology for manufacturing of biomorphous ceramics from naturally grown plant structures. This approach allows the production of ceramic materials with cellular structure, where the microstructural features of the ceramic product are similar to the native plant. After processing, the biomorphic ceramic exhibits directed pore morphology in the micrometer range. Biomorphic SiC fibers were produced from bamboo by carbothermal reduction of SiO{sub 2} originally present in the bamboo structure. Bamboo pieces were heated up to 1500 deg C in argon to promote the reaction between carbon and silica. Biomorphic alumina, mullite and zirconia ceramics were manufactured via the sol-gel route by repeated infiltration of low viscous oxide precursors (sols) into rattan, pine and bamboo structures. The raw samples were pyrolyzed at 800 deg C in nitrogen for 1h and subsequently annealed at 1550 deg C in air. The microstructure and physical properties of the biomorphic ceramics were characterized by X-ray diffraction (XRD) and high temperature-XRD, scanning electron microscopy (SEM), porosimetry and picnometry. Thermal analysis (TGA/DTA) was performed on the infiltrated samples in order to evaluate the reactions and the total weight loss during the thermal process. The mechanical properties were evaluated by compressive strength tests. In contrast to conventional processed ceramic foam of similar porosity, the microstructure highly porous biomorphic ceramics shows uniaxial pore morphology with anisotropic properties. These properties are favorable for applications in catalyst support, filters or low-density heat insulation structures, or as biomaterials. (author)

  16. Characterization of TEMPO-oxidized bacterial cellulose; Caracterizacao de celulose bacteriana tempo-oxidada

    Nascimento, Eligenes S.; Pereira, Andre L.S.; Lima, Helder L.; Barroso, Maria K. de A., E-mail: eligenessampaio@hotmail.com [Universidade Federal Ceara (UFC), Fortaleza, CE (Brazil); Barros, Matheus de O. [Instituto Federal do Ceara (IFCE), Fortaleza, CE (Brazil); Morais, Joao P.S. [Embrapa Algodao, Campina Grande, PB (Brazil); Borges, Maria de F.; Rosa, Morsyleide de F. [Embrapa Agroindustria Tropical, Fortaleza, CE (Brazil)

    2015-07-01

    The aim of this study was to characterize the TEMPO-oxidized bacterial cellulose, as a preliminary research for further application in nanocomposites. Bacterial cellulose (BC) was selectively oxidized at C-6 carbon by TEMPO radical. Oxidized bacterial cellulose (BCOX) was characterized by TGA, FTIR, XRD, and zeta potential. BCOX suspension was stable at pH 7.0, presented a crystallinity index of 83%, in spite of 92% of BC, because of decrease in the free hydroxyl number. FTIR spectra showed characteristic BC bands and, in addition, band of carboxylic group, proving the oxidation. BCOX DTG showed, in addition to characteristic BC thermal events, a maximum degradation peak at 233 °C, related to sodium anhydro-glucuronate groups formed during the cellulose oxidation. Thus, BC can be TEMPO-oxidized without great loss in its structure and properties. (author)

  17. Bio-inspired synthesis and characterization of superparamagnetic particles; Sintese e caracterizacao bioinspirada de particulas superparamagneticas

    Castro, Vinicius F., E-mail: vfc_mg@yahoo.com.br [Universidade Federal de Itajuba (UNIFEI), MG (Brazil); Queiroz, Alvaro A.A. [Universidade Federal de Itajuba (UNIFEI), MG (Brazil). Centro de Estudos e Inovacao em Materiais Biofuncionais Avancados

    2012-08-15

    This paper discusses the bio-inspired synthesis of type YFeAl ferrites encapsulated into polyglycerol dendrimers (PGLD) generation 3. The structure and morphological properties of the system YFeAl/PGLD was characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The magnetic properties were studied through the techniques of Moessbauer spectroscopy and magnetization. The cytotoxicity of the nanoparticles encapsulated in dendrimers PGLD G3 at the cell membrane was studied against mammalian cell line CHO.K1 measuring the amount of lactate dehydrogenase (LDH) released by the cell damage. Microscopy TEM and XRD analysis indicate that spherical nanoparticles were obtained highly crystalline and monodisperse with size 20 nm

  18. Synthesis and characterization of new ionic liquids; Sintese e caracterizacao de novos liquidos ionicos

    Oliveira, L.M.C. de; Mattedi, S.; Boaventura, J.S., E-mail: luanaufrn@hotmail.co [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Escola Politecnica. Programa de Pos-Graduacao em Engenharia Quimica; Iglesias, M. [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Escola Politecnica. Programa de Pos-Graduacao em Engenharia Quimica; Universidad de Santiago de Compostela (Spain). Escuela Tecnica Superior de Ingenieria. Dept. de Ingenieria Quimica

    2010-07-01

    In recent years, ionic liquids have been highlighted for its potential in various industrial applications. Among them, the salts of Broensted has a promising profile for the low toxicity, low cost and simple synthesis. This paper presents the synthesis and characterization of new salts of Bronsted with branched (lactate) or large chain anions (oleate) for future use as additives promoters of proton conductivity in fuel cells of ethanol. Experimental data were measured for density, sound velocity and conductivity of pure ionic liquids and mixtures. The density decreases linearly with increasing temperature, and sound velocity shows a similar trend, but not linear. The conductivity increases according to the Arrhenius model with activation energy less than 10 J/mol. Tests NMR, FTIR and TGA confirm ionic structure and thermal stability up to 165 deg C. (author)

  19. Production and characterization of composite stone; Processamento e caracterizacao de pedra composta

    Leirose, G.D. [Universidade Federal de Ouro Preto (UFOP), MG (Brazil); Lameiras, F.S., E-mail: danileirose@yahoo.com.br [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil)

    2012-07-01

    Composite stone is a product similar to natural granite or marble, produced with particles of these materials. This material is used like natural stone as lining. The fabrication of artificial stones using residues of banded iron formations is a promising alternative to its actual destination (storage in dam). This research aims the characterization of composite stone to prove the efficacy of this kind of processing. It was used first, natural quartz as a raw material. The patterns of the samples were confirmed by IR spectra and XRD patterns, ensuring the reproducibility of processing applied. Moreover, this material is homogeneous, with low porosity and high flexural strength, confirmed by its structural characterization. Thus, it can be affirmed that the process chosen is suitable, enabling the application of this methodology to the use of waste. (author)

  20. Characterization of grog of bricks; Caracterizacao de chamote de blocos de vedacao

    Candido, V.S.; Pinheiro, R.M.; Monteiro, S.N.; Vieira, C.M.F. [Universidade Estadual do Norte Fluminense Darcy Ribeiro (LAMAV/CCT/UENF), Campos dos Goytacazes, RJ (Brazil). Lab. de Materiais Avancados

    2010-07-01

    This work aims to characterize a waste of red ceramic, grog, generated from the milling of defective pieces of bricks fired in a Hoffmann type furnace by a industry from Campos dos Goytacazes-RJ. The grog was tested for X-ray diffraction, X-ray fluorescence, thermogravimetric and differential thermal analysis, dilatometry, sieving and sedimentation by gravity and optical microscopy. The results indicated that the grog is predominantly constituted of quartz, muscovite mica and hematite. The presence of kaolinite indicates that the bricks were fired at low temperatures, below 600 deg C. Finally, the characterization results indicated that the grog presents itself as an alternative non plastic material to be used in mixtures with clays for the production of red ceramics. (author)

  1. Surface characterization of titanium based dental implants; Caracterizacao de implantes odontologicos a base de titanio

    Castilho, Guilherme Augusto Alcaraz

    2006-07-01

    Dental implantology uses metallic devices made of commercially pure titanium in order to replace lost teeth. Titanium presents favorable characteristics as bio material and modern implants are capable of integrate, witch is the union between bone and implant without fibrous tissue development. Three of the major Brazilian implant manufacturers were chosen to join the study. A foreign manufacturer participated as standard. The manufacturers had three specimens of each implant with two different surface finishing, as machined and porous, submitted to analysis. Surface chemical composition and implant morphology were analyzed by X-ray photoelectron spectroscopy (XP S), scanning electron microscopy (SEM) and microprobe. Implant surface is mainly composed of titanium, oxygen and carbon. Few contaminants commonly present on implant surface were found on samples. Superficial oxide layer is basically composed of titanium dioxide (TiO{sub 2}), another oxides as Ti O and Ti{sub 2}O{sub 3} were also found in small amount. Carbon on implant surface was attributed to manufacturing process. Nitrogen, Phosphorous and Silicon appeared in smaller concentration on surface. There was no surface discrepancy among foreign and Brazilian made implants. SEM images were made on different magnification, 35 X to 3500 X, and showed similarity among as machined implants. Porous surface finishing implants presented distinct morphology. This result was attributed to differences on manufacturing process. Implant bioactivity was accessed through immersion on simulated body solution (SBF) in order to verify formation of an hydroxyapatite (HA) layer on surface. Samples were divided on three groups according to immersion time: G1 (7 days), G2 (14 days), G3 (21 days), and deep in SBF solution at 37 deg C. After being removed from solution, XPS analyses were made and then implants have been submitted to microprobe analysis. XPS showed some components of SBF solution on sample surface but microprobe examinations did not confirmed the formation of HA layer. However, it was observed NaCl crystals on some implant surface. (author)

  2. Preparation and characterization of bentonite organo clay; Preparacao de caracterizacao de argilas bentonitas organofilicas

    Bertagnolli, C.; Almeida Neto, A.F. [Universidade Estadual de Campinas (UNICAMP), SP (Brazil). Fac. de Engenharia Quimica. Lab. de Engenharia Ambiental; Silva, M.G.C., E-mail: meuris@feq.unicamp.b [Universidade Estadual de Campinas (UNICAMP), SP (Brazil). Fac. de Engenharia Quimica

    2009-07-01

    Bentonite clays organically modified have great potential use for environmental remediation, especially in the separation of organic compounds from the water. The aim of this work was the preparation of organophilic clays from 'Verde-Lodo' bentonite clay with the quaternary ammonium salts cetyl-pyridinium chloride and benzalkonium chloride. The materials obtained were characterized by XRD, thermogravimetric analyses, Helium picnometry, SEM and energy dispersive X-ray techniques. The results show consistently successful synthesis of the organoclay through the increase in the basal spacing, as well as salt elimination picks and presence of carbon and chlorine in the modified clays; they are inexistent elements in the natural clay. (author)

  3. Characterization of experimental cements with endodontic goal; Caracterizacao de cimentos experimentais com finalidade endodontica

    Dantas, A.M.X.; Sousa, W.J.B.; Oliveira, E.D.C.; Carrodeguas, R.G.; Fook, M.V. Lia, E-mail: alana.mxd@hotmail [Universidade Federal de Campina Grande (CCT/UFCG), PB (Brazil). Unidade Academica de Engenharia de Materiais; Universidade Estadual da Paraiba (UEPB), Campina Grande, PB (Brazil). Departamento de Quimica

    2017-10-01

    The present study aimed to characterize experimental endodontic cements using as comparative parameter MTA cement. Two experimental endodontic cements were assessed: one based on 95% tri-strontium aluminate and 5% gypsum (CE1) and another based on 50% Sr{sub 3}Al{sub 2}O{sub 6} and 50% non-structural white cement (CE2). Experimental cements were manipulated and characterized by scanning electron microscopy (SEM), coupled to EDS mode, X-ray diffractometer (XRD) and Thermogravimetric (TG) analysis. Data analysis demonstrated that the particles of the materials used presented varied shapes and sizes, with similar elements and crystalline behavior. However, CE1 presented increased mass loss. Experimental cements presents similarities to MTA, nevertheless, further studies are encourage to determinate comparative properties with the commercially material. (author)

  4. Characterization of functional polymers by NMR; Caracterizacao de polimeros funcionalizados por ressonancia magnetica nuclear

    Neto, Oscar H.S. A.S.; San Gil, Rosane A.S.; Nakayama, T; Costa Neto, Claudio [Universidade Federal, Rio de Janeiro, RJ (Brazil). Inst. de Quimica

    1994-12-31

    Several synthetic polymers are used in the chemical analysis of complexes mixtures aiming to extract certain specific functional groups for further identification. This work describes the utilization of NMR in the characterization of one of the above mentioned compounds which will be used as reagent for the synthesis of another compound of the same type, which will be further used in the chemical analysis of alcohols and phenols. The methodology is described. The results are described and discussed 4 refs., 2 figs.

  5. Characterization of natural bentonite by NMR; Caracterizacao de bentonitas naturais por ressonancia magnetica nuclear

    Leite, Sidnei Q.M.; Dieguez, Lidia C [Universidade Federal, Rio de Janeiro, RJ (Brazil). Coordenacao dos Programas de Pos-graduacao de Engenharia; Menezes, Sonia M.C. [PETROBRAS, Rio de Janeiro, RJ (Brazil). Centro de Pesquisas; San Gil, Rosane A.S. [Universidade Federal, Rio de Janeiro, RJ (Brazil). Inst. de Quimica

    1994-12-31

    Solid state NMR as well as several other instrumental chemical analysis techniques were used in order to characterize two natural occurring bentonite. The methodology is described. The NMR spectra, together with the other used techniques suggest that the observed differences are due to iron inclusions in tetrahedral and octahedral sites 5 refs., 3 figs., 5 tabs.

  6. Costs characterization for small scale hydroelectric power plants; Caracterizacao dos custos de pequenas centrais hidreletricas

    Oliva, Vagner Jose; Carrocci, Luiz Roberto; Avellar, Luis Henrique Nobre [UNESP, Guaratingueta, SP (Brazil). Faculdade de Engenharia. Dept. de Energia; Florencano, Jose Carlos S. [UNITAU (WEC). Dept. de Engenharia Civil

    1997-12-31

    A set of new projects were developed according the Manuais de Estudos e Projetos de PCH (ELETROBRAS-DNAEE). This paper, initially, shows an analysis of cost for each components of PCH taking into account the real costs of these projects. It also presents a global equation which allows a preliminary estimation of cost for each construction. In a second moment, it shows an another analysis using few second moment, it shows an another analysis using few elements for a better hydraulic utilization. (author) 9 refs., 1 tab.; e-mail: lavellar at feg.unesp.br

  7. Synthesis and characterization of metallic nuclear fuels; Sintese e caracterizacao de combustiveis nucleares metalicos

    Longen, F.R., E-mail: frlongen@utfpr.edu.br [Universidade Tecnologica Federal do Parana (UTFPR), Medianeira, PR (Brazil); Barco, R.; Paesano Junior, A. [Universidade Estadual de Maringa (UEM), PR (Brazil); Pagano Junior, L. [Centro Tecnologico da Marinha (CETEM), Sao Paulo, SP (Brazil)

    2014-07-01

    U-Zr-Mo and U-Zr-Gd ternary alloys, potentially useful as metallic nuclear fuel, were prepared at different concentrations by arc-melting and characterized by X-ray diffraction. Those alloys containing molybdenum were submitted to thermal annealing in inert atmosphere, followed by quenching in water. These samples were measured before and after the thermal treatment. The diffractometric results evidenced that the as-cast alloys solidified mostly with a body centered cubic structure (γphase) and that for the uranium richest samples a second phase formed, with an orthorhombic structure (α phase). For the U-Zr-Gd alloys the X-ray diffractometry revealed the retention of a hexagonal structure (δ phase) and gadolinium traces in the poorest uranium samples. The U{sub 57}(Zr{sub 92}Gd{sub 8}){sub 43} sample resulted monophasic becoming, according to literature, the first time that a solid solution combining uranium and gadolinium is identified. (author)

  8. Production and characterization of ceramics for armor application; Producao e caracterizacao de ceramicas para blindagem balistica

    Alves, J.T.; Lopes, C.M.A. [Instituto Tecnologico de Aeronautica (ITA), Sao Jose dos Campos, SP (Brazil). Div. de Engenharia Mecanica-Aeronautica; Assis, J.M.K.; Melo, F.C.L., E-mail: cmoniz@iae.cta.b [Instituto de Aeronautica e Espaco (IAE), Sao Jose dos Campos, SP (Brazil). Div. de Materiais

    2010-07-01

    The fabrication of devices for ballistic protection as bullet proof vests and helmets and armored vehicles has been evolving over the past years along with the materials and models used for this specific application. The requirements for high efficient light-weight ballistic protection systems which not interfere in the user comfort and mobility has driven the research in this area. In this work we will present the results of characterization of two ceramics based on alumina and silicon carbide. The ceramics were produced in lab scale and the specific mass, scanning electron microscopy (SEM) microstructure, Vickers hardness, flexural resistance at room temperature and X-ray diffraction were evaluated. Ballistic tests performed in the selected materials showed that the ceramics present armor efficiency. (author)

  9. Thermodegradation of biodiesel: thermoanalytical and rheological characterization; Degradacao termica de biodiesel: caracterizacao termoanalitica e reologica

    Silva, Everson L.; Carvalho, Laura H.; Araujo, Gilmar T.; Gadelha, Tatiana S. [Universidade Federal de Campina Grande (UFCG), PB (Brazil)

    2008-07-01

    Brazil is a country of extensive agricultural land and great oil consumption and these factors favor biodiesel production in this country. In order for diesel/biodiesel mixtures to be effectively employed in diesel engines, a rigid quality control of these mixtures is needed. Biodiesel and mixtures must have their quality monitored with respect to oxidative resistance, thermal stability, fluidity and volatility, properties which can be modified by the adverse transport and stock conditions prior to consumption. Oxidation is the main degradation mechanism of products under transport and stock conditions, which can lead to significant economical losses. In this work sought the thermal degradation of neat biodiesel, synthesized in our laboratories was monitored. Thermal aging was conducted at 210 deg C for up to 1000 h. Virgin and thermally degraded samples were characterized by rheological measurements (in different shear conditions); FTIR; density and by color changes. We concluded that the soy biodiesel was successfully synthesized and that thermal exposure caused thermal-oxidative degradation of the biodiesel sample, significantly changing its properties as a function of thermal exposure times. (author)

  10. Characterization of X-ray irradiator RS-2000; Caracterizacao do irradiador de raios X RS-2000

    Mazaro, Sarah Jessica; Pavoni, Juliana Fernandes [Universidade de Sao Paulo (USP), Ribeirao Preto, SP (Brazil). Departamento de Fisica; Silva, Maelson do Nascimento; Bianchini, Adriano L.B.; Amaral, Leonardo Lira do, E-mail: sarahmazaro@yahoo.com.br [Universidade de Sao Paulo (HC/FMRP/USP), Ribeirao Preto, SP (Brazil). Hospital das Clinicas. Faculdade de Medicina. Servico de Radioterapia

    2014-04-15

    Gamma irradiators are being replaced by the x - rays ones which are more economical and have greater safety benefits compared to the radionuclide irradiators. Some tests are usually performed to ensure quality control while working with radiation, as constancy, linearity, repeatability, reproducibility, radiometric survey and security tests. Evaluating the technical parameters and the instrument and equipment performance quickly. The irradiator characterization determines its operation, by ensuring that the deposited dose is the one desired. This study aims to characterize x-rays irradiators through dosimetric tests. The equipment used in this study stable in dose rate free space and regularity for safety test. Furthermore, the measurements were reproducible with a maximum variation of 10% and the radiometric survey showed that the results are consistent with the exemption requirements of radiological protection described in regulatory position 3.01/001:2011. (author)

  11. Ensemble Data Mining Methods

    National Aeronautics and Space Administration — Ensemble Data Mining Methods, also known as Committee Methods or Model Combiners, are machine learning methods that leverage the power of multiple models to achieve...

  12. BDF-methods

    Hostrup, Astrid Kuijers

    1999-01-01

    An introduction to BDF-methods is given. The use of these methods on differential algebraic equations (DAE's) with different indexes with respect to order, stability and convergens of the BDF-methods is presented.......An introduction to BDF-methods is given. The use of these methods on differential algebraic equations (DAE's) with different indexes with respect to order, stability and convergens of the BDF-methods is presented....

  13. Uranium price forecasting methods

    Fuller, D.M.

    1994-01-01

    This article reviews a number of forecasting methods that have been applied to uranium prices and compares their relative strengths and weaknesses. The methods reviewed are: (1) judgemental methods, (2) technical analysis, (3) time-series methods, (4) fundamental analysis, and (5) econometric methods. Historically, none of these methods has performed very well, but a well-thought-out model is still useful as a basis from which to adjust to new circumstances and try again

  14. Methods in aquatic bacteriology

    Austin, B

    1988-01-01

    .... Within these sections detailed chapters consider sampling methods, determination of biomass, isolation methods, identification, the bacterial microflora of fish, invertebrates, plants and the deep...

  15. On the use of a composite moderator at the IBR-2 reactor: Advantages for the neutron-diffraction texture analysis of rocks

    Bulavin, M. V.; Vasin, R.N.; Kulikov, S.A.; Lokajíček, Tomáš; Levin, D.M.

    2016-01-01

    Roč. 10, č. 4 (2016), s. 677-686 ISSN 1027-4510 Institutional support: RVO:67985831 Keywords : cold moderator * neutron-diffraction texture analysis * phase analysis * Rietveld method Subject RIV: DB - Geology ; Mineralogy

  16. The study of disorder and nanocrystallinity in C–S–H, supplementary cementitious materials and geopolymers using pair distribution function analysis

    Meral, Cagla; Benmore, C.J.; Monteiro, Paulo J.M.

    2011-01-01

    Significant progress was achieved with the application of Rietveld method to characterize the crystalline phases in portland cement paste. However, to obtain detailed information on the amorphous or poorly crystalline phases, it is necessary

  17. Preferred orientation of ettringite in concrete fractures

    Wenk, Hans-Rudolf; Monteiro, Paulo J. M.; Kunz, Martin; Chen, Kai; Tamura, Nobumichi; Lutterotti, Luca; Del Arroz, John

    2009-01-01

    distribution of ettringite crystals. Diffraction images are analyzed using the Rietveld method to obtain information on textures. The analysis reveals that the c axes of the trigonal crystallites are preferentially oriented perpendicular to the fracture

  18. Transport equation solving methods

    Granjean, P.M.

    1984-06-01

    This work is mainly devoted to Csub(N) and Fsub(N) methods. CN method: starting from a lemma stated by Placzek, an equivalence is established between two problems: the first one is defined in a finite medium bounded by a surface S, the second one is defined in the whole space. In the first problem the angular flux on the surface S is shown to be the solution of an integral equation. This equation is solved by Galerkin's method. The Csub(N) method is applied here to one-velocity problems: in plane geometry, slab albedo and transmission with Rayleigh scattering, calculation of the extrapolation length; in cylindrical geometry, albedo and extrapolation length calculation with linear scattering. Fsub(N) method: the basic integral transport equation of the Csub(N) method is integrated on Case's elementary distributions; another integral transport equation is obtained: this equation is solved by a collocation method. The plane problems solved by the Csub(N) method are also solved by the Fsub(N) method. The Fsub(N) method is extended to any polynomial scattering law. Some simple spherical problems are also studied. Chandrasekhar's method, collision probability method, Case's method are presented for comparison with Csub(N) and Fsub(N) methods. This comparison shows the respective advantages of the two methods: a) fast convergence and possible extension to various geometries for Csub(N) method; b) easy calculations and easy extension to polynomial scattering for Fsub(N) method [fr

  19. Investigation of structural and electrical properties of La{sub 0.7}(Ba{sub 1-x}Ca{sub x}){sub 0.3}MnO{sub 3} compounds by sol-gel method

    Winarsih, Suci; Kurniawan, Budhy, E-mail: bkuru07@gmail.com; Manaf, Azwar [Physics Department, Universitas Indonesia, Depok 16424 (Indonesia); Nanto, Dwi [Department of Physics Education, Universitas Islam Negeri Syarif Hidayatullah, Jakarta 15412 (Indonesia); Imaduddin, Agung; Hendrik [Metallurgical Research Center, Lembaga Ilmu Pengetahuan Indonesia, Puspiptek-Serpong 15314 (Indonesia); Saptari, Sitti Ahmiatri [Faculty of Science and Technology, Universitas Islam Negeri Syarif Hidayatullah, Jakarta 15412 (Indonesia)

    2016-06-17

    In this paper, we explored structural and electrical properties of La{sub 0.7}(Ba{sub 1-x}Ca{sub x}){sub 0.3}MnO{sub 3} (x = 0; 0.03; and 0.05) compounds. The general structure of perovskite manganites is AMnO{sub 3} (A= trivalent rare earth with divalent ion-doped). Average A-site cation size, external pressure, and the variance of the cation size σ{sup 2} are one of many factors that affected to magneto-transport properties of manganites as reported by others. In this work we focus only on the electrical properties in La{sub 0.7}Ba{sub 0.3}MnO{sub 3} Ca-doped compound which may influence crystal structure resulting resistivity phenomena under magnetic field influence. All samples were synthesized by sol-gel method from which fine powders were obtained. The X-ray powder diffraction pattern of powder materials shows that all samples are fully crystalline with a rhombohedral structure. Rietveld refinement shows that the presence of calcium has changed some crystal structural parameters such lattice parameter, Mn–O bond length, and Mn–O–Mn angles. The electrical resistivity of all synthesized materials investigated by four point probe method using Cryogenic Magnet in the temperature range of 50-300 K under influence a magnetic field shows resistivity temperature dependent. In fact presence of calcium has reduced the resistivity. It might occure because it has made an enhancement in the mobility of hopping electrons. The magnetic external field causes the resistivity decreased for all samples because host spin align by delocalizing the charge carries so electron itinerant through the lattice suggested by other authors. Both calcium dopant concentration and the applied external magnetic field shows strong correlation in reduction of resistivity.

  20. Study of the lattice parameter evolution of PWR irradiated MOX fuel by X-Ray diffraction; Etude de l'evolution du parametre cristallin des combustibles MOX irradies en rep par la methode de diffraction des rayons X

    Clavier, B

    1995-07-01

    Fuel irradiation leads to a swelling resulting from the formation of gaseous (Kr, Xe) or solid fission products which are found either in solution or as solid inclusions in the matrix. This phenomena has to be evaluated to be taken into account in fuel cladding Interaction. Fuel swelling was studied as a function of burn up by measuring the corresponding cell constant evolution by X-Ray diffraction. This study was realized on Mixed Oxide Fuels (MOX) irradiated in a Pressurized Water Reactor (PWR) at different burn-up for 3 initial Pu contents. Lattice parameter evolutions were followed as a function of burn-up for the irradiated fuel with and without an annealing thermal treatment. These experimental evolutions are compared to the theoretical evolutions calculated from the hard sphere model, using the fission product concentrations determined by the APPOLO computer code. Contribution of varying parameters influencing the unit cell value is discussed. Thermal treatment effects were checked by metallography, X-Ray diffraction and microprobe analysis. After thermal treatment, no structural change was observed but a decrease of the lattice parameter was measured. This modification results essentially from self-irradiation defect annealing and not from stoichiometry variations. Microprobe analysis showed that about 15% of the formed Molybdenum is in solid solution In the oxide matrix. Micrographs showed the existence of Pu packs in the oxide matrix which induces a broadening of diffraction lines. The RIETVELD method used to analyze the X-Ray patterns did not allow to characterize independently the Pu packs and the oxide matrix lattice parameters. Nevertheless, with this method, the presence of micro-strains in the irradiated nuclear fuel could be confirmed. (author)

  1. Catalytic oxidation of n-hexane promoted by Ce{sub 1−x}Cu{sub x}O{sub 2} catalysts prepared by one-step polymeric precursor method

    Araújo, Vinícius D., E-mail: dantas@ursa.ifsc.usp.br [Instituto de Física, Universidade de São Paulo – USP, 13560-970 São Carlos, SP (Brazil); Lima, Maurício M. de [Instituto de Ciencia de los Materiales, Universidad de Valencia, E-46071 Valencia (Spain); Fundación General, Universitat de Valencia, Valencia (Spain); Cantarero, Andrés [Instituto de Ciencia de los Materiales, Universidad de Valencia, E-46071 Valencia (Spain); Bernardi, Maria I.B. [Instituto de Física, Universidade de São Paulo – USP, 13560-970 São Carlos, SP (Brazil); Bellido, Jorge D.A. [CAP-Engenharia Química, Universidade Federal de São João Del-Rei – UFSJ, São João Del-Rei, MG (Brazil); Assaf, Elisabete M. [Instituto de Química, Universidade de São Paulo – USP, 13560-970 São Carlos, SP (Brazil); Balzer, Rosana; Probst, Luiz F.D. [Departamento de Química, Universidade Federal de Santa Catarina – UFSC, 88040-900 Florianópolis, SC (Brazil); Fajardo, Humberto V. [Departamento de Química, Universidade Federal de Ouro Preto – UFOP, 35400-000 Ouro Preto, MG (Brazil)

    2013-11-01

    Ceria-supported copper catalysts (Ce{sub 1−x}Cu{sub x}O{sub 2}, with x (mol) = 0, 0.01, 0.03, 0.05 and 0.10) were prepared in one step through the polymeric precursor method. The textural properties of the catalysts were investigated by X-ray diffraction (XRD), Rietveld refinement, N{sub 2}-physisorption (BET surface area), electron paramagnetic resonance (EPR), UV–visible diffuse reflectance and photoluminescence spectroscopies and temperature-programmed reduction (TPR). In a previous study ceria-supported copper catalysts were found to be efficient in the preferential oxidation of CO. In this study, we extended the catalytic application of Ce{sub 1−x}Cu{sub x}O{sub 2} systems to n-hexane oxidation and it was verified that the catalysts were highly efficient in the proposed reaction. The best performance (up to 95% conversion) was observed for the catalysts with low copper loads (Ce{sub 0.97}Cu{sub 0.03}O{sub 2} and Ce{sub 0.99}Cu{sub 0.01}O{sub 2}, respectively). The physicochemical characterizations revealed that these behaviors could be attributed to the copper species present in the catalysts and the interaction between CuO and CeO{sub 2}, which vary according to the copper content. - Highlights: • Synthesis of CuO/CeO2 catalysts by the one-step polymeric precursor method. • 95% n-hexane conversion on Ce0.97Cu0.03O2 catalyst. • Redox properties play a key role in the catalytic performance.

  2. Investigation of structural and electrical properties of La0.7(Ba1-xCax)0.3MnO3 compounds by sol-gel method

    Winarsih, Suci; Kurniawan, Budhy; Manaf, Azwar; Nanto, Dwi; Imaduddin, Agung; Hendrik; Saptari, Sitti Ahmiatri

    2016-01-01

    In this paper, we explored structural and electrical properties of La 0.7 (Ba 1-x Ca x ) 0.3 MnO 3 (x = 0; 0.03; and 0.05) compounds. The general structure of perovskite manganites is AMnO 3 (A= trivalent rare earth with divalent ion-doped). Average A-site cation size, external pressure, and the variance of the cation size σ 2 are one of many factors that affected to magneto-transport properties of manganites as reported by others. In this work we focus only on the electrical properties in La 0.7 Ba 0.3 MnO 3 Ca-doped compound which may influence crystal structure resulting resistivity phenomena under magnetic field influence. All samples were synthesized by sol-gel method from which fine powders were obtained. The X-ray powder diffraction pattern of powder materials shows that all samples are fully crystalline with a rhombohedral structure. Rietveld refinement shows that the presence of calcium has changed some crystal structural parameters such lattice parameter, Mn–O bond length, and Mn–O–Mn angles. The electrical resistivity of all synthesized materials investigated by four point probe method using Cryogenic Magnet in the temperature range of 50-300 K under influence a magnetic field shows resistivity temperature dependent. In fact presence of calcium has reduced the resistivity. It might occure because it has made an enhancement in the mobility of hopping electrons. The magnetic external field causes the resistivity decreased for all samples because host spin align by delocalizing the charge carries so electron itinerant through the lattice suggested by other authors. Both calcium dopant concentration and the applied external magnetic field shows strong correlation in reduction of resistivity.

  3. Advanced differential quadrature methods

    Zong, Zhi

    2009-01-01

    Modern Tools to Perform Numerical DifferentiationThe original direct differential quadrature (DQ) method has been known to fail for problems with strong nonlinearity and material discontinuity as well as for problems involving singularity, irregularity, and multiple scales. But now researchers in applied mathematics, computational mechanics, and engineering have developed a range of innovative DQ-based methods to overcome these shortcomings. Advanced Differential Quadrature Methods explores new DQ methods and uses these methods to solve problems beyond the capabilities of the direct DQ method.After a basic introduction to the direct DQ method, the book presents a number of DQ methods, including complex DQ, triangular DQ, multi-scale DQ, variable order DQ, multi-domain DQ, and localized DQ. It also provides a mathematical compendium that summarizes Gauss elimination, the Runge-Kutta method, complex analysis, and more. The final chapter contains three codes written in the FORTRAN language, enabling readers to q...

  4. Inflow Turbulence Generation Methods

    Wu, Xiaohua

    2017-01-01

    Research activities on inflow turbulence generation methods have been vigorous over the past quarter century, accompanying advances in eddy-resolving computations of spatially developing turbulent flows with direct numerical simulation, large-eddy simulation (LES), and hybrid Reynolds-averaged Navier-Stokes-LES. The weak recycling method, rooted in scaling arguments on the canonical incompressible boundary layer, has been applied to supersonic boundary layer, rough surface boundary layer, and microscale urban canopy LES coupled with mesoscale numerical weather forecasting. Synthetic methods, originating from analytical approximation to homogeneous isotropic turbulence, have branched out into several robust methods, including the synthetic random Fourier method, synthetic digital filtering method, synthetic coherent eddy method, and synthetic volume forcing method. This article reviews major progress in inflow turbulence generation methods with an emphasis on fundamental ideas, key milestones, representative applications, and critical issues. Directions for future research in the field are also highlighted.

  5. Methods of nonlinear analysis

    Bellman, Richard Ernest

    1970-01-01

    In this book, we study theoretical and practical aspects of computing methods for mathematical modelling of nonlinear systems. A number of computing techniques are considered, such as methods of operator approximation with any given accuracy; operator interpolation techniques including a non-Lagrange interpolation; methods of system representation subject to constraints associated with concepts of causality, memory and stationarity; methods of system representation with an accuracy that is the best within a given class of models; methods of covariance matrix estimation;methods for low-rank mat

  6. Consumer Behavior Research Methods

    Chrysochou, Polymeros

    2017-01-01

    This chapter starts by distinguishing consumer behavior research methods based on the type of data used, being either secondary or primary. Most consumer behavior research studies phenomena that require researchers to enter the field and collect data on their own, and therefore the chapter...... emphasizes the discussion of primary research methods. Based on the nature of the data primary research methods are further distinguished into qualitative and quantitative. The chapter describes the most important and popular qualitative and quantitative methods. It concludes with an overall evaluation...... of the methods and how to improve quality in consumer behavior research methods....

  7. Dissolution Methods Database

    U.S. Department of Health & Human Services — For a drug product that does not have a dissolution test method in the United States Pharmacopeia (USP), the FDA Dissolution Methods Database provides information on...

  8. The three circle method

    Garncarek, Z.

    1989-01-01

    The three circle method in its general form is presented. The method is especially useful for investigation of shapes of agglomerations of objects. An example of its applications to investigation of galaxies distribution is given. 17 refs. (author)

  9. Design Methods in Practice

    Jensen, Torben Elgaard; Andreasen, Mogens Myrup

    2010-01-01

    The paper challenges the dominant and widespread view that a good design method will guarantee a systematic approach as well as certain results. First, it explores the substantial differences between on the one hand the conception of methods implied in Pahl & Beitz’s widely recognized text book...... on engineering design, and on the other hand the understanding of method use, which has emerged from micro-sociological studies of practice (ethnomethodology). Second, it reviews a number of case studies conducted by engineering students, who were instructed to investigate the actual use of design methods...... in Danish companies. The paper concludes that design methods in practice deviate substantially from Pahl & Beitz’s description of method use: The object and problems, which are the starting points for method use, are more contested and less given than generally assumed; The steps of methods are often...

  10. Advances in Numerical Methods

    Mastorakis, Nikos E

    2009-01-01

    Features contributions that are focused on significant aspects of current numerical methods and computational mathematics. This book carries chapters that advanced methods and various variations on known techniques that can solve difficult scientific problems efficiently.

  11. Basic Finite Element Method

    Lee, Byeong Hae

    1992-02-01

    This book gives descriptions of basic finite element method, which includes basic finite element method and data, black box, writing of data, definition of VECTOR, definition of matrix, matrix and multiplication of matrix, addition of matrix, and unit matrix, conception of hardness matrix like spring power and displacement, governed equation of an elastic body, finite element method, Fortran method and programming such as composition of computer, order of programming and data card and Fortran card, finite element program and application of nonelastic problem.

  12. Conformable variational iteration method

    Omer Acan

    2017-02-01

    Full Text Available In this study, we introduce the conformable variational iteration method based on new defined fractional derivative called conformable fractional derivative. This new method is applied two fractional order ordinary differential equations. To see how the solutions of this method, linear homogeneous and non-linear non-homogeneous fractional ordinary differential equations are selected. Obtained results are compared the exact solutions and their graphics are plotted to demonstrate efficiency and accuracy of the method.

  13. VALUATION METHODS- LITERATURE REVIEW

    Dorisz Talas

    2015-01-01

    This paper is a theoretical overview of the often used valuation methods with the help of which the value of a firm or its equity is calculated. Many experts (including Aswath Damodaran, Guochang Zhang and CA Hozefa Natalwala) classify the methods. The basic models are based on discounted cash flows. The main method uses the free cash flow for valuation, but there are some newer methods that reveal and correct the weaknesses of the traditional models. The valuation of flexibility of managemen...

  14. Synthesis and characterization of nanosized ceria powders by microwave-hydrothermal method

    Bonamartini Corradi, A.; Bondioli, F.; Ferrari, A.M.; Manfredini, T.

    2006-01-01

    Nanocrystalline ceria powders (CeO 2 ) have been prepared by adding NaOH to a cerium ammonium nitrate aqueous solution under microwave-hydrothermal conditions. In particular the effect of the synthesis conditions (time, pressure and concentration of both the precursor and the precipitant agent solutions) on the physical properties of the crystals have been evaluated. Microwave-hydrothermal treatment of 5 min at 13.4 atm allows to obtain almost crystallized powders (amorphous phase 4%) as underlined by Rietveld-reference intensity ratio (RIR) results

  15. Mixed methods research.

    Halcomb, Elizabeth; Hickman, Louise

    2015-04-08

    Mixed methods research involves the use of qualitative and quantitative data in a single research project. It represents an alternative methodological approach, combining qualitative and quantitative research approaches, which enables nurse researchers to explore complex phenomena in detail. This article provides a practical overview of mixed methods research and its application in nursing, to guide the novice researcher considering a mixed methods research project.

  16. Possibilities of roentgenological method

    Sivash, Eh.S.; Sal'man, M.M.

    1980-01-01

    Literary and experimental data on estimating possibilities of roentgenologic investigations using an electron optical amplifier, X-ray television and roentgen cinematography are generalized. Different methods of studying gastro-intestinal tract are compared. The advantage of the roentgenologic method over the endoscopic method after stomach resection is shown [ru

  17. The Generalized Sturmian Method

    Avery, James Emil

    2011-01-01

    these ideas clearly so that they become more accessible. By bringing together these non-standard methods, the book intends to inspire graduate students, postdoctoral researchers and academics to think of novel approaches. Is there a method out there that we have not thought of yet? Can we design a new method...... generations of researchers were left to work out how to achieve this ambitious goal for molecular systems of ever-increasing size. This book focuses on non-mainstream methods to solve the molecular electronic Schrödinger equation. Each method is based on a set of core ideas and this volume aims to explain...

  18. Mimetic discretization methods

    Castillo, Jose E

    2013-01-01

    To help solve physical and engineering problems, mimetic or compatible algebraic discretization methods employ discrete constructs to mimic the continuous identities and theorems found in vector calculus. Mimetic Discretization Methods focuses on the recent mimetic discretization method co-developed by the first author. Based on the Castillo-Grone operators, this simple mimetic discretization method is invariably valid for spatial dimensions no greater than three. The book also presents a numerical method for obtaining corresponding discrete operators that mimic the continuum differential and

  19. DOE methods compendium

    Leasure, C.S.

    1992-01-01

    The Department of Energy (DOE) has established an analytical methods compendium development program to integrate its environmental analytical methods. This program is administered through DOE's Laboratory Management Division (EM-563). The primary objective of this program is to assemble a compendium of analytical chemistry methods of known performance for use by all DOE Environmental Restoration and Waste Management program. This compendium will include methods for sampling, field screening, fixed analytical laboratory and mobile analytical laboratory analyses. It will also include specific guidance on the proper selection of appropriate sampling and analytical methods in using specific analytical requirements

  20. Methods for assessing geodiversity

    Zwoliński, Zbigniew; Najwer, Alicja; Giardino, Marco

    2017-04-01

    The accepted systematics of geodiversity assessment methods will be presented in three categories: qualitative, quantitative and qualitative-quantitative. Qualitative methods are usually descriptive methods that are suited to nominal and ordinal data. Quantitative methods use a different set of parameters and indicators to determine the characteristics of geodiversity in the area being researched. Qualitative-quantitative methods are a good combination of the collection of quantitative data (i.e. digital) and cause-effect data (i.e. relational and explanatory). It seems that at the current stage of the development of geodiversity research methods, qualitative-quantitative methods are the most advanced and best assess the geodiversity of the study area. Their particular advantage is the integration of data from different sources and with different substantive content. Among the distinguishing features of the quantitative and qualitative-quantitative methods for assessing geodiversity are their wide use within geographic information systems, both at the stage of data collection and data integration, as well as numerical processing and their presentation. The unresolved problem for these methods, however, is the possibility of their validation. It seems that currently the best method of validation is direct filed confrontation. Looking to the next few years, the development of qualitative-quantitative methods connected with cognitive issues should be expected, oriented towards ontology and the Semantic Web.

  1. Investigation of structural and magnetic properties of Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} nano powders prepared by self combustion method

    Sudheesh, V.D.; Nehra, J.; Vinesh, A. [Department of Physics, Mohanlal Sukhadia University, Udaipur 313001, Rajasthan (India); Sebastian, V. [Department of Physics, Nirmalagiri College, Kuthuparamba 670701, Kerala (India); Lakshmi, N., E-mail: nambakkat@yahoo.com [Department of Physics, Mohanlal Sukhadia University, Udaipur 313001, Rajasthan (India); Dutta, Dimple P. [Chemistry Division, Bhabha Atomic Research Centre, Mumbai 400085 (India); Reddy, V.R. [UGC-DAE CSR, University Campus, Khandwa Road, Indore 452001, M.P. (India); Venugopalan, K. [Department of Physics, Mohanlal Sukhadia University, Udaipur 313001, Rajasthan (India); Gupta, Ajay [UGC-DAE CSR, University Campus, Khandwa Road, Indore 452001, M.P. (India)

    2013-02-15

    Graphical abstract: Display Omitted Highlights: ► Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} prepared by self combustion with uniform/nonuniform heating. ► Characterized using TEM, XRD, in-field Mössbauer and DC magnetometry. ► Leads to bimodal (S1) and very narrow size distribution (S2) type nano samples. ► S1 has magnetic properties of bulk Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4}. ► Although very even sized, S2 large magnetic anisotropy distribution. -- Abstract: Nano powders of Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} have been synthesized by the self-combustion method at a relatively low temperature of 473 K under conditions of non-uniform and uniform heating. Rietveld fitting of X-ray diffractograms confirm the formation of the pure spinel phase in both samples. Transmission electron microscopy indicates that the sample prepared under non-uniform heating has a bimodal particle size distribution (average values 16 nm and 6 nm) while the one prepared under uniform heating has a very narrow particle size distribution (average size 4 nm). Low temperature, in-field Mössbauer spectroscopic studies clearly show surface spin contributions. The hyperfine fields and Curie temperature of the non-uniformly heated sample are in good agreement with those reported for the corresponding bulk samples. Despite having a very narrow particle size distribution, the uniformly heated sample has a large anisotropy distribution which is evident in the broad transition visible in the temperature dependent magnetization curve. It is also corroborated by the fact that the experimental magnetization curve at room temperature requires two Langevin functions for satisfactory reproduction.

  2. Methods of Software Verification

    R. E. Gurin

    2015-01-01

    Full Text Available This article is devoted to the problem of software verification (SW. Methods of software verification designed to check the software for compliance with the stated requirements such as correctness, system security and system adaptability to small changes in the environment, portability and compatibility, etc. These are various methods both by the operation process and by the way of achieving result. The article describes the static and dynamic methods of software verification and paid attention to the method of symbolic execution. In its review of static analysis are discussed and described the deductive method, and methods for testing the model. A relevant issue of the pros and cons of a particular method is emphasized. The article considers classification of test techniques for each method. In this paper we present and analyze the characteristics and mechanisms of the static analysis of dependencies, as well as their views, which can reduce the number of false positives in situations where the current state of the program combines two or more states obtained both in different paths of execution and in working with multiple object values. Dependences connect various types of software objects: single variables, the elements of composite variables (structure fields, array elements, the size of the heap areas, the length of lines, the number of initialized array elements in the verification code using static methods. The article pays attention to the identification of dependencies within the framework of the abstract interpretation, as well as gives an overview and analysis of the inference tools.Methods of dynamic analysis such as testing, monitoring and profiling are presented and analyzed. Also some kinds of tools are considered which can be applied to the software when using the methods of dynamic analysis. Based on the work a conclusion is drawn, which describes the most relevant problems of analysis techniques, methods of their solutions and

  3. Radiometric dating methods

    Bourdon, B.

    2003-01-01

    The general principle of isotope dating methods is based on the presence of radioactive isotopes in the geologic or archaeological object to be dated. The decay with time of these isotopes is used to determine the 'zero' time corresponding to the event to be dated. This paper recalls the general principle of isotope dating methods (bases, analytical methods, validation of results and uncertainties) and presents the methods based on natural radioactivity (Rb-Sr, Sm-Nd, U-Pb, Re-Os, K-Ar (Ar-Ar), U-Th-Ra- 210 Pb, U-Pa, 14 C, 36 Cl, 10 Be) and the methods based on artificial radioactivity with their applications. Finally, the methods based on irradiation damages (thermoluminescence, fission tracks, electron spin resonance) are briefly evoked. (J.S.)

  4. Performative Schizoid Method

    Svabo, Connie

    2016-01-01

    is presented and an example is provided of a first exploratory engagement with it. The method is used in a specific project Becoming Iris, making inquiry into arts-based knowledge creation during a three month visiting scholarship at a small, independent visual art academy. Using the performative schizoid......A performative schizoid method is developed as a method contribution to performance as research. The method is inspired by contemporary research in the human and social sciences urging experimentation and researcher engagement with creative and artistic practice. In the article, the method...... method in Becoming Iris results in four audio-visual and performance-based productions, centered on an emergent theme of the scholartist as a bird in borrowed feathers. Interestingly, the moral lesson of the fable about the vain jackdaw, who dresses in borrowed peacock feathers and becomes a castout...

  5. Angular correlation methods

    Ferguson, A.J.

    1974-01-01

    An outline of the theory of angular correlations is presented, and the difference between the modern density matrix method and the traditional wave function method is stressed. Comments are offered on particular angular correlation theoretical techniques. A brief discussion is given of recent studies of gamma ray angular correlations of reaction products recoiling with high velocity into vacuum. Two methods for optimization to obtain the most accurate expansion coefficients of the correlation are discussed. (1 figure, 53 references) (U.S.)

  6. Maximum Quantum Entropy Method

    Sim, Jae-Hoon; Han, Myung Joon

    2018-01-01

    Maximum entropy method for analytic continuation is extended by introducing quantum relative entropy. This new method is formulated in terms of matrix-valued functions and therefore invariant under arbitrary unitary transformation of input matrix. As a result, the continuation of off-diagonal elements becomes straightforward. Without introducing any further ambiguity, the Bayesian probabilistic interpretation is maintained just as in the conventional maximum entropy method. The applications o...

  7. Rossi Alpha Method

    Hansen, G.E.

    1985-01-01

    The Rossi Alpha Method has proved to be valuable for the determination of prompt neutron lifetimes in fissile assemblies having known reproduction numbers at or near delayed critical. This workshop report emphasizes the pioneering applications of the method by Dr. John D. Orndoff to fast-neutron critical assemblies at Los Alamos. The value of the method appears to disappear for subcritical systems where the Rossi-α is no longer an α-eigenvalue

  8. Qualitative methods textbooks

    Barndt, William

    2003-01-01

    Over the past few years, the number of political science departments offering qualitative methods courses has grown substantially. The number of qualitative methods textbooks has kept pace, providing instructors with an overwhelming array of choices. But how to decide which text to choose from this exhortatory smorgasbord? The scholarship desperately needs evaluated. Yet the task is not entirely straightforward: qualitative methods textbooks reflect the diversity inherent in qualitative metho...

  9. The Box Method

    Nielsen, Peter Vilhelm

    The velocity level in a room ventilated by jet ventilation is strongly influenced by the supply conditions. The momentum flow in the supply jets controls the air movement in the room and, therefore, it is very important that the inlet conditions and the numerical method can generate a satisfactor...... description of this momentum flow. The Box Method is a practical method for the description of an Air Terminal Device which will save grid points and ensure the right level of the momentum flow....

  10. Applied Bayesian hierarchical methods

    Congdon, P

    2010-01-01

    ... . . . . . . . . . . . . . . . . . . . . . . . . . . . 1.2 Posterior Inference from Bayes Formula . . . . . . . . . . . . 1.3 Markov Chain Monte Carlo Sampling in Relation to Monte Carlo Methods: Obtaining Posterior...

  11. [Methods of quantitative proteomics].

    Kopylov, A T; Zgoda, V G

    2007-01-01

    In modern science proteomic analysis is inseparable from other fields of systemic biology. Possessing huge resources quantitative proteomics operates colossal information on molecular mechanisms of life. Advances in proteomics help researchers to solve complex problems of cell signaling, posttranslational modification, structure and functional homology of proteins, molecular diagnostics etc. More than 40 various methods have been developed in proteomics for quantitative analysis of proteins. Although each method is unique and has certain advantages and disadvantages all these use various isotope labels (tags). In this review we will consider the most popular and effective methods employing both chemical modifications of proteins and also metabolic and enzymatic methods of isotope labeling.

  12. Methods in ALFA Alignment

    Melendez, Jordan

    2014-01-01

    This note presents two model-independent methods for use in the alignment of the ALFA forward detectors. Using a Monte Carlo simulated LHC run at \\beta = 90m and \\sqrt{s} = 7 TeV, the Kinematic Peak alignment method is utilized to reconstruct the Mandelstam momentum transfer variable t for single-diractive protons. The Hot Spot method uses fluctuations in the hitmap density to pinpoint particular regions in the detector that could signal a misalignment. Another method uses an error function fit to find the detector edge. With this information, the vertical alignment can be determined.

  13. Method of chronokinemetrical invariants

    Vladimirov, Yu.S.; Shelkovenko, A.Eh.

    1976-01-01

    A particular case of a general dyadic method - the method of chronokinemetric invariants is formulated. The time-like dyad vector is calibrated in a chronometric way, and the space-like vector - in a kinemetric way. Expressions are written for the main physical-geometrical values of the dyadic method and for differential operators. The method developed may be useful for predetermining the reference system of a single observer, and also for studying problems connected with emission and absorption of gravitational and electromagnetic waves [ru

  14. Application of Powder Diffraction Methods to the Analysis of the Atomic Structure of Nanocrystals: The Concept of the Apparent Lattice Parameter (ALP)

    Palosz, B.; Grzanka, E.; Gierlotka, S.; Stelmakh, S.; Pielaszek, R.; Bismayer, U.; Weber, H.-P.; Palosz, W.; Curreri, Peter A. (Technical Monitor)

    2002-01-01

    The applicability of standard methods of elaboration of powder diffraction data for determination of the structure of nano-size crystallites is analysed. Based on our theoretical calculations of powder diffraction data we show, that the assumption of the infinite crystal lattice for nanocrystals smaller than 20 nm in size is not justified. Application of conventional tools developed for elaboration of powder diffraction data, like the Rietveld method, may lead to erroneous interpretation of the experimental results. An alternate evaluation of diffraction data of nanoparticles, based on the so-called 'apparent lattice parameter' (alp) is introduced. We assume a model of nanocrystal having a grain core with well-defined crystal structure, surrounded by a surface shell with the atomic structure similar to that of the core but being under a strain (compressive or tensile). The two structural components, the core and the shell, form essentially a composite crystal with interfering, inseparable diffraction properties. Because the structure of such a nanocrystal is not uniform, it defies the basic definitions of an unambiguous crystallographic phase. Consequently, a set of lattice parameters used for characterization of simple crystal phases is insufficient for a proper description of the complex structure of nanocrystals. We developed a method of evaluation of powder diffraction data of nanocrystals, which refers to a core-shell model and is based on the 'apparent lattice parameter' methodology. For a given diffraction pattem, the alp values are calculated for every individual Bragg reflection. For nanocrystals the alp values depend on the diffraction vector Q. By modeling different a0tomic structures of nanocrystals and calculating theoretically corresponding diffraction patterns using the Debye functions we showed, that alp-Q plots show characteristic shapes which can be used for evaluation of the atomic structure of the core-shell system. We show, that using a simple

  15. Nondestructive testing method

    Porter, J.F.

    1996-01-01

    Nondestructive testing (NDT) is the use of physical and chemical methods for evaluating material integrity without impairing its intended usefulness or continuing service. Nondestructive tests are used by manufaturer's for the following reasons: 1) to ensure product reliability; 2) to prevent accidents and save human lives; 3) to aid in better product design; 4) to control manufacturing processes; and 5) to maintain a uniform quality level. Nondestructive testing is used extensively on power plants, oil and chemical refineries, offshore oil rigs and pipeline (NDT can even be conducted underwater), welds on tanks, boilers, pressure vessels and heat exchengers. NDT is now being used for testing concrete and composite materials. Because of the criticality of its application, NDT should be performed and the results evaluated by qualified personnel. There are five basic nondestructive examination methods: 1) liquid penetrant testing - method used for detecting surface flaws in materials. This method can be used for metallic and nonmetallic materials, portable and relatively inexpensive. 2) magnetic particle testing - method used to detect surface and subsurface flaws in ferromagnetic materials; 3) radiographic testing - method used to detect internal flaws and significant variation in material composition and thickness; 4) ultrasonic testing - method used to detect internal and external flaws in materials. This method uses ultrasonics to measure thickness of a material or to examine the internal structure for discontinuities. 5) eddy current testing - method used to detect surface and subsurface flaws in conductive materials. Not one nondestructive examination method can find all discontinuities in all of the materials capable of being tested. The most important consideration is for the specifier of the test to be familiar with the test method and its applicability to the type and geometry of the material and the flaws to be detected

  16. Methods for data classification

    Garrity, George [Okemos, MI; Lilburn, Timothy G [Front Royal, VA

    2011-10-11

    The present invention provides methods for classifying data and uncovering and correcting annotation errors. In particular, the present invention provides a self-organizing, self-correcting algorithm for use in classifying data. Additionally, the present invention provides a method for classifying biological taxa.

  17. Computational methods working group

    Gabriel, T.A.

    1997-09-01

    During the Cold Moderator Workshop several working groups were established including one to discuss calculational methods. The charge for this working group was to identify problems in theory, data, program execution, etc., and to suggest solutions considering both deterministic and stochastic methods including acceleration procedures.

  18. Method for exchanging data

    2014-01-01

    The present invention relates to a method for exchanging data between at least two servers with use of a gateway. Preferably the method is applied to healthcare systems. Each server holds a unique federated identifier, which identifier identifies a single patient (P). Thus, it is possible for the

  19. WWW: The Scientific Method

    Blystone, Robert V.; Blodgett, Kevin

    2006-01-01

    The scientific method is the principal methodology by which biological knowledge is gained and disseminated. As fundamental as the scientific method may be, its historical development is poorly understood, its definition is variable, and its deployment is uneven. Scientific progress may occur without the strictures imposed by the formal…

  20. Methods of numerical relativity

    Piran, T.

    1983-01-01

    Numerical Relativity is an alternative to analytical methods for obtaining solutions for Einstein equations. Numerical methods are particularly useful for studying generation of gravitational radiation by potential strong sources. The author reviews the analytical background, the numerical analysis aspects and techniques and some of the difficulties involved in numerical relativity. (Auth.)

  1. Differential equation method

    Kotikov, A.V.

    1993-01-01

    A new method of massive Feynman diagrams calculation is presented. It provides a fairly simple procedure to obtain the result without the D-space integral calculation (for the dimensional regularization). Some diagrams are calculated as an illustration of this method capacities. (author). 7 refs

  2. DISCOURSE ON METHODS.

    BOUCHER, JOHN G.

    THE AUTHOR STATES THAT BEFORE PRESENT FOREIGN LANGUAGE TEACHING METHODS CAN BE DISCUSSED INTELLIGENTLY, THE RESEARCH IN PSYCHOLOGY AND LINGUISTICS WHICH HAS INFLUENCED THE DEVELOPMENT OF THESE METHODS MUST BE CONSIDERED. MANY FOREIGN LANGUAGE TEACHERS WERE BEGINNING TO FEEL COMFORTABLE WITH THE AUDIOLINGUAL APPROACH WHEN NOAM CHOMSKY, IN HIS 1966…

  3. Research Methods in Education

    Check, Joseph; Schutt, Russell K.

    2011-01-01

    "Research Methods in Education" introduces research methods as an integrated set of techniques for investigating questions about the educational world. This lively, innovative text helps students connect technique and substance, appreciate the value of both qualitative and quantitative methodologies, and make ethical research decisions.…

  4. Attribute-Based Methods

    Thomas P. Holmes; Wiktor L. Adamowicz

    2003-01-01

    Stated preference methods of environmental valuation have been used by economists for decades where behavioral data have limitations. The contingent valuation method (Chapter 5) is the oldest stated preference approach, and hundreds of contingent valuation studies have been conducted. More recently, and especially over the last decade, a class of stated preference...

  5. Proven Weight Loss Methods

    Fact Sheet Proven Weight Loss Methods What can weight loss do for you? Losing weight can improve your health in a number of ways. It can lower ... at www.hormone.org/Spanish . Proven Weight Loss Methods Fact Sheet www.hormone.org

  6. Radiation borehole logging method

    Wylie, A.; Mathew, P.J.

    1977-01-01

    A method of obtaining an indication of the diameter of a borehole is described. The method comprises subjecting the walls of the borehole to monoenergetic gamma radiation and making measurements of the intensity of gamma radiation backscattered from the walls. The energy of the radiation is sufficiently high for the shape to be substantially independent of the density and composition of the borehole walls

  7. Isotope methods in hydrology

    Moser, H.; Rauert, W.

    1980-01-01

    Of the investigation methods used in hydrology, tracer methods hold a special place as they are the only ones which give direct insight into the movement and distribution processes taking place in surface and ground waters. Besides the labelling of water with salts and dyes, as in the past, in recent years the use of isotopes in hydrology, in water research and use, in ground-water protection and in hydraulic engineering has increased. This by no means replaces proven methods of hydrological investigation but tends rather to complement and expand them through inter-disciplinary cooperation. The book offers a general introduction to the application of various isotope methods to specific hydrogeological and hydrological problems. The idea is to place the hydrogeologist and the hydrologist in the position to recognize which isotope method will help him solve his particular problem or indeed, make a solution possible at all. He should also be able to recognize what the prerequisites are and what work and expenditure the use of such methods involves. May the book contribute to promoting cooperation between hydrogeologists, hydrologists, hydraulic engineers and isotope specialists, and thus supplement proven methods of investigation in hydrological research and water utilization and protection wherever the use of isotope methods proves to be of advantage. (orig./HP) [de

  8. Essential numerical computer methods

    Johnson, Michael L

    2010-01-01

    The use of computers and computational methods has become ubiquitous in biological and biomedical research. During the last 2 decades most basic algorithms have not changed, but what has is the huge increase in computer speed and ease of use, along with the corresponding orders of magnitude decrease in cost. A general perception exists that the only applications of computers and computer methods in biological and biomedical research are either basic statistical analysis or the searching of DNA sequence data bases. While these are important applications they only scratch the surface of the current and potential applications of computers and computer methods in biomedical research. The various chapters within this volume include a wide variety of applications that extend far beyond this limited perception. As part of the Reliable Lab Solutions series, Essential Numerical Computer Methods brings together chapters from volumes 210, 240, 321, 383, 384, 454, and 467 of Methods in Enzymology. These chapters provide ...

  9. Adaptive method of lines

    Saucez, Ph

    2001-01-01

    The general Method of Lines (MOL) procedure provides a flexible format for the solution of all the major classes of partial differential equations (PDEs) and is particularly well suited to evolutionary, nonlinear wave PDEs. Despite its utility, however, there are relatively few texts that explore it at a more advanced level and reflect the method''s current state of development.Written by distinguished researchers in the field, Adaptive Method of Lines reflects the diversity of techniques and applications related to the MOL. Most of its chapters focus on a particular application but also provide a discussion of underlying philosophy and technique. Particular attention is paid to the concept of both temporal and spatial adaptivity in solving time-dependent PDEs. Many important ideas and methods are introduced, including moving grids and grid refinement, static and dynamic gridding, the equidistribution principle and the concept of a monitor function, the minimization of a functional, and the moving finite elem...

  10. Bayesian Monte Carlo method

    Rajabalinejad, M.

    2010-01-01

    To reduce cost of Monte Carlo (MC) simulations for time-consuming processes, Bayesian Monte Carlo (BMC) is introduced in this paper. The BMC method reduces number of realizations in MC according to the desired accuracy level. BMC also provides a possibility of considering more priors. In other words, different priors can be integrated into one model by using BMC to further reduce cost of simulations. This study suggests speeding up the simulation process by considering the logical dependence of neighboring points as prior information. This information is used in the BMC method to produce a predictive tool through the simulation process. The general methodology and algorithm of BMC method are presented in this paper. The BMC method is applied to the simplified break water model as well as the finite element model of 17th Street Canal in New Orleans, and the results are compared with the MC and Dynamic Bounds methods.

  11. Methods in Modern Biophysics

    Nölting, Bengt

    2006-01-01

    Incorporating recent dramatic advances, this textbook presents a fresh and timely introduction to modern biophysical methods. An array of new, faster and higher-power biophysical methods now enables scientists to examine the mysteries of life at a molecular level. This innovative text surveys and explains the ten key biophysical methods, including those related to biophysical nanotechnology, scanning probe microscopy, X-ray crystallography, ion mobility spectrometry, mass spectrometry, proteomics, and protein folding and structure. Incorporating much information previously unavailable in tutorial form, Nölting employs worked examples and 267 illustrations to fully detail the techniques and their underlying mechanisms. Methods in Modern Biophysics is written for advanced undergraduate and graduate students, postdocs, researchers, lecturers and professors in biophysics, biochemistry and related fields. Special features in the 2nd edition: • Illustrates the high-resolution methods for ultrashort-living protei...

  12. The surface analysis methods

    Deville, J.P.

    1998-01-01

    Nowadays, there are a lot of surfaces analysis methods, each having its specificity, its qualities, its constraints (for instance vacuum) and its limits. Expensive in time and in investment, these methods have to be used deliberately. This article appeals to non specialists. It gives some elements of choice according to the studied information, the sensitivity, the use constraints or the answer to a precise question. After having recalled the fundamental principles which govern these analysis methods, based on the interaction between radiations (ultraviolet, X) or particles (ions, electrons) with matter, two methods will be more particularly described: the Auger electron spectroscopy (AES) and x-rays photoemission spectroscopy (ESCA or XPS). Indeed, they are the most widespread methods in laboratories, the easier for use and probably the most productive for the analysis of surface of industrial materials or samples submitted to treatments in aggressive media. (O.M.)

  13. Cooperative method development

    Dittrich, Yvonne; Rönkkö, Kari; Eriksson, Jeanette

    2008-01-01

    The development of methods tools and process improvements is best to be based on the understanding of the development practice to be supported. Qualitative research has been proposed as a method for understanding the social and cooperative aspects of software development. However, qualitative...... research is not easily combined with the improvement orientation of an engineering discipline. During the last 6 years, we have applied an approach we call `cooperative method development', which combines qualitative social science fieldwork, with problem-oriented method, technique and process improvement....... The action research based approach focusing on shop floor software development practices allows an understanding of how contextual contingencies influence the deployment and applicability of methods, processes and techniques. This article summarizes the experiences and discusses the further development...

  14. Engaging with mobile methods

    Jensen, Martin Trandberg

    2014-01-01

    This chapter showcases how mobile methods are more than calibrated techniques awaiting application by tourism researchers, but productive in the enactment of the mobile (Law and Urry, 2004). Drawing upon recent findings deriving from a PhD course on mobility and mobile methods it reveals...... the conceptual ambiguousness of the term ‘mobile methods’. In order to explore this ambiguousness the chapter provides a number of examples deriving from tourism research, to explore how mobile methods are always entangled in ideologies, predispositions, conventions and practice-realities. Accordingly......, the engagements with methods are acknowledged to be always political and contextual, reminding us to avoid essentialist discussions regarding research methods. Finally, the chapter draws on recent fieldwork to extend developments in mobilities-oriented tourism research, by employing auto-ethnography to call...

  15. Determination method of radiostrontium

    1984-01-01

    This manual provides determination methods of strontium-90 and strontium-89 in the environment released from nuclear facilities, and it is a revised edition of the previous manual published in 1974. As for the preparation method of radiation counting sample, ion exchange method, oxalate separation method and solvent extraction method were adopted in addition to the method of fuming nitric acid separation adopted in the previous edition. Strontium-90 is determined by the separation and radioactivity determination of yttrium-90 in radioequilibrium with strontium-90. Strontium-89 is determined by subtraction of radioactivity of strontium-90 plus yttrium-90 from gross radioactivity of isolated strontium carbonate. Radioactivity determination should be carried out with a low-background 2 π-gas-flow counting system for the mounted sample on a filter having a chemical form of ferric hydroxide, yttrium oxalate or strontium carbonate. This manual describes sample preparation procedures as well as radioactivity counting procedures for environmental samples of precipitates as rain or snow, airborne dust, fresh water, sea water and soil, and also for ash sample made from biological or food samples such as grains, vegetables, tea leaves, pine needle, milk, marine organisms, and total diet, by employing a method of fuming nitric acid separation, ion exchange separation, oxalate precipitate separation or solvent extraction separation (only for an ash sample). Procedures for reagent chemicals preparation is also attached to this manual. (Takagi, S.)

  16. Basics of Bayesian methods.

    Ghosh, Sujit K

    2010-01-01

    Bayesian methods are rapidly becoming popular tools for making statistical inference in various fields of science including biology, engineering, finance, and genetics. One of the key aspects of Bayesian inferential method is its logical foundation that provides a coherent framework to utilize not only empirical but also scientific information available to a researcher. Prior knowledge arising from scientific background, expert judgment, or previously collected data is used to build a prior distribution which is then combined with current data via the likelihood function to characterize the current state of knowledge using the so-called posterior distribution. Bayesian methods allow the use of models of complex physical phenomena that were previously too difficult to estimate (e.g., using asymptotic approximations). Bayesian methods offer a means of more fully understanding issues that are central to many practical problems by allowing researchers to build integrated models based on hierarchical conditional distributions that can be estimated even with limited amounts of data. Furthermore, advances in numerical integration methods, particularly those based on Monte Carlo methods, have made it possible to compute the optimal Bayes estimators. However, there is a reasonably wide gap between the background of the empirically trained scientists and the full weight of Bayesian statistical inference. Hence, one of the goals of this chapter is to bridge the gap by offering elementary to advanced concepts that emphasize linkages between standard approaches and full probability modeling via Bayesian methods.

  17. Methods in mummy research

    Lynnerup, Niels

    2009-01-01

    Mummies are human remains with preservation of non-bony tissue. Many mummy studies focus on the development and application of non-destructive methods for examining mummies, including radiography, CT-scanning with advanced 3-dimensional visualisations, and endoscopic techniques, as well as minima......Mummies are human remains with preservation of non-bony tissue. Many mummy studies focus on the development and application of non-destructive methods for examining mummies, including radiography, CT-scanning with advanced 3-dimensional visualisations, and endoscopic techniques, as well...... as minimally-destructive chemical, physical and biological methods for, e.g., stable isotopes, trace metals and DNA....

  18. Montessori Method and ICTs

    Athanasios Drigas

    2016-03-01

    Full Text Available This article bridges the gap between the Montessori Method and Information and Communication Technologies (ICTs in contemporary education. It reviews recent research works which recall the Montessori philosophy, principles and didactical tools applying to today’s computers and supporting technologies in children’s learning process. This article reviews how important the stimulation of human senses in the learning process is, as well as the development of Montessori materials using the body and the hand in particular, all according to the Montessori Method along with recent researches over ICTs. Montessori Method within information society age acquires new perspectives, new functionality and new efficacy.

  19. Rubidium-strontium method

    Dubansky, A.

    1980-01-01

    The rubidium-strontium geological dating method is based on the determination of the Rb and Sr isotope ratio in rocks, mainly using mass spectrometry. The method is only practical for silicate minerals and rocks, potassium feldspars and slates. Also described is the rubidium-strontium isochrone method. This, however, requires a significant amount of experimental data and an analysis of large quantities of samples, often of the order of tons. The results are tabulated of rubidium-strontium dating of geological formations in the Czech Socialist Republic. (M.S.)

  20. Structural Reliability Methods

    Ditlevsen, Ove Dalager; Madsen, H. O.

    The structural reliability methods quantitatively treat the uncertainty of predicting the behaviour and properties of a structure given the uncertain properties of its geometry, materials, and the actions it is supposed to withstand. This book addresses the probabilistic methods for evaluation...... of structural reliability, including the theoretical basis for these methods. Partial safety factor codes under current practice are briefly introduced and discussed. A probabilistic code format for obtaining a formal reliability evaluation system that catches the most essential features of the nature...... of the uncertainties and their interplay is the developed, step-by-step. The concepts presented are illustrated by numerous examples throughout the text....

  1. Catalytic reforming methods

    Tadd, Andrew R; Schwank, Johannes

    2013-05-14

    A catalytic reforming method is disclosed herein. The method includes sequentially supplying a plurality of feedstocks of variable compositions to a reformer. The method further includes adding a respective predetermined co-reactant to each of the plurality of feedstocks to obtain a substantially constant output from the reformer for the plurality of feedstocks. The respective predetermined co-reactant is based on a C/H/O atomic composition for a respective one of the plurality of feedstocks and a predetermined C/H/O atomic composition for the substantially constant output.

  2. Nuclear physics mathematical methods

    Balian, R.; Gervois, A.; Giannoni, M.J.; Levesque, D.; Maille, M.

    1984-01-01

    The nuclear physics mathematical methods, applied to the collective motion theory, to the reduction of the degrees of freedom and to the order and disorder phenomena; are investigated. In the scope of the study, the following aspects are discussed: the entropy of an ensemble of collective variables; the interpretation of the dissipation, applying the information theory; the chaos and the universality; the Monte-Carlo method applied to the classical statistical mechanics and quantum mechanics; the finite elements method, and the classical ergodicity [fr

  3. Methods for RNA Analysis

    Olivarius, Signe

    of the transcriptome, 5’ end capture of RNA is combined with next-generation sequencing for high-throughput quantitative assessment of transcription start sites by two different methods. The methods presented here allow for functional investigation of coding as well as noncoding RNA and contribute to future...... RNAs rely on interactions with proteins, the establishment of protein-binding profiles is essential for the characterization of RNAs. Aiming to facilitate RNA analysis, this thesis introduces proteomics- as well as transcriptomics-based methods for the functional characterization of RNA. First, RNA...

  4. Electromigration method in radiochemistry

    Makarova, T.P.; Stepanov, A.V.

    1977-01-01

    Investigations are reviewd of the period 1969-1975 accomplished by such methods as zonal electrophoresis in countercurrent, focusing electrophoresis, isotachophoresis, electrophoresis with elution, continuous two-dimensional electrophoresis. Since the methods considered are based on the use of porous fillers for stabilizing the medium, some attention is given to the effect of the solid-solution interface on the shape and rate of motion of the zones of the rare-earth elements investigated, Sr and others. The trend of developing electrophoresis as a method for obtaining high-purity elements is emphasized

  5. Numerical methods using Matlab

    Lindfield, George

    2012-01-01

    Numerical Methods using MATLAB, 3e, is an extensive reference offering hundreds of useful and important numerical algorithms that can be implemented into MATLAB for a graphical interpretation to help researchers analyze a particular outcome. Many worked examples are given together with exercises and solutions to illustrate how numerical methods can be used to study problems that have applications in the biosciences, chaos, optimization, engineering and science across the board. Numerical Methods using MATLAB, 3e, is an extensive reference offering hundreds of use

  6. Model Correction Factor Method

    Christensen, Claus; Randrup-Thomsen, Søren; Morsing Johannesen, Johannes

    1997-01-01

    The model correction factor method is proposed as an alternative to traditional polynomial based response surface techniques in structural reliability considering a computationally time consuming limit state procedure as a 'black box'. The class of polynomial functions is replaced by a limit...... of the model correction factor method, is that in simpler form not using gradient information on the original limit state function or only using this information once, a drastic reduction of the number of limit state evaluation is obtained together with good approximations on the reliability. Methods...

  7. Imaging methods in otorhinolaryngology

    Frey, K.W.; Mees, K.; Vogl, T.

    1989-01-01

    This book is the work of an otorhinolaryngologist and two radiologists, who combined their experience and efforts in order to solve a great variety and number of problems encountered in practical work, taking into account the latest technical potentials and the practical feasibility, which is determined by the equipment available. Every chapter presents the full range of diagnostic methods applicable, starting with the suitable plain radiography methods and proceeding to the various tomographic scanning methods, including conventional tomography. Every technique is assessed in terms of diagnostic value and drawbacks. (orig./MG) With 778 figs [de

  8. Generalized subspace correction methods

    Kolm, P. [Royal Institute of Technology, Stockholm (Sweden); Arbenz, P.; Gander, W. [Eidgenoessiche Technische Hochschule, Zuerich (Switzerland)

    1996-12-31

    A fundamental problem in scientific computing is the solution of large sparse systems of linear equations. Often these systems arise from the discretization of differential equations by finite difference, finite volume or finite element methods. Iterative methods exploiting these sparse structures have proven to be very effective on conventional computers for a wide area of applications. Due to the rapid development and increasing demand for the large computing powers of parallel computers, it has become important to design iterative methods specialized for these new architectures.

  9. Influence of Y and La substitution on particle size, structural and magnetic properties of nanosized nickel ferrite prepared by using citrate precursor method

    Anh, Luong Ngoc [International Training Institute for Materials Science (ITIMS), Hanoi University of Science and Technology, 1 Dai Co Viet Road, Hanoi (Viet Nam); Loan, To Thanh, E-mail: totloan@itims.edu.vn [International Training Institute for Materials Science (ITIMS), Hanoi University of Science and Technology, 1 Dai Co Viet Road, Hanoi (Viet Nam); Duong, Nguyen Phuc [International Training Institute for Materials Science (ITIMS), Hanoi University of Science and Technology, 1 Dai Co Viet Road, Hanoi (Viet Nam); Vietnam-Japan International Institute for Science of Technology (VJIIST), Hanoi University of Science and Technology, 1 Dai Co Viet Road, Hanoi (Viet Nam); Soontaranon, Siriwat [Synchrotron Light Research Institute, 111 University Avenue, Suranaree, Muang, Nakhon Ratchasima 30000 (Thailand); Viet Nga, Tran Thi; Hien, Than Duc [International Training Institute for Materials Science (ITIMS), Hanoi University of Science and Technology, 1 Dai Co Viet Road, Hanoi (Viet Nam)

    2015-10-25

    The compounds with the formulas NiFe{sub 2}O{sub 4}, NiFe{sub 1.9}Y{sub 0.1}O{sub 4} and NiFe{sub 1.9}La{sub 0.1}O{sub 4} were prepared by citrate precursor method and followed by heat treatment in air at 600 °C for 5 h. Crystal structure, valence state, chemical bonding and composition of the samples were studied rigorously by XRD, SXRD, XANES, FTIR and ICP–AES. Rietveld refinement of XRD and SXRD patterns reveals that the samples crystallize in single spinel phase with almost inverted structure in which the substituted ions Y{sup 3+} and La{sup 3+} locate in the octahedral sites and about ten percents of nickel atoms were found at the tetrahedral sites. Morphology and particle size were studied by SEM and TEM. The results show that the samples are composed of clustered nanoparticles with mean particle size decreases approximately from 20 nm in NiFe{sub 2}O{sub 4} sample to 10 nm in the substituted ones. The magnetic measurements were carried out by means of a VSM. Spontaneous magnetization, magnetic coercivity, Curie temperature, superparamagnetic transition temperature, interparticle interaction energy and effective anisotropy were determined and explained on the basis of the surface and finite–size effects and cation distribution. - Highlights: • Y{sup 3+} and La{sup 3+} substituted NiFe{sub 2}O{sub 4} nanoparticles are synthesized by citrate precursor method involving less energy. • XRD, SXRD and FTIR spectra reveal the crystallographic site occupancy of Y{sup 3+} and La{sup 3+}. • Compositions and valence states of cations are verified by ICP-AES and XANES. • Y{sup 3+} and La{sup 3+} substitution decreases the mean particle size to about 10 nm. • Influence of rare earth substitution and finite size in magnetic properties are investigated.

  10. Concrete compositions and methods

    Chen, Irvin; Lee, Patricia Tung; Patterson, Joshua

    2015-06-23

    Provided herein are compositions, methods, and systems for cementitious compositions containing calcium carbonate compositions and aggregate. The compositions find use in a variety of applications, including use in a variety of building materials and building applications.

  11. Ensemble Data Mining Methods

    Oza, Nikunj C.

    2004-01-01

    Ensemble Data Mining Methods, also known as Committee Methods or Model Combiners, are machine learning methods that leverage the power of multiple models to achieve better prediction accuracy than any of the individual models could on their own. The basic goal when designing an ensemble is the same as when establishing a committee of people: each member of the committee should be as competent as possible, but the members should be complementary to one another. If the members are not complementary, Le., if they always agree, then the committee is unnecessary---any one member is sufficient. If the members are complementary, then when one or a few members make an error, the probability is high that the remaining members can correct this error. Research in ensemble methods has largely revolved around designing ensembles consisting of competent yet complementary models.

  12. Diagnostic method and reagent

    Edgington, T.S.; Plow, E.F.

    1979-01-01

    The discovery of an isomeric species of carcinoembryonic antigen and methods of isolation, identification and utilization as a radiolabelled species of the same as an aid in the diagnosis of adenocarcinomas of the gastrointestinal tract are disclosed. 13 claims

  13. Methods of dating

    Gatty, B

    1986-04-01

    Scientific methods of dating, born less than thirty years ago, have recently improved tremendously. First the dating principles will be given; then it will be explained how, through natural radioactivity, we can have access to the age of an event or an object; the case of radiocarbon will be especially emphasized. The principle of relative methods such as thermoluminescence or paleomagnetism will also be shortly given. What is the use for dating. The fields of its application are numerous; through these methods, relatively precise ages can be given to the major events which have been keys in the history of universe, life and man; thus, dating is a useful scientific tool in astrophysics, geology, biology, anthropology and archeology. Even if certain ages are still subject to controversies, we can say that these methods have confirmed evolution's continuity, be it on a cosmic, biologic or human scale, where ages are measured in billions, millions or thousands of years respectively.

  14. Energy consumption assessment methods

    Sutherland, K S

    1975-01-01

    The why, what, and how-to aspects of energy audits for industrial plants, and the application of energy accounting methods to a chemical plant in order to assess energy conservation possibilities are discussed. (LCL)

  15. Stochastic optimization methods

    Marti, Kurt

    2005-01-01

    Optimization problems arising in practice involve random parameters. For the computation of robust optimal solutions, i.e., optimal solutions being insensitive with respect to random parameter variations, deterministic substitute problems are needed. Based on the distribution of the random data, and using decision theoretical concepts, optimization problems under stochastic uncertainty are converted into deterministic substitute problems. Due to the occurring probabilities and expectations, approximative solution techniques must be applied. Deterministic and stochastic approximation methods and their analytical properties are provided: Taylor expansion, regression and response surface methods, probability inequalities, First Order Reliability Methods, convex approximation/deterministic descent directions/efficient points, stochastic approximation methods, differentiation of probability and mean value functions. Convergence results of the resulting iterative solution procedures are given.

  16. Predictive Methods of Pople

    Chemistry for their pioneering contri butions to the development of computational methods in quantum chemistry and density functional theory .... program of Pop Ie for ab-initio electronic structure calculation of molecules. This ab-initio MO ...

  17. Methods for cellobiosan utilization

    Linger, Jeffrey; Beckham, Gregg T.

    2017-07-11

    Disclosed herein are enzymes useful for the degradation of cellobiosan in materials such a pyrolysis oils. Methods of degrading cellobiosan using enzymes or organisms expressing the same are also disclosed.

  18. Methods of neutron spectrometry

    Doerschel, B.

    1981-01-01

    The different methods of neutron spectrometry are based on the direct measurement of neutron velocity or on the use of suitable energy-dependent interaction processes. In the latter case the measuring effect of a detector is connected with the searched neutron spectrum by an integral equation. The solution needs suitable unfolding procedures. The most important methods of neutron spectrometry are the time-of-flight method, the crystal spectrometry, the neutron spectrometry by use of elastic collisions with hydrogen nuclei, and neutron spectrometry with the aid of nuclear reactions, especially of the neutron-induced activation. The advantages and disadvantages of these methods are contrasted considering the resolution, the measurable energy range, the sensitivity, and the experimental and computational efforts. (author)

  19. Methods in Modern Biophysics

    Nölting, Bengt

    2010-01-01

    Incorporating recent dramatic advances, this textbook presents a fresh and timely introduction to modern biophysical methods. An array of new, faster and higher-power biophysical methods now enables scientists to examine the mysteries of life at a molecular level. This innovative text surveys and explains the ten key biophysical methods, including those related to biophysical nanotechnology, scanning probe microscopy, X-ray crystallography, ion mobility spectrometry, mass spectrometry, proteomics, and protein folding and structure. Incorporating much information previously unavailable in tutorial form, Nölting employs worked examples and about 270 illustrations to fully detail the techniques and their underlying mechanisms. Methods in Modern Biophysics is written for advanced undergraduate and graduate students, postdocs, researchers, lecturers, and professors in biophysics, biochemistry and related fields. Special features in the 3rd edition: Introduces rapid partial protein ladder sequencing - an important...

  20. Lean Government Methods Guide

    This Guide focuses primarily on Lean production, which is an organizational improvement philosophy and set of methods that originated in manufacturing but has been expanded to government and service sectors.

  1. Number projection method

    Kaneko, K.

    1987-01-01

    A relationship between the number projection and the shell model methods is investigated in the case of a single-j shell. We can find a one-to-one correspondence between the number projected and the shell model states

  2. Etching method employing radiation

    Chapman, B.N.; Winters, H.F.

    1982-01-01

    This invention provides a method for etching a silicon oxide, carbide, nitride, or oxynitride surface using an electron or ion beam in the presence of a xenon or krypton fluoride. No additional steps are required after exposure to radiation

  3. GEM simulation methods development

    Tikhonov, V.; Veenhof, R.

    2002-01-01

    A review of methods used in the simulation of processes in gas electron multipliers (GEMs) and in the accurate calculation of detector characteristics is presented. Such detector characteristics as effective gas gain, transparency, charge collection and losses have been calculated and optimized for a number of GEM geometries and compared with experiment. A method and a new special program for calculations of detector macro-characteristics such as signal response in a real detector readout structure, and spatial and time resolution of detectors have been developed and used for detector optimization. A detailed development of signal induction on readout electrodes and electronics characteristics are included in the new program. A method for the simulation of charging-up effects in GEM detectors is described. All methods show good agreement with experiment

  4. Improved radioanalytical methods

    Erickson, M.D.; Aldstadt, J.H.; Alvarado, J.S.; Crain, J.S.; Orlandini, K.A.; Smith, L.L.

    1995-01-01

    Methods for the chemical characterization of the environment are being developed under a multitask project for the Analytical Services Division (EM-263) within the US Department of Energy (DOE) Office of Environmental Management. This project focuses on improvement of radioanalytical methods with an emphasis on faster and cheaper routine methods. We have developed improved methods, for separation of environmental levels of technetium-99 and strontium-89/90, radium, and actinides from soil and water; and for separation of actinides from soil and water matrix interferences. Among the novel separation techniques being used are element- and class-specific resins and membranes. (The 3M Corporation is commercializing Empore trademark membranes under a cooperative research and development agreement [CRADA] initiated under this project). We have also developed methods for simultaneous detection of multiple isotopes using inductively coupled plasma-mass spectrometry (ICP-MS). The ICP-MS method requires less rigorous chemical separations than traditional radiochemical analyses because of its mass-selective mode of detection. Actinides and their progeny have been isolated and concentrated from a variety of natural water matrices by using automated batch separation incorporating selective resins prior to ICP-MS analyses. In addition, improvements in detection limits, sample volume, and time of analysis were obtained by using other sample introduction techniques, such as ultrasonic nebulization and electrothermal vaporization. Integration and automation of the separation methods with the ICP-MS methodology by using flow injection analysis is underway, with an objective of automating methods to achieve more reproducible results, reduce labor costs, cut analysis time, and minimize secondary waste generation through miniaturization of the process

  5. Continuation Newton methods

    Axelsson, Owe; Sysala, Stanislav

    2015-01-01

    Roč. 70, č. 11 (2015), s. 2621-2637 ISSN 0898-1221 R&D Projects: GA ČR GA13-18652S Institutional support: RVO:68145535 Keywords : system of nonlinear equations * Newton method * load increment method * elastoplasticity Subject RIV: IN - Informatics, Computer Science Impact factor: 1.398, year: 2015 http://www.sciencedirect.com/science/article/pii/S0898122115003818

  6. Nuclear methods monitor nutrition

    Allen, B.J.

    1988-01-01

    Neutron activation of nitrogen and hydrogen in the body, the isotope dilution technique and the measurement of naturally radioactive potassium in the body are among the new nuclear methods, now under collaborative development by the Australian Nuclear Scientific and Technology Organization and medical specialists from several Sydney hospitals. These methods allow medical specialists to monitor the patient's response to various diets and dietary treatments in cases of cystic fibrosis, anorexia nervosa, long-term surgical trauma, renal diseases and AIDS. ills

  7. The fission track method

    Hansen, K.

    1990-01-01

    During the last decade fission track (FT) analysis has evolved as an important tool in exploration for hydrocarbon resources. Most important is this method's ability to yield information about temperatures at different times (history), and thus relate oil generation and time independently of other maturity parameters. The purpose of this paper is to introduce the basics of the method and give an example from the author's studies. (AB) (14 refs.)

  8. Experimental physics method

    Jeong, Yang Su; Oh, Byeong Seong

    2010-05-01

    This book introduces measurement and error, statistics of experimental data, population, sample variable, distribution function, propagation of error, mean and measurement of error, adjusting to rectilinear equation, common sense of error, experiment method, and record and statement. It also explains importance of error of estimation, systematic error, random error, treatment of single variable, significant figure, deviation, mean value, median, mode, sample mean, sample standard deviation, binomial distribution, gauss distribution, and method of least squares.

  9. Methods for measuring shrinkage

    Chapman, Paul; Templar, Simon

    2006-01-01

    This paper presents findings from research amongst European grocery retailers into their methods for measuring shrinkage. The findings indicate that: there is no dominant method for valuing or stating shrinkage; shrinkage in the supply chain is frequently overlooked; data is essential in pinpointing where and when loss occurs and that many retailers collect data at the stock-keeping unit (SKU) level and do so every 6 months. These findings reveal that it is difficult to benc...

  10. Method of saccharifying cellulose

    Johnson, E.A.; Demain, A.L.; Madia, A.

    1983-05-13

    A method is disclosed of saccharifying cellulose by incubation with the cellulase of Clostridium thermocellum in a broth containing an efficacious amount of thiol reducing agent. Other incubation parameters which may be advantageously controlled to stimulate saccharification include the concentration of alkaline earth salts, pH, temperature, and duration. By the method of the invention, even native crystalline cellulose such as that found in cotton may be completely saccharified.

  11. Method of treating depression

    Henn, Fritz [East Patchogue, NY

    2012-01-24

    Methods for treatment of depression-related mood disorders in mammals, particularly humans are disclosed. The methods of the invention include administration of compounds capable of enhancing glutamate transporter activity in the brain of mammals suffering from depression. ATP-sensitive K.sup.+ channel openers and .beta.-lactam antibiotics are used to enhance glutamate transport and to treat depression-related mood disorders and depressive symptoms.

  12. Methods of experimental physics

    Williams, Dudley

    1962-01-01

    Methods of Experimental Physics, Volume 3: Molecular Physics focuses on molecular theory, spectroscopy, resonance, molecular beams, and electric and thermodynamic properties. The manuscript first considers the origins of molecular theory, molecular physics, and molecular spectroscopy, as well as microwave spectroscopy, electronic spectra, and Raman effect. The text then ponders on diffraction methods of molecular structure determination and resonance studies. Topics include techniques of electron, neutron, and x-ray diffraction and nuclear magnetic, nuclear quadropole, and electron spin reson

  13. The ICARE Method

    Henke, Luke

    2010-01-01

    The ICARE method is a flexible, widely applicable method for systems engineers to solve problems and resolve issues in a complete and comprehensive manner. The method can be tailored by diverse users for direct application to their function (e.g. system integrators, design engineers, technical discipline leads, analysts, etc.). The clever acronym, ICARE, instills the attitude of accountability, safety, technical rigor and engagement in the problem resolution: Identify, Communicate, Assess, Report, Execute (ICARE). This method was developed through observation of Space Shuttle Propulsion Systems Engineering and Integration (PSE&I) office personnel approach in an attempt to succinctly describe the actions of an effective systems engineer. Additionally it evolved from an effort to make a broadly-defined checklist for a PSE&I worker to perform their responsibilities in an iterative and recursive manner. The National Aeronautics and Space Administration (NASA) Systems Engineering Handbook states, engineering of NASA systems requires a systematic and disciplined set of processes that are applied recursively and iteratively for the design, development, operation, maintenance, and closeout of systems throughout the life cycle of the programs and projects. ICARE is a method that can be applied within the boundaries and requirements of NASA s systems engineering set of processes to provide an elevated sense of duty and responsibility to crew and vehicle safety. The importance of a disciplined set of processes and a safety-conscious mindset increases with the complexity of the system. Moreover, the larger the system and the larger the workforce, the more important it is to encourage the usage of the ICARE method as widely as possible. According to the NASA Systems Engineering Handbook, elements of a system can include people, hardware, software, facilities, policies and documents; all things required to produce system-level results, qualities, properties, characteristics

  14. Synthesis and characterization of nanoparticles ferrites of the type ZN{sub x}Cu{sub 1-x}FE{sub 2}O{sub 4} and your application catalyst in acetylation vegetable oils; Sintese e caracterizacao de nanoparticulas de ferritas do tipo Zn{sub x}Cu{sub 1-x}Fe{sub 2}O{sub 4} e a sua aplicacao como catalisador em acetilacao em oleos vegetais

    Casagrande, D.S; Costa, W.V; Hechenleitner, A.A.W.; Oliveira, D.M.F. de; Pineda, E.A.G., E-mail: diogo_casagrande@msn.com [Universidade Estadual de Maringa (UEM), PR (Brazil)

    2016-07-01

    In this work were synthesized copper and zinc ferrites (0 - 10% mol with respect to copper), by the combustion method, using citrate as stabilizer. The obtained products were analyzed by Infrared spectrometry (FTIR), Raman spectroscopy (RAMAN) and x-ray diffractometry (DRX). Synthesized ferrites present hematite phase, maghemite phase and copper ferrite phases. The analysis indicated that increasing the zinc content leads to decreased of hematite phase. Increasing of zinc content lead to an increase of particle size. The best results of oil acylation were obtained with ferrites containing 2 and 4% of zinc, wherein the increase the increase of yield of acetylated product reached at 19% when compared with the yield obtained whit copper ferrite without zinc. (author)

  15. Preparation and characterization of electroluminescent devices based on complexes of {beta}-diketonates of Tb{sup 3+}, Eu{sup 3+}, Gd{sup 3+} ions with macrocyclic ligands and UO{sub 2}{sup 2+} films; Preparacao e caracterizacao de dispositivos eletroluminescentes de complexos de {beta}-dicetonados de ions Tb{sup 3+}, Eu{sup 3+}, Gd{sup 3+} com ligantes macrociclicos e filmes de UO{sub 2}{sup 2+}

    Gibelli, Edison Bessa

    2010-07-01

    Complexes containing Rare Earth ions are of great interest in the manufacture of electro luminescent devices as organic light emitting devices (OLED). These devices, using rare earth trivalent ions (TR{sup 3+}) as emitting centers, show high luminescence with extremely fine spectral bands due to the structure of their energy levels, long life time and high quantum efficiency. This work reports the preparation of Rare Earth {beta}-diketonate complexes (Tb{sup 3+}, Eu{sup 3+} and Gd{sup 3+}) and (tta - thenoyltrifluoroacetonate and acac - acetylacetonate) containing a ligand macrocyclic crown ether (DB18C6 - dibenzo18coroa6) and polymer films of UO{sub 2}{sup 2+}. The materials were characterized by complexometric titration with EDTA, CH elemental analysis, near infrared absorption spectroscopy, thermal analysis, X-ray diffraction (powder method) and luminescence spectroscopy. For manufacturing the OLED it was used the technique of deposition of thin films by physical vapor (PVD, Physical Vapor Deposition). (author)

  16. VALUATION METHODS- LITERATURE REVIEW

    Dorisz Talas

    2015-07-01

    Full Text Available This paper is a theoretical overview of the often used valuation methods with the help of which the value of a firm or its equity is calculated. Many experts (including Aswath Damodaran, Guochang Zhang and CA Hozefa Natalwala classify the methods. The basic models are based on discounted cash flows. The main method uses the free cash flow for valuation, but there are some newer methods that reveal and correct the weaknesses of the traditional models. The valuation of flexibility of management can be conducted mainly with real options. This paper briefly describes the essence of the Dividend Discount Model, the Free Cash Flow Model, the benefit from using real options and the Residual Income Model. There are a few words about the Adjusted Present Value approach as well. Different models uses different premises, and an overall truth is that if the required premises are real and correct, the value will be appropriately accurate. Another important condition is that experts, analysts should choose between the models on the basis of the purpose of valuation. Thus there are no good or bad methods, only methods that fit different goals and aims. The main task is to define exactly the purpose, then to find the most appropriate valuation technique. All the methods originates from the premise that the value of an asset is the present value of its future cash flows. According to the different points of view of different techniques the resulted values can be also differed from each other. Valuation models and techniques should be adapted to the rapidly changing world, but the basic statements remain the same. On the other hand there is a need for more accurate models in order to help investors get as many information as they could. Today information is one of the most important resources and financial models should keep up with this trend.

  17. The lod score method.

    Rice, J P; Saccone, N L; Corbett, J

    2001-01-01

    The lod score method originated in a seminal article by Newton Morton in 1955. The method is broadly concerned with issues of power and the posterior probability of linkage, ensuring that a reported linkage has a high probability of being a true linkage. In addition, the method is sequential, so that pedigrees or lod curves may be combined from published reports to pool data for analysis. This approach has been remarkably successful for 50 years in identifying disease genes for Mendelian disorders. After discussing these issues, we consider the situation for complex disorders, where the maximum lod score (MLS) statistic shares some of the advantages of the traditional lod score approach but is limited by unknown power and the lack of sharing of the primary data needed to optimally combine analytic results. We may still learn from the lod score method as we explore new methods in molecular biology and genetic analysis to utilize the complete human DNA sequence and the cataloging of all human genes.

  18. Advances in iterative methods

    Beauwens, B.; Arkuszewski, J.; Boryszewicz, M.

    1981-01-01

    Results obtained in the field of linear iterative methods within the Coordinated Research Program on Transport Theory and Advanced Reactor Calculations are summarized. The general convergence theory of linear iterative methods is essentially based on the properties of nonnegative operators on ordered normed spaces. The following aspects of this theory have been improved: new comparison theorems for regular splittings, generalization of the notions of M- and H-matrices, new interpretations of classical convergence theorems for positive-definite operators. The estimation of asymptotic convergence rates was developed with two purposes: the analysis of model problems and the optimization of relaxation parameters. In the framework of factorization iterative methods, model problem analysis is needed to investigate whether the increased computational complexity of higher-order methods does not offset their increased asymptotic convergence rates, as well as to appreciate the effect of standard relaxation techniques (polynomial relaxation). On the other hand, the optimal use of factorization iterative methods requires the development of adequate relaxation techniques and their optimization. The relative performances of a few possibilities have been explored for model problems. Presently, the best results have been obtained with optimal diagonal-Chebyshev relaxation

  19. Independent random sampling methods

    Martino, Luca; Míguez, Joaquín

    2018-01-01

    This book systematically addresses the design and analysis of efficient techniques for independent random sampling. Both general-purpose approaches, which can be used to generate samples from arbitrary probability distributions, and tailored techniques, designed to efficiently address common real-world practical problems, are introduced and discussed in detail. In turn, the monograph presents fundamental results and methodologies in the field, elaborating and developing them into the latest techniques. The theory and methods are illustrated with a varied collection of examples, which are discussed in detail in the text and supplemented with ready-to-run computer code. The main problem addressed in the book is how to generate independent random samples from an arbitrary probability distribution with the weakest possible constraints or assumptions in a form suitable for practical implementation. The authors review the fundamental results and methods in the field, address the latest methods, and emphasize the li...

  20. Grid generation methods

    Liseikin, Vladimir D

    2017-01-01

    This new edition provides a description of current developments relating to grid methods, grid codes, and their applications to actual problems. Grid generation methods are indispensable for the numerical solution of differential equations. Adaptive grid-mapping techniques, in particular, are the main focus and represent a promising tool to deal with systems with singularities. This 3rd edition includes three new chapters on numerical implementations (10), control of grid properties (11), and applications to mechanical, fluid, and plasma related problems (13). Also the other chapters have been updated including new topics, such as curvatures of discrete surfaces (3). Concise descriptions of hybrid mesh generation, drag and sweeping methods, parallel algorithms for mesh generation have been included too. This new edition addresses a broad range of readers: students, researchers, and practitioners in applied mathematics, mechanics, engineering, physics and other areas of applications.

  1. Bayesian methods in reliability

    Sander, P.; Badoux, R.

    1991-11-01

    The present proceedings from a course on Bayesian methods in reliability encompasses Bayesian statistical methods and their computational implementation, models for analyzing censored data from nonrepairable systems, the traits of repairable systems and growth models, the use of expert judgment, and a review of the problem of forecasting software reliability. Specific issues addressed include the use of Bayesian methods to estimate the leak rate of a gas pipeline, approximate analyses under great prior uncertainty, reliability estimation techniques, and a nonhomogeneous Poisson process. Also addressed are the calibration sets and seed variables of expert judgment systems for risk assessment, experimental illustrations of the use of expert judgment for reliability testing, and analyses of the predictive quality of software-reliability growth models such as the Weibull order statistics.

  2. Energy methods in dynamics

    Le, Khanh Chau

    2012-01-01

    The above examples should make clear the necessity of understanding the mechanism of vibrations and waves in order to control them in an optimal way. However vibrations and waves are governed by differential equations which require, as a rule, rather complicated mathematical methods for their analysis. The aim of this textbook is to help students acquire both a good grasp of the first principles from which the governing equations can be derived, and the adequate mathematical methods for their solving. Its distinctive features, as seen from the title, lie in the systematic and intensive use of Hamilton's variational principle and its generalizations for deriving the governing equations of conservative and dissipative mechanical systems, and also in providing the direct variational-asymptotic analysis, whenever available, of the energy and dissipation for the solution of these equations. It will be demonstrated that many well-known methods in dynamics like those of Lindstedt-Poincare, Bogoliubov-Mitropolsky, Ko...

  3. Nuclear methods for tribology

    Racolta, P.M.

    1994-01-01

    The tribological field of activity is mainly concerned with the relative movement of different machine components, friction and wear phenomena and their dependence upon lubrication. Tribological studies on friction and wear processes are important because they lead to significant parameter-improvements of engineering tools and machinery components. A review of fundamental aspects of both friction and wear phenomena is presented. A number of radioindicator-based methods have been known for almost four decades, differing mainly with respect to the mode of introducing the radio-indicators into the machine part to be studied. All these methods briefly presented in this paper are based on the measurement of the activity of wear products and therefore require high activity levels of the part. For this reason, such determinations can be carried out only in special laboratories and under conditions which do not usually agree with the conditions of actual use. What is required is a sensitive, fast method allowing the determination of wear under any operating conditions, without the necessity of stopping and disassembling the machine. The above mentioned requirements are the features that have made the Thin Layer Activation technique (TLA) the most widely used method applied in wear and corrosion studies in the last two decades. The TLA principle, taking in account that wear and corrosion processes are characterised by a loss of material, consists in an ion beam irradiation of a well defined volume of a machine part subjected to wear. The radioactivity level changes can usually be measured by gamma-ray spectroscopy methods. A review of both main TLA fields of application in major laboratories abroad and of those performed at the U-120 cyclotron of I.P.N.E.-Bucharest together with the existing trends to extend other nuclear analytical methods to tribological studies is presented as well. (author). 25 refs., 6 figs., 2 tabs

  4. Methods for pretreating biomass

    Balan, Venkatesh; Dale, Bruce E; Chundawat, Shishir; Sousa, Leonardo

    2017-05-09

    A method for pretreating biomass is provided, which includes, in a reactor, allowing gaseous ammonia to condense on the biomass and react with water present in the biomass to produce pretreated biomass, wherein reactivity of polysaccharides in the biomass is increased during subsequent biological conversion as compared to the reactivity of polysaccharides in biomass which has not been pretreated. A method for pretreating biomass with a liquid ammonia and recovering the liquid ammonia is also provided. Related systems which include a biochemical or biofuel production facility are also disclosed.

  5. Exploring Monte Carlo methods

    Dunn, William L

    2012-01-01

    Exploring Monte Carlo Methods is a basic text that describes the numerical methods that have come to be known as "Monte Carlo." The book treats the subject generically through the first eight chapters and, thus, should be of use to anyone who wants to learn to use Monte Carlo. The next two chapters focus on applications in nuclear engineering, which are illustrative of uses in other fields. Five appendices are included, which provide useful information on probability distributions, general-purpose Monte Carlo codes for radiation transport, and other matters. The famous "Buffon's needle proble

  6. Research on teaching methods.

    Oermann, M H

    1990-01-01

    Research on teaching methods in nursing education was categorized into studies on media, CAI, and other nontraditional instructional strategies. While the research differed, some generalizations may be made from the findings. Multimedia, whether it is used for individual or group instruction, is at least as effective as traditional instruction (lecture and lecture-discussion) in promoting cognitive learning, retention of knowledge, and performance. Further study is needed to identify variables that may influence learning and retention. While learner attitudes toward mediated instruction tended to be positive, investigators failed to control for the effect of novelty. Control over intervening variables was lacking in the majority of studies as well. Research indicated that CAI is as effective as other teaching methods in terms of knowledge gain and retention. Attitudes toward CAI tended to be favorable, with similar problems in measurement as those evidenced in studies of media. Chang (1986) also recommends that future research examine the impact of computer-video interactive instruction on students, faculty, and settings. Research is needed on experimental teaching methods, strategies for teaching problem solving and clinical judgment, and ways of improving the traditional lecture and discussion. Limited research in these areas makes generalizations impossible. There is a particular need for research on how to teach students the diagnostic reasoning process and encourage critical thinking, both in terms of appropriate teaching methods and the way in which those strategies should be used. It is interesting that few researchers studied lecture and lecture-discussion except as comparable teaching methods for research on other strategies. Additional research questions may be generated on lecture and discussion in relation to promoting concept learning, an understanding of nursing and other theories, transfer of knowledge, and development of cognitive skills. Few

  7. Carbon 14 dating method

    Fortin, Ph.

    2000-01-01

    This document gives a first introduction to 14 C dating as it is put into practice at the radiocarbon dating centre of Claude-Bernard university (Lyon-1 univ., Villeurbanne, France): general considerations and recalls of nuclear physics; the 14 C dating method; the initial standard activity; the isotopic fractioning; the measurement of samples activity; the liquid-scintillation counters; the calibration and correction of 14 C dates; the preparation of samples; the benzene synthesis; the current applications of the method. (J.S.)

  8. Methods of Multivariate Analysis

    Rencher, Alvin C

    2012-01-01

    Praise for the Second Edition "This book is a systematic, well-written, well-organized text on multivariate analysis packed with intuition and insight . . . There is much practical wisdom in this book that is hard to find elsewhere."-IIE Transactions Filled with new and timely content, Methods of Multivariate Analysis, Third Edition provides examples and exercises based on more than sixty real data sets from a wide variety of scientific fields. It takes a "methods" approach to the subject, placing an emphasis on how students and practitioners can employ multivariate analysis in real-life sit

  9. Tautomerism methods and theories

    Antonov, Liudmil

    2013-01-01

    Covering the gap between basic textbooks and over-specialized scientific publications, this is the first reference available to describe this interdisciplinary topic for PhD students and scientists starting in the field. The result is an introductory description providing suitable practical examples of the basic methods used to study tautomeric processes, as well as the theories describing the tautomerism and proton transfer phenomena. It also includes different spectroscopic methods for examining tautomerism, such as UV-VIs, time-resolved fluorescence spectroscopy, and NMR spectrosc

  10. Speeding Fermat's factoring method

    McKee, James

    A factoring method is presented which, heuristically, splits composite n in O(n^{1/4+epsilon}) steps. There are two ideas: an integer approximation to sqrt(q/p) provides an O(n^{1/2+epsilon}) algorithm in which n is represented as the difference of two rational squares; observing that if a prime m divides a square, then m^2 divides that square, a heuristic speed-up to O(n^{1/4+epsilon}) steps is achieved. The method is well-suited for use with small computers: the storage required is negligible, and one never needs to work with numbers larger than n itself.

  11. High frequency asymptotic methods

    Bouche, D.; Dessarce, R.; Gay, J.; Vermersch, S.

    1991-01-01

    The asymptotic methods allow us to compute the interaction of high frequency electromagnetic waves with structures. After an outline of their foundations with emphasis on the geometrical theory of diffraction, it is shown how to use these methods to evaluate the radar cross section (RCS) of complex tri-dimensional objects of great size compared to the wave-length. The different stages in simulating phenomena which contribute to the RCS are reviewed: physical theory of diffraction, multiple interactions computed by shooting rays, research for creeping rays. (author). 7 refs., 6 figs., 3 insets

  12. Practical methods of optimization

    Fletcher, R

    2013-01-01

    Fully describes optimization methods that are currently most valuable in solving real-life problems. Since optimization has applications in almost every branch of science and technology, the text emphasizes their practical aspects in conjunction with the heuristics useful in making them perform more reliably and efficiently. To this end, it presents comparative numerical studies to give readers a feel for possibile applications and to illustrate the problems in assessing evidence. Also provides theoretical background which provides insights into how methods are derived. This edition offers rev

  13. Electrorheological fluids and methods

    Green, Peter F.; McIntyre, Ernest C.

    2015-06-02

    Electrorheological fluids and methods include changes in liquid-like materials that can flow like milk and subsequently form solid-like structures under applied electric fields; e.g., about 1 kV/mm. Such fluids can be used in various ways as smart suspensions, including uses in automotive, defense, and civil engineering applications. Electrorheological fluids and methods include one or more polar molecule substituted polyhedral silsesquioxanes (e.g., sulfonated polyhedral silsesquioxanes) and one or more oils (e.g., silicone oil), where the fluid can be subjected to an electric field.

  14. Method of sterilization

    Peel, J.L.; Waites, W.M.

    1981-01-01

    A method of sterilisation of food packaging is described which comprises treating microorganisms with an ultraviolet irradiated solution of hydrogen peroxide to render the microorganisms non-viable. The wavelength of ultraviolet radiation used is wholly or predominantly below 325 nm and the concentration of the hydrogen peroxide is no greater than 10% by weight. The method is applicable to a wide variety of microorganisms including moulds, yeasts, bacteria, viruses and protozoa and finds particular application in the destruction of spore-forming bacteria, especially those which are dairy contaminants. (U.K.)

  15. Unorthodox theoretical methods

    Nedd, Sean [Iowa State Univ., Ames, IA (United States)

    2012-01-01

    The use of the ReaxFF force field to correlate with NMR mobilities of amine catalytic substituents on a mesoporous silica nanosphere surface is considered. The interfacing of the ReaxFF force field within the Surface Integrated Molecular Orbital/Molecular Mechanics (SIMOMM) method, in order to replicate earlier SIMOMM published data and to compare with the ReaxFF data, is discussed. The development of a new correlation consistent Composite Approach (ccCA) is presented, which incorporates the completely renormalized coupled cluster method with singles, doubles and non-iterative triples corrections towards the determination of heats of formations and reaction pathways which contain biradical species.

  16. Monte Carlo methods

    Bardenet Rémi

    2013-07-01

    Full Text Available Bayesian inference often requires integrating some function with respect to a posterior distribution. Monte Carlo methods are sampling algorithms that allow to compute these integrals numerically when they are not analytically tractable. We review here the basic principles and the most common Monte Carlo algorithms, among which rejection sampling, importance sampling and Monte Carlo Markov chain (MCMC methods. We give intuition on the theoretical justification of the algorithms as well as practical advice, trying to relate both. We discuss the application of Monte Carlo in experimental physics, and point to landmarks in the literature for the curious reader.

  17. The SPH homogeneization method

    Kavenoky, Alain

    1978-01-01

    The homogeneization of a uniform lattice is a rather well understood topic while difficult problems arise if the lattice becomes irregular. The SPH homogeneization method is an attempt to generate homogeneized cross sections for an irregular lattice. Section 1 summarizes the treatment of an isolated cylindrical cell with an entering surface current (in one velocity theory); Section 2 is devoted to the extension of the SPH method to assembly problems. Finally Section 3 presents the generalisation to general multigroup problems. Numerical results are obtained for a PXR rod bundle assembly in Section 4

  18. Splines and variational methods

    Prenter, P M

    2008-01-01

    One of the clearest available introductions to variational methods, this text requires only a minimal background in calculus and linear algebra. Its self-contained treatment explains the application of theoretic notions to the kinds of physical problems that engineers regularly encounter. The text's first half concerns approximation theoretic notions, exploring the theory and computation of one- and two-dimensional polynomial and other spline functions. Later chapters examine variational methods in the solution of operator equations, focusing on boundary value problems in one and two dimension

  19. Probabilistic methods for physics

    Cirier, G

    2013-01-01

    We present an asymptotic method giving a probability of presence of the iterated spots of R d by a polynomial function f. We use the well-known Perron Frobenius operator (PF) that lets certain sets and measure invariant by f. Probabilistic solutions can exist for the deterministic iteration. If the theoretical result is already known, here we quantify these probabilities. This approach seems interesting to use for computing situations when the deterministic methods don't run. Among the examined applications, are asymptotic solutions of Lorenz, Navier-Stokes or Hamilton's equations. In this approach, linearity induces many difficult problems, all of whom we have not yet resolved.

  20. METHOD OF ROLLING URANIUM

    Smith, C.S.

    1959-08-01

    A method is described for rolling uranium metal at relatively low temperatures and under non-oxidizing conditions. The method involves the steps of heating the uranium to 200 deg C in an oil bath, withdrawing the uranium and permitting the oil to drain so that only a thin protective coating remains and rolling the oil coated uranium at a temperature of 200 deg C to give about a 15% reduction in thickness at each pass. The operation may be repeated to accomplish about a 90% reduction without edge cracking, checking or any appreciable increase in brittleness.

  1. Supercritical fluid analytical methods

    Smith, R.D.; Kalinoski, H.T.; Wright, B.W.; Udseth, H.R.

    1988-01-01

    Supercritical fluids are providing the basis for new and improved methods across a range of analytical technologies. New methods are being developed to allow the detection and measurement of compounds that are incompatible with conventional analytical methodologies. Characterization of process and effluent streams for synfuel plants requires instruments capable of detecting and measuring high-molecular-weight compounds, polar compounds, or other materials that are generally difficult to analyze. The purpose of this program is to develop and apply new supercritical fluid techniques for extraction, separation, and analysis. These new technologies will be applied to previously intractable synfuel process materials and to complex mixtures resulting from their interaction with environmental and biological systems

  2. A flexible homework method

    Bao, Lei; Stonebraker, Stephen R.; Sadaghiani, Homeyra

    2008-09-01

    The traditional methods of assigning and grading homework in large enrollment physics courses have raised concerns among many instructors and students. In this paper we discuss a cost-effective approach to managing homework that involves making half of the problem solutions available to students before the homework is due. In addition, students are allowed some control in choosing which problems to solve. This paper-based approach to homework provides more detailed and timely support to students and increases the amount of self-direction in the homework process. We describe the method and present preliminary results on how students have responded.

  3. Molecular methods for biofilms

    Ferrera, Isabel; Balagué , Vanessa; Voolstra, Christian R.; Aranda, Manuel; Bayer, Till; Abed, Raeid M.M.; Dobretsov, Sergey; Owens, Sarah M.; Wilkening, Jared; Fessler, Jennifer L.; Gilbert, Jack A.

    2014-01-01

    This chapter deals with both classical and modern molecular methods that can be useful for the identification of microorganisms, elucidation and comparison of microbial communities, and investigation of their diversity and functions. The most important and critical steps necessary for all molecular methods is DNA isolation from microbial communities and environmental samples; these are discussed in the first part. The second part provides an overview over DNA polymerase chain reaction (PCR) amplification and DNA sequencing methods. Protocols and analysis software as well as potential pitfalls associated with application of these methods are discussed. Community fingerprinting analyses that can be used to compare multiple microbial communities are discussed in the third part. This part focuses on Denaturing Gradient Gel Electrophoresis (DGGE), Terminal Restriction Fragment Length Polymorphism (T-RFLP) and Automated rRNA Intergenic Spacer Analysis (ARISA) methods. In addition, classical and next-generation metagenomics methods are presented. These are limited to bacterial artificial chromosome and Fosmid libraries and Sanger and next-generation 454 sequencing, as these methods are currently the most frequently used in research. Isolation of nucleic acids: This chapter discusses, the most important and critical steps necessary for all molecular methods is DNA isolation from microbial communities and environmental samples. Nucleic acid isolation methods generally include three steps: cell lysis, removal of unwanted substances, and a final step of DNA purification and recovery. The first critical step is the cell lysis, which can be achieved by enzymatic or mechanical procedures. Removal of proteins, polysaccharides and other unwanted substances is likewise important to avoid their interference in subsequent analyses. Phenol-chloroform-isoamyl alcohol is commonly used to recover DNA, since it separates nucleic acids into an aqueous phase and precipitates proteins and

  4. Molecular methods for biofilms

    Ferrera, Isabel

    2014-08-30

    This chapter deals with both classical and modern molecular methods that can be useful for the identification of microorganisms, elucidation and comparison of microbial communities, and investigation of their diversity and functions. The most important and critical steps necessary for all molecular methods is DNA isolation from microbial communities and environmental samples; these are discussed in the first part. The second part provides an overview over DNA polymerase chain reaction (PCR) amplification and DNA sequencing methods. Protocols and analysis software as well as potential pitfalls associated with application of these methods are discussed. Community fingerprinting analyses that can be used to compare multiple microbial communities are discussed in the third part. This part focuses on Denaturing Gradient Gel Electrophoresis (DGGE), Terminal Restriction Fragment Length Polymorphism (T-RFLP) and Automated rRNA Intergenic Spacer Analysis (ARISA) methods. In addition, classical and next-generation metagenomics methods are presented. These are limited to bacterial artificial chromosome and Fosmid libraries and Sanger and next-generation 454 sequencing, as these methods are currently the most frequently used in research. Isolation of nucleic acids: This chapter discusses, the most important and critical steps necessary for all molecular methods is DNA isolation from microbial communities and environmental samples. Nucleic acid isolation methods generally include three steps: cell lysis, removal of unwanted substances, and a final step of DNA purification and recovery. The first critical step is the cell lysis, which can be achieved by enzymatic or mechanical procedures. Removal of proteins, polysaccharides and other unwanted substances is likewise important to avoid their interference in subsequent analyses. Phenol-chloroform-isoamyl alcohol is commonly used to recover DNA, since it separates nucleic acids into an aqueous phase and precipitates proteins and

  5. Software specification methods

    Habrias, Henri

    2010-01-01

    This title provides a clear overview of the main methods, and has a practical focus that allows the reader to apply their knowledge to real-life situations. The following are just some of the techniques covered: UML, Z, TLA+, SAZ, B, OMT, VHDL, Estelle, SDL and LOTOS.

  6. Leak detection method

    1978-01-01

    This invention provides a method for removing nuclear fuel elements from a fabrication building while at the same time testing the fuel elements for leaks without releasing contaminants from the fabrication building or from the fuel elements. The vacuum source used, leak detecting mechanism and fuel element fabrication building are specified to withstand environmental hazards. (UK)

  7. Photovoltaic device and method

    Cleereman, Robert J; Lesniak, Michael J; Keenihan, James R; Langmaid, Joe A; Gaston, Ryan; Eurich, Gerald K; Boven, Michelle L

    2015-01-27

    The present invention is premised upon an improved photovoltaic device ("PVD") and method of use, more particularly to an improved photovoltaic device with an integral locator and electrical terminal mechanism for transferring current to or from the improved photovoltaic device and the use as a system.

  8. Methods for Risk Analysis

    Alverbro, Karin

    2010-01-01

    Many decision-making situations today affect humans and the environment. In practice, many such decisions are made without an overall view and prioritise one or other of the two areas. Now and then these two areas of regulation come into conflict, e.g. the best alternative as regards environmental considerations is not always the best from a human safety perspective and vice versa. This report was prepared within a major project with the aim of developing a framework in which both the environmental aspects and the human safety aspects are integrated, and decisions can be made taking both fields into consideration. The safety risks have to be analysed in order to be successfully avoided and one way of doing this is to use different kinds of risk analysis methods. There is an abundance of existing methods to choose from and new methods are constantly being developed. This report describes some of the risk analysis methods currently available for analysing safety and examines the relationships between them. The focus here is mainly on human safety aspects

  9. HEV and cirrhosis: methods

    First page Back Continue Last page Overview Graphics. HEV and cirrhosis: methods. Study group. Patients with cirrhosis and recent jaundice for <30 d. Controls. Patients with liver cirrhosis but no recent worsening. Exclusions. Significant alcohol consumption. Recent hepatotoxic drugs. Recent antiviral therapy. Recent ...

  10. Method of killing microorganisms

    Tensmeyer, L.G.

    1980-01-01

    A method of sterilizing the contents of containers involves exposure to a plasma induced therein by focusing a high-power laser beam in an electromagnetic field preferably for a period of from 1.0 millisec to 1.0 secs. (U.K.)

  11. Method of signal analysis

    Berthomier, Charles

    1975-01-01

    A method capable of handling the amplitude and the frequency time laws of a certain kind of geophysical signals is described here. This method is based upon the analytical signal idea of Gabor and Ville, which is constructed either in the time domain by adding an imaginary part to the real signal (in-quadrature signal), or in the frequency domain by suppressing negative frequency components. The instantaneous frequency of the initial signal is then defined as the time derivative of the phase of the analytical signal, and his amplitude, or envelope, as the modulus of this complex signal. The method is applied to three types of magnetospheric signals: chorus, whistlers and pearls. The results obtained by analog and numerical calculations are compared to results obtained by classical systems using filters, i.e. based upon a different definition of the concept of frequency. The precision with which the frequency-time laws are determined leads then to the examination of the principle of the method and to a definition of instantaneous power density spectrum attached to the signal, and to the first consequences of this definition. In this way, a two-dimensional representation of the signal is introduced which is less deformed by the analysis system properties than the usual representation, and which moreover has the advantage of being obtainable practically in real time [fr

  12. TRAC methods and models

    Mahaffy, J.H.; Liles, D.R.; Bott, T.F.

    1981-01-01

    The numerical methods and physical models used in the Transient Reactor Analysis Code (TRAC) versions PD2 and PF1 are discussed. Particular emphasis is placed on TRAC-PF1, the version specifically designed to analyze small-break loss-of-coolant accidents

  13. The Prescribed Velocity Method

    Nielsen, Peter Vilhelm

    The- velocity level in a room ventilated by jet ventilation is strongly influenced by the supply conditions. The momentum flow in the supply jets controls the air movement in the room and, therefore, it is very important that the inlet conditions and the numerical method can generate a satisfactory...

  14. Immunocytochemical methods and protocols

    Javois, Lorette C

    1999-01-01

    ... monoclonal antibodies to study cell differentiation during embryonic development. For a select few disciplines volumes have been published focusing on the specific application of immunocytochemical techniques to that discipline. What distinguished Immunocytochemical Methods and Protocols from earlier books when it was first published four years ago was i...

  15. Adhesive compositions and methods

    Allen, Scott D.; Sendijarevic, Vahid; O'Connor, James

    2017-12-05

    The present invention encompasses polyurethane adhesive compositions comprising aliphatic polycarbonate chains. In one aspect, the present invention encompasses polyurethane adhesives derived from aliphatic polycarbonate polyols and polyisocyanates wherein the polyol chains contain a primary repeating unit having a structure:. In another aspect, the invention provides articles comprising the inventive polyurethane compositions as well as methods of making such compositions.

  16. Ferrari's Method and Technology

    Althoen, Steve

    2005-01-01

    Some tips that combine knowledge of mathematics history and technology for adapting Ferrar's method to factor quintics with a TI-83 graphing calculator are presented. A demonstration on the use of the root finder and regression capabilities of the graphing calculator are presented, so that the tips can be easily adapted for any graphing calculator…

  17. Truth and Methods.

    Dasenbrock, Reed Way

    1995-01-01

    Examines literary theory's displacing of "method" in the New Historicist criticism. Argues that Stephen Greenblatt and Lee Paterson imply that no objective historical truth is possible and as a result do not give methodology its due weight in their criticism. Questions the theory of "truth" advanced in this vein of literary…

  18. Sparse Classification - Methods & Applications

    Einarsson, Gudmundur

    for analysing such data carry the potential to revolutionize tasks such as medical diagnostics where often decisions need to be based on only a few high-dimensional observations. This explosion in data dimensionality has sparked the development of novel statistical methods. In contrast, classical statistics...

  19. Method of complex scaling

    Braendas, E.

    1986-01-01

    The method of complex scaling is taken to include bound states, resonances, remaining scattering background and interference. Particular points of the general complex coordinate formulation are presented. It is shown that care must be exercised to avoid paradoxical situations resulting from inadequate definitions of operator domains. A new resonance localization theorem is presented

  20. Alternative methods in criticality

    Pedicini, J.M.

    1982-01-01

    In this thesis two new methods of calculating the criticality of a nuclear system are introduced and verified. Most methods of determining the criticality of a nuclear system depend implicitly upon knowledge of the angular flux, net currents, or moments of the angular flux, on the system surface in order to know the leakage. For small systems, leakage is the predominant element in criticality calculations. Unfortunately, in these methods the least accurate fluxes, currents, or moments are those occurring near system surfaces or interfaces. This is due to a mathematical inability to satisfy rigorously with a finite order angular polynomial expansion or angular difference technique the physical boundary conditions which occur on these surfaces. Consequently, one must accept large computational effort or less precise criticality calculations. The methods introduced in this thesis, including a direct leakage operator and an indirect multiple scattering leakage operator, obviate the need to know angular fluxes accurately at system boundaries. Instead, the system wide scalar flux, an integral quantity which is substantially easier to obtain with good precision is sufficient to obtain production, absorption, scattering, and leakage rates