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\n 31_P-XRF<\/b> \/ An improved method for Ed-XRF background subtraction\n <\/div>\n
\n Paula Rangel Pestana Allegro\n <\/div>\n <\/div>\n
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\n Energy dispersive X-ray fluorescence (ED-XRF) is a versatile tool to qualitatively and quantitatively determine major, minor and trace elements in different materials, such as glasses [1], metals [2], biological materials [3] paintings [4], etc. Without taking samples of the analysed material, it is possible to determine which elements are present in the material and, in some cases, also determine their concentrations. However, the background due to Compton and Rayleigh scatterings and due the interaction between the characteristic X-rays of the material and the detecting instrument has a significant effect on the detection limits and precision, especially for the trace elements [5]. Several methods have been proposed to estimate and subtract the background from the X-ray spectra, such as stripping peaks to fit the background [6], orthogonal polynomial decomposition [7], the least squares method [8], wavelet analysis [9] and cubic spline interpolation [10]. With the exception of the cubic spline interpolation, the above methods are not suitable for automated batched analysing spectra, since they require user assisted iterative calculations. The cubic spline interpolation can be automated, however, it does not take into account the correct subtraction of two neighbouring peaks separated by less than 2 times the detector resolution. In this work we propose an alternative method of automated background subtraction based on the preconditioning of the interpolating background points by removing the intermediate minima of under-resolved close maxima and requiring monotonicity of each interpolant. The new method presents an improvement of existing ones in cases where consecutive peaks are not well spaced and the fluorescence background cannot be well approximated by known functions. We have tested the method in a real case of X-ray spectra measured in the painting "Natura Morta" (1946), by Mario Mafai.\r\n\r\n[1] M. Hlo\u017eek, T. Trojek, Radiat. Phys. Chem. 116 (2015) 332.\r\n[2] F. Bilo et al., Appl. Surf. Sci. 359 (2015) 215. \r\n[3] X. Li, Z. Yu, Appl. Radiat. Isot. 111 (2016) 45.\r\n[4] T. Trojek, D. Trojková, , Radiat. Phys. Chem. 116 (2015) 321.\r\n[5] R. M. Rousseau, Rigaku J. 18 (2001) 33\r\n[6] CG Clayton, R. Spackman, Nucl Geophys 1 (1987) 25.\r\n[7] S. Steenstrup, J Appl Crystallogr 14 (1981) 226.\r\n[8] B. Vekemans et al., X\u2010Ray Spectrom 23 (1994) 278. \r\n[9] P. Bury et al., Nucl Instrum Methods Phys Res Sect A 383 (1996) 572.\r\n[10] L. Yi et al., Nuclear Instruments and Methods in Physics Research A 775 (2015) 12. \n <\/div>\n <\/div>\n<\/div>\n
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\n 26_P-XRF<\/b> \/ ANÁLISE MULTIELEMENTAR EM AMOSTRAS DE SOLO COM EMPREGO DE EDXRF\n <\/div>\n
\n Marialina Sá da Silva\n <\/div>\n <\/div>\n
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\n O descarte inadequado de resíduos sólidos é um problema para a sociedade e a situação agrava-se em países subdesenvolvidos e\/ ou em desenvolvimento, como o Brasil. Considerando o depósito de lixo sobre o solo, o objetivo deste trabalho é caracterizar qualitativa e quantitativamente a composição de cinco amostras de solo coletadas em uma área específica utilizada para descarte de lixo como depósito ou área de transbordo há pelo menos duas décadas. Para identificar elementos contaminantes, como metais pesados, foi selecionada uma amostra de solo para controle, coletada na mesma região, porém onde nunca houve contato com resíduos sólidos descartados. A amostra controle permite determinar as especificidades do solo padrão da região de interesse. Todas as amostras de solo foram coletadas superficialmente a uma profundidade máxima de 5 cm e acondicionadas em estufa a 60ºC por 8 horas. A partir daí, foram moídas manualmente e totalmente peneiradas a fim de se alcançar a homogeneidade das partículas em 75 µm. Retornando as amostras para a estufa, aplicou-se um processo de secagem a 60ºC por cerca de 30 horas. Para a análise por Fluorescência de Raios X foi empregado um sistema portátil de EDXRF, que consiste de um mini tubo de raio X de baixa potência com anodo de prata (Ag) operando em 15 (baixo Z) e-35 keV (alto Z)\/100 µA e um detector de silício (Si). Para a análise, 500 mg de massa composto por parcelas de 300 mg de amostra e 200 mg de ácido bórico (H3BO3), foram prensadas a aproximadamente 200 MPa por cerca de 15 minutos a fim de se obter pastilhas finas com diâmetro de 2,54 centímetros e densidade superficial de 100 mg\/ cm². Foram detectados dezesseis elementos: K, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Br, Rb, Sr, Zr, Nb e Pb. A fração mássica dos elementos varia discretamente e para determinar a concentração destes foi realizado um cálculo considerando a Intensidade da Radiação, a Absorção da Amostra, a Sensibilidade do Sistema, entre outros parâmetros. O estudo do nível do acúmulo de poluição no solo através da técnica de EDXRF revelou-se como uma técnica de baixo custo e eficiente na determinação da concentração elementar dos poluentes. \n <\/div>\n <\/div>\n<\/div>\n
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\n 25_P-XRF<\/b> \/ Analysis of collimators made of different materials through Monte Carlo simulation for a total reflection X-ray fluorescence spectrometry system\n <\/div>\n
\n Marcio Henrique dos Santos\n <\/div>\n <\/div>\n
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\n In 2014, Costa et al. developed a total reflection X-ray fluorescence portable spectrometer at Nuclear Instrumentation Laboratory (COPPE\/UFRJ-Brazil). This spectrometer includes a lucite collimator with optical properties in its system. The presence of lucite with this feature tends to improve the nature of a traditional collimator. In this case, the adequacy of the transmitted beam geometry joins the increasing intensity on account of total reflections that can happen in lucite, thus minimizing the possibility of scattering or refraction. The goal of the paper is to verify that this lucite collimator with optical properties can be called “optimized collimator”. To do so, it compares the intensities of the beams transmitted for five collimators with the same geometrical definition but each with a specific chemical composition: aluminum, lead, lucite without optical properties, lucite with optical properties, and finally, a trio of lead slits. The analysis was done by simulating each case and based on 10^8 events for each one. The results showed that the intensities of direct transmission (without interaction with any medium) are similar as a reference. Thus, the spreading percentage (elastic plus inelastic plus refraction) that were transmitted by the collimators were 0.62%, 0.09% e 14.36% for aluminum, lead, and lucite, respectively. And the beam spread percentage by total reflection and which was transmitted by the collimator was 60.79% for lucite with optical properties. As a conclusion of this analysis, it can be said that the lucite with optical properties makes the most efficient collimator, increasing the intensity of the transmitted beam around 60%, surpassing the other collimators (without optical properties) and thus justifying its use in the total reflection X-ray fluorescence spectrometry system.\n <\/div>\n <\/div>\n<\/div>\n
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\n 34_P-XRF<\/b> \/ ANALYSIS OF METALS IN AIR SAMPLES USING APDC PRECONCENTRATION AND X-RAY FLUORESCENCE TECHNIQUE\n <\/div>\n
\n Raysa Costa Nardes\n <\/div>\n <\/div>\n
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\n Air pollution has become one of the leading quality degradation factors of life for people in large urban centers. Studies indicate that the suspended particulate matter in the atmosphere is directly associated with risks to public health, in addition, it can cause damage to fauna, flora and public \/ cultural patrimonies. The inhalable particulate materials can cause the emergence and \/ or worsening of chronic diseases related to respiratory system and other diseases, such as reduced physical strength. In this study, we propose a new method to measure the concentration of total suspended particulate matter (TSP) in the air using an impinger as an air cleaning apparatus. Thus, the heavy metals analysis was performed using APDC preconcentratin and Total Reflection X-ray Fluorescence technique (TXRF). The samples were collected from five random points in the city of Rio de Janeiro\/Brazil. Analyses of TXRF were performed at the Brazilian Synchrotron Light Laboratory (LNLS). The technique proved viable because it was able to detect five important metallic elements to environmental studies: Cr, Fe, Ni, Cu and Zn. This technique presented substantial efficiency in determining the elementary concentration of air pollutants, in addition to low cost. It can be concluded that the metals analysis technique in air samples using an impinger as sample collection instrument associated with a complexing agent (APDC) was viable because it is a low-cost technique, moreover, it was possible the detection of five important metal elements in environmental studies associated with industrial emissions and urban traffic.\n <\/div>\n <\/div>\n<\/div>\n
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\n 32_P-XRF<\/b> \/ CARACTERIZAÇÃO DE PIGMENTOS EM DUAS AMOSTRAS DE VALOR HISTÓRICO-CULTURAL UTILIZANDO UM SISTEMA PORTÁTIL DE FLUORESCÊNCIA DE RAIOS X\n <\/div>\n
\n Ramon Silva dos Santos\n <\/div>\n <\/div>\n
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\n O estudo dos pigmentos utilizados na composição de pinturas em uma variedade de materiais é extremamente importante na Arqueometria. Além disto, a caracterização de pigmentos pode auxiliar no estabelecimento de uma provável data para a pintura, reconstruindo sua história, processos de restauro antigos, técnicas que possam ter sido utilizadas em sua conservação e, ainda, detectando possíveis falsificações. Assim, o objetivo deste estudo foi realizar a análise de pigmentos em duas obras em suporte sobre papel de valor histórico-cultural, usando um sistema portátil de Fluorescência de Raios X (35 kV, 50 μA e tempos de aquisição do espectro de 300 s). As amostras analisadas foram: uma Planta Urbanística de Petrópolis de1846 e um croqui topográfico da Grande Medição Judicial de 1762. Os resultados mostraram que foi possível obter uma assinatura para cada uma das amostras analisada a partir dos espectros de fluorescência de Raios X obtidos associados às regiões com e sem pigmentos. No caso da Planta Urbanística de Petrópolis de1846 os resultados obtidos mostram que os pigmentos pretos apresentaram evidência de terem origem nas tintas ferrogálicas. Os pigmentos azuis provavelmente estariam associados a presença de cobre na tinta utilizada. Por outro lado, as regiões descoloradas também apresentaram evidências de pigmentação azul (predominância do elemento cobre nos pigmentos). Os pigmentos amarelos apresentaram predominância dos elementos Ti e Zn. Além disso, nas regiões restauradas foram encontradas assinaturas de Zn, Ba e Pb. No caso da análise de pigmentos no Croqui topográfico da Grande Medição Judicial de 1762 os resultados indicam fortemente que as tintas utilizadas nos desenhos e linhas no Croqui topográfico são oriundas de tintas Ferrogálicas.\n <\/div>\n <\/div>\n<\/div>\n
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\n 29_P-XRF<\/b> \/ CHARACTERIZATION OF YELLOW AND BLUE PIGMENTS BY X-RAY TECHNIQUES\n <\/div>\n
\n Natasha Fioretto Aguero\n <\/div>\n <\/div>\n
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\n Archeometry is an important area of analysis and characterization of materials, mainly those used in cultural heritage objects. Systematic analyzes with different archeometric methodologies in paintings allow studies on both the technique and the palette of a particular artist, and can assist in new and better preventive conservation and restoration practices.\r\nThe motivation for this work originated from problems related with pigments degradation, which have been presented by various works in recent years. Lead-based pigments can undergo a color change and in particular the photodegradation of the chrome yellow pigment (PbCrO4) has been discussed in literature [1]. This pigment usually presents itself in two crystalline forms: monoclinic and orthorhombic, each presenting different trends of degradation [1], hence the need to discriminate the crystal phases of this compound to better characterize it. Another yellow hue compound, cadmium yellow (CdS), can suffer degradation due to exposure to light [2]. Other white pigments and their mixtures also have reports of degradation processes, such as the titanium white used by Brazilian artist Candido Portinari [3].\r\nThis work presents results of our analyses of yellow and blue pigments from different manufacturers by the use of X-ray diffraction, X-ray fluorescence and Raman spectroscopy in order to better characterize and understand them. We will also present the reflectance results of the photodegradation process of some of these pigments, which was induced in the TGM line of the Brazilian Synchrotron Light Laboratory. All results are presented in comparison with the data in literature, as well as the inherent characteristics of each pigment are discussed.\r\n\r\n[1]“Degradation Process of Lead Chromate Yellows in Paintings by Vincent Van Gogh” Letizia Monico. PhD thesis. University of Antwerp and University of Perugia.\r\n[2]“Combined use of Synchrotron Radiation Based Micro-X-ray Fluorescence, Micro-X-ray Diffraction, Micro-X-ray Absorption Near-Edge, and Micro-Fourier Transform Infrared Spectroscopies for Revealing an Alternative Degradation Pathway of the Pigment Cadmium Yellow in a Painting by Van Gogh”, Geert Van der Snickt, Koen Janssens, Joris Dik, Wout De Nolf, Frederik Vanmeert, Jacub Jaroszewicz, Marine Cotte, Gerald Falkenberg, and Luuk Van der Loeff, Analytical Chemistry 2012 84 (23), 10221-10228.\r\n[3] “Material and Technical Studies of a Selected Group of Paintings by Candido Portinari, a Major Brazilian Modernist Painter”, A. Rosado, I. Mendes, E. Motta Jr., C. V. Teixeira, L. A. C. Souza, Book: Science and Art: The Painted Surface, The Royal Society of Chemistry, 2014.\r\n\r\nAcknowledgement: We are grateful for the financial support of FAPESP for this project and for the support of the IFUSP Crystallography Laboratory and the Brazilian Synchrotron Light Laboratory. \r\n\n <\/div>\n <\/div>\n<\/div>\n
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\n 27_P-XRF<\/b> \/ COMPARAÇÃO DAS TÉCNICAS DE XRF E XRD NA ANÁLISE DE MISTURA DE PIGMENTOS HISTÓRICOS \n <\/div>\n
\n Mariane Lucena da Silva\n <\/div>\n <\/div>\n
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\n A caracterização de pigmentos em obra de arte é de fundamental importância, para a compressão histórica e artística de uma obra, além de auxiliar na resolução de problemas relacionados com sua conservação, restauração, datação e autenticação. Atualmente a Fluorescência de Raios X (XRF) destaca-se como uma das técnicas mais empregadas neste tipo de investigação. No entanto, por tratar-se de uma técnica de análise elementar, esta pode fornecer resultados dúbios especialmente na análise de pigmentos cujas tonalidades são provenientes de misturas. Para estes casos torna-se fundamental a aplicação de técnicas complementares de análise. Para demostrar as limitações da XRF na análise de mistura de pigmentos, neste trabalho três pigmentos verdes e um pigmento laranja provenientes de misturas foram estudados através da Difração de Raios X (XRD) e XRF. As misturas foram produzidas a partir de pigmentos inorgânicos em pó. Para simular uma situação real as misturas foram diluídas em óleo de linhaça e seguindo métodos tradicionais de cromatização, foram pintadas sobre uma camada de preparação feita com branco de chumbo [2PbCO3.Pb(OH)2]. Para realizar as análises por XRD, uma tela foi depositada no porta-amostra do difratômetro e os pigmentos pintados sobre ela. As misturas foram investigadas utilizando o difratômetro modelo XRD-6000 da Shimadzu, com ânodo de cobre, operando com tensão de 30 kV e 40 mA. As análises de XRF foram realizadas no sistema modelo TRACER IV da Bruker, que possui ânodo de Rh, que foi ajustado com tensão de 40 kV e corrente de 10 μA. Os pigmentos foram produzidos a partir das seguintes misturas: (a) amarelo de Nápoles [Pb3(SbO4)2] + azul cobalto [(Co,Zn)2Al2O4] =verde; (b) amarelo ocre [α-FeOOH+argila+sílica] + azul da Prússia [Fe4[Fe(CN)6]314-16H2O] = verde; (c) amarelo de cromo [PbCrO4] + azul da Prússia = verde; (d) vermelho de chumbo [Pb3O4] + amarelo de cromo = laranja. Por ser uma técnica de análise elementar, a caracterização de pigmentos por XRF é a combinação dos elementos detectados no espectro com a tonalidade visível do pigmento. Portanto nos casos estudados não foi possível caracterizar os pigmentos originais, mas apenas possíveis pigmentos para cada caso (ex: verde cobalto [CoO.nZnO], terra verde [K [[Al,FeIII],[FeII,Mg][AlSi3,Si4]O10[OH]2], óxido de cromo [Cr2O3], laranja de cromo [PbCrO4.PbH2O], etc). Já os dados fornecidos pela XRD, permitiu caracterizar todos os componentes presente em cada uma das misturas. Os resultados indicam a necessidade da aplicação de múltiplas técnicas na investigação de pigmentos em obras de artes, além de comprovar a eficácia da XRD para este tipo de análise.\n <\/div>\n <\/div>\n<\/div>\n
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\n 24_P-XRF<\/b> \/ COMPARAÇÃO DE SIMULAÇÕES REALIZADAS NO GEANT4, MCNPX E XRMC\n <\/div>\n
\n Luiz Fernando Rosalba Telles de Sousa\n <\/div>\n <\/div>\n
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\n O presente trabalho apresenta os resultados da comparação entre os resultados obtidos nos programas de simulação da passagem de radiação através da matéria GEANT4 versão 10.1, XRMC versão 6.4 e MNCPX versão26e. São utilizados 1e8 eventos de raios X coplanares, monoenergéticos em 15 keV que incidem sobre a amostra simulada em um ângulo de 22,5º com a perpendicular à superfície de incidência. São comparados os espectros de simulações e as respectivas razões características entre os picos Kα\/Kβ de substratos de cobre e aço 1020 de espessura 1000 micrômetros com e sem revestimento de zinco com espessuras de 10 micrômetros. Para análise dos espectros foi utilizado como técnica de interpolação o método ajuste gaussiano deslocado e para cálculo da área sobre o gráfico o método de integração de Simpson composto com 1e4 pontos. A tabela 1 apresenta o resultado das comparações entre os programas. Os resultados se mostraram mais similares entre os programas GEANT4 e XRMC quando utilizadas as técnicas de análise propostas. \n <\/div>\n <\/div>\n<\/div>\n
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\n 33_P-XRF<\/b> \/ METALS BIOMONITORING AIR POLLUTION IN RIO DE JANEIRO CITY USING LEAVES OF NERIUM OLEANDER L. AND X-RAY FLUORESCENCE TECHNIQUE \n <\/div>\n
\n Ramon Silva dos Santos\n <\/div>\n <\/div>\n
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\n In this study, Nerium oleander L. leaves were used as biomonitors to evaluate the levels of environmental pollutants in a sub-region in the Metropolitan Area of Rio de Janeiro – Brazil through Energy Dispersive X-ray Fluorescence technique – EDXRF. The control samples were collected in the Parque Nacional da Pedra Branca\/RJ. The samples were collected during all seasons of 2013 (summer, fall, winter and spring). The EDXRF system consist of a portable XRF system formed by a mini X-ray tube of low power (anode of Ag and operated in 15 kV\/50 μA and 35 kV\/50 μA) and a SiPIN detector. It was determined the concentration of 11 elements: Cl, K, Ca, Mn, Fe, Cu, Zn, Br, Rb, Sr and Pb. The Pearson's correlation analysis shows a significant correlation between the elements Fe, Zn, and Pb; besides that, it shows a significant correlation between the elements Ca and Sr and a significant correlation between the elements Cl, K and Rb. The principal component analysis (PCA) showed the grouping of the elements in two main factors that can be associated to emission sources of these elements. The elements Cl, K, Ca, Cu, Rb and Sr can be associated as a possible influence from the soil (root uptake and\/or resuspension). On the other hand, the elements Fe, Cu, Zn, and Pb can be associated to vehicle and industry emission sources. Through the elemental concentration distribution maps, it was possible to verify the difference in the dispersion of these elements in sampling sites during the seasons. The study shows that the use of EDXRF technique associated to the Nerium oleander L. leaves used as biomonitor is efficient, precise, fast and low-cost option for air pollutants monitoring in Metropolitan Areas.\n <\/div>\n <\/div>\n<\/div>\n
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\n 19_P-XRD<\/b> \/ MICROSTRUCTURE OF EFV USING SYNCHROTRON AND CONVENTIONAL X-RAY DIFRACTION SOURCES\n <\/div>\n
\n Renata Guimarães\n <\/div>\n <\/div>\n
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\n Polymorphism and particle size distribution can impact the dissolution behaviour and, as a consequence,\r\nbioavailability and bioequivalence of poorly soluble drugs, such as Efavirenz (EFV). Nevertheless, these\r\ncharacteristics do not explain some failures occurring in in vitro assays and in in vivo studies. EFV\r\nbelongs to class II of the biopharmaceutics classification system and the high activity antiretroviral\r\ntherapy (HAART) is considered the best choice in the treatment of adults and children. In a previous\r\nstudy, Fandaruff et. al. demonstrated the biorrelevance of the microstructure (crystalline domain sizes) in\r\nEFV and the correlation between changes in dissolution properties and changes in crystallite size rather than\r\nparticle size [1]. The microstructure study of these samples was done using synchrotron radiation X-ray\r\ndiffraction at ELETTRA facility (Italy). The aim of this work is to expand the previous study of the effect of\r\nmicrostructure on different commercial raw materials and crystallized samples of EFV. A further extension\r\nof the method of crystallite size analysis to anisotropic crystallite shape and a reproducibility of the results obtained\r\nin X-ray diffraction experiments using synchrotron and conventional radiation sources are reported.\n <\/div>\n <\/div>\n<\/div>\n
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\n 28_P-XRF<\/b> \/ PIGMENTS ANALYSIS OF BARROQUE SCULPTURE OF XVIII CENTURY BY EDXRF¬¬¬\n <\/div>\n
\n Matheus Antonio Teixeira de Oliveira\n <\/div>\n <\/div>\n
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\n The identification of pigments on substrates like polychrome canvas and sculptures is very important for the comprehension of the history of a work of art, beyond, it helps to solve problems related to conservation, restoration and dating of the work. Nowadays, X-Ray Fluorescence (XRF) is the most employed analysis technique for pigment characterization in works of art. The frequent application of this technique is mainly due to the technological innovations which occurred in the last decade that enabled the construction of XRF portable systems, allowing elemental analysis in situ and non-destructive of a work of art with a good precision. In this work, analysis by XRF technique was employed, in little samples extracted from the São João Evangelista wood polychrome sculpture, which is lying in Santo Inácio School (Rio de Janeiro, Brazil). The statue is dated of the beginning of XVIII century was originally sculpted by unknown artists, for the Jesuits Church's altar builded at Castle's Hill in 1567, however with the Hill's overthrow, in 1922, the artworks were been saved at School's hall. The XRF analysis were made utilizing a portable model TRACER IV of Bruker, the spectrums were collected with operating system voltage 40kV and 10μA and 120 seconds of acquisition time. The results obtained of the samples extracted from the red mantle indicated the presence of Hg, it is a Vermilion pigment [HgS] key element. On the green samples extracted from the tunic were characterized Cu and Pb, these results associate with microstructure images taken from Optical Microscopy (OM), reveal that the green tone is from mixture of the pigments azurite [Cu(CO3)2(OH)2] and massicot [PbO]. Also were analysed golden sample extracted from the sculpture, in which was characterized Au by XRF, being such metal widely used in Brazilian sculptures of the period baroque. As the identified pigments and Au were widely utilized at the same period of the sculpture manufacture, the results reveal that the sculpture is consistent with its manufacturing period (XVII century) and does not have recent interventions. \n <\/div>\n <\/div>\n<\/div>\n
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\n 18_P-XRD<\/b> \/ REGION OF INTEREST IN ALVEOLAR BONE ANALYSIS USING X-RAY MICROTOMOGRAPHY\n <\/div>\n
\n Olga Maria Oliveira de Araújo\n <\/div>\n <\/div>\n
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\n X-ray microtomography has become the gold standard for evaluation of the architecture of trabecular bone, one of its main advantages is ability to provide quantitative results without destruction of the sample. Region of interest in evaluation studies of periodontal disease may be difficult, the selection is the interproximal region between the first and second molars in the jaw. Periodontal disease is characterized by an inflammatory process culminating in destruction of the supporting tissues of the teeth, (ie, gum, periodontal ligament and alveolar bone). The aim of this study is to analyse and compare the results between the selection of the interpolated region of interest with continuous and variable geometry for morphometric evaluation of alveolar bone using X-ray microtomography. The measurement results for bone area, total volume, porosity, bone mineral density in volumetric measurements, which are the most representative morphometric indices to detect the loss of alveolar bone in periodontal disease do not show large differences related to definition of the region of interest analysed, which validates the continuous interest region used despite the irregular nature of the region in the jaw.\n <\/div>\n <\/div>\n<\/div>\n
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\n 17_P-XRD<\/b> \/ SÍNTESIS Y CARACTERIZACIÓN CRISTALOGRÁFICA DEL COMPUESTO MoO2Br2-4,7-DIMETILFENANTROLINA\n <\/div>\n
\n Margareth Yaniry Barón Márquez\n <\/div>\n <\/div>\n
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\n El compuesto MoO2Br2-4,7-dimetilfenantrolina se obtuvo a partir de 290 mg de Na2MoO4 (1.2 equiv.) en 4mL de HBr (47%) y se agitó durante 10 minutos hasta que el sólido se disolvió totalmente y la solución adquirió una coloración amarilla, a la cual se adicionaron 15mL de éter etílico. Las fases se separaron con un embudo de extracción y este proceso se repitió 5 veces (10 mL de éter etílico) combinando las fases orgánicas sobre sulfato de sodio anhidro. La fase de éter etílico se adicionó lentamente sobre 208 mg de 4,7-dimetil-1,10-fenantrolina previamente disueltos en 50mL de acetona, la mezcla de reacción se mantuvo bajo agitación durante 3 horas a temperatura ambiente (Figura 1). La mezcla de reacción se filtró al vacío y el sólido obtenido se lavó varias veces con éter etílico obteniendo un sólido ligeramente amarillo [2].\r\nPosteriormente se realizó la caracterización estructural por difracción de rayos-X de muestras policristalinas, encontrando que el compuesto de interés cristaliza en el sistema monoclínico con constantes de celda celda: a = 23.782 (4) Å, b = 8.705 (2) Å, c = 9.815 (3) Å, ß = 99.3° (4) y V = 2005.36 Å3.\r\n\n <\/div>\n <\/div>\n<\/div>\n
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\n 30_P-XRF<\/b> \/ THE USE OF EDXRF TECHNIQUE TO STUDY PHOTOGRAPHICS AND PHOTOMECHANICS PROCESS\n <\/div>\n
\n Paula Aline Durães Almeida de Souza Santos\n <\/div>\n <\/div>\n
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\n Photographic and photochemical processes were important in the late nineteenth and early twentieth centuries, as they were routinely used to record images. During the manufacturing photographic processes it was common for some photographers to carry out toning with substances such as gold and selenium that guaranteed greater longevity to images recorded on paper with the objective to preserve it from the degradation under the effect of light. Several Museum collections present materials with different kinds of photomechanical and photographic processes and the studies of those supports were scarce. The Museu Paulista collection has a variety of iconographic materials (salt print, albumen paper, phototype among others) from the 19th , as well as good examples of postcards in several different print processes) Many of this iconographic materials were part of the 19th and 20th European tourist circuit. There are representations of cities, art and "sights" in the different kinds of print processes – carbon prints, rotogravures, half-tones, collotypes. Through this kind of documentation is possible understand the circuit of production and consumption of printed representations, associated with tourism practices in many cities of European countries – such as Germany, Spain, Italy and France. With the use of non-destructive techniques such as Energy Dispersive X-Ray Fluorescence - EDXRF, one can characterize the types of tonings that have occurred in the photographic prints, as well as identify them their different processes. The analyses led to the identification of both the type of photographic process and the different toning applied, such as gold or selenium toning. The identification of the use of different tonings is an example of the importance of EDXRF technique for the analysis of such materials. Thus, in this work we will present some results and the advantages of the use of non-destructive technique EDXRF to study different types of photographic and photochemical process that are available in the Museu Paulista collections. \n <\/div>\n <\/div>\n<\/div>\n"}