Program of SARX 2016

Na área de Ciência e Tecnologia os espalhamentos Rayleigh e Compton de raios X têm papel importante porque podem ser utilizados para caracterizar um material compósito através do seu número atômico efetivo (Zef). A importância do desenvolvimento desta metodologia estar relacionada à forma de se obter o Zef de um material e consequentemente o coeficiente de atenuação de massa (µ) por técnicas de espalhamento sem usar a transmissão de radiação. Isto é importante na região de baixas energias (E<30 keV) onde as técnicas de transmissão são inviáveis. O Zef e o µ são parâmetros importantes em várias aplicações tecnológicas, principalmente em dosimetria da radiações ionizantes e Física médica com fótons de baixa energias. Neste trabalho foram analisadas 128 amostras de polímeros; sendo 6 do tipo 1, 8 do tipo 2, 8 do tipo 3, 4 do tipo 4, 12 do tipo 5, 13 do tipo 6, 15 do tipo 7 e 62 polímeros com classificações desconhecidas. Todos os perfis de espalhamento foram obtidos num ângulo de espalhamento de 128 graus, usando um tubo de raios X com anodo de prata (35 kV e 100 µA) e um detector semicondutor do tipo SiDrift (SDD). A energia associada aos fótons do feixe incidente foi a linha Kα da Prata (22,16 keV). Foi mostrado que existe uma relação linear entre a razão R/C e Zef dos materiais analisados, principalmente, no intervalo de Zef de 6 – 14. Foram caracterizados nove polímeros pelo Zef e o coeficiente de atenuação de massa (µ). Polímeros do tipo 1, tipo 2, tipo 3, tipo 4, tipo 5, tipo 6, Teflón, EVA e acrílico. Além disso, foi possível caracterizar 73 % dos polímeros desconhecidos. Deste grupo foi possível classificar 6 polímeros como do tipo 1, 13 do tipo 2, 2 do tipo 3, 12 do tipo 4, 7 do tipo 5, 9 do tipo 6 e 14 do tipo 7 (acrílico). Não puderam ser classificados 17 polímeros por que a faixa de Zef (6,50 – 11,84) estava fora dos intervalos de confiança dos Zef dos polímeros estudados neste trabalho.

Crude oil is a complex matrix with the presence of several types of contaminants (metallorganic compounds, sulfur containing compounds, sediments, among others). The deleterious effects of metallorganic in petroleum are associated with poisoning of catalysts, equipment corrosion and toxic emissions to the atmosphere. On the other hand, their contents are used as geochemical oil origin markers and for classification. In this study, two methodologies of sample preparation (deposition on solid substrate and thin film) aiming the determination of V and Ni in oils have been studied, comparing different benchtop EDXRF spectrometer configurations and calibration approaches. The achieved results were compared to the ones obtained using the traditional direct analysis. The methodologies were validated by analysis of reference materials from NIST and ASTM proficiency test programs, whose results showed to be precise and accurate (Table 1). Unlike the usual sample preparation methods for the analysis of petroleum by XRF, AA, or ICP, the proposed methodologies require smaller amounts of sample and solvents, minimizing labor and cost of analysis.

Crude oil is a complex matrix containing different contaminants (for instance, metallorganic compounds, sulfur containing compounds, sediments and water). Al and S could be present in oil, at relevant quantities, mainly as finely divided solids. Evaluating the presence of water and sediments in crude oil is important as they bring problems during refining, equipment corrosion; irregular operation of the distillation unit; blocking of the heat exchangers and affect product quality. In X-ray fluorescence (XRF) spectrometry, the usual strategy to determine sulfur and metals in crude oil involves the use of organic standards in mineral oil, providing some degree of matrix matching. In this study, Energy Dispersive (ED) XRF spectrometry was used to develop a method to determinate silicon and aluminium in crude oil samples, using proper strategy as these elements are not present in samples as organic specimens. The analytical curves were prepared using: i) inorganic standards in lithium tetraborate (as in ASTM D5863) ii) organic standards in mineral oil. Both strategies used the standards (solution) in a solid substrate to measure the elements intensity. The results showed that the specimen form used as standards in calibration has a direct influence on the results obtained, indicating that such a study should always be performed when developing a XRF based method for crude oils. In Figure 1 it is shown the calibration curves for Al and Si using both calibration strategies and Table 1 contains the results obtained using both approaches for the analysis of ASTM proficiency test samples and for crude oil samples provided by Petrobras.

The analysis of trace elements in cancer research has gained interest in recent years due to reported correlations between abnormal concentrations and tumour growth. Quantitative topographic elemental studies using synchrotron µ-XRF enables investigations even at the single cell level, but it requires a proper sample preparing technique to ensure that the measured elemental distribution accurately reflects the spatial variations in the real samples. Two sample preparation techniques (formalin fixed followed by paraffin embedded and formalin fixed followed by cryostat sectioning) were analysed in a total of 10 paired breast carcinoma samples. Measurements were performed at the XRF beamline of the Laboratório Nacional de Luz Síncrotron, Campinas - Brazil. Comparison between trance elements maps and histological slices showed that both techniques preserve spatial distribution of trace elements. It was observed an increase in the signal to noise ratio of Ca, Fe Cu and Zn in the paraffin embedded samples, compared to cryostat cut ones, possibly due to the removal of adipose tissue. The quartile coefficient of dispersion analysis showed similar variability in both sample preparations. Also, the ratios Fe/Ca, Zn/Ca and Cu/Ca showed similar tendencies in both sample preparations, suggesting that these procedures affect all analysed elements in a proportional way. Finally, our results suggest that paraffin embedded procedure is preferable for breast cancer analysis using µ-XRF, since it preserves morphological and chemical aspects of the samples while provides an increasing in the signal to noise ratio.

O estudo e a caracterização de objetos de valor arqueológico ou histórico, utilizando técnicas físico-químicas de análise vêm se intensificando nos últimos anos. Este tipo de estudo multidisciplinar é também conhecido como arqueometria. Os artefatos cerâmicos usualmente constituem o tipo de objeto mais encontrado em escavações arqueológicas, por isso é um tipo de amostra frequentemente estudada na arqueometria. A análise da cerâmica pode complementar as informações obtidas em documentos escritos para produzir um melhor conhecimento. A Fluorescência de Raios X (XRF) é uma das técnicas, que possuem grande destaque na análise de artefatos cerâmicos, isto, por que a mesma possibilita caracterizar a composição elementar das amostras, com boa precisão e acurácia de forma não-destrutiva. Neste trabalho foram caracterizados por XRF, doze fragmentos cerâmicos escavados, por pesquisadores do Museu Nacional da UFRJ em uma antiga fazenda no município de Pirenópolis, Goiás (Brasil), cuja fundação é datada de 1800. Sendo, que as amostras foram escavadas principalmente no quintal da sede e nas senzalas. Os resultados obtidos pela XRF foram comparados através de testes estatísticos multivariado – Análise por Componentes Principais (PCA) – no intuito de estabelecer similaridades ou diferenças a nível elementar entre as amostras investigadas. Os espectros de XRF foram coletados no sistema modelo TRACER IV da Bruker, utilizando tensão de 40 kV e corrente de 10 μA, durante quatro minutos. Foram obtidos três espectros de XRF para cada amostra, onde em seguida foi realizada a média dessas três contagens de cada amostra para serem comparadas no PCA. Os resultados da XRF revelaram que todas as amostras possuem os seguintes elementos: K, Ca, Mn, Fe, Cu, Y, Sr, Nb, Mo. Sendo a diferença entre os espectros de XRF a despeito das intensidades dos elementos. A comparação das amostras por PCA permitiram identificar que algumas amostras da senzala e do quintal da sede possuem grandes semelhanças à nível elementar, permitindo inferir que o material cerâmico utilizado pelos escravos e senhores do engenho possuem a mesma proveniência. Este resultado permite respaldar a hipótese sobre o modelo de escravidão adotado na propriedade, que incluía atitudes paternalistas do proprietário, que englobava a distribuição de materiais cerâmicos de uso cotidiano para os escravos.

El compuesto (1E,2E)-N-(4-clorofenil)-3-fenilprop-2-en-1-imina [3], se sintetizó a partir de una mezcla estequiométrica de 4-cloroanilina [1] (1.5mmol) y trans-cinamaldehído [2] (1.5mmol). La caracterización molecular se llevó a cabo mediante espectroscopía infrarroja (IR) y resonancia magnética nuclear (RMN). En la Figura 1 se muestra el esquema sintético realizado para la obtención del compuesto [3]. La caracterización cristalográfica del compuesto (1E,2E)-N-(4-clorofenil)-3-fenilprop-2-en-1-imina se realizó por medio de la técnica de Difracción de Rayos-X de muestras policristalinas, obteniendo que el compuesto [3] cristaliza en un sistema monoclínico con grupo espacial P21/c (Nº 14) y presenta las siguientes constantes de celda: a = 14.824 (7) Å, b = 16.48 (1) Å, c = 5.137 (3) Å, ß = 96.83° (7) y V = 1246.2 (9) Å3, con figuras de mérito de M(20) = 10.8 y F(20) = 21.5 (2.9332, 0.0186).

De acuerdo a las diferentes teorías sobre el origen del petróleo, se puede asumir que el petróleo y el gas se originan principalmente en rocas sedimentarias, a partir de la evolución térmica de la materia orgánica. En tal sentido, las rocas generadoras de petróleo deben contener suficiente materia orgánica, adicionalmente a la calidad se debe de considerar la cantidad y madurez que haya alcanzado en la ventana de generación de petróleo y gas. Teniendo en cuenta que algunas formaciones se caracterizan por su alto contenido orgánico de proveniencia marina, afecta que no existan contenidos apreciables del macerales como la vitrinita. Lo que conlleva a tener limitaciones para determinar la madurez térmica de la materia orgánica a partir de la reflactancia de la vitrinita (Ro). Esta desventaja es frecuentemente suplida por el uso de otros indicadores como el de la Ro equivalente de la Tmax calculada a partir de la ecuación de Jarvie (2011). Esta investigación propuso el uso de variables cristalográficas tales como FWHM y tamaño del cristalito como método alternativo para estimar la madurez termal de la roca. Para tal efecto, se calcularon las variables cristalográficas en la reflexión (001) de Caolinita y se analizaron mediante una correlación lineal multivariada con algunos datos experimentales y calculados de Ro de una formación colombiana. Con la correlación obtenida se pudo confirmar que la caolinita se encuentra afectada por el grado de madurez de la roca y que las rocas de la formación en estudio corresponden a rocas maduras que se encuentran en la ventana de aceite.

El análisis y control en tiempo real de un yacimiento sea en un pozo exploratorio o un pozo de producción nos permite reducir el tiempo de respuesta durante las decisiones operacionales de perforación o recobro y obtener una correlación más acertada de la litoestratigrafía del yacimiento. Ante la necesidad de optimizar los procesos de exploración y producción en la industria petrolera, los analizadores portables prometen ser una tecnología de fácil operación en las campañas onsite particulares de esta industria. Esta metodología propuso el uso del análisis por DRX de montajes desorientados tanto a nivel de la roca total como a nivel de la fracción menor de 2 µm mediante el uso de un difractómetro de rayos-x portable marca Olympus modelo Terra-441 bajo condiciones de ensayo de 30 kV de energía y 350 µA de intensidad. La validación de esta metodología se desarrolló con mezclas de referencia y rocas del subsuelo colombiano de yacimientos convencionales y no convencionales.

Five gold samples were analysed using laser ablation and multi collector mass spectrometer. Four of these samples were from goldfields in Cuiabá, Peixoto, Lacerda and Colombia. The last one was a modern British coin, which is supposed to be a gold mix of different provenances. The process evaluated Pb isotopes 204, 206, 207 and 208. At the same time the isotope 202 from Hg was measured in order to correct superposition of 204 Hg present in buffer gas with 204 Pb. X-Ray fluorescence measurements were also made in order to evaluate copper and silver concentrations in the samples. All results are interesting and characterize quite well these gold samples. This is the first step in order to develop the methodology to analyse old artifacts like coins and other metal objects and therefore, this is an important technique largely used in Archeometry. Furthermore, this is an important method to fingerprinting gold provenance in Brazil.

El compuesto 4-cloro-N-(9H-fluoren-9-iliden)anilina se obtuvo a partir de 0.31g (1.72mmoles) de 9-fluorenona [1] y 0.22g (1.72mmoles) de 4-cloroanilina [2]. La reacción se llevó a cabo utilizando etanol como solvente y reflujo constante durante 72 horas. La formación de cristales amarillos con punto de fusión de 153°C y la caracterización molecular mediante técnicas analíticas instrumentales como Infrarrojo y espectrometría de masas evidenciaron la formación del compuesto [3]. El proceso de síntesis se aprecia en la Figura 1. Figura 1 – Síntesis del compuesto 4-chloro-N-(9H-fluoren-9-ylidene)anilina Posteriormente se realizó la caracterización cristalográfica por difracción de rayos-X de muestras policristalinas, encontrando que el compuesto de interés cristaliza en el sistema monoclínico con constantes de celda: a = 14.261 (2) Å, b = 5.205(4) Å, c = 19.428(2) Å, ß = 99.147° (2) y V = 1426.4 (1)

O Brasil é um dos maiores produtores de gemas, ou pedras preciosas, do mundo, além de conter uma enorme variedade gemológica, sua produção é reconhecida internacionalmente pela sua qualidade e beleza. Algumas das gemas brasileiras usadas em joias são: a Esmeralda, a Água-marinha, o Topázio, a Turmalina, o Quartzo e a Ametista, diferindo uma das outras quanto à cor, transparência e dureza. Certas gemas, embora valiosas e bonitas, não possuem a dureza e a fragilidade desejável para serem usadas em joias, mas são exibidas em museus e procuradas por colecionadores. As gemas são classificadas de acordo com diferentes especificações técnicas como a composição química e os sistemas cristalinos. Muitas gemas são da classe dos silicatos e dos óxidos. Buscando uma compreensão melhor quanto às composições químicas, foram feitas análises em diferentes amostras de gemas através da técnica de fluorescência de raios X por dispersão em energia utilizando dois espectrômetros de raio X, o mini-XRF da Amptek e o ARTAX 200 da Bruker. Nas amostras foram detectados os picos característicos dos principais elementos como o Silício, Nióbio, Ferro e Cromo, além de impurezas, que em muitas pedras são as responsáveis pela denominação das cores.

Os meteoritos despertam a curiosidade da humanidade desde a antiguidade. No entanto, o estudo desses materiais vai muito além de uma simples curiosidade. A pesquisa que desenvolvemos possui a finalidade de realizar um estudo científico de amostras de meteoritos, através de análises sistemáticas[1]. Desse modo, pretendemos propor possíveis modelos de caracterização desses objetos por meio de diferentes técnicas instrumentais não destrutivas, tais como, fluorescência de raios X (XRF) e microtomografia computadorizada (µTC). Assim, acreditamos que poderemos neste trabalho averiguar, caracterizar, fornecer e estabelecer empiricamente, informações fundamentais para compreendermos melhor a evolução do Sistema Solar através desses objetos[2]. Referências: [1] Hutchison, R. Meteorites: a petrologic, chemical and isotopic synthesis.2a Ed. Cambridge planetary science series. 2004. [2]Patterson, C. Age of meteorites and the Earth. Geochimica et Cosmochimica Acta, 1956, Vol. 10, 230-257.

Inicialmente tida como arte exótica, a tatuagem, adquiriu conotação artística e foi inserida em novos contextos sociais. No entanto, a preocupação com o bem-estar, assume relevantes preocupações na hora de tomar decisões que envolvam algum risco à saúde. De acordo com a Resolução da Diretoria Colegiada – RDC 55/2008 ANVISA, a qual regulariza o uso de pigmentação permanente para pele, há no Brasil apenas quatro marcas autorizadas para a prática da tatuagem. Este trabalho teve como proposta a caracterização elementar de pigmentos utilizados para fazer tatuagem, com a finalidade de identificar os metais presentes na composição das tintas e avaliar os possíveis riscos que estes materiais, quando inseridos no organismo, podem acarretar. A análise foi realizada pela técnica de fluorescência de raios X por energia dispersiva (EDXRF). O sistema de EDXRF é composto por um tubo de raios X com alvo de Mo, colimador de 0,65mm e um detector XFlash (SDD), o ARTAX 200 (BRUKER). Foram analisadas amostras de tintas, as quais foram desidratadas e prensadas, transformadas em pastilhas à fim de evitar o aumento do background nos espectros gerados pelo software, uma vez que amostras liquidas possuem essa característica, que dificulta leitura dos gráficos. Os parâmetros de exposição foram de 30kV e 102μA durante o tempo de 300s para cada amostra. O resultado dos espectros de emissão, apresentou os seguintes elementos Cl, Ti, Cr, Fe, Cu, Zr, Ni e Nb como componentes dos pigmentos. A reação de alguns destes metais com a derme, de acordo com referências, podem causar alergias e dermatites de menor ou maior grau na região tatuada, o que constitui um problema a longo prazo.

The process of proliferation and differentiation of hematopoietic cells is a complex mechanism which depends on the presence of nuclear proteins, cytoplasmic proteins and the action of various genes. These genes can be mutated so that the differentiation program is changed. Changing the program is related to the onset of leukemia which is characterized by disorder of cell proliferation or the production of abnormal cell clone. This differentiation mechanism has been widely studied in relation to normal human cells and leukemic myeloid type. Myeloid Leukemia can be subdivided according to the degree of cellular maturity. Immature forms present an acute evolution and mature forms have a chronic evolution. The Chronic Myeloid Leukemia (CML) is responsible for 20% of all cases of leukemia and about 3% of childhood leukemia. The predominant age group is between 25 and 60 years, with a greater number of patients with males. The Acute Myeloid Leukemia (AML) is the most common type of acute leukemia and more than 80% of cases occurring in adults. This type of leukemia is around 15-20% of acute leukemia in childhood with a peak incidence between 40 and 60 years. AML is more common in men than in women. The determination of multielemental concentrations in physiological fluids is of considerable interest in clinical chemistry. Since it has been established this levels in human serum can be utilized as indicators for several pathological conditions. The multielement composition determination in human serum is important for the investigation of their role in human physiology and metabolism. We studied hundred serum samples from each group of patients (AML and CML) of both sexes with ages ranging from 19 to 70 years and hundred and twenty healthy volunteers aged 19 to 65 years. All the serum samples were collected from people who live in the urban area of Rio de Janeiro City/Brazil. All of them were submitted to medical history. This study was performed with the approval of the ethics committee. The measurements were performed at the X-Ray Fluorescence Beamline at the Brazilian National Synchrotron Light Laboratory (LNLS), in Campinas, São Paulo. It was possible to determine the concentrations of the following six elements: Na, P, S, Cl, K and Ca. In this work we used statistical analysis by principal components (PCA) SPSS for windows version 20.0. For this analysis, it was performed the test of Kaiser-Meyer-Olklin (KMO) and the Test of Sphericity Bartelett (TSB).

Saquinavir (SQV) is an important protease inhibitor used for AIDS/HIV antiretroviral therapy. It is commercialized as mesylate salt (SQVM) and classified as belonging to class IV (low permeability and solubility). The dissolution properties were investigated by SQVM in the medium containing the anionic surfactant Sodium Lauryl Sulphate (SLS). It was expected that the electrostatic interactions between the anions of SLS and the cationic drug species could cause a decrease in the repulsive forces of the head groups of the surfactant molecules leading to enhanced solubilization. However, for the SQVM profile in the anionic surfactant medium the result obtained was contradictory. Therefore, the aim of this study was to explain the anomalous dissolution behavior of SQVM in SLS medium through a structural analysis. The anionic portion of SLS remaining molecules interact with the cationic species of SQV to form an insoluble salt which precipitates out (Figure 1) and results in desolubilization phenomenon. Through crystallographic investigation it was possible to demonstrate the crystallization of SQVM with SLS. Therefore, SLS is not an appropriate dissolution medium to analyse the dissolution properties of SQVM. Figure 1 – (A) Dissolution profile of SQVM raw material and (B) Turbidity of SQVM in SLS 0.25% medium

A Floresta Amazônica é rica em sua biodiversidade, por isso, existe a necessidade de realizar mais estudos científicos para aumentar o conhecimento sobre sua heterogeneidade. A ecologia de muitas espécies arbóreas, principalmente no que se refere à composição química inorgânica, é ainda desconhecida. Esse é o caso da família Burseraceae, composta de 18 gêneros e aproximadamente 700 espécies. Sendo o Protium Burm.f. o principal gênero da família. Uma característica marcante em deste gênero é a presença de espécies que exsudam resina aromática no tronco. Essas resinas, conhecidas popularmente por “breu”, têm usos documentados como repelente de insetos, acendedor de fogo, calafeto de canoas e no tratamento de diferentes problemas físicos. Este trabalho tem como objetivo diferenciar a composição química inorgânica do breu, coletado da espécie Protium strumosum Daly, a partir de dois métodos de extração diferentes, natural e com a aplicação do ethephon (5%), mostrando o quanto qualitativamente e quantitativamente a resina excretada difere uma da outra. Foram coletadas 15 amostras de breu, que foram posteriormente analisadas pelo método de Fluorescência de Raios-X por dispersão de onda (FRXDO). Após análise qualitativa das amostras, foram encontrados elementos como Potássio, Cloro, Sódio, Silício, Enxofre, Cálcio, Magnésio, Fósforo, Ferro, Prata, Iodo, Cádmio, Bromo, Ítrio, Molibdênio, Nióbio, Zircônio, Estanho, Manganês e Rubídio. Já nos estudos qualitativos, observa-se a diferença de composição nas amostras extraídas com e sem o estimulante. Com as análises quantitativas, esta observação ganha respaldo numérico e tem-se a confirmação de que a composição da resina exudada naturalmente é diferente da estimulada artificialmente.

A utilização de resíduos de EVA na construção civil vem sendo intensificada na última década. É notório o grande potencial que estes resíduos possuem para emprego como agregados leves, em substituição aos agregados naturais, e na elaboração de compósitos cimentícios alternativos. Neste trabalho são analisados os elementos químicos presentes na composição dos pigmentos em amostras de EVA da empresa Start Impermeabilizantes a partir de uma análise da espectroscopia por fluorescência de Raios X utilizando um micro espectrômetro da AMPTEK em diversas amostras com cores distintas. A avaliação dos elementos presentes no EVA busca viabilizar a utilização dos resíduos deste material como agregado na produção de concreto permeável, que permite que a água das chuvas passe através dele e seja armazenada nas camadas inferiores, base e sub-base. Os resultados foram obtidos para amostras com sete cores diferentes, de modo a aferir os elementos presentes em diferentes tipos de pigmentos. A partir da análise foram encontrados como elementos principais o cálcio (Ca), titânio (Ti), zinco (Zn) e ferro (Fe). Segundo a literatura a presença de tais elementos pode ser atribuída a substâncias largamente utilizadas na indústria de pigmentos como o carbonato de cálcio, dióxido de titânio, óxido de zinco e óxido de ferro II. Por fim, a partir dos resultados obtidos é possível estudar a utilização dos refugos de EVA como agregado através da interação do EVA com o cimento na produção de concreto permeável bem como a avaliação ambiental de modo que, durante a passagem de água, substâncias poluentes não sejam carreadas para o lençol freático, causando o fenômeno conhecido como lixiviação.

Alzheimer disease (AD) is an insidious, progressive and irreversible brain disorder. Its incidence is highest in people aged over 65 [1]. The cause of AD is not fully understood. The pathological features of AD include β-amyloid (Aβ) plaques, intracellular neurofibrillary tangles, loss of neurons and synapses, and activation of glia cells. Recently, several groups have raised the “metal hypothesis” of AD [2]. This hypothesis is mainly based upon experimental results. First, several metal ions, such as zinc, iron and copper, are all increased in the ageing brain. It has been reported that the content of metal ions in the brain of AD patients is 3-7 times that of normal people and that the metal ions in brain homeostasis may result in the development of AD [3]. Second, these metal ions can interact with Aβ, resulting in the promotion of Aβ deposition and plaque formation. Total reflection X-ray fluorescence analysis (TXRF) is a multielement analytical technique, which is capable of yielding quantitative information on the elemental composition of a variety of materials. This method can be used for elemental trace analysis [4]. In this work, three groups were studied: control, AD10 and AD100. The groups AD10 and AD100 were given a single intracerebroventricular injection of 10 pmol and 100 pmol of oligomers of β-amyloid peptide respectively to be induced AD. Seven days after the injection was carried out craniectomy and subsequently evaluated five brain compartments: frontal cortex, temporal cortex, hypothalamus, hippocampus and cerebellum. All samples were submitted to acid digestion (HNO3 + H2O2). After that, they were diluted with Milli-Q water and added an internal standard (Ga).The TXRF measurements were performed at the X-Ray Fluorescence Beamline at Brazilian National Synchrotron Light Laboratory (LNLS), in Campinas, São Paulo using a monochromatic beam (11.5 keV) for the excitation and an Silicon drift detector with energy resolution of 133 eV at 5.9 keV. It was possible to determine the concentrations of the following elements: P, S, K, Ca, Fe, Cu and Zn.

This project intends to develop a remote control to micro X-ray fluorescence (µXRF) system. X-ray microfluorescence represents a relatively specialized form of XRF analysis, it is becoming increasingly adopted in specialized applications because of its unique analytical capabilities and the complementary nature of results in comparison with other microprobe techniques. The system utilized was developed by Laboratório de Instrumentação Eletrônica e Técnicas Analíticas (LIETA) group and named Sistema Integrado de Controle (SIC). The system consists in three main integrated modules: X-ray tube, digital pulse processor and high accurate table. A microcomputer connect all the modules and process the data acquisition. This equipment has a graphic user interface by means of a website. The website control enables the final user to perform µXRF measurment by any device with web browser available. With simple steps, the automated system initiates all computacional commands of the routine and generate photon counts per channel data files. All the generated data is processed at PyMca analysis software.

The purpose of investigating technology choices is to question the techniques and materials used by potters and the consequences of their choices (Sillar & Tite 2000) [1]. To understand the differentiation of technologies and possibly the people who produced these artifacts in different chronological moments and geographical areas the first step is the chemical characterization to define the variability of each region and link the results to the archaeological and chronological results. In this work we show the results of the analyzes made by the XRF technique of ceramic fragments from three different regions of the Amazon rainforest: Oriental, West and South region. Thus it was possible an assessment of the range of results that are relevant to the study of archaeological ceramics of the Amazon rainforest and to the understanding of potters populations that produced them.

Cerium oxide (CeO2) nanoparticle (NP) has unique physical and chemical properties. These particular features enable the CeO2 NP to a wide variety of recent application, such as UV absorption, catalysis, solid oxide fuel cells use, and so forth. However, the environmental risks of CeO2 NP have not been extensively studied so far and it has been a matter of currently concern worldwide. In this context, this study aims at the CeO2 NP (20 nm particle size) mobility as well as its conceivable transformation in Typic Hapludox and Rhodic Hapludox soils. For the soil CeO2 NP mobility evaluation, an acrylic column filled with the abovementioned soils top covered with 350 mg CeO2 NP was employed as shown in Figure 1. Breakthrough assays using a volume of synthetic rain water equivalent to average precipitation from Jan-Mar were carried out. The translocation of Br- and CeO2 were investigated for both soils. Benchtop energy dispersive X-ray fluorescence (EDXRF) was used to detect the presence of Br and Ce in the eluate. Br- was highly mobile whereas CeO2 did not leach. Further EDXRF analysis showed that CeO2 remained adsorbed at the first two centimetres of the soil column. Another matter of concern regards possible chemical transformations undergone by CeO2 NP in the soil. To assess CeO2 NP reactivity the NP was incubated in Typic Hapludox and Rhodic Hapludox soils aqueous suspensions for two weeks under stirring. Then, Ce-L3 X-ray absorption spectra were recorded at the XAFAS2 beamline at the Brazilian Synchrotron Light Source (LNLS). Figure 2 shows the near edged fine structure spectra for the NP incubated in Typic Hapludox and the pristine one. The preliminary results indicate that only slight changes have been observed. The whiteline increasing might be related to changes at the electronic structure of the incubated NP. Seemingly, the density of empty states increases, which could be promoted by oxygen vacancies. Anyway, for this short period, i.e. two weeks, under mild environmental conditions we have not find any dramatic changes on CeO2 chemical environment.

The Hurter & Driffield curve, primary tool for evaluation of characteristics of radiographic films is defined as the optical density as function of exposure. This optical density is traditionally measured by the transmittance of a beam light across the film, and its response is important to understand the film behaviour in sensitometry, in scanning by optical scanners and also in the viewing with our eyes against a light source such as light box. There are many mathematical and computational models to characterize the behaviour of this curve and its properties, but is not among them some models that consider the interference that the equipment used can have about sensitometric curves. When trying to adjust curves from theoretical models to experimental data, it was estimated that, for high exposure values, there was inconsistency between data, and this inconsistency would suggest a limitation in optical density. When trying to make the measurement of silver depending on exposure through another method than optical, such as X-rays fluorescense, it was realized that these data was reasonably agree with the models, and that the limitation in optical density is mainly caused by its measurement. The objectives of this work were: 1 - characterize this limitation of the measurement of optical density; 2 - Suggest the X-ray fluorescence as a technique that bypasses the resulting difficulty caused by this limitation; and 3 - by X-ray microfluorescense, reconstruct images and show what kind of information is lost and that the new method can be revealed. The study shows that the transmittance of light is a limited way to measuring the concentration of silver, and gave birth to a mathematical characterization of this limitation, which set a reasonable fit to experimental data. Also characterized and suggested the X-ray fluorescence method which can solve this problem, showing data that are more consistent with models that do not consider the limitation. The mapping was successful in reconstructing images and present a visual way that a good portion of the dynamic range is lost with the measurement by light transmittance.

El sitio arqueológico Pampas Gramalote (Figura 1-a) se ubica en el centro poblado menor de Huanchaquito, provincia de Trujillo. Los trabajos que se vienen realizando en el sitio están ayudando a entender el proceso de complejización social desde la perspectiva de las comunidades o centros residenciales domésticos. Se trata de estudiar la configuración y dinámica interna de una comunidad y como ésta se articuló en las diferentes esferas y escalas sociales y económicas del valle de Moche y la costa norte en general. Los trabajos de investigación que se han venido realizando desde la década de 1970 y específicamente las investigaciones arqueológicas llevadas a cabo por Prieto entre 2010 y 2014, han permitido tener una perspectiva más amplia del sitio, enfocando su estudio en las dinámicas económicas y las interacciones sociales de sus pobladores con otros grupos contemporáneos. En este contexto, considerando que el sitio ha probado ser uno de los asentamientos con el uso más antiguo de vasijas de cerámica (Figura 1-b) en la costa peruana y para entender la introducción y/o uso de esta técnica en los Andes Centrales, fueron investigados estos artefactos. Fragmentos cerámicos encontrados en el sitio fueron estudiados por difracción de rayos-X, a fin de conocer su composición y características estructurales. Las medidas de la reflectividad fueron evaluadas por refinamiento estructural aplicando el método de Rietveld. Resultados de este estudio son presentados en este trabajo, con lo que esperamos contribuir al esclarecimiento de estos hallazgos.

Métodos de análise multivariada tais como, PLS tem sido amplamente utilizado em conjunto com outras técnicas analíticas para estudos de objetos arqueológicos e do patrimônio cultural. O procedimento de PLS utilizando compreende duas etapas: a validação e calibração. A etapa de calibração é utilizada para o estabelecimento de uma relação entre a matriz de dados X (sinais instrumentais, variáveis independentes) e as propriedades amostras usando amostras de referência (variáveis dependentes) organizadas na matriz Y. A etapa de validação permite a verificação se o modelo é capaz de prever as propriedades das novas amostras. Foi estudado uma moldura dourada da peça intitulada Mulher Enxugando o Braço Esquerdo (Após o Banho) realizada em 1884, de autoria do pintor Degas, Hilaire-Germain Edgar de Gas com dimensões de 58 x 64 cm. Seis pontos foram analisados por PXRF durante 300 segundos. Para obter os padrões (variáveis dependentes) utilizados no modelo PLS folhas de ouro com espessuras conhecidas foram utilizadas correspondendo aos valores 0,094, 0,188, 0,564, 1,128, 2,068 µm, respectivamente. Para a regressão PLS, os dados dos espectros de calibração foram arranjados em uma matriz 5x1024 (X) e uma matriz de 5x1 (Y) com os valores de espessuras. Os dados de validação foram arranjados em uma matriz 6x1024 (X) com os espectros a partir da moldura. Foi usado um filtro de média como um passo de pré-processamento dos dados, e todos os espectros foram normalizados para o mesmo tempo de medição. A metodologia proposta com base em uma abordagem PLS foi capaz de prever as espessuras de Au numa moldura de madeira dourada de uma pintura. A diferença relativa entre os dois métodos permaneceu entre 6 até 16%, e os valores de espessura podem ser consideradas equivalentes, dentro das barras de erro.

O presente trabalho faz parte de um projeto maior, o qual pretende através silicofitólitos, δ 13C, datações por 14C-AMS e diversas análises pedológicas em perfis de solo, realizar a reconstituição paleoambiental no Médio Vale do rio Paraíba do Sul - RJ. Para isso, conhecer as características dos solos, bem como as concentrações de elementos presentes, pode auxiliar a interpretação de resultados, tornando a pesquisa mais fidedigna. Desta forma, 35 amostras de solo foram secas a 50°C, destorroadas, peneiras a 250 μm e analisadas por Fluorescência de Raios X por Dispersão de Energia (EDXRF). Foi utilizado um equipamento comercial produzido pela Shimadzu Corporation. Os parâmetros de operação foram: tubo de raios X de Ródio, tensão de 5 KV; corrente ajustada automaticamente de no máximo 1 mA; colimador de 10 mm; detector de silício; resfriamento termoelétrico; tempo de medida de 200 s e 3 varreduras por análise. Foi utilizada a metodologia de Parâmetros Fundamentas para a determinação quali-quantitativa. Os seguintes elementos foram encontrados: Si, Fe, Ca, Ti, K, Mn, Sr e Zr.

Intended primarily for decoration, currently thin films are used as the basis of high technology. Among the physical quantities that characterize it, thickness strongly influences other properties of the film. Thickness measurements are performed using sophisticated and high cost equipment, which often need a proper treatment of the sample to accomplish the desired measurement. Thus, the methodology of X-Ray Fluorescence with portable equipment (PXRF) shows a highly suitable tool to determine these thicknesses. Thus, it was proposed and developed a procedure for the determination of film thickness by PXRF employing K lines attenuation. The thin films were deposited by thermal evaporation from the pellets with 100 mg, 70 mg and 35 mg of V2O5 powder (Sigma-Aldrich, 99.9%). Knowing that Calcium (Ca) is one of the constituents of the glass substrate, it is used the differential attenuation of the K lines of this element after traversing the layer of V2O5. It was employed a Portable X-ray Fluorescence system (PXRF) composed of a Si-Pin detector with a 6 mm2 crystal and 500 μm thickness, a 12.5 μm thickness Beryllium window and a silver anode X-ray tube with silver collimator and filter. Thickness obtained by PXRF was compared with the measurements obtained by scanning electron microscopy. Through the PXRF technique values of 54, 98 and 167 nm for film thicknesses of 35, 70 and 100 mg were obtained. These values are in good agreement with measures by electron microscopy, 50 ± 7, 110 ± 3 and 160 ± 5 nm, respectively. It is observed that the values of the calculated thicknesses are slightly larger than the values measured by the scanning micrographs, due to the fact that a small residual deposits in the boat evaporation. Thus, the PXRF methodology is a highly suitable tool to determine the thickness of nanometric thin.

The white marble sculpture of Leopoldo e Silva (1879-1948), called "Menina e Moça" (23 x 147 x 40 cm), is kept in exposition in one of the hallway of the museum Pinacoteca de São Paulo, in which the public has direct access to it and it is even possible to touch the sculpture. As a result, the sculpture has dirt stains with brown shades over the white marble. A helical vortex cleaning system employing an air flux with calcite was performed as a blasting cleaning process. The calcite has a medium abrasiveness and its composition is similar to the marble sculpture. After the cleaning process a hydrophobic product based on silicon nanoparticles was applied (Silano®). This study consists in the surface qualitative characterization of the sculpture, which objective was to verify if the helical vortex cleaning process as well as if the hydrophobic sealant modify the surface chemical composition of the sculpture. A laboratory-made portable energy dispersive X-ray fluorescence (EDXRF) equipment, developed in the Applied Nuclear Physics Laboratory of the Universidade Estadual de Londrina, was taken to the Pinacoteca museum for the study. Fourteen measurements in different points were performed before helical vortex application, 7 measurements after the helical vortex cleaning and 3 measurements after the hydrophobic sealant application. Due to the limited available time for measurements, it was not possible to perform the same number of points before the cleaning. The operation conditions of the portable EDXRF equipment were: 35 kV, 5 µA and 200s excitatin/ measurement time. In all the spectra the chemical elements P, S, Ca, Fe, Sr appeared. The highest intensity peaks were from Ca and Sr which are the major components of the marble. In some point Zn was detected before the cleaning process. It was noted that the Fe and Zn intensity peaks decreased after the helical vortex cleaning attesting that the surface was cleaned because Fe is the major component of dust. The spectra of the measurements after the sealant application were identical to the ones made just with the helical vortex cleaning. However, the detection limit of the portable EDXRF equipment is in tens of ppm for light elements, therefore the Si nanoparticles were enabled to be identified. In conclusion, the helical vortex cleaning process and the hydrophobic application are efficient for sculpture conservation and do not alter significantly the surface composition of the marble.

In recent decades, it has been a large increase in the use of electronic devices as well as their batteries consumption. However, the improper disposal of these materials can cause soil and groundwater contamination by potentially toxic metals. In this context, the present study aims to evaluate the total elemental content and their leaching from soil exposed to Zn-C and alkaline batteries and electronic components from printed circuit boards. Test soil columns 40 cm in length containing the above mentioned materials were prepared. The soil columns were exposed to artificial rain and the leachate were collected. The leachate samples were analyzed by the synchrotron radiation total reflection X-Ray fluorescence spectrometry (SRTXRF) at the Brazilian Synchrotron Light Laboratory D09-XRF beam line. The Cr, Mn, Fe, Cu, Zn and Pb content in the leachate were lower than the set maximum values CONAMA 369/2008 resolution. The SRTXRF K, Ca, Ti, Cr, Mn, Fe, Cu, Zn and Pb detection limits ranged from 0.22 μg L^(-1) to 4.32 μg L^(-1). The results showed a higher leaching of K, Mn, Zn and Pb in the columns containing batteries. For soil analysis, Al, Si, K, Ca, Ti, Cr, Mn, Fe, Cu, Zn, Zr and Pb were evaluated using a benchtop energy dispersive X-Ray fluorescence spectrometer (EDXRF) and the detection limits ranged from 5390 to 16 mg kg^(-1). For soil columns batteries containing, higher K, Mn and Zn levels were found in the surface soil layer compared to the control. For soil columns printed circuit boards containing, an increase of Ti, Mn and Pb were evident. In addition, the metal concentration variation in soil was evident only in surface soil, up to 10 cm. From 10 to 40 cm the difference soil was minimal compared to the blank. SRTXRF and EDXRF were showed promising techniques for evaluation of metals in the leachate and soil, respectively.

Nowadays men and women spend a lot of time, resources and efforts to the cultivation of personal hygiene and the best possible look, as a result, the cosmetics industry plays an important role in the economy of most developed countries. The raw materials used in cosmetics are classified as active principles or excipients. Excipient is all inert ingredient added to a formulation to give consistency, in order that the product can be applied, handled and packaged appropriately. The active ingredients are substances that effectively work and promote changes on the body regions in which the cosmetics are applied, e.g., skin, eyelids, nails, etc., thus their amounts need to be controlled due to the application acceptable limits, its toxicity, the consequences of excessive doses, possible side effects, and the possibility of sensitization and allergic reactions. The concentration and quality of the raw material used in the manufacture of a cosmetics product can be verified by analytical methods, among them the X-ray fluorescence, since X-ray fluorescence technique is suitable for performing multi-elemental analysis with low cost and fast results. This study, developed in Applied Nuclear Physics Laboratory (LFNA) of the Londrina State University (UEL), had as objective inorganic elements determination in cosmetic samples, as well as its matrix characterization. It was used a portable energy dispersive X-ray fluorescence (EDXRF) system associated with principal components analysis (PCA). For the measurements was used a home-made portable system which consists of a X-ray tube with Ag target and filter (MAGNUM MUHV50, Moxtek); a high voltage source (FTC-200, Moxtek) for control of the voltage and electric current applied to the X-ray tube; the X-123 complete X-ray spectrometer with Si-PIN detector (Amptek) with FWHM@5.9 keV: 153 eV; and a laptop for acquisition, storage and data treatment. A total of 40 eye shadows samples from 4 manufacturers and suppliers in the Brazilian market representing different colors and shades were analyzed. It was possible to identify and quantify the elements Cl, K, Ca, Ti, Cr, Fe, Cu, Zn and Bi. In order to verify tendencies in the classification of the samples, the set of X-ray spectra was evaluated by principal components analysis. The whole X-ray spectrum was considered in the analysis and it was possible to verify a separation of the samples in groups in accordance with manufacturer. From the multi-elemental data obtained by X-ray fluorescence and the information revealed by the principal component analysis it was possible to identify the differences in the composition of each set of samples. Based on these results it can be seen that the combination of X-ray fluorescence technique with the principal component analysis presents a valuable tool for the classification and characterization of cosmetics samples.

An important aspect for the evaluation of fire effects in slash-and-burn agricultural system, as well as in wildfire, is the soil burn severity. The objective of this study is to estimate the maximum temperature reached in real soil burn events using energy dispersive X-ray fluorescence (EDXRF) as an analytical tool, combined with partial least square (PLS) regression. Muffle-heated soil samples were used for PLS regression model calibration and two real slash-and-burn soils were tested as external samples in the model. It was possible to associate EDXRF spectra alterations to the maximum temperature reached in the heat affected soils with about 17% relative standard deviation. Table 1 presents the measured values with thermocouple on burned fields samples with its respective predicted values by partial least square regression model using EDXRF spectra for the maximum temperature reached on surface soil. The results are promising since the analysis is fast, non destructive, and determined after the burn event, although local calibration for each type of burned soil is necessary.

La técnica de fluorescencia de rayos X (XRF) permite la identificación y cuantificación de elementos en muestras de diversa naturaleza. En particular su aplicación en tejidos biológicos es ventajosa porque no exige una preparación de muestras compleja en comparación con técnicas instrumentales alternativas. Los estudios por XRF permiten realizar un seguimiento de las concentraciones de elementos metálicos contribuyendo de esta manera al entendimiento de diversos procesos fisiológicos de los organismos vivos donde los metales son partícipes esenciales. Sin embargo, las concentraciones de metales en tejidos biológicos se encuentran en niveles traza por lo que su análisis requiere una cuidadosa optimización de la sensitividad del espectrómetro y del proceso de preparación de muestras. En este trabajo se desarrolló un dispositivo compacto que permita modificar el haz de excitación en energía y tamaño, para esto fue utilizado un cristal de silicio (100) y colimadores de láminas paralelas de vidrio tanto en el canal de excitación como en el canal de detección tanto antes como después del cristal. El dispositivo se acopló a un tubo de rayos X de difracción Philips modelo PW2275/20 con ánodo de molibdeno de modo de seleccionar la línea Kα de emisión característica. El haz de rayos x de excitación resultante es altamente monocromatizado (E= 0,8 keV), intenso y con sección transversal de 1mm×3,5mm, permitiendo registrar espectros por XRF con muy baja señal de fondo y alta tasa de conteo, lo cual incrementa considerablemente la sensitividad del espectrómetro. Para alcanzar límites de detección en el orden de las partes por millón, las muestras de tejidos biológicos deben además ser liofilizadas. En el presente trabajo se muestran los resultados de la caracterización del espectrómetro desarrollado (límites de detección, propiedades del haz de excitación) y algunas aplicaciones sobre tejidos biológicos (especialmente tumores malignos de mama).

El control de calidad de las aleaciones empleadas en la industria nuclear es muy importante, los datos emitidos lleva a la toma de decisiones de alto impacto. En este trabajo se desarrolla una nueva metodología para determinar aleantes e impurezas en aleaciones de zirconio (zircaloy), de titanio y de aluminio. La escasa cantidad de materiales de referencia necesarios para el análisis elemental de aleaciones por fluorescencia de rayos X convencional (WDXRF) nos llevó al desarrollo de una nueva forma de determinación empleando la fluorescencia de rayos X por reflexión total, donde el material sólido inicial se lleva a estado líquido en un simple paso de digestión, empleando mínimos volúmenes, y soluciones estándares trazables para la calibración del equipo. El espectrómetro utilizado es el S2 Picofox (Bruker), versión automática, con tubo de Mo, a 50kV y 0,6mA. En el caso de aleaciones de zirconio, se trabajó con una solución acuosa de ácido fluorhídrica para la solubilización de las virutas y posteriormente se analizan los aleantes y minoritarios: Sn, Fe y Cr, y luego las impurezas como Pb, Ni, Cu, Ti, Mn, V, Ta y W, empleando soportes de plástico, con un tiempo de medición de 300 segundos y la validación del método con un material de referencia NIST 360b para estimar los parámetros de exactitud y precisión, junto con los límites de detección. En el caso de aleaciones de titanio, las muestras se llevan a digestión en ácido fluorhídrico/ clorhídrico, los elementos analizados como impurezas son Fe, Al, Sn, Zr y Si. El material de referencia empleado en la optimización y validación del método es Ti 6-2-4-2. Finalmente, las aleaciones de aluminio se tratan con ácido clorhídrico y luego se realiza una solución con etanol al 20 % para disminuir el fenómeno higroscópico. Se optimiza el método para determinar Fe, Mn, Zn y Cr. El material de referencia empleado en la optimización del método es AA5052. La técnica de fluorescencia de rayos X por reflexión total es una herramienta muy útil para determinar impurezas en aleaciones, empleando mínimos volúmenes de muestra, con un proceso sencillo de tratamiento del material, a cortos tiempos de medición, utilizando soluciones trazables para su calibración y un material de referencia para la validación. Las fuentes de incertidumbre se identifican y los principales aportes se refieren al tratamiento de la muestra. Actualmente se emplea la TXRF para caracterizar aleaciones especiales de interés nuclear en ausencia materiales de referencia para su calibración.

A técnica de fluorescência de raios X por dispersão em energia (EDXRF) é amplamente empregada em análises de obras de artes e em objetos de patrimônio histórico por ser uma técnica não invasiva, capaz de fornecer informações sobre a composição química e a concentração dos elementos. Muitos objetos de valor arqueológico são compostos por uma estrutura de duas ou mais camadas de diferentes materiais, sendo uma de substrato e uma ou mais camadas de revestimento. A técnica de EDXRF tem sido avaliada como uma possível ferramenta para determinar a espessura de duas e/ou várias camadas de materiais, podendo auxiliar na conservação e restauração de objetos do patrimônio cultural [1]. O objetivo desse trabalho consiste na avaliação da metodologia de medida de espessura de camadas depositadas sobre uma base usando a razão entre as linhas de fluorescência de raios X (Kα/Kβ ou Lα/Lβ) emitidas por elementos da base. As análises das espessuras foram realizadas em folhas de alumínio de diferentes espessuras (12 μm, 36 μm e 60 μm) depositadas em dois materiais de base: cobre e chumbo. O sistema de XRF utilizado para as medidas de espessura é formado por um mini tubo de raios X de baixa potência com anodo de Ag e um detector SiPIN. Variando a posição do tubo de raios X e do detector foram avaliadas três configurações do sistema de XRF para o cálculo da espessura: tubo de raios X perpendicular a amostra, detector perpendicular a amostra e , por fim, tubo de raios X e detector simétricos a amostra. Em cada geometria variou-se o ângulo entre o feixe incidente e detector. Foi possível determinar as três espessuras das folhas de alumínio nas três geometrias analisadas, tanta na base de cobre quanto na base de chumbo. As medidas de espessura obtidas com a segunda geometria (detector perpendicular a amostra) foram as que apresentaram menores exatidões quando comparadas com o valor esperado das espessuras das folhas de alumínio. Os resultados mostraram que a primeira e a terceira geometrias foram mais eficientes para o cálculo da espessura de camadas. Além disso, os resultados demonstraram que quanto menor o ângulo entre o detector e a amostra mais preciso se torna o cálculo da espessura.

The materials analysis by Energy Dispersive X-ray Fluorescence (EDXRF) depends on the elementary composition and the layer thickness studied. Samples with many layers are common in historical artifacts, with pigments overlapping paintings or metal layers of recoating. In this work, the layer’s thickness measurement method using the intensity of Ka/Kb or La/Lb characteristic X-ray peaks was studied. Using few samples extracted from the baroque sculpture in polychrome wood from Saint João Evangelista, from XVIII century, it was measured the gold layer thickness that overlies gold details of the image. The sculpture was carved to the Jesuits Church's altar built at Castelo's Hill in 1567. After the Hill’s overthrow, in 1922, the artworks were been saved at Saint Inácio School's hall (Rio de Janeiro, Brazil). For the X-ray peaks intensity analysis, was used 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 from the technique using the X-ray peaks were compared to the results obtained using the high resolution optical microscope automated, model Axio Imager M2m from Carl Zeiss. The founded results prove the technique efficiency, it is important when are only available sample’s fragments that do not allow using optical microscope

A radiação espalhada tende a ser uma fonte de problemas em técnicas radiológicas, tanto a para a qualidade da imagem quanto para a radioproteção. Ela pode aumentar o ruído da radiografia, prejudicando a uniformidade e o contraste da imagem, mas também pode aumentar a exposição do operador, pois torna a amostra uma fonte secundária de radiação ionizante. A consciência da existência e do comportamento da radiação espalhada é um importante fator para práticas de proteção radiológica, mas também para a otimização dos parâmetros da técnica, otimizando a imagem. Imagens computacionais representativas deste tipo de radiação são excelentes materiais para a demonstração destes. O processo de interação da radiação ionizante com a matéria, que gera radiação espalhada tem algumas similaridades com o processo de luz visível, mas não acontece apenas na superfície de um determinado corpo. O objetivo deste trabalho é criar um simulador de baixo custo computacional para cálculo e demonstração gráfica do comportamento da radiação espalhada, em função de diversos fatores como energia e intensidade do feixe, material e meio radiografado, assim como os efeitos da mesma na imagem gerada. O simulador será construído na linguagem C e na plataforma de cálculo numérico OCTAVE. Todo o processo será executado dentro do ambiente virtual que fará parte do simulador. Mantendo a possibilidade de mudança e criações de condições diferenciadas e mantendo interatividade com o usuário final. O principal produto do simulador serão imagens do ambiente virtual da radiografia, assim como das radiografias geradas. Estas imagens terão predominantemente viés educativo, mas com capacidade para simular testes reais.

The AlGaSb layers grown on [100] GaSb substrates could create structures that operate in the 0.7-1.7 µm range, this makes suitable for its potentially use in optoelectronic devices, these includes lasers and detectors working in optical fiber communication systems. In this work, the liquid phase epitaxy (LPE) technique was used to grow Al(x)Ga(1-x)Sb layers with different thicknesses on GaSb substrate and after the growth the layers were annealed at 450°C during four hours. The High Resolution X-ray diffraction (HRXRD) was used to analyze the crystalline quality and stress change of AlGaSb layers and the optical features of AlGaSb/GaSb system were observed through low temperature photoluminescence (PL). In this study the release of tensile stress and its transformation into compressive stress modifies the near band edge at low temperature causing a shift to lower wavelength. Also, the emission increased its PL intensity attributed to interdiffusion and intermixing of species and the reduction of non-radiative recombination centres in the layer.

Occupational exposures are important parameters that need to be investigated to evaluate the radiological effects. On this work we used Geant4, version 9.6.p03 and low energy model Livermore, to define the energy correction factor (ECF) to be used on correction of thermoluminescent dosimeters (TLDs) measurements. The simulated TLDs were positioned over Bomb phantoms, representing occupational workers involved in fluoroscopic paediatric procedures. We calculated the ECF to X-ray scattered spectra by different paediatric phantoms (newborn, 1 year old, 5 years old and 10 years old), representing patients of different size undergoing fluoroscopic barium meal procedure at 60 kVp and 75 kVp. The TLDs were fixed over three regions of the occupational workers simulated: eyes (left and right), thyroid (over and under the collar of protection) and hands (left and right). The primary spectrum and scattered spectrum, that interact to each TLD, were recorded and used to calculate the ECF. We used a systematic analyses to observe de significance on influences and tendencies observed. As results we found that: (i) the scattered dimensions (paediatric phantoms simulated) does influence on ECF, in a way that an increase on scatterer size tends to increase the ECF to a fixed position of the TLD; (ii) the incident spectra energy (ripple and peak tension) can change the ECF significantly.

The study in avian neurology has been largely enrichened by the use of CT scans. This methodology presents obvious advantages. Materials usually do not need treatment before entering the scanner, no deterioration occurs during the scan, and the results allow the reconstruction of high-quality 3D models, which represent an essential step in order to perform more complex anatomical and biomechanical studies. The datasets obtained by the scans are longlasting and easily portable, facilitating the comparison and study of the 3D models obtained, which are easily manipulated, sectioned and redescribed. More importantly, this methodology provides data on extant taxa characterized as ‘very rare’ or endangered, andsvn add extinct birds rare in the fossil record. In order to explore brain anatomy in several bird species, X-raysvn add micro-CT data were obtained using an experiemntal micro-CT scanner available at Facultad desvn add Matemática, Astronomía y Física (FaMAF). This equipment allows to obtain 2D and 3D images up to 20svn add cm x 20 cm with resolutions of 194 microns. It is also possible to maximize the quality of the images fromsvn add the control of main parameters involved in the image acquisition: conformation of the X-ray beam (spatialsvn add and spectral distribution), counting statistics, number of projections, relative position of the sample andsvn add detector. Different reconstruction algorithms and filtering algorithms were implemented in order to obtainsvn add highest quality 3D models. This is actually possible thanks to the interdisciplinary work of professionalssvn add from different areas of knowledge.

The novel Cr1-xTixSe compounds have been synthesized for x = 0, 0.05, 0.10 and 0.15. Although both CrSe and TiSe are individually reported as NiAs-type phases, solid solutions in this system have not been previously synthesized. Structural characterization was made using X-Ray Powder Diffraction (XRD) data. All samples belong to the P63/mmc space group and share the nickel arsenide (NiAs) structure type. Chromium and titanium are known to have different oxidation states in selenide compounds, both varying between +2 and +4 oxidation states. In the case of study stoichiometry suggests a +2 oxidation state for the metals. However, the NiAs structure presents a very short cation-cation distance that can lead to some degree of bonding, affecting oxidation states. X-ray Emission Spectroscopy (XES) measurements were carried out in order to study the oxidation state of chromium in these new compounds. A high-resolution Kβ spectrum of a common chromium selenide is shown in Figure 1. By calculating the difference between the Kβ5and Kβ1,3 peak positions (DE) and comparing with appropriate standards, oxidation states can be inferred for each sample. All three substituted samples contain chromium in an average +2 oxidation state within experimental error. Additional sample characterization included resistivity measurements, which will also be discussed and complemented by the conclusions of the structural characterization as a whole.

Double perovskites Ba1+xLa1-xMnSbO6 were synthesized by traditional ceramic method in air as polycrystalline powders. The 0.1≤x≤0.2 compounds belong to the I 2/m monoclinic space group, while the x≥0.3 perovskites belong to the I 4/m tetragonal space group. Effective presence of mixture of Mn2+/Mn3+ has been well established by X-ray Emission Spectroscopy (XES) using high resolution Kβ emission for the set. The system Ba1+xLa1-xMnSbO6 displays signs of ferromagnetism at low temperature by magnetometry analysis. Also, Neutron Powder Diffraction data reveals that at 4 K, there is a presence of long range order that begins to disappear with increasing doping. We will show crystallographic and magnetic cell, magnetometry measurements, and XES measurements. Figure 1 – Room temperature Powder X-Ray Diffraction patterns for Ba1+xLa1-xMnSbO6 samples a) 0.1≤x≤0.4. and b) 0.5≤x≤0.7. Zoom view for the higher angles region for c) 0.1≤x≤0.4.and d) 0.5≤x≤0.7.

Para este estudio seleccionamos muestras de cerámicas y adobes del yacimiento de Cerro Cepero localizado en la comarca de Baza, Andalucía (España). Cronológicamente su fase de ocupación abarca desde la época del Bronce Final hasta el siglo VII d.C. Esa región tuvo diversas excavaciones irregulares desde hace muchos años, por diferentes equipos de arqueólogos. Y actualmente el yacimiento es objeto de estudio del Centro de Estudios de Arqueología Bastetana. En este yacimiento fue posible recuperar materiales cerámicos de gran relevancia y estudiar adobes de estructuras ibéricas, siendo la principal de ellas la muralla que aflora en la zona norte. La caracterización de las muestras fue hecha mediante el empleo de Difracción de Rayos X y Fluorescencia de Rayos X, teniendo otras técnicas complementarias como el estudio de Análisis de Imágenes, Análisis Petrográfica y Colorimetria. La Difracción de Rayos X fue utilizada para definir las fases mineralógicas que componen los adobes y las cerámicas, además de estimar su posible temperatura de cocción. El estudio de la composición química fue hecho mediante la Fluorescencia de Rayos X, donde se han discriminado los elementos mayoritarios y los trazas. Los datos obtenidos fueron tratados por el método de Análisis de Componentes Principales (PCA) con el fin de comparar las variables químicas.

Se preparó una solución (a temperatura ambiente) de 0,1 mL de trietilamina en 10 mL de tolueno. Posteriormente, se preparó otra solución de 4 mL de DMF con una mezcla de 0,2 g del nitrato de zinc hexahidratado [Zn(NO3)2.6H2O] y 0,08 g del ácido tereftálico diluido en 16 mL de tolueno. Las soluciones anteriores se mezclaron con agitación constante durante 16 horas. Finalmente se filtró al vacío, se secó el producto, obteniendo un sólido blanco con punto de fusión de 211°C. El rendimiento de la reacción fue de 51%. El compuesto fue caracterizado molecularmente por diversas técnicas analíticas y cristalográficamente por difracción de rayos-X obteniendo que cristaliza en el sistema monoclínico con constantes de celda: a = 23.689 (7) Å, b = 5.007 (5) Å, c = 23.349 (9) Å, ß = 115.93° (3) y V = 2491.21 Å3.

This work provides some applications of Total Reflection X-ray Fluorescence (TXRF) in the field of food analysis. The main reason for food analysis is because it is becoming more demanding safety and quality in this field by the regulatory agencies to ensure compliance with current standards. The concentrations of major, minor and traces elements were investigate by TXRF. A fast analysis allows an early detection before food could reach consumers. The following food samples were considered: wine, milk and cheese The samples may be separated in two different groups. The first two may be directly analyzed by TXRF, since they are liquid and can be diluted in water. The last must be digested to be analyzed in a microwave digester using nitric acid and oxygen peroxide. In the case of wines an important application is the classification of them through the elemental analysis as a fingerprint the possible vineyard. For milk, analysis of the elements it has an important role because it is one of the main nutrients for children. Furthermore dairy farms located in arsenicism areas were checked the presence of As in both milk and cheese samples. Milk and wine analysis was done directly over a dilution (1:5) of the samples. Cheese analysis needed a previous mineralization. In all case Ga (1mg/L) was used as internal standard. Total reflection X-Ray Analysis was perfomed in a S2 Picofox Bruker, X-rays from Mo tube at 50KV 0.6mA. . The accuracy of the measurements was calculated by determining the concentration of the elements in a standard solution (ICP-multielement standard solution). For milk samples the equipment was calibrate by adding elements that no are included in the sample in order to perform de sensitivity curves for K and L X- rays lines. In the case of wines calibration was performed using standard solution 20 % in ethanol. The results were satisfactory and allow propose the use of TXRF as a promising technique in the field of food analysis, in a wide scope, that is both environmental or quality control, or any other issues.

One of the most important preconditions in the analysis of historical/artistic materials is the use of nondestructive techniques. For this reason, X-ray techniques are the most popular and used in the analysis of these types of materials in Museums. The Energy Dispersive X-Ray Fluorescence (EDXRF) technique allows a nondestructive qualitative and quantitative multi-elemental analysis on various types of samples in Art/Archaeometry applications. This work analyzed ancient gold artifacts from different ages using an EDXRF portable system. Ten different types of gold samples were analyzed: earrings, pendants, figurines and clothing adornments. All samples analyzed are part of the gold collection of the Instituto de Pesquisa Histórica e Arqueologia do Rio de Janeiro (IPHARJ). The XRF analyses were performed using an EDXRF commercial system (ARTAX 200, Mo anode, 40 kV and 250 µA). The concentrations of Cu, Au and Ag were obtained from calibration curves obtained with gold standards of 24k, 18k, 16k, 14k, 12k and 10k. The results showed that the samples have different concentrations of gold. Thus, it was possible to classify the samples with respect to gold purity (karat gold). Besides that, two samples were classified as tumbagas since their copper and gold concentrations were very similar to those found in the literature.

Los medicamentos genéricos, ocupan cada día más un lugar de privilegio en el mercado nacional y mundial. La principal razón, se centra en el suministro de medicamentos a bajos costos que puedan ser asequibles a la población de escasos recursos económicos. Sin embargo, el suministro de medicamentos genéricos al ser humano, puede estar ligado a efectos secundarios o colaterales de gran impacto para la salud pública, debido a que no es únicamente necesario suministrar el principio activo específico, sino que además se requiere evaluar la forma cristalina de dicho principio activo (estudio del polimorfismo) y los excipientes que se proporcionan en el medicamento para garantizar que el genérico tenga la misma biodisponibilidad del medicamento original. En el presente trabajo se realizó un estudio estructural comparativo entre diversas presentaciones sólidas de la carbamazepina distribuidas en el área metropolitana de Bucaramanga (Colombia). Así mismo, se caracterizó molecular y cristalográficamente el principio activo de los medicamentos y se estudió el fenómeno del polimorfismo, evaluando el efecto de la temperatura y el solvente en el proceso de cristalización. Finalmente, se realizó la comparación de las formas polimórficas encontradas mediante la técnica de difracción de rayos-X de muestras policristalinas.

Nanomaterials present unique properties that strongly differ from those exhibited by bulk materials. Such singular features may be used to boost crop production. In this context, our group has been investigating the absorption, transport and metabolism of nanomaterials by plants. The present work has addressed the effects of nano ZnO on the germination of seeds of Phaseolus vulgaris. Seeds were soaked for 20 min in aqueous dispersions of 20, 40 and 60 nm ZnO at 1000 mg L-1. Germination was monitored during five days. The results showed that, compared to control seeds, 20 nm particles promoted the radicle development, whereas 40 nm and 60 nm prevented it. Aiming at understanding such effects, we have employed X-rays to monitor Zn behaviour. EDXRF analysis showed that Zn penetrates the seed coat reaching the embryo. For treated seeds Zn level goes from thousands to hundreds of mg kg-1 at the coat and embryo, respectively. In control seeds, it remains at tens of mg kg-1regardless the location. Figure 1a shows the distribution of Zn at the seed treated with 60 nm ZnO. The map indicates a gradient from the outer to inner region, Zn is mainly present at coat. µ-XANES was recorded at locations shown by Figure 1b. Conversely to control seed, Zn chemical species depends on the tissue nature. At the external part of seed coat, Zn remains as ZnO. At the middle of the coat it is mixture of ZnO + Zn-malate and at embryo it is found as Zn-hystidine + Zn-phytate. The seeds treated with 20 nm presented an important fraction of Zn-hystidine at the seed coat. Thus, at the current stage of our research, the results indicate that Zn-hystidine complex could be more beneficial for the seeds development. Figure 1 – (a) µ-XRF image showing Zn distribution (30 µm beam), (b) Magnified optical image highlighting the spots where µ-XANES (12 x 25 µm2 beam) were recorded and (c) Normalized Zn-K µ-XANES spectra. Seeds treated with 60 nm particles. Acknowledgement: This project has been funded by FAPESP Young Investigators Awards 2015/05942-0 and FAPESP Multi-User Equipment Grant 2015/19121. The µ-XANES measurements were performed at XRF beamline at LNLS, CNPEM. We are grateful to Dr. Carlos A. Perez and Douglas Galante for their assistance during beamtime.

A espécie Plagioscion squamosissimus, pertence à família Scianidae, conhecida popularmente como corvina ou pescada branca, sendo originária da bacia amazônica e amplamente comercializada nas regiões norte e nordeste do Brasil. Alimenta-se de peixes menores e camarões. Como peixe ósseo possui três pares de corpos inorgânicos chamados otólitos, cada par tendo um nome especifico. São eles: sagittae, lapillus e asteriscus, sendo o sagittae, em várias espécies, mais notório em dimensão e objeto de vários estudos. Otólitos são concreções calcárias em volta de uma matriz protéica, presentes no ouvido dos peixes ósseos (atrás dos olhos), com funções específicas de equilíbrio, sentido de direção e receptor de vibrações sonoras. Nele está contida informações da idade, crescimento, local de nascimento, padrões migratórios, determinação de eventos importantes no ciclo de vida do peixe. Com a determinação química inorgânica do otólito é possível saber como o peixe está interagindo com o meio, uma vez que biomineraliza os minerais que consome por meio de sua alimentação. Os otólitos utilizados para análise foram retirados de exemplares coletados na região pesqueira de Manacapuru, interior do Amazonas, Baixo Solimões, os mesmos triturados e aglutinados em pastilhas de ácido bórico para análise qualitativa e quantitativa no equipamento de fluorescência de raios-x por dispersão de ondas. Os elementos encontrados nas amostras foram Ca, Na, Al, Si, P, S, Cl, K, Fe, Sr, Ag, Rb e Mo, sendo o cálcio presente em maior quantidade, uma vez que os otólitos são concreções calcárias sob a forma mineral de aragonita.

During the last 20 years the archaeological research in the Oriental Pyrenees, especially in the Cerdanya region (Girona, NE Spain), has evidenced the presence of an important Iron Age population, the Cerretani, mentioned in the ancient literary sources. They occupied the central valleys of the eastern Pyrenees, from the planes (up to 1100 m. asl) to the main hills and the pasture lands (up to 2.000 m. asl). This cerretani were settled in several oppida, the typical Iron age hill forts, of modest dimensions (0,6 Ha.), placed along the course of the Segre river. The main site discovered, the Castellot oppidum (Bolvir), has been excavated in the last ten years, showing the presence of a limited population (about 200-250 people) since the beginning of the 4th c. B.C. The excavations have shown the presence of an Iberian community but with some specificities, like the importance of the livestock strategies or the low presence of imported materials. The recent discovery of several objects in archaeological context in the Oriental Pyrenees (la Cerdanya region, Catalonia) has aroused the question of the Roman presence in this mountain area, and the development of some metallurgical activities in this previously considered marginal zone. . About the middle half of 2nd c. B.C. these cerretani oppida were remodelled, as we have documented: the setting up of a new urbanism, the opening of a fortified gate, and specially the uses of new metallurgical technologies, show the potential impact of the Roman presence, probably in a military context. Coming from different sites, we have collected some metallurgical objects (earring, rings and coins) that use gold and silver in an elaborated technology, and pointed out the question of the use of gold in pre-Roman and Roman times in this Pyrenean area. The use of gold and silver in some objects has to be also connected with the recent identification of a metallurgical workshop in the Castellot site, dating from the 2nd half of 2nd c. B.C. It seems the technology of the Gold earring from the Castellot site, and specially the gilded ring from Baltarga, had to be connected directly with the Roman military presence in the region from the middle 2nd c. B.C. The iron and silver ring found in the archaeological sites evidence also the use of a complex metallurgical technology, characterized by X-ray techniques, by the local communities' long time before the Roman presence, and likely the knowledge and exploitation of silver and gold resources.

Antoni Gaudí was an architect from Catalonia, Spain, who belonged to the Modernist (Art Nouveau) movement and was famous for his unique style and highly individualistic designs. Gaudi is the author of many of the most famous and representative buildings of Barcelona architectural landscape, such as the Sagrada Familia basilique, the Park Guell, Guell Palace, Casa Milá and Casa Batlló. Gaudí studied at the High School of Architecture in Barcelona from 1873 to 1877, obtaining the title of architect in 1878. The newly named architect immediately began to plan and design innovative buildings, and collaborated with the School his entire life. The Modernist movement was prodigious in its use of ceramics not only in Catalonia, but also in other places throughout the Iberian Peninsula or in many other European countries. Ceramics are certainly omnipresent in Gaudí’s work; their use is perhaps one of their most distinctive characteristics. In 1879, Gaudí’s name first appeared on the books of the Pujol I Bausis ceramic factory which mention a shade of yellow called “Gaudí.” This suggests that from his very first projects, Gaudí used ceramic tile overlay as an essential component of his work. All of Gaudí’s works display a notable wealth of ceramic decoration, well represented in one of its first work: Casa Vicens, built between 1883 and 1888. It is significant because it is an outstanding work dominated by ceramic elements with widely contrasting chromaticism. Casa Vicens was named a UNESCO World Heritage Site in 2005 along with a selection of the architect's other works. Nowadays the home is being restored and it is planned to be opened as a museum next year. Casa Vicens suffered several architectural modifications around 1925 and also some restoration ending the 1990's. In each in each of these modifications some of the tiles were replaced with new identical colour but different manufacturing process. The aim of the present work is focussed on identifying the composition of the body ceramic pieces and the characterization the glazes, approaching to their production techniques and the process they were decorated. The complete characterization of the materials used in Cultural Heritage monuments is a crucial step, enabling to make decisions about restoration and preventive conservation methods. We mainly used non-invasive instrumentation, such as "in-situ" and laboratory Energy dispersive X-ray fluorescence, X-ray diffraction, SEM/EDX and optical microscopy.

Nowadays, the production and use of engineered nanomaterials (ENMs) for industrial applications has been grown. Among the different types of ENMs, metallic nanoparticles have been increasingly used, being silver nanoparticles (AgNPs) one of the most utilised due to their antibacterial properties. Because of the expansion of their fabrication, the release of these emerging pollutants into the environment has enhanced, especially in soils that are the main fate. Consequently, vegetables that grow in agricultural soils can absorb AgNPs suspended in soil fluids. Therefore, it is important to develop and improve analytical techniques in order to monitor these particles in the environment. With this purpose, we tested the possibilities of using total X-ray reflection spectrometry (TXRF) to monitor the silver content in soil adsorption kinetic studies and in the evaluation of AgNPs bioavailability to vegetal samples. For soil adsorption studies, an amount of soil was put in contact with a volume of a solution containing the analyte (AgNPs). Then, the analyte in the supernatant was monitored over the time, allowing its adsorption kinetics study on the soil. For TXRF analysis of soil extracts, it was found that using a deposition volume of 10 μL and a measuring time of 2000 s the limit of detection of Ag (Ag-Kα detection) was around 40 μg·L-1, which was suitable to carry out this kind of lab-controlled studies. TXRF results were compared with those obtained by inductively coupled plasma optic emission spectrometry (ICP-OES) and good agreement was found. Furthermore, we explored the possibilities to analyse directly the Ag adsorbed in the soil after performing the kinetic studies. In this case, the limit of detection for Ag using 50 mg of soil was around 1.5 mg·Kg-1. Results obtained using such approach was compared with those obtained after acidic microwave digestion of the soil and similar values were obtained. The evaluation of the transference of AgNPs to crops was performed through hydroponic experiments. These experiments consist on growing the plant in a hydroponic solution that contains the analyte. In this study, lettuces were grown in hydroponic media containing AgNPs or ionic silver (Ag+) during 9 days in lab-controlled conditions. After 9 days, an acid microwave digestion of the vegetal samples (roots and leaves) was done. The TXRF analysis of vegetal digests was performed using the same instrumental conditions as the soil kinetics studies. In the results obtained, the uptake AgNPs or Ag+ by roots was confirmed but not translocation to leaves. Results obtained were also compared with those obtained by ICP-OES. In conclusion, TXRF spectrometry can be considered a faster, simpler and cost-effective tool for AgNPs determination in soil adsorption studies as well as in investigations of their exposure to vegetables. It uses small sample volumes and it provides simultaneous multi-elemental information that can be useful to improve the understanding of the controlling factors on Ag mobility and bioavailability.

Presentamos el efecto estructural y composicional del aluminio en nanopartículas de ZnO sintetizadas mediante el método de sonoquímica, la impurificación con aluminio se hace in situ y varía de 0 al 2% atómico. Para la síntesis se empleó nitrato de zinc hexahidratado (Zn(NO3•6H2O) e hidróxido de amonio (NH4OH) y AlCl3 (fuente del ión Al+3) en medio acuoso. Se estudio el efecto del tiempo de irradiación ultrásonica para la obtención del material. La cristalinidad fue evaluada mediante Difracción de Rayos X (XRD) indicando la presencia de la estructura hexagonal tipo wurtzita, con orientación en el plano (002) y la composición se realizó mediante Fluorescencia de Rayos X, de longitud de onda dispersiva (WDXRF). La espectroscopia Raman confirmo la presencia de la fase. Se determinó el valor de banda prohibida mediante la caracterización óptica y se estudio el efecto del dopante sobre la estructura cristalina.

os compuestos de la familia tipo Ruddlesden-Popper (K2NiF4) como La4LiNiO8 y Nd4LiNiO8 pertenecientes al sistema cristalino tetragonal (I4/mmm) fueron sintetizados mediante la ruta nitrato-citrato (método Pechini), permitiendo así la obtención de una fase pura a baja temperatura y corto tiempo de calcinación. Para su preparación, se empleó un 50 % de exceso de hidróxido de litio, con el objetivo de estabilizar el alto estado de oxidación del metal de transición en el material [1]. El estudio de las fases cristalinas se llevó a cabo mediante el refinamiento Rietveld/Lebail con el fin confirmar los valores de las constantes de celda. El estudio de reactividad química de los compuestos preparados con los materiales 8YSZ ((ZrO2)0.92(Y2O3)0.08)0.926 y 10GDC (Gd0.10Ce0.90O1.95), que son los electrolitos más usados para las celdas SOFC, se llevó a cabo a una temperatura de reacción de 850 °C durante 3 horas con flujo de aire. Los materiales estudiados presentaron difusión de iones al ponerlos en contacto con los electrolitos dando lugar a la formación de otras fases; sin embargo, se encontró una cierta compatibilidad en el caso de 10GDC en comparación a 8YSZ.

O ferro é um importante elemento no transporte respiratório do oxigênio e dióxido de carbono e nas enzimas envolvidas no transporte celular. A anemia ferropriva é um problema de saúde pública no mundo que afeta cerca de dois bilhões de pessoas, especialmente nos países em desenvolvimento. No Brasil os programas de prevenção e tratamento da anemia fazem a reposição do ferro utilizando de forma padronizada o sulfato ferroso devido ao seu baixo custo aliado à sua alta biodisponibilidade. Neste estudo foram preparadas amostras com quantidades conhecidas de F2SO4 em base de celulose e construir uma curva apropriada para identificação rápida de conteúdo deste material em medicamentos adquiridos no comércio. Foram produzidas amostras e com duas granulometrias e com quantidades de F2SO4 entre 80 e 375mg por grama de celulose, de modo a observar a influência da granulometria no resultado. As amostras produzidas foram medidas num sistema de XRF da Amptek com tubo de raios X com anodo de Au (com tensão de 20keV e corrente de 20µA)e espectrômetro 123 (SDD). Os resultados mostraram que para quantidades até 300mg/g a resposta é linear e essa técnica pode ser utilizado neste tipo de amostra. Novas medidas estão sendo feitas com base de lactose, pois são estas as bases mais utilizadas em medicamentos comerciais.

El algoritmo para reconstrucción tridimensional de imágenes tomográficas más usado en la actualidad es el algoritmo FDK. Dependiendo del tamaño y la cantidad de radiografías de entrada y las dimensiones de las imágenes de salida el costo del procesamiento computacional puede ser elevado. Con el objetivo de acelerar el procesamiento varios trabajos han sido desarrollados usando diferentes configuraciones de hardware para procesamiento paralelo. En el presente trabajo presentamos los resultados de la paralelización del algoritmo FDK usando procesadores multicore (PM) e unidades gráficas de procesamiento (GPUs), las muestras usadas para testes fueron dados reales de tomografias. Las tablas 1 y 2 muestran los resultados alcanzados para las versiones paralelas del algoritmo en los dos hardwares paralelos testados. Para los testes fueron utilizadas tres muestras de diferentes tamaños 1 (400x308 pixels), 3 (1024x1024 pixels) y 4 (2000x1048 pixels). La versión paralela para GPUs fue testada en dos GPUs de diferentes capacidades GPU3 (NVIDIA GT 740M) y GPU4 (NVIDIA TESLA20KM). La versión paralela para PM fue testada en dos procesadores XEON E5-2420 Hexa Core de Intel, disponibilizando 12 núcleos físicos y 12 núcleos hypertreading. Las dos versiones paralelas del algoritmo consiguen acelerar el procesamiento. De los dos hardwares testados las GPUs consiguieron la mayor aceleración, sin embargo la limitada capacidade de memória de las GPUs disponibles actualmente no mercado limita su uso para paralelizar este tipo de aplicaciones. Considerando los resultados obtenidos, los costos financieros de los hardwares testados e los costos de desarrollo de las aplicaciones paralelas; sugerimos que para paralelizar el algoritmo FDK resulta más viable usar procesadores multicore en vez de GPUs.

Las celdas solares de películas delgadas están conformadas por capas de diferentes materiales, constituidas por dos contactos eléctricos, la capa absorbente y la ventana óptica. El objetivo principal en el avance tecnológico de estos dispositivos fotovoltaicos es reducir el precio de fabricación de los sistemas, desarrollar nuevos materiales con bajo nivel de toxicidad y que tengan las propiedades adecuadas para la fabricación de celdas solares, los cuales le permitan ser competitivos frente a las fuentes convencionales. En este trabajo se propone la síntesis y estudio de la composición química, morfología, propiedades estructurales y ópticas de los materiales ZnS, Zn(1-x)In(x)S y Zn(1-z)Nd(z)S. Los compuestos azufrados se depositaron sobre sustratos de cuarzo por la técnica sol gel mediante Spin-coating y posteriormente la sulfurización de las películas delgadas. Para la caracterización detallada de los recubrimientos se emplearon las técnicas de fluorescencia de rayos X (FRX), microscopia electrónica de barrido (SEM), difracción de rayos X (DRX), y espectroscopia UV-Vis. Un análisis cualitativo de los difractogramas empleando el programa Search March, confirmó la presencia de las fases cristalinas en estudio. Igualmente, mediante la fluorescencia de rayos X se realizó el análisis químico de los recubrimientos y se corroboró la concentración de cada uno de los elementos presentes en el compuesto. Los resultados obtenidos son de interés especial para evaluar su aplicación potencial como ventana óptica en celdas solares.

In interventional procedures using fluoroscopy, the medical staff is exposed to ionizing radiation, often above the limit allowed to occupationally exposed individuals and are only seen at the end of the procedure or after a month when using individual dosimeters. The aim of this study was to develop a system to estimate the equivalent dose of ionizing radiation in real time during the interventional medical procedure using fluoroscopy. The performance of the remote-controlled fluoroscopy system of scattered radiation measurements was operated at 50 kVp and 30 mA and 9DP model ionization chamber Ludlum and phantom PMMA. Dose rates were collected by the ionization chamber for the regions of the gonads, 90 cm, the trunk 128 cm eyes, 166 cm and the distance of the main beam 19, 38, 76 and 152 cm, alternately turning 45.O and 45.O around the fluoroscopy table. The rates above 10μSv/h doses and the reproducibility of the measurements were considered. The criterion of Chauvenet was used to eliminate the discrepant results data, and were calculated the mean and standard deviation for each position. The result of this selection was used to construct isodose curves using interpolation techniques. System linearity tests were conducted by varying the voltage obtaining the correlation coefficient of 0.97 and 0.99 respectively for the interventional physician and nurse positions. For viewing in real time dose rates ionization chamber was set at the top of the fluoroscopy table as a fixed reference point. The collected data were sent to the computer to determine the dose rates estimated indirectly in relation to the predetermined isodose and positioning of the medical staff in interventional procedure. Dose rates and the estimated cumulative dose are shown in real time via a TV monitor located visibly showing the intensities of dose rates with a visual indication of color scale to the doses received by members of the medical team. Student's test was used to validate the system with p < 0.05. The exposure of ionizing radiation was reduced when the medical team changed its position or increasing distance in relation to the main beam during the interventional procedure.

En esta investigación se estudia la transformación y reducción térmica de mineral de ilmenita pulverizado ~ (75µm) al pasar a través de una antorcha modificada de acetileno bajo condiciones reductoras y el diseñado de la antorcha es realizado por los autores y debe proveer los medios de obtención de dichas partículas. Se analiza el proceso desde el punto de vista termodinámico por medio de minimización de energía libre de Gibbs obtenidas mediante el software CSIRO Versión 5 y se describen las diferentes etapas del proceso hasta alcanzar la formación de las partículas de carburo de titanio y hierro. Por medio de una serie de simulaciones en diferentes herramientas, se determinan distribuciones de temperatura, análisis estructural del funcionamiento del sistema y comportamiento de las partículas. Posteriormente se realizan ensayos experimentales de una muestra de ilmenita pulverizada, para corroborar las condiciones de experimentación planteadas. Donde la ilmenita se descompone y se produce la nucleación de partículas de carburo de titanio sólidas, las cuales sirven de núcleos para la condensación posterior del hierro en estado líquido. El producto obtenido fue caracterizado por medio de difracción de rayos X (DRX), estos resultados indican un grado significativo de segregación del (Fe) sobre el carburo de titanio (TiC).

Los materiales zeolíticos son conocidos por su capacidad de intercambio catiónico, absorción y adsorción de molécula gaseosas en sus poros, como soportes enzimáticos y agregados alimentarios. Las propiedades descritas anteriormente dependen de su equilibrio superficial y de los poros de los grupos hidroxilo e hidrogeniones, los cuales se pueden modificar al aplicar intercambios iónicos. En el presente trabajo se sintetizaron sodalitas sódicas a partir de materiales de desecho y luego se sometieron a intercambio iónico con soluciones de cloruro de amonio a diferentes condiciones y tiempos de exposición en ultrasonido. Los sólidos obtenidos se caracterizaron estructuralmente mediante el método de Rietveld empleando el software comercial RIQAS, apoyados en los resultados de Flurescencia de Rayos-X, Resonancia Magnética Nuclear de Sólidos y Espectroscopia Raman; concluyendo que a mayor porcentaje de N3- sustituido en la ocupancia del Na+, mayor precipitación de sulfato, logrando un 60% de remoción del anión presente en 16mL de una solución 0,02M CuSO4 Authors express their acknowledgement to Universidad Industrial de Santander and Laboratorio de Rayos-X, Parque Tecnológico Guatiguará-PTG (Bucaramanga-Colombia) for data collection

A resistência à compressão do concreto é uma propriedade fundamental do material, estando diretamente relacionada com a estrutura da matriz cimentícia. Verifica-se que a presença de poros na matriz cimentícia diminui essa resistência, onde além da quantidade de poros, devem ser consideradas também a área específica e a distribuição dos poros por tamanho. Estes fatores influenciam diretamente na resistência do material. Devido à variação das dimensões dos poros, bem como às suas formas irregulares, as técnicas tradicionais variam desde operações e equipamentos simples até muito sofisticados, ocasionando diferenças significativas nos resultados. Este trabalho apresenta um método de ensaio não destrutivo (END) para obtenção da porosidade do concreto utilizando microtomografia por Raio X com processamento de imagens digitais para caracterização da distribuição, tamanho e volume dos poros presentes na matriz cimentícia. Foram utilizadas imagens microtomográficas das amostras de concreto de 20MPa e 30Mpa com 256 tons de cinza, ajustadas em contraste, binarizadas e filtradas para a caracterização da distribuição, volume e tamanho dos poros na matriz cimentícia. Os resultados dos valores de porosidade mostram compatibilidade entre o método apresentado e o método proposto pela NBR 9778 (2009).

El compuesto MoO2Cl2-4,4-dimetilbipiridina se obtuvo a partir de de la disolucion de 238,mg MoO2Cl2 (1.2 equiv) en 10ml de diclorometano seco bajo atmosfera de nitrogeno en un schlenk, al cual se le adicionaron lentamente 184 mg de dimetilpiridina disueltos en 10ml de diclorometano seco bajo atmósfera de nitrógeno. La reacción se agitó durante 3 horas a temperatura ambiente protegida de la luz. La mezcla de reaccion se filtró al vacio y el sólido resultante se lavó varias veces con éter etílico para obtener un sólido gris. La caracterización cristalográfica muestra que el compuesto cristaliza en el sistema monoclínico con constantes de celda: a=12.014(4)Å b=10.375(5)Å c=11.784(5)Å ß=103.233° V=1429.74 Å3

Nowadays, renewable energy resources as well as more efficient energy storage systems have taken a starring role, since more sustainable energy systems are being demanded due mainly to the increasing needs of modern society together with the collateral effects of conventional energy sources. This situation has driven to a search for improved electrochemical storage systems that can safely store energy from sustainable sources, proving the energy needed, for example, for transportation and residential uses. As an example of everyday technology, the use of portable electronic devices has been feasible thanks to the lithium-ion batteries (LIB). The energy storage capacity of the LIB system is 5 times higher than lead-acid batteries, and it shows an average voltage of 3.8 V per cell in comparison with the average 2.0-2.2 V of the lead-acid batteries. In addition, lithium-ion batteries have the advantage of lower weight, higher energy density and faster charge and discharge rates compared to other similar battery technologies. Even though they are the most widely batteries employed in portable electronics, it is important to attend several issues regarding safety, and to improve its energy storage capacity in order to be used at larger scales, in, for example, electric vehicles. Lithium titanate, Li4Ti5O12 (LTO), is a promising candidate for anode material at the moment because of many its advantages. Due to this, a better knowledge regarding the LTO structure and how changes are related with its ulterior performance is of great importance. In this work, Resonant Inelastic X-ray Scattering (RIXS) has been used for studying titanium local environment changes in the LTO molecule when different levels of charge are applied. As complementary technique, XANES spectra of the Ti-K edge were also measured. The measurements were carried out at the Brazilian Synchrotron Light Source (LNLS, Campinas) in the D09B beamline and at ELETTRA Sincrotrone Trieste (Italy) in the IAEA end-station of the XRF-beamline. Several samples with different levels of charge (not charged, partially charged and fully charged) were studied. Reflection geometry was used together with monochromatic photons of 4900 eV (just beneath the K absorption edge of titanium) for the RIXS measurements and XANES spectra were acquired scanning the incident beam energy in the range 4930-5080 eV, i.e., around the Ti-K edge. For data analysis, and in order to discriminate the changes on the titanium chemical state of the LTO molecule, Principal Component Analysis (PCA) was used on both RIXS and XANES spectra. The results show that RIXS allows the detection of minor changes in the structure of the lithium-based compound due to the particular level of charge. In this way, typical chemical studies as the ones performed with conventional absorption techniques (XANES, EXAFS) can be achieved with this technique, with the advantageous characteristics of shorter measuring times and suppressing any energy scan during the analysis, between others.

El compuesto MoO2Cl2-4,7-dimetilfenantrolina se obtuvo a partir de la disolución de 238 mg de MoO2Cl2 ( 1.2 equiv) en 10 mL de diclorometano seco bajo atmósfera de nitrógeno en un schlenk al cual se le adicionaron lentamente 28mg de 4,7-dimetil-1,10-fenantrolina disueltos en 15 mL de diclorometano seco bajo atmósfera de nitrógeno. La reacción se agitó durante 4 horas a temperatura ambiente protegida de la luz. La mezcla de reacción se filtró al vacío y el sólido resultante se lavó varias veces con éter etílico para obtener un sólido gris. Posteriormente se realizó la caracterización cristalográfica por difracción de rayos-X policristalinas, encontrando que el compuesto de interés cristaliza en el sistema monoclínico con constantes de celda celda: a = 12.918 (4) Å, b = 9.768 (2) Å, c = 11.998 (4) Å, ß = 101.68° (2) y V = 14826.61 Å3

O estudo dos ossos e de suas características histomorfométricas é fundamental para a correta classificação de várias espécias de animais. Estas medidas, em sua maioria, são feitas através da separação dos tecidos ósseos dos demais tecidos biológicos da amostra e posterior medição. É muito comum o uso de técnicas como a diafanização e a maceração no estudo de vertebrados. Estes processos, apesar de amplamente utilizados, são processos destrutivos que em muitos casos não pode ser aplicado devido ao tamanho reduzido dos ossos de alguns exemplares. Para contornar estas limitações o uso de técnicas de diagnósticos por imagens não destrutivas tem sido amplamente utilizado para a obtenção das informações volumétricas internas e externas dos ossos. Neste trabalho utilizamos a microtomografia computadorizada para aquisição destas informações. Agregando a este cenário uma crescente oferta de tecnologias para prototipagem rápidas a custos cada vez mais reduzidos, torna possível com auxílio de software de CAD a construção de modelos biológicos que permitem a reprodução de inúmeras réplicas da estrutura óssea. Estes modelos podem ser reproduzidos em diferentes dimensões, posições e materiais, tanto na parte externa ou interna do osso. No entanto, este é um processo complexo que exige a manipulação das imagens por diversos programas específicos até a obtenção do modelo tridimensional a ser prototipado. Os resultados obtidos em ossos de codornas (Coturnix Coturnix) e em pequenos sapos da espécie Proceratophrys bigibbosa, mostraram o grande potencial de aplicação desta ferramenta computacional na construção de biomodelos para estudos biológicos e didáticos de pequenos animais.

Cancer is a worldwide public health problem, and its incidence in the world grew by 20% in the last decade. Zinc, an essential trace element, is involved in many cellular processes. The main function of the prostate is the high production and secretion of citrate which is possible due to the unique accumulation of zinc by prostatic epithelial cells. In relation to prostate cancer, it can inhibit the growth of tumor cells, due to the stop of cell cycle and / or induction of apoptosis. The X-ray microfluorescence technique (μXRF) is a tool for modern analysis of elemental composition of different samples with high sensitivity and negligible damage to the sample. This study investigated the behavior of cells in spheroids of human prostate cells, tumor cell line (DU145) and normal cell line (RWPE- 1), after supplementation with zinc chloride by 24 hours and 48 hours using synchrotron X-ray microfluorescence (µSRXRF) and analyzed cell viability through colorimetric cytotoxicity assay (MTT). The measurements were performed with a standard geometry of 45º of incidence, excited by a white beam using a pixel of 25 μm and a time of 300 ms/pixel at the XRF beamline at the Synchrotron Light National Laboratory (Campinas, Brazil). The results by µSRXRF showed that Zn intensity decreased in tumor cells despite supplementation and the treatment time, while in normal cells that intensity increases with supplementation and the treatment time. MTT assay's results were not significant, which indicates that the cell viability was not changed, regardless of treatment in both cell types tested, so the cells are viable.

Se disolvieron 238,mg de MoO2Cl2 (1.2 equiv) en 10mL diclorometano seco bajo atmosfera de nitrógeno en un schlenk, al cual se le adicionaron lentamente 184 mg de dimetilbipiridina disueltos en 10mL diclorometano seco bajo atmosfera de nitrógeno. La reacción se agitó durante 3 horas a temperatura ambiente protegida de la luz. La mezcla de reacción se filtró al vacío y el sólido resultante (3) se lavó varias veces con éter etílico para obtener un sólido gris. La caracterización molecular se realizó por diversas técnicas instrumentales y la caracterización cristalográfica por difracción de rayos-X de muestras policirstalinas, obteniendo que el compuesto de interés cristaliza en el sistema monoclínico con constantes de celda: a = 22.343 (1) Å, b = 4.923 (3) Å, c =17.176 (1) Å, ß = 99.78° (6) y V = 1861.71 Å3.

A utilização de técnicas não destrutivas na análise de material arqueológico é recomendada a fim de garantir sua preservação. Neste estudo foi analisada uma moeda do Império Romano datada do século IV D.C. do governo de Constantine II. Sua composição química superficial foi obtida de forma qualitativa através da técnica de Fluorescência de Raios X por Energia Dispersiva (EDXRF) e a homogeneidade da liga foi avaliada por Microtomografia Computadorizada (µ-CT). A leitura por EDXRF em três pontos distintos da moeda é apresentado na Tabela 1. É possível perceber um aumento da quantidade de prata e chumbo no ponto b em relação aos outros pontos medidos. A µ-CT revelou uma variação de densidade na superfície da moeda, especialmente na região do ponto b, como pode ser observado na Figura 1. Estes resultados são compatíveis com o processo térmico/mecânico conhecido como enriquecimento superficial de prata, que promove a migração destes metais para a superfície e confere um brilho prateado à moeda.

O mapeamento da concentração de elementos químicos, através da fluorescência de raios-X é um importante elemento no estudo de amostras superficiais, como pinturas e quadros. Existem sistemas de fluorescência industriais que são fabricados para tal fim, mas, além de serem demasiadamente custosos para o pequeno usuário, são específicos para determinadas faixas de dimensões de amostras e limitam o pesquisador ou usuário a um procedimento padrão, não dando liberdade a variações metodológicas e novos tratamentos dos dados. Os equipamentos portáteis normalmente não são fabricados para tal finalidade, mas podem ser adaptados com os ajustes certos. Ter o controle sobre o procedimento passo a passo tanto do equipamento, quanto do software que faz a reconstrução deste mapa é um passo importante para utilização em casos adversos e a implementação de novidades dentro desta técnica. Desta forma, a criação de algoritmos, que variam do padrão e possibilitam ao usuário improvisar e criar alterações nas rotinas, tanto computacionais quanto experimentais seria um fator interessante para contornar alguns tipos de dificuldades. O presente trabalho pretende criar um algoritmo para a criação de imagens de mapa de concentração a partir de arquivos resultantes de medidas de fluorescências de raios-X pontuais, implementando, quando possível, rotinas de pré e pós-processamento. Este último visando combinar os resultados com outras técnicas de medidas O algoritmo será criado e executado inicialmente na linguagem computacional matemática OCTAVE, que já possui pacotes próprios e simples para trabalhar com aquisição e manipulação de imagens, sendo de código fonte aberto. Os dados experimentais serão extraídos manualmente de um equipamento de fluorescência portátil, e toda a adaptação necessária tenderá a ser minimizada por soluções computacionais. Variações de modos de aquisição, para diferenciar medidas, otimizar tempo de aquisição de dados e até otimizar a qualidade das imagens poderão ser aplicados também para a melhoria dos resultados.

La validación de los métodos analíticos permite al laboratorio asegurar, mediante evidencia objetiva, que los resultados emitidos aplicando dicho método son confiables. Actualmente, está muy difundida la sistemática para validar métodos cuantitativos; sin embargo cuando se intenta aplicar en cualitativos no es fácil definir la metodología a aplicar. La fluorescencia de rayos X por reflexión total permite determinar en forma simultánea la presencia de elementos desde el Na hasta el U, en una mínima muestra liquida o suspensión que es evaporada en un portamuestra, obteniendo un espectro dispersivo en energía característico. El objetivo del trabajo fue establecer una metodología para determinaren forma inequívoca presencia de elementos en una muestra con un tratamiento estadístico de datos. La técnica a validar involucra la determinación simultanea de elementos desde el S (Z=16) al U (Z=92) con excepción de Mo, en muestras acuosas y en suspensiones. El procedimiento para la medición de muestras acuosas o suspensiones incluye la toma de una alícuota de 5ul en soportes adecuados de cuarzo (discos de 3cm de diámetro), los cuales se llevan a sequedad bajo lámpara IR. Luego de la evaporación, el residuo es excitado en el espectrómetro y finalmente, se adquiere un espectro dispersivo en energía característico de la muestra. El tiempo de medición se establece en 300 segundos para todas las muestras. Los parámetros seleccionados para evaluar el método fueron la selectividad y el límite de corte. En cuanto a la selectividad, la fluorescencia de rayos X implica la medición de longitudes de onda específicos para cada elemento. Asimismo, como todo método analítico no cuantitativo, se evalúa mediante un comportamiento dicotómico y como respuesta analítica se obtiene una distribución binaria en el formato de resultados positivos y negativos. La interacción entre ellos y el grado en que influyen en la determinación de una muestra están dados por el límite de corte. Para establecer los valores del límite de corte se trabajó con soluciones estándares de Ni, K, Fe y U en concentraciones cercanas a 0,005 mg/L.v Las verificaciones de los limites para los elementos desde el K hasta el U se realizaron con soluciones multielementales trazables al NIST. Se realizaron ensayos independientes de 20 blancos que permitieron verificar los cálculos de límites de detección emitidos por el equipo y más de 30 muestras con soluciones estándares a concentraciones variables de sólidos disueltos. Las mediciones se realizaron en un espectrómetro fluorescencia de rayos X por reflexión total (TXRF) S2 Picofox (Bruker) con tubo de Mo, con potencia máxima de 50W, detector tipo SDD con área de 10mm2 y resolución de 160 eV. Los portamuestras empleados fueron de cuarzo y el tiempo de medición seleccionado fue de 300 segundos para los blancos, los estándares y las muestras. Este método validado actualmente es empleado en forma rutinaria para muestras acuosas o en suspensión provenientes de distintas áreas de las centrales nucleares e industrias afines (CONUAR, NASA, etc.) donde se requiere la detección temprana de elementos trazas que puedan estar presentes: polvos residuales provenientes de fisuras en tuberías, impurezas en pastillas de uranio, impurezas en efluentes, etc

Enxofre, vanádio e níquel são contaminantes naturais importantes para estudos geoquímicos de origem e classificação do petróleo. Entretanto, as suas presenças são prejudiciais para a qualidade do petróleo e dos produtos, pois são associadas à corrosão de equipamentos, às desativações dos catalisadores de craqueamento e de hidrotratamento e à poluição atmosférica. Com o propósito de obtenção de uma metodologia alternativa aos métodos oficiais (ASTM D2622, ASTM D5863, ISO 14597 e ISO 51790, por exemplo) que utilizasse menores quantidades de amostra e de solvente, abordagem simples de correção do efeito matriz e instrumentação analítica acessível foi desenvolvido um método onde esses analitos são quantificados em filmes finos de petróleos por meio de um espectrômetro EDX comercial de bancada e de baixa potência. Os resultados da validação mostraram que a metodologia é suficientemente sensível (limites de detecção de 0,02 % em massa para o enxofre, 0,8 mg/kg para o vanádio e 1,0 mg/kg para o níquel), seletiva, robusta, acurada (recuperações médias de 100,3 % para o enxofre, 98,7 % para o vanádio e 99,7 % para o níquel) e precisa (precisões globais médias de 7,1 % para o enxofre, 5,3 % para o vanádio e 5,2 % para o níquel) para finalidades acadêmicas e industriais quando aplicadas para petróleos similares aos brasileiros (traços de vanádio e níquel e enxofre até 1 % em massa). As amostras devem ter o parâmetro BSW enquadrado (teores de água inferior a 0,5 % em volume e de sais e sedimentos menores que 275 mg/L), pois as precisões são sensíveis a teores elevados de cloro no petróleo.

O teor de biodiesel no diesel, em volume, aumentará dos atuais 7 % até 10 % em 2019, podendo chegar a 15 % se os testes e os ensaios com motores validarem essa adição. O Programa de Monitoramento da Qualidade dos Combustíveis da ANP referencia as normas ASTM D5453, ASTM D2622, ASTM D4294, ASTM D7039 e ABNT NBR 14533 para a determinação de enxofre em diesel comercializado no Brasil que, à exceção da primeira, baseiam-se na espectrometria de fluorescência de raios X, cuja acurácia depende da correta correção do efeito matriz. Tendo isso em mente, foram estudados o efeito matriz devido à presença de biodiesel, ou seja, de oxigênio, na intensidade de emissão da radiação S-Kα de amostras de diesel contendo traços de enxofre e algoritmos de correção do efeito matriz por meio de coeficientes de influência empíricos e teóricos. A avaliação da estatística erro relativo mostrou que o algoritmo de De Jongh considerando o oxigênio foi o que melhor corrigiu o efeito do oxigênio na quantificação de enxofre em misturas de diesel S5 e S10, ambos contendo até 10 % de biodiesel em volume.

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.

Neste trabalho 68 contas de vidro encontradas no sítio arqueológico do Cais do Valongo na zona portuário do Rio de Janeiro foram analisadas usando a técnica de fluorescência de raios de raios X (XRF). Para análise por XRF as contas foram separadas seguindo as suas formas e coloração: nove de cor branca e cilíndricas, quinze de cor vermelha e cilíndricas e quarenta e quatro de cor azul e facetadas. Para a análise das contas foi utilizado um sistema comercial de XRF (ARTAX 200 - Bruker) composto por um tubo de raios X com anodo de Molibdênio e um detector XFlash. As condições operacionais de análise foram: 35 kV, 500 µA e tempo de exposição de 600 s. Foi possível detectar 16 elementos: Si, K, Ca, Ti, Mn, Fe, Co, Ni, Cu, Zn, As, Rb, Sr, Sb, Pb e Bi. Na análise dos resultados utilizou-se a correlação de Pearson, a fim de se observar como as variáveis se comportavam entre si, e a análise de componentes principais (PCA) a fim de investigar possíveis semelhanças ou diferenças entre as contas de acordo com cada conjunto de cores. Associado ao PCA também foi realizada a análise por agrupamento hierárquico (HCA). Os resultados mostraram que o grupo de contas brancas se separou em dois grandes grupos e em duas contas que se separam entre si e dos grupos; uma devido a contribuição maior de Ca e a outra devido as contribuições de Cu e Zn. Apenas nas contas brancas foi detectado o elemento Sb que é normalmente utilizado na formação dos vidros brancos opacos No caso das contas vermelhas, observou-se a separação das contas em três grupos e uma conta que se separou dos grupos (grandes concentrações de Cu e Pb). As contas azuis apresentaram a formação de três grupos e uma conta que se separou bastante das outras contas azuis devido a grande concentração de Pb. Assim, com o uso da técnica de fluorescência de raios X e análises por PCA e HCA foi possível caracterizar as diferenças entre as contas de forma eficaz sem qualquer tipo de alteração física e preservando integralmente o material estudado.

Marcelo Rubio1, María F. Mera2, Carlos A. Pérez3, Sofía Cazón4 1 CEPROCOR, Álvarez de Arenales 230, (5000), Córdoba, Argentina. CONICET, Buenos Aires, Argentina. FAMAF, Universidad Nacional de Córdoba, Córdoba, Argentina. {mrubiocba@yahoo.com} 2 CEPROCOR, Álvarez de Arenales 230, (5000), Córdoba, Argentina {mariafernanda.mera@gmail.com} 3 LNLS, Laboratório Nacional de Luz Síncrotron, Caixa Postal 6192, CEP 13083-970, Campinas, SP, Brazil. {carlos.perez@lnls.br} 4 CEPROCOR, Álvarez de Arenales 230, (5000), Córdoba, Argentina {soficazon@gmail.com} ABSTRACT Phytoextraction technologies uses plants to extract toxics metals from contaminated soils and accumulate them in the harvestable parts of the plants, which can then be removed from site. This work describe inconclusive results of the phytoextracion capacity of three kind of plants: 1) hyperaccumulator plant species such as Brassica napus, 2) fast-growing non-hyperaccumulator plants such as Festuca arundinacea (Both 1 and 2 grown in Pb industrial level contaminated soil), and 3) Lolium perenne grown in Pb contaminated soil and in crops of hydroponics. SR µXRF technique offers a powerful approach for probing and mapping the distribution of Pb in selected sections of plant tissues. The measurements were carried out at the D09B XRF Fluorescence beamline of the LNLS. Preparation of contaminated soil, seed selection, seeding, control of handling plant growth variables, selective harvesting and preparation of samples for SR µXRF were done at CEPROCOR. Keywords: X-Ray; Fluorescence; Synchrotron Acknowledgement: This work was developed at Brazilian National Synchrotron Light Laboratory under the proposal XRF-18934. The authors would like to thank the LNLS staff for its technical support. We are grateful for the financial support of CEPROCOR and LNLS for this project. References [1] Scheckel K., and col., In Vivo Synchrotron Study of Thallium Speciation and Compartmentation in Iberis intermedia, Environ. Sci. Technol. 2004, 38, 5095-5100. [2] Donner E and col, Mapping Element Distributions in Plant Tissues Using Synchrotron XRF Techniques. Chapter 9, 2012. [3] Lombi E and col, In situ analysis of metal(loid)s in plants: State of the art and artefacts. Environmental and Experimental, Botany, 72, 2011, 3-17. [4] EPA Phytoremediation resourse guide, United States Environmental Protection Agency, EPA 542-B-99-003 June 1999. [5] Sarret G and col., Use of Synchrotron-Based Techniques to Elucidate Metal Uptake and Metabolism in Plants, Chapter 1, Advances in Agronomy, 2013, 1. [6] Rubio M et al. Study of lead levels in soils by weathering of metallic Pb bullets used in dove hunting in Córdoba, Argentina. X-Ray Spectrom. March 2014.

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.

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]. Posteriormente 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.

El presente estudio se basa en la preparación de un material composite a partir de hidroxiapatita (HAp) y titania (TiO2) mediante radiación ultrasónica en una relación 1:1. La Hidroxiapatita (HA) es un fosfato de calcio Ca10(PO4)6 OH que presenta una composición muy similar a la parte mineral del tejido óseo, por lo que es un material biocompatible y bioactivo ideal para regeneración ósea por lo que es considerado un material de elevada aplicación médica. Por su parte el TiO2 presenta propiedades mecánicas como alta dureza y resistencia al desgaste, además de ser bioinerte y biocompatible, haciéndolo un candidato idóneo para obtener un material biomaterial. La caracterización de las fases presentes fue evaluada a través de difracción de rayos X y espectrometría Raman. Los patrones de difracción mostraron los picos característicos de la HA en fase hexagonal y fueron confirmados mediante la base de datos PDF-4 (ficha 9-0432). El estudio composicional fue realizado mediante fluorescencia de rayos X.

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.

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.

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.

In the recent years different nanoparticles agents have been proposed for produce diagnostic images of tumor areas and simultaneously the application of highly localized treatment. The most studied are the Gold nanoparticles (GNPs) that are enhancer of local dose delivery for orthovoltage radiotherapy and a contrast agent with a better attenuation that the traditional compounds used. One of the common challenges that presented the using these new agents is to develop methodologies for detection in vivo, quickly, efficiently and with greater sensitivity when are provided to the organism. Given that the effectiveness of their applications require knowing exactly the concentration and distribution in the volumes of study. In this work is optimized a benchtop L X-ray system of low power (4 W), which allow quantify in vivo low concentrations of gold nanoparticles into tumor phantoms, with the minimum surface dose. The studied dephs for the tumor phantoms were 0-4 mm of depths in tissue equivalent, with a fixed volumen of 0.3 cm3. The composition of the doped tumor phantoms consisted of a solution of GNPs (1.9 nm AurovistTM, Nanoprobes Inc.) suspended in de-ionized water. For the optimization procces, a set of measurement were carried out for determining the optimal incident spectrum which minimized the limit of detection and the dosis. Several tube voltages (kVp) and alluminium filters of different thicknesses (0.75 mm to 3 mm) for each kVp were configured to obtain a non-symmetrical narrow spectrum with a fixed FWHM and centered between the 8-20 keV. For determining the experimental detection limit, several GNPs concentrations ranging from 0.05 to 10 mgAu/ml were measured into the tumor phantoms at the dephs previously selected and considering a statistical fluctuantion with a 95% of confidence level. The ranging of concentration and depths selected, corresponds to the possible tumour gold concentrations for in vivo aplication.

Previous X ray diffraction studies indicate distortions of geometric parameters (length and / or bond angles) in many first row coordination complexes. Distortions that result in clearly different coordination geometries described for each coordination number, and several times to raise doubt about the existence of chemical bonds. A recent study of [Zn(Phem)2Ac]BF4 (B.L. Rodrigues. Acta Cryst. (2004). E60, m1166) shows asymmetry coordination in Zn-O bonds, with d[Zn-O1] = 2.293(3)A and d[Zn-O2] = 2.149(3)A. This work presents crystallographic and spectroscopic studies of two new nickel compounds. Compound [Ni(Bipi)2Ac]BF4 shows the metal and the acetate in crystallographic special position (axis 2), which requires equivalence between the bonds Ni-O. [Ni(Phem)2Ac]BF4, on the other hand, does not present the metal and acetate in special positions. Despite of this, this compound also presents equivalence in the coordination between the metal and each acetate oxygen. Furthermore, through studies of Hirsfeld surfaces intermolecular interactions are identified, between individual molecules in the crystal, hydrogen bonds. Diffraction results for polycrystalline samples and compared to the simulated diffraction patterns from single crystal diffraction, indicate that crystalline materials are pure. UV-Vis spectra suggest close proximity between the forces of bipyridine and phenanthroline ligands.

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. The 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]. This 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. [1]“Degradation Process of Lead Chromate Yellows in Paintings by Vincent Van Gogh” Letizia Monico. PhD thesis. University of Antwerp and University of Perugia. [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. [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. Acknowledgement: 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.

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.

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.

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. [1] M. Hložek, T. Trojek, Radiat. Phys. Chem. 116 (2015) 332. [2] F. Bilo et al., Appl. Surf. Sci. 359 (2015) 215. [3] X. Li, Z. Yu, Appl. Radiat. Isot. 111 (2016) 45. [4] T. Trojek, D. Trojková, , Radiat. Phys. Chem. 116 (2015) 321. [5] R. M. Rousseau, Rigaku J. 18 (2001) 33 [6] CG Clayton, R. Spackman, Nucl Geophys 1 (1987) 25. [7] S. Steenstrup, J Appl Crystallogr 14 (1981) 226. [8] B. Vekemans et al., X‐Ray Spectrom 23 (1994) 278. [9] P. Bury et al., Nucl Instrum Methods Phys Res Sect A 383 (1996) 572. [10] L. Yi et al., Nuclear Instruments and Methods in Physics Research A 775 (2015) 12.

The use of X-ray Fluorescence is very often restricted to the analysis of bulk materials by the average user. The technique is also considered as not being fit for the lower ppm or even ppb concentration range. Much of this is true, but appropriate sample preparation techniques, the additional hardware and software show that XRF is capable in analysing much more than only the "traditional" samples. For the analysis of light elements (H - O) XRF cannot be considered as THE technique. Nevertheless, adequate fundamental parameter software makes it possible to calculate a very good estimate of the total concentration of light components and therefore also the results of other elements of interest will be improved drastically. What about analysing ppb levels in aqueous solutions? It is possible with the appropriate sample preparation technique. Did you ever think about performing mapping analysis on inorganic or even organic samples? Also this is something XRF will do excellently with adapted soft- and hardware tools. This presentation will show you the flexibility and strength of WDXRF, a technique that becomes more and more a complete analysis tool.

AlGaSb layers grown on [100] GaSb substrates could build structures in order to use in optoelectronic devices such as lasers or detectors for operate in the 0.7-1.7 µm range. In this work, the liquid phase epitaxy (LPE) technique was used to grow Al(x)Ga(1-x)Sb layers with different composition of x value from 0.03 to 0.15 on GaSb substrate, this cause a substitution of gallium by aluminium atoms. The High Resolution X-ray diffraction (HRXRD) was used to determine the lattice parameters of AlGaSb layers, the mismatch to substrate and the relaxation of layer. The composition was studied by x-ray fluorescence (XRF). In this study the substitution of atoms creates tensile stress and relaxation, its lattice parameters follows the Vegard's law in function of composition, also, the composition changes the operation wavelength for the potential use in optoelectronic device.

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.

A fluorescência de raios X (XRF) é uma técnica analítica multielementar bastante difundida e com aplicações variadas. Uma das características importantes de um sistema de XRF é a sua capacidade de ser portátil; o que permite a aplicações em várias áreas da ciência e tecnologia concomitantemente. O objetivo desse trabalho foi o desenvolvimento de um sistema de XRF portátil (APOENA X) abrasileirado e competitivo com os sistemas comerciais. O sistema Apoena X é formado por um mini tubo de raios X de baixa potência (anodo de Ag, 40kV/200µA), um detector SiPIN e uma micro câmera digital para alinhamento do feixe de raios X sobre a amostra. A microcâmera digital foi fixada entre o detector e o tubo de raios X de forma que a imagem do ponto de medida pudesse ser visualizada na tela de um microcomputador e que um feixe de laser mostrasse pontualmente o local de interseção entre o feixe de raios X incidente sobre a amostra e o feixe emergente que é produzido na direção do detector. O software de posicionamento da microcâmera digital foi desenvolvido no próprio laboratório (LIETA). O sistema portátil é alimentado por uma bateria gerando maior portabilidade e permitindo aplicações em ambientes externos onde o acesso a rede elétrica é impossível. O sistema APOENA X é compacto, funcional, inovador e fora dos padrões comerciais dos equipamentos importados. Além de gerar tecnologia na área de espectrometria de raios X, o sistema portátil tem função multiaplicativa que permite a análise de uma variedade grande de tipos diferentes de amostras.

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.

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.

Polymorphism and particle size distribution can impact the dissolution behaviour and, as a consequence, bioavailability and bioequivalence of poorly soluble drugs, such as Efavirenz (EFV). Nevertheless, these characteristics do not explain some failures occurring in in vitro assays and in in vivo studies. EFV belongs to class II of the biopharmaceutics classification system and the high activity antiretroviral therapy (HAART) is considered the best choice in the treatment of adults and children. In a previous study, Fandaruff et. al. demonstrated the biorrelevance of the microstructure (crystalline domain sizes) in EFV and the correlation between changes in dissolution properties and changes in crystallite size rather than particle size [1]. The microstructure study of these samples was done using synchrotron radiation X-ray diffraction at ELETTRA facility (Italy). The aim of this work is to expand the previous study of the effect of microstructure on different commercial raw materials and crystallized samples of EFV. A further extension of the method of crystallite size analysis to anisotropic crystallite shape and a reproducibility of the results obtained in X-ray diffraction experiments using synchrotron and conventional radiation sources are reported.

In the pharmaceutical industry is important characterize the active pharmaceutical ingredients (APIs) involved in the manufacture of a drug. It is well-known that a number of physicochemical properties of the APIs depend on the structural characteristics in the solid state. Thiocolchicoside is an active pharmaceutical ingredient used as a muscle relaxant. The only crystal structure thiocolchicoside-related reported in the Cambridge Structural Database corresponds to an ethanol solvate hydrate (Refcode: THCLCS). However, the hydrogen atoms information and intermolecular interactions is not reported. Yellow prism crystals were obtained from an ethanol/water solution at room temperature. Integration and reduction of the single diffraction data produced an orthorhombic cell with space group P212121 (No. 19) and parameters a= 9.8311(7) Å, b= 12.0923(8) Å, c= 28.180(2) Å, V= 3350.1(4) Å3, similar to THCLCS. The present X-ray diffraction study consists in a crystal structure, hydrogen bonding and CH...π interactions analysis which play an important role in the crystal packing and have not been reported previously for this material.

Synchrotron Micro X-Ray Fluorescence (µSRXRF) is a non-destructive technique very often used in biological investigations to obtain information regarding the distribution of elements in tissue and cell samples. Diseases of the prostate are very frequent in men over 40 years of age. Prostate cancer and benign prostatic hyperplasia (BPH) represents, worldwide, a significant risk in terms of morbidity and mortality. In this context, the aim of this work was to investigate the distribution of Fe, Cu and Cu/Zn using synchrotron X-ray microfluorescence (SRµXRF) in cell spheroids in benign prostate hyperplasia (BPH) and prostate cancer (DU145) supplemented with Zinc and to analyze the influence on intensity of Fe, Cu and Cu/Zn after Zinc supplementation. The SRµXRF measurements were performed in standard geometry of 45º incidence, exciting with a white beam and using an optical capillary with 20 μm diameter collimation in the XRF beam line at the Synchrotron Light National Laboratory (Campinas, Brazil). The results showed non-uniform distribution of Fe and Cu in all the spheroids analyzed. It was possible observed that intensity of Fe, Cu and Cu/Zn were changed with the Zn supplementation. Therefore, the Zn supplementation changes the metabolic of prostate cell.

During the last years has been proposed the utilization of Gold and Silver nanoparticles like bio-markers when are bound to molecules like antibodies, which are linked to specifics cell receptors. This would provide useful information like the spatial distribution and radiosensibility of the tumor cells in the cancer treatment. Because the distribution of malignant cells is heterogeneous in tumour volume, the dose could be modulated considering different bio-parameters that will affect the distribution and radiosensitivity of cells, as the concentration of intracellular oxygen and cell redistribution. Therefore use gold and silver nanoparticles with specific markers would provide information of these bio-parameters, and thus individualize treatments depending on the conditions of the tumor microenvironment. In this work is optimized a bench-top EDXRF system, which allow quantify in vivo low concentrations of silver and gold nanoparticles into tumor phantoms. In the first state, the system was previously configured using XMI- MSIM software designed to predict the XRF spectral response using Monte Carlo simulations. The studied setup is comprised of an mini X-ray tube and a set of filter of Se, Sr, Y, Zr, (for exiting the gold L3-edge) and Cd, In and Sn (for exiting the silver K-edge), configured with variable thickness, for emit simultaneously two spectrally narrow beam centered on a specific excitation energy. The figures of merit used for adjusted the composition and thickness of the filters were minimizing the detection limit and radiation exposure. In the second state, the experimental verification was realized in a tissue equivalent phantom, made of a mixture of 96% cellulose and 4% salt Merck. Tumor phantoms of 0.3 cm3 embedded with the nanoparticles agent consisted of a solution of GNPs (1.9 nm AurovistTM, Nanoprobes Inc.) and Silver nanoparticles (in-house by LIIFAMIRx) suspended in de-ionized water. For determining the experimental detection limit, several concentrations ranging from 0.05 to 10 mgAu/ml were measured into the tumor phantoms considering a statistical fluctuation with a 95% of confidence level. The ranging of concentration studied corresponds to the possible gold and silver concentrations expected to be found in future in vivo application in human.

Our society has an urgent and growing demand for energy. Because of this need, each day new materials and routes that promise to meet this demand emerges. However, many of these strategies require large areas to become effective or are heavily dependent on weather conditions. And, due to global warming, these energy alternatives cannot be sustained, and this impacts negatively on operating costs. One of the possible energy routes use nuclear energy, this route faces strong resistance, especially from environmentalists and it gains strength when there are accidents like Chernobyl and Fukushima. Despite all the controversy, nuclear power has gained more space in our society, including our country. Brazil has, for decades, nuclear power plants in full operation and, as we have no reports of any problems. Our country has also a huge uranium reserves which has a positive impact on the final cost of energy produced by nuclear route. Because of all that, there are negotiations for the installation of a new plant in the northeast of the country. This region is strategic due to its energy demand and also to the proximity of biggest uranium reserves. Two Brazilian states are always highlighted, from the installation of nuclear power plants, Ceará and Sergipe. This possibility, combined with the intrinsic fears of nuclear energy, led us to seek alternative materials that can be used as radiation levels indicators. In this work, we chose to study usual materials of civil construction for the purpose of employing them in retrospective dosimetry, which aims to determine the excessive dose of radiation exposure, either chronological or acute. The materials studied were sand, mortar, tiles, tile, brick and concrete are commonly present everywhere. The samples here studied were collected in Sergipe cities. The characterization of these materials was done by analytical techniques, initially XRF and XRD were used. After the chemical characterization became clear that we would need to resort to chemical extraction strategies specific to be able to extract the quartz grain which is in fact the species susceptible to radiation. Once applied to acid leaching, named by us as Campos method, new aliquots were characterized by microscopy, ICP-MS and EPR. The results obtained by combining these strategies, demonstrated the potential of using these materials as radiation indicators. However, the high iron content combined with the prohibition of using chemical leaching procedureswith that promote the heating of the sample, showed that more studies are needed in order to establish a routine protocol.

La fluorescencia de rayos X (FRX) es una técnica que permite, en el área de exploración y explotación de hidrocarburos, el análisis de metales en muestras geológicas de reservorios. La información obtenida puede utilizarse para el modelado del reservorio, el análisis de potencialidad de roca a través de la determinación de correlaciones estratigráficas, inferir el ambiente de deposición y ayudar a entender la mineralogía como la mecánica de la roca. Al igual que cualquier técnica analítica, un punto clave en la confiabilidad del análisis cuantitativo en las mediciones por FRX es la preparación de muestra. En el caso del análisis de muestras geológicas existen tres posibilidades de preparación para la medición; molienda y análisis directo en polvo, medición en pastillas prensadas o fusión de la muestra. Este último, presenta diversas ventajas como la eliminación de efectos de tamaño de partículas y de matriz. En el siguiente trabajo se realizó una optimización del método por fusión para el análisis de metales en rocas de reservorio por FRX. La misma se realizó seleccionando por medio de un diseño exploratorio los factores significativos del tratamiento de la muestra que afectan a la señal. Posteriormente, se encontraron las condiciones óptimas de trabajo empleando una metodología de superficie de respuesta. Finalmente, empleando las condiciones optimizadas se realizó el análisis cuantitativo de las muestras construyendo las curvas de calibración para los metales de interés. Los límites de detección y cuantificación encontrados fueron: Fe: 0,5 y 2,6 ppm; Ti: 0,4 y 1,0 ppm; Ca: 1,8 y 6,0 ppm y K: 0,9 y 2,0, respectivamente. La metodología se validó mediante estándares geológicos certificados y se comparó con la técnica de referencia por ICP, encontrando que la metodología utilizada es adecuada para el análisis de metales en rocas de reservorio.

O objetivo deste trabalho é classificar padrões em imagens de Raios X. Para isso, foi desenvolvida uma ferramenta computacional: o SDPI - Sistema de Detecção de Padrões em Imagens. A base da metodologia de classificação, utilizado pelo SDPI, são os Descritores de Textura. O SDPI extrai os Descritores de Textura da imagem a ser analisada, e utiliza estas informações para treinar uma Rede Neural Artificial (RNA). Para testar a ferramenta desenvolvida, foram utilizados dois conjuntos distintos de imagens de mamografia. Após a obtenção dos Descritores de Textura nos dois conjuntos de imagens, utilizamos o primeiro conjunto de imagens para treinar uma RNA, e o segundo conjunto de imagens para testes. Após o treinamento, a RNA determina imagens com calcificações, no conjunto de teste, com uma precisão de 87,50%. Os resultados mostram que a classificação das imagens por Descritores de Textura é uma ferramenta poderosa, que independe de análise visual, que pode sofrer subjetividades. Este processo pode ser utilizado em outras aplicações, tais como localizações de desmatamentos em aerofotografias e determinação de padrões em plantações.

Se realizó la caracterización estructural del compuesto 4-cloro-N-(9H-fluoren-9-iliden)anilina por medio de difracción de rayos-X de monocristales. Mediante este estudio se obtuvieron las posiciones atómicas, longitudes y ángulos de enlace. Adicionalmente, se determinaron las constantes de celda a= 14.2571 (12) Å b= 5.2035 (4) Å c= 19.4321 (18) Å β= 99.152(15)°, el volumen de celda determinado 1423.25 Å3 y el grupo espacial P 21/n. En la Figura 1 se aprecia la celda unidad del compuesto de interés Figura 1 – Celda unidad del compuesto 4-chloro-N-(9H-fluoren-9-ylidene)anilina Finalmente se determinaron las principales interacciones intra e intermoleculares del compuesto de interés.

The antiretroviral drug Nevirapine (NVP) (11-Cyclo-propyl-5,11-dihydro-4-methyl-6H-dipyrido[3,2- b:2’,3’-e][1,4]diazepin-6-one) is a non-nucleoside reverse transcriptase inhibitor, used in the treatment of HIV-1 infection. It is a class II drug according the Biopharmaceutics Classification System (BSC)1, exhibiting low solubility and high permeability. To increase the drug dissolution and its bioavailability, the different preparation methods with crystal modification such as co-crystals were studied. Co-crystals are multicomponent crystalline solids which have different drug molecules or a drug and a non-volatile substance in its structure. NVP molecule has a conformationally rigid amide group that allows a co-crystal formation with soluble carboxylic acids or amide co-formers2. Caira et al. reported the crystal structure and solid state properties of several NVP co-crystals2. We prepared different co-crystals of NVP and there were identified using their crystal structure Caira published data. The only case where we observed differences was for NVP-salicylic acid (NVP-AS). Our data presented different reflections in comparison with reported data. Therefore, the goal of this work was to determinate the crystal structure of NVP-AS using single crystal X-ray diffraction in combination with solid state NMR spectroscopy in order to confirm our crystal structure results. 1 Lindenberga, M.; Koppb, S.; Dressmana, J. B. European Journ. of Pharm. and Biopharmaceutics. 2004, 265-278. 2 Caira, M.R. et. al. CrystEngComm. 2012, 17-23. Acknowledgement: We are grateful for the financial support of CAPES for this project.

In the present study jewels from the tomb of the lady of Cao were studied, a Moche “queen” of a period around 300 AD (in the Museum “Señora de Cao” in Magdalena de Cao, north of Peru). To this aim a X-ray digital radiography system (XDR) was employed, using a mini X-ray flat-panel sensor. The objective of these analyses was to obtain structure information of the jewelry (mainly nose ornaments composed of gold and silver sheets), particularly about manufacturing mode and soldering between gold and silver sheets and thickness quantification. A portable XDR system was employed, consisting of a flat-panel detector using APS-CMOS technology produced by Schick Technologies and a mini X-ray tube with Au anode from Amptek, which works at 50 kV and 100 µA maximum voltage and current. The radiographic images of the jewels revealed interesting details on the manufacturing process and on how the silver and gold sheets were glued or soldered .

The x-ray microtomography is an important non-destructive technique to investigate fossils and other prehistories specimens, because of its capacity of preserve their physics integrity. Currently, is frequent the search for the technique for studies with palaeontology. This study is about the use of X-ray microtomography to survey a fossil compared with actual specimen of blowfish. The aim of this study is identify the changes that occur over the years. This images were obtained through of system SkyScan 1173. The acquisition parameters 130 kV of voltage, 61uA of current, pixel size 26 µm and the rotation degree was 0.5°. After the scanning was realized the reconstruction and it allows to realize a qualitative analysis with 2D and 3D images. This images allowed to observe a change in orientation of jaw. This result showed that the technique is very important to analyse this type of specimens because is a non-destructive technique that provides qualitative and quantitative tools essentials to allow the visualization of the internal structures preserving the integrity of specimens.

O bjetivo deste estudo foi à caracterização química do material particulado em suspensão na atmosfera da região metropolitana de Goiânia (GO). A amostragem foi realizada no inverno e no verão de 2012. Utilizou-se na coleta o amostrador do tipo Stacker, capaz de amostrar simultaneamente partículas finas (partículas com um diâmetro de até 2,5 µm) e grossas (partículas com um diâmetro entre 2,5 e 10 µm). Neste estudo foram utilizados filtros de policarbonato com diâmetro de 47 milímetros, com tamanho de poro de 0,4 e 8,0 µm, para coleta de PM2,5 e PM10 respectivamente. A massa de aerosol nos filtros PM10 e PM2,5 apresentaram os seguintes valores médios e desvios-padrão: PM10 inverno e verão de 15 ± 7 μg/m³e 90 ± 70 μg/m³, respectivamente; Goiânia PM2,5 inverno 27 ± 7 μg/m³ , verão 14 ± 9 μg/m³. A determinação elementar foi realizada pela técnica de Fluorescência de Raios X Dispersiva em Energia excitada com luz sínctrotron (SRXRF). As concentrações elementares médias e desvios-padrão das amostras coletadas em Goiânia são apresentados da seguinte forma: PM10 inverno (Si 1500 ± 400 ng/m³; S 150 ± 30 ng/m³; Ca 600 ± 200 ng/m³; K 240 ± 90 ng/m³; Ti 130 ± 50 ng/m³; Cr 3,7 ± 0,8 ng/m³; Mn 11 ± 3 ng/m³; Fe 1430 ± 400 ng/m³; Cu 13 ± 4 ng/m³; Zn 22 ± 8 ng/m³ e PM2,5 inverno (Si 650 ± 20 ng/m³; S 120 ± 20 ng/m³; Ca 150 ± 180 ng/m³; K 80 ± 70 ng/m³; Ti 40 ± 30 ng/m³; Cr 1,8 ± 0,6 ng/m³; Mn 3 ± 2 ng/m³; Fe 300 ± 300 ng/m³; Cu 5,6 ± 1,7 ng/m³; Zn 8 ± 4 ng/m³. Verão PM10 (Si 1100 ± 300 ng/m³; S 150 ± 50 ng/m³; Ca 430 ± 140 ng/m³; K 150 ± 60 ng/m³; Ti 70 ± 30 ng/m³; Cr 5 ± 3 ng/m³; Mn 7 ± 2 ng/m³; Fe 800 ± 300 ng/m³; Cu 7 ± 3 ng/m³; Zn 21 ± 7 ng/m³ e PM2,5 verão (Si <LQ, S 130 ± 40 ng/m³; Ca 40 ± 40 ng/m³; K 50 ± 30 ng/m³; Ti 8 ± 7 ng/m³; Cr 1,2 ± 0,8 ng/m³; Mn 1,8 ± 0,7 ng/m³; Fe 60 ± 60 ng/m³; Cu 2,8 ± 0,4 ng/m³; Zn 4,5 ± 1,9 ng/m³). A massa total média (μg/m³) do PM2,5 no inverno foi maior que a do PM10, fenômeno causado pela maior emissão de particulado fino ou devido ao menor tePMo de resiliência do PM10 na atmosfera. No verão o PM10 apresentou concentrações (μg/m³) maiores do que no inverno, cerca de seis vezes maior, já para o PM2,5 a concentração média foi maior no inverno. No geral, os elementos determinados apresentaram concentrações médias maiores no particulado grosso que no fino. A campanha de amostragem de inverno apresentou concentrações médias maiores para as duas frações coletadas. Salva exceção do S, elemento normalmente associado ao PM2,5, não apresentou variação significativa entre as frações coletadas e nem entre as épocas de amostragem. A presença de S no PM10 pode ter ocorrido devido à adsorção de dióxido de enxofre na superfície das partículas sólidas, aderido através de reações com oxidantes já presentes nessas partículas (MARTINS C. R., ANDRADE J. B., 2002).

Este trabalho apresenta o desenvolvimento e caracterização de um sistema portátil automatizado de fluorescência de raios X por reflexão total (TXRF) de alta tecnologia e baixo custo para realizar análises não destrutivas, que pode ser empregado para análise de vários tipos de amostras: biológicas, ambientais, engenharia de materiais e na indústria. O sistema é constituído por um tubo de raios X de 50 W, ânodo de Mo, um guia de onda, um detector Si-PIN, refletores de quartzo, posicionadores para os eixos X, Y e Z, movimentados por dois motores de passos controlados usando a plataforma Arduino e um micro computador. O sistema TXRF foi avaliado e caracterizado a partir de testes de repetibilidade, otimização da posição do feixe de raios X, ângulo de reflexão total e curva de sensibilidade. A operação do sistema foi realizada com 40 kV e 0,4 mA, com contagens de 200 segundos. A precisão e exatidão foram realizadas utilizando-se amostras certificadas de fígado bovino (NIST – Bovine liver 1577b). No teste de repetibilidade, o sistema apresentou um coeficiente de variação menor que 3,2 %. Na condição de reflexão total, o ângulo critico foi de 0,10 ± 0,01 graus, valor que está de acordo com a previsão teórica para a energia do feixe incidente (ânodo de Mo) e o refletor de quartzo. As concentrações determinadas com o sistema automatizado portátil de TXRF apresentaram variação no intervalo de 9 -14 % para os elementos majoritários (P, S e K) e de 2-20 % para os elementos traços (Ca, Mn, Fe, Cu, Zn e Rb). O sistema portátil automatizado de TXRF mostrou que é capaz de efetuar analises de fluorescência de raios X por reflexão total com um sistema de alta tecnologia e baixo custo e analisar elementos em um intervalo de Z=15 a Z=38.

Disposal of industrial wastes and application of fertilizers and pesticides in agriculture has contributed to a continuous accumulation of contaminants in certain areas. Release of toxic soluble substances onto the soil as a result of agricultural and industrial activities may pose a serious threat to the environment. One aspect of sustainability is the accumulation of metals in soil which causes problems if certain levels are exceeded. When a liquid comes in contact with soil, some of their constituents will dissolve to a greater or lesser extent. Leaching of chemical substances occurs across the soil by percolation of water solutions. The leaching potential refers to the risk that soluble contaminants could be transferred through the soil to the groundwater reservoir. The degree of dissolution of individual particles in the contact phase (liquid/soil) determines the leachate composition. The mobility of metals in soil depends on their bond strength with the soil surface. Metal ions generally associate with the hydroxides, sulfides or carbonates of the soil organic matter by different mechanisms such as complexation. The most important factors that affect these processes are pH, redox potential, and organic matter concentration in soil. The binding of the metal to the dissolved organic matter can increase their solubility by more than 2 orders of magnitude. In this research, chromium adsorption in soils coming from the Pampean region of Argentina was studied and compared with the same soils amended with food waste compost. This region shows a high industrial activity that includes tanneries and metallurgical industries. Chromium, as CrVI (anion) and CrIII (cation), was chosen as a representative metal to study the adsorption or retention capacities of these soils. Energy Dispersive X-Ray Fluorescence spectrometry (EDXRF) was employed for the characterization of soils samples and Total Reflection X-Ray Fluorescence Spectrometry (TXRF) for the solutions. This research gives an interesting contribution to be extended for other types of soils allowing in this way to estimate the groundwater contamination risk based on the soil quantitative elemental information and the advantages of the mixing with food waste compost.

Pollution from heavy metals is becoming an increasing concern, since pollution can affect different environmental compartments namely, soil, air and water. Groundwater geochemical arsenic contamination is still a serious problem in Argentina. There is an increased necessity to develop processes to eliminate arsenic or at least to minimize their concentration in wastewaters prior to their release into the environment. Research and development of low-cost procedures in order to recover natural resources of water, superficial or groundwater, have become a very important task and a great challenge. Traditionally, the methods used to remove metals from a solution are chemical precipitation, adsorption, cations-exchange, reverse osmosis, electrodialysis, electrochemical reduction, etc. Adsorption process is the most frequently applied in industries due to low cost, easy procedure, versatility and the possibility to re-use the adsorbent. In this sense, many studies having been carried out in this field. Among natural adsorbents, the hydroxyapatites (HA) are known for their ability to retain various metals and metalloids, due to their surface characteristics; these are calcium phosphates that exist in some phosphate rocks, but especially in teeth and bone tissue of animals. Bovine bones represent an option. Bones are primarily composed of calcium phosphate, hydroxyapatite and collagen; HA was reported as an effective heavy metals adsorbent. The aim of this study was to evaluate the ability of bovine hydroxyapatite (HA) to act as adsorbent of arsenic to be used for remediation purposes. The specific surface area and total pore volume was calculated for the HA by developing an adsorption isotherm in nitrogen gas to its boiling temperature at atmospheric pressure. The method used was the conventional Brunauer– Emmett–Teller (BET) in order to measure the specific surface area of a material. The adsorbent was found to be a non-porous material. To develop the adsorption isotherms, batch experiments were carried out with different As solutions with initial concentrations ranging from 3 mg L-1 to 6 mg L-1 of As and different doses of HA (0.2 to 2 g per 50 mL). The amount of pollutant removed was determined from the difference between the initial concentration of arsenic and the remainder. The employed analytical technique was Total Reflection X-ray Fluorescence spectrometry (TXRF). According to the obtained results it can conclude that HA can be a possible low-cost adsorbent forAs showinga removal of 43%.Reactors water treatment, for reducing As concentration in drinking water,at laboratory scale, is presented. The effect of chemical variables as pH, temperature, competitively with other analytes is also considered.

A Fluorescência de Raios X por Dispersão em Energia (EDXRF) é um método que permite fazer análises quantitativas e qualitativas multielementares dos amostras de forma não destrutiva. Neste trabalho o espectrômetro de XRF da Amptek®, composto por um tubo com anodo de ouro e um detector SDD, foi utilizado para caracterizar amostras de ouro, tendo como referência três amostras de ouro padrão de 14, 16 e 18 quilates. Uma tabela foi montada com os resultados obtidos nas amostras padrão, que teve como base a razão Kα Cu / Lα Au. Posteriormente, amostras de joias de ouro foram comparadas com os padrões de medição e foi verificada a quantidade de ouro. Essa metodologia se mostrou adequada para análise de baixo custo da qualidade de objetos de ouro.

Duplex Stainless Steel is widely used in oil & gas, chemical, petrochemical and nuclear power industries because of its combination of good mechanical properties and high corrosion resistance characteristics. Microstructure of duplex stainless steel is an example of composite material with approximately equal amounts of austenite and ferrite phases. Residual stress measurements in ferrite and austenite phases were made in duplex steel plates jointed by the GTAW welding technology. Software for processing of experimental data obtained by X-ray diffraction method was developed especially for stress measurements in duplex stainless steels. Using of this software allows to improve the accuracy and precision of stress measurements in ferrite and austenite phases and to minimize processing time.

The conservation of cultural heritage metal artworks is a major challenge. The main concern is related with corrosion: a physicochemical interaction between the metal and its environment, involving oxidation process trigged by the exposure of the metallic surface to various substances widely found in the air, such as Oxygen, Chloride and Sulfur Dioxide, intensified by moisture and dust, impurities that settle on the surface and act as catalysts in the metal degradation process. Regarding cultural heritage artefacts, corrosion could be related with the loss of some specific values (artistic, historic, scientific, social, etc.) of that object. There are several approaches regarding methods for cleaning surfaces in order to remove impurities and thereby, to preserve the object and maybe to restore it. One of the most common methods involves wet chemical process using hard abrasives. Indeed, these treatments are effective (for some purposes), and they have a low cost. However, details of the morphology of the surface of the samples are lost by such treatments. Taking into account that when it comes to cultural heritage objects, the goal is find a cleaning treatment which provides the lowest possible damage. The purpose of the present work is therefore study the possible effectiveness and also the advantages and disadvantages of the Glow Discharge Cleaning (GDC) method, through the analysis of coins obtained from Mr. Wilson Gennari's personal collection. In other to stablish an adequate procedure for our goal, we performed analyses in coins with corrosion in the surface. The effectiveness of the cleaning process was monitored with an X-Ray Fluorescence (XRF) portable equipment (Ampetk) before and after the cleaning. Also the coins mass also was monitored during the process. The conditions of Glow Discharge used was: pressure 6,0 x 10־¹torr, current 70 - 90mA, voltage 1,0 - 1,4kV and time 9 minutes. Photographic images were also obtained to follow up the cleaning process. Moreover, was possible to suggest that the physical properties of the alloy were not affected by this GDC process, once a very small reduction was observed in only one of the element matrix (Zinc) without any alteration on Copper content. The results obtained in this study suggest that the GDC procedure can be used to clean metallic surface, with clear advantages when compared to chemical cleaning due the fact that, there was no matrix lost (no mass reduction) and no signs of chemical degradation were found.

A sociedade moderna assiste um crescimento exponencial da violência que atinge todo o mundo. O emprego de armas de fogo (AF) está relacionado significativamente com este evento. Diversos são os trabalhos científicos voltados ao desenvolvimento de meios para se reduzir os índices de criminalidade e prestar suporte tecnológico aos meios de investigação criminal. Este trabalho consiste na pesquisa para a identificação de resíduos de disparos de armas de fogo, gunshot residue (GSR), que podem se depositar sobre as mãos de atiradores. Para o experimento foi utilizado um espectrômetro portátil de raios X produzido pela Amptek, com tubo de raios X com anodo de Au. As amostras forma submetidas a um feixe de 25kV de tensão e 25µA de corrente por um intervalo de 600s. Os espectros foram construídos e analisados com auxílio do programa DppMca, também fornecido pela Amptek. Amostras extraídas das mãos de atiradores mostram que com o emprego da técnica de fluorescência de raios X por dispersão de energia (EDXRF) torna possível identificar traços característicos de GSR.

Five gold samples were analysed using laser ablation and multi collector mass spectrometer. Four of these samples were from goldfields in Cuiabá, Peixoto, Lacerda and Colombia. The last one was a modern British coin, which is supposed to be a gold mix of different provenances. The process evaluated Pb isotopes 204, 206, 207 and 208. At the same time the isotope 202 from Hg was measured in order to correct superposition of 204 Hg present in buffer gas with 204 Pb. X-Ray fluorescence measurements were also made in order to evaluate copper and silver concentrations in the samples. All results are interesting and characterize quite well these gold samples. This is the first step in order to develop the methodology to analyse old artifacts like coins and other metal objects and therefore, this is an important technique largely used in Archeometry. Furthermore, this is an important method to fingerprinting gold provenance in Brazil.

Os meteoritos despertam a curiosidade da humanidade desde a antiguidade. No entanto, o estudo desses materiais vai muito além de uma simples curiosidade. A pesquisa que desenvolvemos possui a finalidade de realizar um estudo científico de amostras de meteoritos, através de análises sistemáticas[1]. Desse modo, pretendemos propor possíveis modelos de caracterização desses objetos por meio de diferentes técnicas instrumentais não destrutivas, tais como, fluorescência de raios X (XRF) e microtomografia computadorizada (µTC). Assim, acreditamos que poderemos neste trabalho averiguar, caracterizar, fornecer e estabelecer empiricamente, informações fundamentais para compreendermos melhor a evolução do Sistema Solar através desses objetos[2]. Referências: [1] Hutchison, R. Meteorites: a petrologic, chemical and isotopic synthesis.2a Ed. Cambridge planetary science series. 2004. [2]Patterson, C. Age of meteorites and the Earth. Geochimica et Cosmochimica Acta, 1956, Vol. 10, 230-257.

Saquinavir (SQV) is an important protease inhibitor used for AIDS/HIV antiretroviral therapy. It is commercialized as mesylate salt (SQVM) and classified as belonging to class IV (low permeability and solubility). The dissolution properties were investigated by SQVM in the medium containing the anionic surfactant Sodium Lauryl Sulphate (SLS). It was expected that the electrostatic interactions between the anions of SLS and the cationic drug species could cause a decrease in the repulsive forces of the head groups of the surfactant molecules leading to enhanced solubilization. However, for the SQVM profile in the anionic surfactant medium the result obtained was contradictory. Therefore, the aim of this study was to explain the anomalous dissolution behavior of SQVM in SLS medium through a structural analysis. The anionic portion of SLS remaining molecules interact with the cationic species of SQV to form an insoluble salt which precipitates out (Figure 1) and results in desolubilization phenomenon. Through crystallographic investigation it was possible to demonstrate the crystallization of SQVM with SLS. Therefore, SLS is not an appropriate dissolution medium to analyse the dissolution properties of SQVM. Figure 1 – (A) Dissolution profile of SQVM raw material and (B) Turbidity of SQVM in SLS 0.25% medium

Alzheimer disease (AD) is an insidious, progressive and irreversible brain disorder. Its incidence is highest in people aged over 65 [1]. The cause of AD is not fully understood. The pathological features of AD include β-amyloid (Aβ) plaques, intracellular neurofibrillary tangles, loss of neurons and synapses, and activation of glia cells. Recently, several groups have raised the “metal hypothesis” of AD [2]. This hypothesis is mainly based upon experimental results. First, several metal ions, such as zinc, iron and copper, are all increased in the ageing brain. It has been reported that the content of metal ions in the brain of AD patients is 3-7 times that of normal people and that the metal ions in brain homeostasis may result in the development of AD [3]. Second, these metal ions can interact with Aβ, resulting in the promotion of Aβ deposition and plaque formation. Total reflection X-ray fluorescence analysis (TXRF) is a multielement analytical technique, which is capable of yielding quantitative information on the elemental composition of a variety of materials. This method can be used for elemental trace analysis [4]. In this work, three groups were studied: control, AD10 and AD100. The groups AD10 and AD100 were given a single intracerebroventricular injection of 10 pmol and 100 pmol of oligomers of β-amyloid peptide respectively to be induced AD. Seven days after the injection was carried out craniectomy and subsequently evaluated five brain compartments: frontal cortex, temporal cortex, hypothalamus, hippocampus and cerebellum. All samples were submitted to acid digestion (HNO3 + H2O2). After that, they were diluted with Milli-Q water and added an internal standard (Ga).The TXRF measurements were performed at the X-Ray Fluorescence Beamline at Brazilian National Synchrotron Light Laboratory (LNLS), in Campinas, São Paulo using a monochromatic beam (11.5 keV) for the excitation and an Silicon drift detector with energy resolution of 133 eV at 5.9 keV. It was possible to determine the concentrations of the following elements: P, S, K, Ca, Fe, Cu and Zn.

The purpose of investigating technology choices is to question the techniques and materials used by potters and the consequences of their choices (Sillar & Tite 2000) [1]. To understand the differentiation of technologies and possibly the people who produced these artifacts in different chronological moments and geographical areas the first step is the chemical characterization to define the variability of each region and link the results to the archaeological and chronological results. In this work we show the results of the analyzes made by the XRF technique of ceramic fragments from three different regions of the Amazon rainforest: Oriental, West and South region. Thus it was possible an assessment of the range of results that are relevant to the study of archaeological ceramics of the Amazon rainforest and to the understanding of potters populations that produced them.

The Hurter & Driffield curve, primary tool for evaluation of characteristics of radiographic films is defined as the optical density as function of exposure. This optical density is traditionally measured by the transmittance of a beam light across the film, and its response is important to understand the film behaviour in sensitometry, in scanning by optical scanners and also in the viewing with our eyes against a light source such as light box. There are many mathematical and computational models to characterize the behaviour of this curve and its properties, but is not among them some models that consider the interference that the equipment used can have about sensitometric curves. When trying to adjust curves from theoretical models to experimental data, it was estimated that, for high exposure values, there was inconsistency between data, and this inconsistency would suggest a limitation in optical density. When trying to make the measurement of silver depending on exposure through another method than optical, such as X-rays fluorescense, it was realized that these data was reasonably agree with the models, and that the limitation in optical density is mainly caused by its measurement. The objectives of this work were: 1 - characterize this limitation of the measurement of optical density; 2 - Suggest the X-ray fluorescence as a technique that bypasses the resulting difficulty caused by this limitation; and 3 - by X-ray microfluorescense, reconstruct images and show what kind of information is lost and that the new method can be revealed. The study shows that the transmittance of light is a limited way to measuring the concentration of silver, and gave birth to a mathematical characterization of this limitation, which set a reasonable fit to experimental data. Also characterized and suggested the X-ray fluorescence method which can solve this problem, showing data that are more consistent with models that do not consider the limitation. The mapping was successful in reconstructing images and present a visual way that a good portion of the dynamic range is lost with the measurement by light transmittance.

El sitio arqueológico Pampas Gramalote (Figura 1-a) se ubica en el centro poblado menor de Huanchaquito, provincia de Trujillo. Los trabajos que se vienen realizando en el sitio están ayudando a entender el proceso de complejización social desde la perspectiva de las comunidades o centros residenciales domésticos. Se trata de estudiar la configuración y dinámica interna de una comunidad y como ésta se articuló en las diferentes esferas y escalas sociales y económicas del valle de Moche y la costa norte en general. Los trabajos de investigación que se han venido realizando desde la década de 1970 y específicamente las investigaciones arqueológicas llevadas a cabo por Prieto entre 2010 y 2014, han permitido tener una perspectiva más amplia del sitio, enfocando su estudio en las dinámicas económicas y las interacciones sociales de sus pobladores con otros grupos contemporáneos. En este contexto, considerando que el sitio ha probado ser uno de los asentamientos con el uso más antiguo de vasijas de cerámica (Figura 1-b) en la costa peruana y para entender la introducción y/o uso de esta técnica en los Andes Centrales, fueron investigados estos artefactos. Fragmentos cerámicos encontrados en el sitio fueron estudiados por difracción de rayos-X, a fin de conocer su composición y características estructurales. Las medidas de la reflectividad fueron evaluadas por refinamiento estructural aplicando el método de Rietveld. Resultados de este estudio son presentados en este trabajo, con lo que esperamos contribuir al esclarecimiento de estos hallazgos.

O presente trabalho faz parte de um projeto maior, o qual pretende através silicofitólitos, δ 13C, datações por 14C-AMS e diversas análises pedológicas em perfis de solo, realizar a reconstituição paleoambiental no Médio Vale do rio Paraíba do Sul - RJ. Para isso, conhecer as características dos solos, bem como as concentrações de elementos presentes, pode auxiliar a interpretação de resultados, tornando a pesquisa mais fidedigna. Desta forma, 35 amostras de solo foram secas a 50°C, destorroadas, peneiras a 250 μm e analisadas por Fluorescência de Raios X por Dispersão de Energia (EDXRF). Foi utilizado um equipamento comercial produzido pela Shimadzu Corporation. Os parâmetros de operação foram: tubo de raios X de Ródio, tensão de 5 KV; corrente ajustada automaticamente de no máximo 1 mA; colimador de 10 mm; detector de silício; resfriamento termoelétrico; tempo de medida de 200 s e 3 varreduras por análise. Foi utilizada a metodologia de Parâmetros Fundamentas para a determinação quali-quantitativa. Os seguintes elementos foram encontrados: Si, Fe, Ca, Ti, K, Mn, Sr e Zr.

The white marble sculpture of Leopoldo e Silva (1879-1948), called "Menina e Moça" (23 x 147 x 40 cm), is kept in exposition in one of the hallway of the museum Pinacoteca de São Paulo, in which the public has direct access to it and it is even possible to touch the sculpture. As a result, the sculpture has dirt stains with brown shades over the white marble. A helical vortex cleaning system employing an air flux with calcite was performed as a blasting cleaning process. The calcite has a medium abrasiveness and its composition is similar to the marble sculpture. After the cleaning process a hydrophobic product based on silicon nanoparticles was applied (Silano®). This study consists in the surface qualitative characterization of the sculpture, which objective was to verify if the helical vortex cleaning process as well as if the hydrophobic sealant modify the surface chemical composition of the sculpture. A laboratory-made portable energy dispersive X-ray fluorescence (EDXRF) equipment, developed in the Applied Nuclear Physics Laboratory of the Universidade Estadual de Londrina, was taken to the Pinacoteca museum for the study. Fourteen measurements in different points were performed before helical vortex application, 7 measurements after the helical vortex cleaning and 3 measurements after the hydrophobic sealant application. Due to the limited available time for measurements, it was not possible to perform the same number of points before the cleaning. The operation conditions of the portable EDXRF equipment were: 35 kV, 5 µA and 200s excitatin/ measurement time. In all the spectra the chemical elements P, S, Ca, Fe, Sr appeared. The highest intensity peaks were from Ca and Sr which are the major components of the marble. In some point Zn was detected before the cleaning process. It was noted that the Fe and Zn intensity peaks decreased after the helical vortex cleaning attesting that the surface was cleaned because Fe is the major component of dust. The spectra of the measurements after the sealant application were identical to the ones made just with the helical vortex cleaning. However, the detection limit of the portable EDXRF equipment is in tens of ppm for light elements, therefore the Si nanoparticles were enabled to be identified. In conclusion, the helical vortex cleaning process and the hydrophobic application are efficient for sculpture conservation and do not alter significantly the surface composition of the marble.

An important aspect for the evaluation of fire effects in slash-and-burn agricultural system, as well as in wildfire, is the soil burn severity. The objective of this study is to estimate the maximum temperature reached in real soil burn events using energy dispersive X-ray fluorescence (EDXRF) as an analytical tool, combined with partial least square (PLS) regression. Muffle-heated soil samples were used for PLS regression model calibration and two real slash-and-burn soils were tested as external samples in the model. It was possible to associate EDXRF spectra alterations to the maximum temperature reached in the heat affected soils with about 17% relative standard deviation. Table 1 presents the measured values with thermocouple on burned fields samples with its respective predicted values by partial least square regression model using EDXRF spectra for the maximum temperature reached on surface soil. The results are promising since the analysis is fast, non destructive, and determined after the burn event, although local calibration for each type of burned soil is necessary.

El control de calidad de las aleaciones empleadas en la industria nuclear es muy importante, los datos emitidos lleva a la toma de decisiones de alto impacto. En este trabajo se desarrolla una nueva metodología para determinar aleantes e impurezas en aleaciones de zirconio (zircaloy), de titanio y de aluminio. La escasa cantidad de materiales de referencia necesarios para el análisis elemental de aleaciones por fluorescencia de rayos X convencional (WDXRF) nos llevó al desarrollo de una nueva forma de determinación empleando la fluorescencia de rayos X por reflexión total, donde el material sólido inicial se lleva a estado líquido en un simple paso de digestión, empleando mínimos volúmenes, y soluciones estándares trazables para la calibración del equipo. El espectrómetro utilizado es el S2 Picofox (Bruker), versión automática, con tubo de Mo, a 50kV y 0,6mA. En el caso de aleaciones de zirconio, se trabajó con una solución acuosa de ácido fluorhídrica para la solubilización de las virutas y posteriormente se analizan los aleantes y minoritarios: Sn, Fe y Cr, y luego las impurezas como Pb, Ni, Cu, Ti, Mn, V, Ta y W, empleando soportes de plástico, con un tiempo de medición de 300 segundos y la validación del método con un material de referencia NIST 360b para estimar los parámetros de exactitud y precisión, junto con los límites de detección. En el caso de aleaciones de titanio, las muestras se llevan a digestión en ácido fluorhídrico/ clorhídrico, los elementos analizados como impurezas son Fe, Al, Sn, Zr y Si. El material de referencia empleado en la optimización y validación del método es Ti 6-2-4-2. Finalmente, las aleaciones de aluminio se tratan con ácido clorhídrico y luego se realiza una solución con etanol al 20 % para disminuir el fenómeno higroscópico. Se optimiza el método para determinar Fe, Mn, Zn y Cr. El material de referencia empleado en la optimización del método es AA5052. La técnica de fluorescencia de rayos X por reflexión total es una herramienta muy útil para determinar impurezas en aleaciones, empleando mínimos volúmenes de muestra, con un proceso sencillo de tratamiento del material, a cortos tiempos de medición, utilizando soluciones trazables para su calibración y un material de referencia para la validación. Las fuentes de incertidumbre se identifican y los principales aportes se refieren al tratamiento de la muestra. Actualmente se emplea la TXRF para caracterizar aleaciones especiales de interés nuclear en ausencia materiales de referencia para su calibración.

The AlGaSb layers grown on [100] GaSb substrates could create structures that operate in the 0.7-1.7 µm range, this makes suitable for its potentially use in optoelectronic devices, these includes lasers and detectors working in optical fiber communication systems. In this work, the liquid phase epitaxy (LPE) technique was used to grow Al(x)Ga(1-x)Sb layers with different thicknesses on GaSb substrate and after the growth the layers were annealed at 450°C during four hours. The High Resolution X-ray diffraction (HRXRD) was used to analyze the crystalline quality and stress change of AlGaSb layers and the optical features of AlGaSb/GaSb system were observed through low temperature photoluminescence (PL). In this study the release of tensile stress and its transformation into compressive stress modifies the near band edge at low temperature causing a shift to lower wavelength. Also, the emission increased its PL intensity attributed to interdiffusion and intermixing of species and the reduction of non-radiative recombination centres in the layer.

Double perovskites Ba1+xLa1-xMnSbO6 were synthesized by traditional ceramic method in air as polycrystalline powders. The 0.1≤x≤0.2 compounds belong to the I 2/m monoclinic space group, while the x≥0.3 perovskites belong to the I 4/m tetragonal space group. Effective presence of mixture of Mn2+/Mn3+ has been well established by X-ray Emission Spectroscopy (XES) using high resolution Kβ emission for the set. The system Ba1+xLa1-xMnSbO6 displays signs of ferromagnetism at low temperature by magnetometry analysis. Also, Neutron Powder Diffraction data reveals that at 4 K, there is a presence of long range order that begins to disappear with increasing doping. We will show crystallographic and magnetic cell, magnetometry measurements, and XES measurements. Figure 1 – Room temperature Powder X-Ray Diffraction patterns for Ba1+xLa1-xMnSbO6 samples a) 0.1≤x≤0.4. and b) 0.5≤x≤0.7. Zoom view for the higher angles region for c) 0.1≤x≤0.4.and d) 0.5≤x≤0.7.

This work provides some applications of Total Reflection X-ray Fluorescence (TXRF) in the field of food analysis. The main reason for food analysis is because it is becoming more demanding safety and quality in this field by the regulatory agencies to ensure compliance with current standards. The concentrations of major, minor and traces elements were investigate by TXRF. A fast analysis allows an early detection before food could reach consumers. The following food samples were considered: wine, milk and cheese The samples may be separated in two different groups. The first two may be directly analyzed by TXRF, since they are liquid and can be diluted in water. The last must be digested to be analyzed in a microwave digester using nitric acid and oxygen peroxide. In the case of wines an important application is the classification of them through the elemental analysis as a fingerprint the possible vineyard. For milk, analysis of the elements it has an important role because it is one of the main nutrients for children. Furthermore dairy farms located in arsenicism areas were checked the presence of As in both milk and cheese samples. Milk and wine analysis was done directly over a dilution (1:5) of the samples. Cheese analysis needed a previous mineralization. In all case Ga (1mg/L) was used as internal standard. Total reflection X-Ray Analysis was perfomed in a S2 Picofox Bruker, X-rays from Mo tube at 50KV 0.6mA. . The accuracy of the measurements was calculated by determining the concentration of the elements in a standard solution (ICP-multielement standard solution). For milk samples the equipment was calibrate by adding elements that no are included in the sample in order to perform de sensitivity curves for K and L X- rays lines. In the case of wines calibration was performed using standard solution 20 % in ethanol. The results were satisfactory and allow propose the use of TXRF as a promising technique in the field of food analysis, in a wide scope, that is both environmental or quality control, or any other issues.

One of the most important preconditions in the analysis of historical/artistic materials is the use of nondestructive techniques. For this reason, X-ray techniques are the most popular and used in the analysis of these types of materials in Museums. The Energy Dispersive X-Ray Fluorescence (EDXRF) technique allows a nondestructive qualitative and quantitative multi-elemental analysis on various types of samples in Art/Archaeometry applications. This work analyzed ancient gold artifacts from different ages using an EDXRF portable system. Ten different types of gold samples were analyzed: earrings, pendants, figurines and clothing adornments. All samples analyzed are part of the gold collection of the Instituto de Pesquisa Histórica e Arqueologia do Rio de Janeiro (IPHARJ). The XRF analyses were performed using an EDXRF commercial system (ARTAX 200, Mo anode, 40 kV and 250 µA). The concentrations of Cu, Au and Ag were obtained from calibration curves obtained with gold standards of 24k, 18k, 16k, 14k, 12k and 10k. The results showed that the samples have different concentrations of gold. Thus, it was possible to classify the samples with respect to gold purity (karat gold). Besides that, two samples were classified as tumbagas since their copper and gold concentrations were very similar to those found in the literature.

Los medicamentos genéricos, ocupan cada día más un lugar de privilegio en el mercado nacional y mundial. La principal razón, se centra en el suministro de medicamentos a bajos costos que puedan ser asequibles a la población de escasos recursos económicos. Sin embargo, el suministro de medicamentos genéricos al ser humano, puede estar ligado a efectos secundarios o colaterales de gran impacto para la salud pública, debido a que no es únicamente necesario suministrar el principio activo específico, sino que además se requiere evaluar la forma cristalina de dicho principio activo (estudio del polimorfismo) y los excipientes que se proporcionan en el medicamento para garantizar que el genérico tenga la misma biodisponibilidad del medicamento original. En el presente trabajo se realizó un estudio estructural comparativo entre diversas presentaciones sólidas de la carbamazepina distribuidas en el área metropolitana de Bucaramanga (Colombia). Así mismo, se caracterizó molecular y cristalográficamente el principio activo de los medicamentos y se estudió el fenómeno del polimorfismo, evaluando el efecto de la temperatura y el solvente en el proceso de cristalización. Finalmente, se realizó la comparación de las formas polimórficas encontradas mediante la técnica de difracción de rayos-X de muestras policristalinas.

Nanomaterials present unique properties that strongly differ from those exhibited by bulk materials. Such singular features may be used to boost crop production. In this context, our group has been investigating the absorption, transport and metabolism of nanomaterials by plants. The present work has addressed the effects of nano ZnO on the germination of seeds of Phaseolus vulgaris. Seeds were soaked for 20 min in aqueous dispersions of 20, 40 and 60 nm ZnO at 1000 mg L-1. Germination was monitored during five days. The results showed that, compared to control seeds, 20 nm particles promoted the radicle development, whereas 40 nm and 60 nm prevented it. Aiming at understanding such effects, we have employed X-rays to monitor Zn behaviour. EDXRF analysis showed that Zn penetrates the seed coat reaching the embryo. For treated seeds Zn level goes from thousands to hundreds of mg kg-1 at the coat and embryo, respectively. In control seeds, it remains at tens of mg kg-1regardless the location. Figure 1a shows the distribution of Zn at the seed treated with 60 nm ZnO. The map indicates a gradient from the outer to inner region, Zn is mainly present at coat. µ-XANES was recorded at locations shown by Figure 1b. Conversely to control seed, Zn chemical species depends on the tissue nature. At the external part of seed coat, Zn remains as ZnO. At the middle of the coat it is mixture of ZnO + Zn-malate and at embryo it is found as Zn-hystidine + Zn-phytate. The seeds treated with 20 nm presented an important fraction of Zn-hystidine at the seed coat. Thus, at the current stage of our research, the results indicate that Zn-hystidine complex could be more beneficial for the seeds development. Figure 1 – (a) µ-XRF image showing Zn distribution (30 µm beam), (b) Magnified optical image highlighting the spots where µ-XANES (12 x 25 µm2 beam) were recorded and (c) Normalized Zn-K µ-XANES spectra. Seeds treated with 60 nm particles. Acknowledgement: This project has been funded by FAPESP Young Investigators Awards 2015/05942-0 and FAPESP Multi-User Equipment Grant 2015/19121. The µ-XANES measurements were performed at XRF beamline at LNLS, CNPEM. We are grateful to Dr. Carlos A. Perez and Douglas Galante for their assistance during beamtime.

Nowadays, the production and use of engineered nanomaterials (ENMs) for industrial applications has been grown. Among the different types of ENMs, metallic nanoparticles have been increasingly used, being silver nanoparticles (AgNPs) one of the most utilised due to their antibacterial properties. Because of the expansion of their fabrication, the release of these emerging pollutants into the environment has enhanced, especially in soils that are the main fate. Consequently, vegetables that grow in agricultural soils can absorb AgNPs suspended in soil fluids. Therefore, it is important to develop and improve analytical techniques in order to monitor these particles in the environment. With this purpose, we tested the possibilities of using total X-ray reflection spectrometry (TXRF) to monitor the silver content in soil adsorption kinetic studies and in the evaluation of AgNPs bioavailability to vegetal samples. For soil adsorption studies, an amount of soil was put in contact with a volume of a solution containing the analyte (AgNPs). Then, the analyte in the supernatant was monitored over the time, allowing its adsorption kinetics study on the soil. For TXRF analysis of soil extracts, it was found that using a deposition volume of 10 μL and a measuring time of 2000 s the limit of detection of Ag (Ag-Kα detection) was around 40 μg·L-1, which was suitable to carry out this kind of lab-controlled studies. TXRF results were compared with those obtained by inductively coupled plasma optic emission spectrometry (ICP-OES) and good agreement was found. Furthermore, we explored the possibilities to analyse directly the Ag adsorbed in the soil after performing the kinetic studies. In this case, the limit of detection for Ag using 50 mg of soil was around 1.5 mg·Kg-1. Results obtained using such approach was compared with those obtained after acidic microwave digestion of the soil and similar values were obtained. The evaluation of the transference of AgNPs to crops was performed through hydroponic experiments. These experiments consist on growing the plant in a hydroponic solution that contains the analyte. In this study, lettuces were grown in hydroponic media containing AgNPs or ionic silver (Ag+) during 9 days in lab-controlled conditions. After 9 days, an acid microwave digestion of the vegetal samples (roots and leaves) was done. The TXRF analysis of vegetal digests was performed using the same instrumental conditions as the soil kinetics studies. In the results obtained, the uptake AgNPs or Ag+ by roots was confirmed but not translocation to leaves. Results obtained were also compared with those obtained by ICP-OES. In conclusion, TXRF spectrometry can be considered a faster, simpler and cost-effective tool for AgNPs determination in soil adsorption studies as well as in investigations of their exposure to vegetables. It uses small sample volumes and it provides simultaneous multi-elemental information that can be useful to improve the understanding of the controlling factors on Ag mobility and bioavailability.

Presentamos el efecto estructural y composicional del aluminio en nanopartículas de ZnO sintetizadas mediante el método de sonoquímica, la impurificación con aluminio se hace in situ y varía de 0 al 2% atómico. Para la síntesis se empleó nitrato de zinc hexahidratado (Zn(NO3•6H2O) e hidróxido de amonio (NH4OH) y AlCl3 (fuente del ión Al+3) en medio acuoso. Se estudio el efecto del tiempo de irradiación ultrásonica para la obtención del material. La cristalinidad fue evaluada mediante Difracción de Rayos X (XRD) indicando la presencia de la estructura hexagonal tipo wurtzita, con orientación en el plano (002) y la composición se realizó mediante Fluorescencia de Rayos X, de longitud de onda dispersiva (WDXRF). La espectroscopia Raman confirmo la presencia de la fase. Se determinó el valor de banda prohibida mediante la caracterización óptica y se estudio el efecto del dopante sobre la estructura cristalina.

os compuestos de la familia tipo Ruddlesden-Popper (K2NiF4) como La4LiNiO8 y Nd4LiNiO8 pertenecientes al sistema cristalino tetragonal (I4/mmm) fueron sintetizados mediante la ruta nitrato-citrato (método Pechini), permitiendo así la obtención de una fase pura a baja temperatura y corto tiempo de calcinación. Para su preparación, se empleó un 50 % de exceso de hidróxido de litio, con el objetivo de estabilizar el alto estado de oxidación del metal de transición en el material [1]. El estudio de las fases cristalinas se llevó a cabo mediante el refinamiento Rietveld/Lebail con el fin confirmar los valores de las constantes de celda. El estudio de reactividad química de los compuestos preparados con los materiales 8YSZ ((ZrO2)0.92(Y2O3)0.08)0.926 y 10GDC (Gd0.10Ce0.90O1.95), que son los electrolitos más usados para las celdas SOFC, se llevó a cabo a una temperatura de reacción de 850 °C durante 3 horas con flujo de aire. Los materiales estudiados presentaron difusión de iones al ponerlos en contacto con los electrolitos dando lugar a la formación de otras fases; sin embargo, se encontró una cierta compatibilidad en el caso de 10GDC en comparación a 8YSZ.

El algoritmo para reconstrucción tridimensional de imágenes tomográficas más usado en la actualidad es el algoritmo FDK. Dependiendo del tamaño y la cantidad de radiografías de entrada y las dimensiones de las imágenes de salida el costo del procesamiento computacional puede ser elevado. Con el objetivo de acelerar el procesamiento varios trabajos han sido desarrollados usando diferentes configuraciones de hardware para procesamiento paralelo. En el presente trabajo presentamos los resultados de la paralelización del algoritmo FDK usando procesadores multicore (PM) e unidades gráficas de procesamiento (GPUs), las muestras usadas para testes fueron dados reales de tomografias. Las tablas 1 y 2 muestran los resultados alcanzados para las versiones paralelas del algoritmo en los dos hardwares paralelos testados. Para los testes fueron utilizadas tres muestras de diferentes tamaños 1 (400x308 pixels), 3 (1024x1024 pixels) y 4 (2000x1048 pixels). La versión paralela para GPUs fue testada en dos GPUs de diferentes capacidades GPU3 (NVIDIA GT 740M) y GPU4 (NVIDIA TESLA20KM). La versión paralela para PM fue testada en dos procesadores XEON E5-2420 Hexa Core de Intel, disponibilizando 12 núcleos físicos y 12 núcleos hypertreading. Las dos versiones paralelas del algoritmo consiguen acelerar el procesamiento. De los dos hardwares testados las GPUs consiguieron la mayor aceleración, sin embargo la limitada capacidade de memória de las GPUs disponibles actualmente no mercado limita su uso para paralelizar este tipo de aplicaciones. Considerando los resultados obtenidos, los costos financieros de los hardwares testados e los costos de desarrollo de las aplicaciones paralelas; sugerimos que para paralelizar el algoritmo FDK resulta más viable usar procesadores multicore en vez de GPUs.

Las celdas solares de películas delgadas están conformadas por capas de diferentes materiales, constituidas por dos contactos eléctricos, la capa absorbente y la ventana óptica. El objetivo principal en el avance tecnológico de estos dispositivos fotovoltaicos es reducir el precio de fabricación de los sistemas, desarrollar nuevos materiales con bajo nivel de toxicidad y que tengan las propiedades adecuadas para la fabricación de celdas solares, los cuales le permitan ser competitivos frente a las fuentes convencionales. En este trabajo se propone la síntesis y estudio de la composición química, morfología, propiedades estructurales y ópticas de los materiales ZnS, Zn(1-x)In(x)S y Zn(1-z)Nd(z)S. Los compuestos azufrados se depositaron sobre sustratos de cuarzo por la técnica sol gel mediante Spin-coating y posteriormente la sulfurización de las películas delgadas. Para la caracterización detallada de los recubrimientos se emplearon las técnicas de fluorescencia de rayos X (FRX), microscopia electrónica de barrido (SEM), difracción de rayos X (DRX), y espectroscopia UV-Vis. Un análisis cualitativo de los difractogramas empleando el programa Search March, confirmó la presencia de las fases cristalinas en estudio. Igualmente, mediante la fluorescencia de rayos X se realizó el análisis químico de los recubrimientos y se corroboró la concentración de cada uno de los elementos presentes en el compuesto. Los resultados obtenidos son de interés especial para evaluar su aplicación potencial como ventana óptica en celdas solares.

En esta investigación se estudia la transformación y reducción térmica de mineral de ilmenita pulverizado ~ (75µm) al pasar a través de una antorcha modificada de acetileno bajo condiciones reductoras y el diseñado de la antorcha es realizado por los autores y debe proveer los medios de obtención de dichas partículas. Se analiza el proceso desde el punto de vista termodinámico por medio de minimización de energía libre de Gibbs obtenidas mediante el software CSIRO Versión 5 y se describen las diferentes etapas del proceso hasta alcanzar la formación de las partículas de carburo de titanio y hierro. Por medio de una serie de simulaciones en diferentes herramientas, se determinan distribuciones de temperatura, análisis estructural del funcionamiento del sistema y comportamiento de las partículas. Posteriormente se realizan ensayos experimentales de una muestra de ilmenita pulverizada, para corroborar las condiciones de experimentación planteadas. Donde la ilmenita se descompone y se produce la nucleación de partículas de carburo de titanio sólidas, las cuales sirven de núcleos para la condensación posterior del hierro en estado líquido. El producto obtenido fue caracterizado por medio de difracción de rayos X (DRX), estos resultados indican un grado significativo de segregación del (Fe) sobre el carburo de titanio (TiC).

Los materiales zeolíticos son conocidos por su capacidad de intercambio catiónico, absorción y adsorción de molécula gaseosas en sus poros, como soportes enzimáticos y agregados alimentarios. Las propiedades descritas anteriormente dependen de su equilibrio superficial y de los poros de los grupos hidroxilo e hidrogeniones, los cuales se pueden modificar al aplicar intercambios iónicos. En el presente trabajo se sintetizaron sodalitas sódicas a partir de materiales de desecho y luego se sometieron a intercambio iónico con soluciones de cloruro de amonio a diferentes condiciones y tiempos de exposición en ultrasonido. Los sólidos obtenidos se caracterizaron estructuralmente mediante el método de Rietveld empleando el software comercial RIQAS, apoyados en los resultados de Flurescencia de Rayos-X, Resonancia Magnética Nuclear de Sólidos y Espectroscopia Raman; concluyendo que a mayor porcentaje de N3- sustituido en la ocupancia del Na+, mayor precipitación de sulfato, logrando un 60% de remoción del anión presente en 16mL de una solución 0,02M CuSO4 Authors express their acknowledgement to Universidad Industrial de Santander and Laboratorio de Rayos-X, Parque Tecnológico Guatiguará-PTG (Bucaramanga-Colombia) for data collection

A resistência à compressão do concreto é uma propriedade fundamental do material, estando diretamente relacionada com a estrutura da matriz cimentícia. Verifica-se que a presença de poros na matriz cimentícia diminui essa resistência, onde além da quantidade de poros, devem ser consideradas também a área específica e a distribuição dos poros por tamanho. Estes fatores influenciam diretamente na resistência do material. Devido à variação das dimensões dos poros, bem como às suas formas irregulares, as técnicas tradicionais variam desde operações e equipamentos simples até muito sofisticados, ocasionando diferenças significativas nos resultados. Este trabalho apresenta um método de ensaio não destrutivo (END) para obtenção da porosidade do concreto utilizando microtomografia por Raio X com processamento de imagens digitais para caracterização da distribuição, tamanho e volume dos poros presentes na matriz cimentícia. Foram utilizadas imagens microtomográficas das amostras de concreto de 20MPa e 30Mpa com 256 tons de cinza, ajustadas em contraste, binarizadas e filtradas para a caracterização da distribuição, volume e tamanho dos poros na matriz cimentícia. Os resultados dos valores de porosidade mostram compatibilidade entre o método apresentado e o método proposto pela NBR 9778 (2009).

El compuesto MoO2Cl2-4,4-dimetilbipiridina se obtuvo a partir de de la disolucion de 238,mg MoO2Cl2 (1.2 equiv) en 10ml de diclorometano seco bajo atmosfera de nitrogeno en un schlenk, al cual se le adicionaron lentamente 184 mg de dimetilpiridina disueltos en 10ml de diclorometano seco bajo atmósfera de nitrógeno. La reacción se agitó durante 3 horas a temperatura ambiente protegida de la luz. La mezcla de reaccion se filtró al vacio y el sólido resultante se lavó varias veces con éter etílico para obtener un sólido gris. La caracterización cristalográfica muestra que el compuesto cristaliza en el sistema monoclínico con constantes de celda: a=12.014(4)Å b=10.375(5)Å c=11.784(5)Å ß=103.233° V=1429.74 Å3

Cancer is a worldwide public health problem, and its incidence in the world grew by 20% in the last decade. Zinc, an essential trace element, is involved in many cellular processes. The main function of the prostate is the high production and secretion of citrate which is possible due to the unique accumulation of zinc by prostatic epithelial cells. In relation to prostate cancer, it can inhibit the growth of tumor cells, due to the stop of cell cycle and / or induction of apoptosis. The X-ray microfluorescence technique (μXRF) is a tool for modern analysis of elemental composition of different samples with high sensitivity and negligible damage to the sample. This study investigated the behavior of cells in spheroids of human prostate cells, tumor cell line (DU145) and normal cell line (RWPE- 1), after supplementation with zinc chloride by 24 hours and 48 hours using synchrotron X-ray microfluorescence (µSRXRF) and analyzed cell viability through colorimetric cytotoxicity assay (MTT). The measurements were performed with a standard geometry of 45º of incidence, excited by a white beam using a pixel of 25 μm and a time of 300 ms/pixel at the XRF beamline at the Synchrotron Light National Laboratory (Campinas, Brazil). The results by µSRXRF showed that Zn intensity decreased in tumor cells despite supplementation and the treatment time, while in normal cells that intensity increases with supplementation and the treatment time. MTT assay's results were not significant, which indicates that the cell viability was not changed, regardless of treatment in both cell types tested, so the cells are viable.

Enxofre, vanádio e níquel são contaminantes naturais importantes para estudos geoquímicos de origem e classificação do petróleo. Entretanto, as suas presenças são prejudiciais para a qualidade do petróleo e dos produtos, pois são associadas à corrosão de equipamentos, às desativações dos catalisadores de craqueamento e de hidrotratamento e à poluição atmosférica. Com o propósito de obtenção de uma metodologia alternativa aos métodos oficiais (ASTM D2622, ASTM D5863, ISO 14597 e ISO 51790, por exemplo) que utilizasse menores quantidades de amostra e de solvente, abordagem simples de correção do efeito matriz e instrumentação analítica acessível foi desenvolvido um método onde esses analitos são quantificados em filmes finos de petróleos por meio de um espectrômetro EDX comercial de bancada e de baixa potência. Os resultados da validação mostraram que a metodologia é suficientemente sensível (limites de detecção de 0,02 % em massa para o enxofre, 0,8 mg/kg para o vanádio e 1,0 mg/kg para o níquel), seletiva, robusta, acurada (recuperações médias de 100,3 % para o enxofre, 98,7 % para o vanádio e 99,7 % para o níquel) e precisa (precisões globais médias de 7,1 % para o enxofre, 5,3 % para o vanádio e 5,2 % para o níquel) para finalidades acadêmicas e industriais quando aplicadas para petróleos similares aos brasileiros (traços de vanádio e níquel e enxofre até 1 % em massa). As amostras devem ter o parâmetro BSW enquadrado (teores de água inferior a 0,5 % em volume e de sais e sedimentos menores que 275 mg/L), pois as precisões são sensíveis a teores elevados de cloro no petróleo.

Marcelo Rubio1, María F. Mera2, Carlos A. Pérez3, Sofía Cazón4 1 CEPROCOR, Álvarez de Arenales 230, (5000), Córdoba, Argentina. CONICET, Buenos Aires, Argentina. FAMAF, Universidad Nacional de Córdoba, Córdoba, Argentina. {mrubiocba@yahoo.com} 2 CEPROCOR, Álvarez de Arenales 230, (5000), Córdoba, Argentina {mariafernanda.mera@gmail.com} 3 LNLS, Laboratório Nacional de Luz Síncrotron, Caixa Postal 6192, CEP 13083-970, Campinas, SP, Brazil. {carlos.perez@lnls.br} 4 CEPROCOR, Álvarez de Arenales 230, (5000), Córdoba, Argentina {soficazon@gmail.com} ABSTRACT Phytoextraction technologies uses plants to extract toxics metals from contaminated soils and accumulate them in the harvestable parts of the plants, which can then be removed from site. This work describe inconclusive results of the phytoextracion capacity of three kind of plants: 1) hyperaccumulator plant species such as Brassica napus, 2) fast-growing non-hyperaccumulator plants such as Festuca arundinacea (Both 1 and 2 grown in Pb industrial level contaminated soil), and 3) Lolium perenne grown in Pb contaminated soil and in crops of hydroponics. SR µXRF technique offers a powerful approach for probing and mapping the distribution of Pb in selected sections of plant tissues. The measurements were carried out at the D09B XRF Fluorescence beamline of the LNLS. Preparation of contaminated soil, seed selection, seeding, control of handling plant growth variables, selective harvesting and preparation of samples for SR µXRF were done at CEPROCOR. Keywords: X-Ray; Fluorescence; Synchrotron Acknowledgement: This work was developed at Brazilian National Synchrotron Light Laboratory under the proposal XRF-18934. The authors would like to thank the LNLS staff for its technical support. We are grateful for the financial support of CEPROCOR and LNLS for this project. References [1] Scheckel K., and col., In Vivo Synchrotron Study of Thallium Speciation and Compartmentation in Iberis intermedia, Environ. Sci. Technol. 2004, 38, 5095-5100. [2] Donner E and col, Mapping Element Distributions in Plant Tissues Using Synchrotron XRF Techniques. Chapter 9, 2012. [3] Lombi E and col, In situ analysis of metal(loid)s in plants: State of the art and artefacts. Environmental and Experimental, Botany, 72, 2011, 3-17. [4] EPA Phytoremediation resourse guide, United States Environmental Protection Agency, EPA 542-B-99-003 June 1999. [5] Sarret G and col., Use of Synchrotron-Based Techniques to Elucidate Metal Uptake and Metabolism in Plants, Chapter 1, Advances in Agronomy, 2013, 1. [6] Rubio M et al. Study of lead levels in soils by weathering of metallic Pb bullets used in dove hunting in Córdoba, Argentina. X-Ray Spectrom. March 2014.

El presente estudio se basa en la preparación de un material composite a partir de hidroxiapatita (HAp) y titania (TiO2) mediante radiación ultrasónica en una relación 1:1. La Hidroxiapatita (HA) es un fosfato de calcio Ca10(PO4)6 OH que presenta una composición muy similar a la parte mineral del tejido óseo, por lo que es un material biocompatible y bioactivo ideal para regeneración ósea por lo que es considerado un material de elevada aplicación médica. Por su parte el TiO2 presenta propiedades mecánicas como alta dureza y resistencia al desgaste, además de ser bioinerte y biocompatible, haciéndolo un candidato idóneo para obtener un material biomaterial. La caracterización de las fases presentes fue evaluada a través de difracción de rayos X y espectrometría Raman. Los patrones de difracción mostraron los picos característicos de la HA en fase hexagonal y fueron confirmados mediante la base de datos PDF-4 (ficha 9-0432). El estudio composicional fue realizado mediante fluorescencia de rayos X.

In the recent years different nanoparticles agents have been proposed for produce diagnostic images of tumor areas and simultaneously the application of highly localized treatment. The most studied are the Gold nanoparticles (GNPs) that are enhancer of local dose delivery for orthovoltage radiotherapy and a contrast agent with a better attenuation that the traditional compounds used. One of the common challenges that presented the using these new agents is to develop methodologies for detection in vivo, quickly, efficiently and with greater sensitivity when are provided to the organism. Given that the effectiveness of their applications require knowing exactly the concentration and distribution in the volumes of study. In this work is optimized a benchtop L X-ray system of low power (4 W), which allow quantify in vivo low concentrations of gold nanoparticles into tumor phantoms, with the minimum surface dose. The studied dephs for the tumor phantoms were 0-4 mm of depths in tissue equivalent, with a fixed volumen of 0.3 cm3. The composition of the doped tumor phantoms consisted of a solution of GNPs (1.9 nm AurovistTM, Nanoprobes Inc.) suspended in de-ionized water. For the optimization procces, a set of measurement were carried out for determining the optimal incident spectrum which minimized the limit of detection and the dosis. Several tube voltages (kVp) and alluminium filters of different thicknesses (0.75 mm to 3 mm) for each kVp were configured to obtain a non-symmetrical narrow spectrum with a fixed FWHM and centered between the 8-20 keV. For determining the experimental detection limit, several GNPs concentrations ranging from 0.05 to 10 mgAu/ml were measured into the tumor phantoms at the dephs previously selected and considering a statistical fluctuantion with a 95% of confidence level. The ranging of concentration and depths selected, corresponds to the possible tumour gold concentrations for in vivo aplication.

Previous X ray diffraction studies indicate distortions of geometric parameters (length and / or bond angles) in many first row coordination complexes. Distortions that result in clearly different coordination geometries described for each coordination number, and several times to raise doubt about the existence of chemical bonds. A recent study of [Zn(Phem)2Ac]BF4 (B.L. Rodrigues. Acta Cryst. (2004). E60, m1166) shows asymmetry coordination in Zn-O bonds, with d[Zn-O1] = 2.293(3)A and d[Zn-O2] = 2.149(3)A. This work presents crystallographic and spectroscopic studies of two new nickel compounds. Compound [Ni(Bipi)2Ac]BF4 shows the metal and the acetate in crystallographic special position (axis 2), which requires equivalence between the bonds Ni-O. [Ni(Phem)2Ac]BF4, on the other hand, does not present the metal and acetate in special positions. Despite of this, this compound also presents equivalence in the coordination between the metal and each acetate oxygen. Furthermore, through studies of Hirsfeld surfaces intermolecular interactions are identified, between individual molecules in the crystal, hydrogen bonds. Diffraction results for polycrystalline samples and compared to the simulated diffraction patterns from single crystal diffraction, indicate that crystalline materials are pure. UV-Vis spectra suggest close proximity between the forces of bipyridine and phenanthroline ligands.

The use of X-ray Fluorescence is very often restricted to the analysis of bulk materials by the average user. The technique is also considered as not being fit for the lower ppm or even ppb concentration range. Much of this is true, but appropriate sample preparation techniques, the additional hardware and software show that XRF is capable in analysing much more than only the "traditional" samples. For the analysis of light elements (H - O) XRF cannot be considered as THE technique. Nevertheless, adequate fundamental parameter software makes it possible to calculate a very good estimate of the total concentration of light components and therefore also the results of other elements of interest will be improved drastically. What about analysing ppb levels in aqueous solutions? It is possible with the appropriate sample preparation technique. Did you ever think about performing mapping analysis on inorganic or even organic samples? Also this is something XRF will do excellently with adapted soft- and hardware tools. This presentation will show you the flexibility and strength of WDXRF, a technique that becomes more and more a complete analysis tool.

AlGaSb layers grown on [100] GaSb substrates could build structures in order to use in optoelectronic devices such as lasers or detectors for operate in the 0.7-1.7 µm range. In this work, the liquid phase epitaxy (LPE) technique was used to grow Al(x)Ga(1-x)Sb layers with different composition of x value from 0.03 to 0.15 on GaSb substrate, this cause a substitution of gallium by aluminium atoms. The High Resolution X-ray diffraction (HRXRD) was used to determine the lattice parameters of AlGaSb layers, the mismatch to substrate and the relaxation of layer. The composition was studied by x-ray fluorescence (XRF). In this study the substitution of atoms creates tensile stress and relaxation, its lattice parameters follows the Vegard's law in function of composition, also, the composition changes the operation wavelength for the potential use in optoelectronic device.

A fluorescência de raios X (XRF) é uma técnica analítica multielementar bastante difundida e com aplicações variadas. Uma das características importantes de um sistema de XRF é a sua capacidade de ser portátil; o que permite a aplicações em várias áreas da ciência e tecnologia concomitantemente. O objetivo desse trabalho foi o desenvolvimento de um sistema de XRF portátil (APOENA X) abrasileirado e competitivo com os sistemas comerciais. O sistema Apoena X é formado por um mini tubo de raios X de baixa potência (anodo de Ag, 40kV/200µA), um detector SiPIN e uma micro câmera digital para alinhamento do feixe de raios X sobre a amostra. A microcâmera digital foi fixada entre o detector e o tubo de raios X de forma que a imagem do ponto de medida pudesse ser visualizada na tela de um microcomputador e que um feixe de laser mostrasse pontualmente o local de interseção entre o feixe de raios X incidente sobre a amostra e o feixe emergente que é produzido na direção do detector. O software de posicionamento da microcâmera digital foi desenvolvido no próprio laboratório (LIETA). O sistema portátil é alimentado por uma bateria gerando maior portabilidade e permitindo aplicações em ambientes externos onde o acesso a rede elétrica é impossível. O sistema APOENA X é compacto, funcional, inovador e fora dos padrões comerciais dos equipamentos importados. Além de gerar tecnologia na área de espectrometria de raios X, o sistema portátil tem função multiaplicativa que permite a análise de uma variedade grande de tipos diferentes de amostras.

In the pharmaceutical industry is important characterize the active pharmaceutical ingredients (APIs) involved in the manufacture of a drug. It is well-known that a number of physicochemical properties of the APIs depend on the structural characteristics in the solid state. Thiocolchicoside is an active pharmaceutical ingredient used as a muscle relaxant. The only crystal structure thiocolchicoside-related reported in the Cambridge Structural Database corresponds to an ethanol solvate hydrate (Refcode: THCLCS). However, the hydrogen atoms information and intermolecular interactions is not reported. Yellow prism crystals were obtained from an ethanol/water solution at room temperature. Integration and reduction of the single diffraction data produced an orthorhombic cell with space group P212121 (No. 19) and parameters a= 9.8311(7) Å, b= 12.0923(8) Å, c= 28.180(2) Å, V= 3350.1(4) Å3, similar to THCLCS. The present X-ray diffraction study consists in a crystal structure, hydrogen bonding and CH...π interactions analysis which play an important role in the crystal packing and have not been reported previously for this material.

Synchrotron Micro X-Ray Fluorescence (µSRXRF) is a non-destructive technique very often used in biological investigations to obtain information regarding the distribution of elements in tissue and cell samples. Diseases of the prostate are very frequent in men over 40 years of age. Prostate cancer and benign prostatic hyperplasia (BPH) represents, worldwide, a significant risk in terms of morbidity and mortality. In this context, the aim of this work was to investigate the distribution of Fe, Cu and Cu/Zn using synchrotron X-ray microfluorescence (SRµXRF) in cell spheroids in benign prostate hyperplasia (BPH) and prostate cancer (DU145) supplemented with Zinc and to analyze the influence on intensity of Fe, Cu and Cu/Zn after Zinc supplementation. The SRµXRF measurements were performed in standard geometry of 45º incidence, exciting with a white beam and using an optical capillary with 20 μm diameter collimation in the XRF beam line at the Synchrotron Light National Laboratory (Campinas, Brazil). The results showed non-uniform distribution of Fe and Cu in all the spheroids analyzed. It was possible observed that intensity of Fe, Cu and Cu/Zn were changed with the Zn supplementation. Therefore, the Zn supplementation changes the metabolic of prostate cell.

During the last years has been proposed the utilization of Gold and Silver nanoparticles like bio-markers when are bound to molecules like antibodies, which are linked to specifics cell receptors. This would provide useful information like the spatial distribution and radiosensibility of the tumor cells in the cancer treatment. Because the distribution of malignant cells is heterogeneous in tumour volume, the dose could be modulated considering different bio-parameters that will affect the distribution and radiosensitivity of cells, as the concentration of intracellular oxygen and cell redistribution. Therefore use gold and silver nanoparticles with specific markers would provide information of these bio-parameters, and thus individualize treatments depending on the conditions of the tumor microenvironment. In this work is optimized a bench-top EDXRF system, which allow quantify in vivo low concentrations of silver and gold nanoparticles into tumor phantoms. In the first state, the system was previously configured using XMI- MSIM software designed to predict the XRF spectral response using Monte Carlo simulations. The studied setup is comprised of an mini X-ray tube and a set of filter of Se, Sr, Y, Zr, (for exiting the gold L3-edge) and Cd, In and Sn (for exiting the silver K-edge), configured with variable thickness, for emit simultaneously two spectrally narrow beam centered on a specific excitation energy. The figures of merit used for adjusted the composition and thickness of the filters were minimizing the detection limit and radiation exposure. In the second state, the experimental verification was realized in a tissue equivalent phantom, made of a mixture of 96% cellulose and 4% salt Merck. Tumor phantoms of 0.3 cm3 embedded with the nanoparticles agent consisted of a solution of GNPs (1.9 nm AurovistTM, Nanoprobes Inc.) and Silver nanoparticles (in-house by LIIFAMIRx) suspended in de-ionized water. For determining the experimental detection limit, several concentrations ranging from 0.05 to 10 mgAu/ml were measured into the tumor phantoms considering a statistical fluctuation with a 95% of confidence level. The ranging of concentration studied corresponds to the possible gold and silver concentrations expected to be found in future in vivo application in human.

La fluorescencia de rayos X (FRX) es una técnica que permite, en el área de exploración y explotación de hidrocarburos, el análisis de metales en muestras geológicas de reservorios. La información obtenida puede utilizarse para el modelado del reservorio, el análisis de potencialidad de roca a través de la determinación de correlaciones estratigráficas, inferir el ambiente de deposición y ayudar a entender la mineralogía como la mecánica de la roca. Al igual que cualquier técnica analítica, un punto clave en la confiabilidad del análisis cuantitativo en las mediciones por FRX es la preparación de muestra. En el caso del análisis de muestras geológicas existen tres posibilidades de preparación para la medición; molienda y análisis directo en polvo, medición en pastillas prensadas o fusión de la muestra. Este último, presenta diversas ventajas como la eliminación de efectos de tamaño de partículas y de matriz. En el siguiente trabajo se realizó una optimización del método por fusión para el análisis de metales en rocas de reservorio por FRX. La misma se realizó seleccionando por medio de un diseño exploratorio los factores significativos del tratamiento de la muestra que afectan a la señal. Posteriormente, se encontraron las condiciones óptimas de trabajo empleando una metodología de superficie de respuesta. Finalmente, empleando las condiciones optimizadas se realizó el análisis cuantitativo de las muestras construyendo las curvas de calibración para los metales de interés. Los límites de detección y cuantificación encontrados fueron: Fe: 0,5 y 2,6 ppm; Ti: 0,4 y 1,0 ppm; Ca: 1,8 y 6,0 ppm y K: 0,9 y 2,0, respectivamente. La metodología se validó mediante estándares geológicos certificados y se comparó con la técnica de referencia por ICP, encontrando que la metodología utilizada es adecuada para el análisis de metales en rocas de reservorio.

Se realizó la caracterización estructural del compuesto 4-cloro-N-(9H-fluoren-9-iliden)anilina por medio de difracción de rayos-X de monocristales. Mediante este estudio se obtuvieron las posiciones atómicas, longitudes y ángulos de enlace. Adicionalmente, se determinaron las constantes de celda a= 14.2571 (12) Å b= 5.2035 (4) Å c= 19.4321 (18) Å β= 99.152(15)°, el volumen de celda determinado 1423.25 Å3 y el grupo espacial P 21/n. En la Figura 1 se aprecia la celda unidad del compuesto de interés Figura 1 – Celda unidad del compuesto 4-chloro-N-(9H-fluoren-9-ylidene)anilina Finalmente se determinaron las principales interacciones intra e intermoleculares del compuesto de interés.

The antiretroviral drug Nevirapine (NVP) (11-Cyclo-propyl-5,11-dihydro-4-methyl-6H-dipyrido[3,2- b:2’,3’-e][1,4]diazepin-6-one) is a non-nucleoside reverse transcriptase inhibitor, used in the treatment of HIV-1 infection. It is a class II drug according the Biopharmaceutics Classification System (BSC)1, exhibiting low solubility and high permeability. To increase the drug dissolution and its bioavailability, the different preparation methods with crystal modification such as co-crystals were studied. Co-crystals are multicomponent crystalline solids which have different drug molecules or a drug and a non-volatile substance in its structure. NVP molecule has a conformationally rigid amide group that allows a co-crystal formation with soluble carboxylic acids or amide co-formers2. Caira et al. reported the crystal structure and solid state properties of several NVP co-crystals2. We prepared different co-crystals of NVP and there were identified using their crystal structure Caira published data. The only case where we observed differences was for NVP-salicylic acid (NVP-AS). Our data presented different reflections in comparison with reported data. Therefore, the goal of this work was to determinate the crystal structure of NVP-AS using single crystal X-ray diffraction in combination with solid state NMR spectroscopy in order to confirm our crystal structure results. 1 Lindenberga, M.; Koppb, S.; Dressmana, J. B. European Journ. of Pharm. and Biopharmaceutics. 2004, 265-278. 2 Caira, M.R. et. al. CrystEngComm. 2012, 17-23. Acknowledgement: We are grateful for the financial support of CAPES for this project.

In the present study jewels from the tomb of the lady of Cao were studied, a Moche “queen” of a period around 300 AD (in the Museum “Señora de Cao” in Magdalena de Cao, north of Peru). To this aim a X-ray digital radiography system (XDR) was employed, using a mini X-ray flat-panel sensor. The objective of these analyses was to obtain structure information of the jewelry (mainly nose ornaments composed of gold and silver sheets), particularly about manufacturing mode and soldering between gold and silver sheets and thickness quantification. A portable XDR system was employed, consisting of a flat-panel detector using APS-CMOS technology produced by Schick Technologies and a mini X-ray tube with Au anode from Amptek, which works at 50 kV and 100 µA maximum voltage and current. The radiographic images of the jewels revealed interesting details on the manufacturing process and on how the silver and gold sheets were glued or soldered .

Na área de Ciência e Tecnologia os espalhamentos Rayleigh e Compton de raios X têm papel importante porque podem ser utilizados para caracterizar um material compósito através do seu número atômico efetivo (Zef). A importância do desenvolvimento desta metodologia estar relacionada à forma de se obter o Zef de um material e consequentemente o coeficiente de atenuação de massa (µ) por técnicas de espalhamento sem usar a transmissão de radiação. Isto é importante na região de baixas energias (E<30 keV) onde as técnicas de transmissão são inviáveis. O Zef e o µ são parâmetros importantes em várias aplicações tecnológicas, principalmente em dosimetria da radiações ionizantes e Física médica com fótons de baixa energias. Neste trabalho foram analisadas 128 amostras de polímeros; sendo 6 do tipo 1, 8 do tipo 2, 8 do tipo 3, 4 do tipo 4, 12 do tipo 5, 13 do tipo 6, 15 do tipo 7 e 62 polímeros com classificações desconhecidas. Todos os perfis de espalhamento foram obtidos num ângulo de espalhamento de 128 graus, usando um tubo de raios X com anodo de prata (35 kV e 100 µA) e um detector semicondutor do tipo SiDrift (SDD). A energia associada aos fótons do feixe incidente foi a linha Kα da Prata (22,16 keV). Foi mostrado que existe uma relação linear entre a razão R/C e Zef dos materiais analisados, principalmente, no intervalo de Zef de 6 – 14. Foram caracterizados nove polímeros pelo Zef e o coeficiente de atenuação de massa (µ). Polímeros do tipo 1, tipo 2, tipo 3, tipo 4, tipo 5, tipo 6, Teflón, EVA e acrílico. Além disso, foi possível caracterizar 73 % dos polímeros desconhecidos. Deste grupo foi possível classificar 6 polímeros como do tipo 1, 13 do tipo 2, 2 do tipo 3, 12 do tipo 4, 7 do tipo 5, 9 do tipo 6 e 14 do tipo 7 (acrílico). Não puderam ser classificados 17 polímeros por que a faixa de Zef (6,50 – 11,84) estava fora dos intervalos de confiança dos Zef dos polímeros estudados neste trabalho.

Crude oil is a complex matrix with the presence of several types of contaminants (metallorganic compounds, sulfur containing compounds, sediments, among others). The deleterious effects of metallorganic in petroleum are associated with poisoning of catalysts, equipment corrosion and toxic emissions to the atmosphere. On the other hand, their contents are used as geochemical oil origin markers and for classification. In this study, two methodologies of sample preparation (deposition on solid substrate and thin film) aiming the determination of V and Ni in oils have been studied, comparing different benchtop EDXRF spectrometer configurations and calibration approaches. The achieved results were compared to the ones obtained using the traditional direct analysis. The methodologies were validated by analysis of reference materials from NIST and ASTM proficiency test programs, whose results showed to be precise and accurate (Table 1). Unlike the usual sample preparation methods for the analysis of petroleum by XRF, AA, or ICP, the proposed methodologies require smaller amounts of sample and solvents, minimizing labor and cost of analysis.

Crude oil is a complex matrix containing different contaminants (for instance, metallorganic compounds, sulfur containing compounds, sediments and water). Al and S could be present in oil, at relevant quantities, mainly as finely divided solids. Evaluating the presence of water and sediments in crude oil is important as they bring problems during refining, equipment corrosion; irregular operation of the distillation unit; blocking of the heat exchangers and affect product quality. In X-ray fluorescence (XRF) spectrometry, the usual strategy to determine sulfur and metals in crude oil involves the use of organic standards in mineral oil, providing some degree of matrix matching. In this study, Energy Dispersive (ED) XRF spectrometry was used to develop a method to determinate silicon and aluminium in crude oil samples, using proper strategy as these elements are not present in samples as organic specimens. The analytical curves were prepared using: i) inorganic standards in lithium tetraborate (as in ASTM D5863) ii) organic standards in mineral oil. Both strategies used the standards (solution) in a solid substrate to measure the elements intensity. The results showed that the specimen form used as standards in calibration has a direct influence on the results obtained, indicating that such a study should always be performed when developing a XRF based method for crude oils. In Figure 1 it is shown the calibration curves for Al and Si using both calibration strategies and Table 1 contains the results obtained using both approaches for the analysis of ASTM proficiency test samples and for crude oil samples provided by Petrobras.

The analysis of trace elements in cancer research has gained interest in recent years due to reported correlations between abnormal concentrations and tumour growth. Quantitative topographic elemental studies using synchrotron µ-XRF enables investigations even at the single cell level, but it requires a proper sample preparing technique to ensure that the measured elemental distribution accurately reflects the spatial variations in the real samples. Two sample preparation techniques (formalin fixed followed by paraffin embedded and formalin fixed followed by cryostat sectioning) were analysed in a total of 10 paired breast carcinoma samples. Measurements were performed at the XRF beamline of the Laboratório Nacional de Luz Síncrotron, Campinas - Brazil. Comparison between trance elements maps and histological slices showed that both techniques preserve spatial distribution of trace elements. It was observed an increase in the signal to noise ratio of Ca, Fe Cu and Zn in the paraffin embedded samples, compared to cryostat cut ones, possibly due to the removal of adipose tissue. The quartile coefficient of dispersion analysis showed similar variability in both sample preparations. Also, the ratios Fe/Ca, Zn/Ca and Cu/Ca showed similar tendencies in both sample preparations, suggesting that these procedures affect all analysed elements in a proportional way. Finally, our results suggest that paraffin embedded procedure is preferable for breast cancer analysis using µ-XRF, since it preserves morphological and chemical aspects of the samples while provides an increasing in the signal to noise ratio.

O estudo e a caracterização de objetos de valor arqueológico ou histórico, utilizando técnicas físico-químicas de análise vêm se intensificando nos últimos anos. Este tipo de estudo multidisciplinar é também conhecido como arqueometria. Os artefatos cerâmicos usualmente constituem o tipo de objeto mais encontrado em escavações arqueológicas, por isso é um tipo de amostra frequentemente estudada na arqueometria. A análise da cerâmica pode complementar as informações obtidas em documentos escritos para produzir um melhor conhecimento. A Fluorescência de Raios X (XRF) é uma das técnicas, que possuem grande destaque na análise de artefatos cerâmicos, isto, por que a mesma possibilita caracterizar a composição elementar das amostras, com boa precisão e acurácia de forma não-destrutiva. Neste trabalho foram caracterizados por XRF, doze fragmentos cerâmicos escavados, por pesquisadores do Museu Nacional da UFRJ em uma antiga fazenda no município de Pirenópolis, Goiás (Brasil), cuja fundação é datada de 1800. Sendo, que as amostras foram escavadas principalmente no quintal da sede e nas senzalas. Os resultados obtidos pela XRF foram comparados através de testes estatísticos multivariado – Análise por Componentes Principais (PCA) – no intuito de estabelecer similaridades ou diferenças a nível elementar entre as amostras investigadas. Os espectros de XRF foram coletados no sistema modelo TRACER IV da Bruker, utilizando tensão de 40 kV e corrente de 10 μA, durante quatro minutos. Foram obtidos três espectros de XRF para cada amostra, onde em seguida foi realizada a média dessas três contagens de cada amostra para serem comparadas no PCA. Os resultados da XRF revelaram que todas as amostras possuem os seguintes elementos: K, Ca, Mn, Fe, Cu, Y, Sr, Nb, Mo. Sendo a diferença entre os espectros de XRF a despeito das intensidades dos elementos. A comparação das amostras por PCA permitiram identificar que algumas amostras da senzala e do quintal da sede possuem grandes semelhanças à nível elementar, permitindo inferir que o material cerâmico utilizado pelos escravos e senhores do engenho possuem a mesma proveniência. Este resultado permite respaldar a hipótese sobre o modelo de escravidão adotado na propriedade, que incluía atitudes paternalistas do proprietário, que englobava a distribuição de materiais cerâmicos de uso cotidiano para os escravos.

El compuesto (1E,2E)-N-(4-clorofenil)-3-fenilprop-2-en-1-imina [3], se sintetizó a partir de una mezcla estequiométrica de 4-cloroanilina [1] (1.5mmol) y trans-cinamaldehído [2] (1.5mmol). La caracterización molecular se llevó a cabo mediante espectroscopía infrarroja (IR) y resonancia magnética nuclear (RMN). En la Figura 1 se muestra el esquema sintético realizado para la obtención del compuesto [3]. La caracterización cristalográfica del compuesto (1E,2E)-N-(4-clorofenil)-3-fenilprop-2-en-1-imina se realizó por medio de la técnica de Difracción de Rayos-X de muestras policristalinas, obteniendo que el compuesto [3] cristaliza en un sistema monoclínico con grupo espacial P21/c (Nº 14) y presenta las siguientes constantes de celda: a = 14.824 (7) Å, b = 16.48 (1) Å, c = 5.137 (3) Å, ß = 96.83° (7) y V = 1246.2 (9) Å3, con figuras de mérito de M(20) = 10.8 y F(20) = 21.5 (2.9332, 0.0186).

De acuerdo a las diferentes teorías sobre el origen del petróleo, se puede asumir que el petróleo y el gas se originan principalmente en rocas sedimentarias, a partir de la evolución térmica de la materia orgánica. En tal sentido, las rocas generadoras de petróleo deben contener suficiente materia orgánica, adicionalmente a la calidad se debe de considerar la cantidad y madurez que haya alcanzado en la ventana de generación de petróleo y gas. Teniendo en cuenta que algunas formaciones se caracterizan por su alto contenido orgánico de proveniencia marina, afecta que no existan contenidos apreciables del macerales como la vitrinita. Lo que conlleva a tener limitaciones para determinar la madurez térmica de la materia orgánica a partir de la reflactancia de la vitrinita (Ro). Esta desventaja es frecuentemente suplida por el uso de otros indicadores como el de la Ro equivalente de la Tmax calculada a partir de la ecuación de Jarvie (2011). Esta investigación propuso el uso de variables cristalográficas tales como FWHM y tamaño del cristalito como método alternativo para estimar la madurez termal de la roca. Para tal efecto, se calcularon las variables cristalográficas en la reflexión (001) de Caolinita y se analizaron mediante una correlación lineal multivariada con algunos datos experimentales y calculados de Ro de una formación colombiana. Con la correlación obtenida se pudo confirmar que la caolinita se encuentra afectada por el grado de madurez de la roca y que las rocas de la formación en estudio corresponden a rocas maduras que se encuentran en la ventana de aceite.

El compuesto 4-cloro-N-(9H-fluoren-9-iliden)anilina se obtuvo a partir de 0.31g (1.72mmoles) de 9-fluorenona [1] y 0.22g (1.72mmoles) de 4-cloroanilina [2]. La reacción se llevó a cabo utilizando etanol como solvente y reflujo constante durante 72 horas. La formación de cristales amarillos con punto de fusión de 153°C y la caracterización molecular mediante técnicas analíticas instrumentales como Infrarrojo y espectrometría de masas evidenciaron la formación del compuesto [3]. El proceso de síntesis se aprecia en la Figura 1. Figura 1 – Síntesis del compuesto 4-chloro-N-(9H-fluoren-9-ylidene)anilina Posteriormente se realizó la caracterización cristalográfica por difracción de rayos-X de muestras policristalinas, encontrando que el compuesto de interés cristaliza en el sistema monoclínico con constantes de celda: a = 14.261 (2) Å, b = 5.205(4) Å, c = 19.428(2) Å, ß = 99.147° (2) y V = 1426.4 (1)

O Brasil é um dos maiores produtores de gemas, ou pedras preciosas, do mundo, além de conter uma enorme variedade gemológica, sua produção é reconhecida internacionalmente pela sua qualidade e beleza. Algumas das gemas brasileiras usadas em joias são: a Esmeralda, a Água-marinha, o Topázio, a Turmalina, o Quartzo e a Ametista, diferindo uma das outras quanto à cor, transparência e dureza. Certas gemas, embora valiosas e bonitas, não possuem a dureza e a fragilidade desejável para serem usadas em joias, mas são exibidas em museus e procuradas por colecionadores. As gemas são classificadas de acordo com diferentes especificações técnicas como a composição química e os sistemas cristalinos. Muitas gemas são da classe dos silicatos e dos óxidos. Buscando uma compreensão melhor quanto às composições químicas, foram feitas análises em diferentes amostras de gemas através da técnica de fluorescência de raios X por dispersão em energia utilizando dois espectrômetros de raio X, o mini-XRF da Amptek e o ARTAX 200 da Bruker. Nas amostras foram detectados os picos característicos dos principais elementos como o Silício, Nióbio, Ferro e Cromo, além de impurezas, que em muitas pedras são as responsáveis pela denominação das cores.

Inicialmente tida como arte exótica, a tatuagem, adquiriu conotação artística e foi inserida em novos contextos sociais. No entanto, a preocupação com o bem-estar, assume relevantes preocupações na hora de tomar decisões que envolvam algum risco à saúde. De acordo com a Resolução da Diretoria Colegiada – RDC 55/2008 ANVISA, a qual regulariza o uso de pigmentação permanente para pele, há no Brasil apenas quatro marcas autorizadas para a prática da tatuagem. Este trabalho teve como proposta a caracterização elementar de pigmentos utilizados para fazer tatuagem, com a finalidade de identificar os metais presentes na composição das tintas e avaliar os possíveis riscos que estes materiais, quando inseridos no organismo, podem acarretar. A análise foi realizada pela técnica de fluorescência de raios X por energia dispersiva (EDXRF). O sistema de EDXRF é composto por um tubo de raios X com alvo de Mo, colimador de 0,65mm e um detector XFlash (SDD), o ARTAX 200 (BRUKER). Foram analisadas amostras de tintas, as quais foram desidratadas e prensadas, transformadas em pastilhas à fim de evitar o aumento do background nos espectros gerados pelo software, uma vez que amostras liquidas possuem essa característica, que dificulta leitura dos gráficos. Os parâmetros de exposição foram de 30kV e 102μA durante o tempo de 300s para cada amostra. O resultado dos espectros de emissão, apresentou os seguintes elementos Cl, Ti, Cr, Fe, Cu, Zr, Ni e Nb como componentes dos pigmentos. A reação de alguns destes metais com a derme, de acordo com referências, podem causar alergias e dermatites de menor ou maior grau na região tatuada, o que constitui um problema a longo prazo.

A Floresta Amazônica é rica em sua biodiversidade, por isso, existe a necessidade de realizar mais estudos científicos para aumentar o conhecimento sobre sua heterogeneidade. A ecologia de muitas espécies arbóreas, principalmente no que se refere à composição química inorgânica, é ainda desconhecida. Esse é o caso da família Burseraceae, composta de 18 gêneros e aproximadamente 700 espécies. Sendo o Protium Burm.f. o principal gênero da família. Uma característica marcante em deste gênero é a presença de espécies que exsudam resina aromática no tronco. Essas resinas, conhecidas popularmente por “breu”, têm usos documentados como repelente de insetos, acendedor de fogo, calafeto de canoas e no tratamento de diferentes problemas físicos. Este trabalho tem como objetivo diferenciar a composição química inorgânica do breu, coletado da espécie Protium strumosum Daly, a partir de dois métodos de extração diferentes, natural e com a aplicação do ethephon (5%), mostrando o quanto qualitativamente e quantitativamente a resina excretada difere uma da outra. Foram coletadas 15 amostras de breu, que foram posteriormente analisadas pelo método de Fluorescência de Raios-X por dispersão de onda (FRXDO). Após análise qualitativa das amostras, foram encontrados elementos como Potássio, Cloro, Sódio, Silício, Enxofre, Cálcio, Magnésio, Fósforo, Ferro, Prata, Iodo, Cádmio, Bromo, Ítrio, Molibdênio, Nióbio, Zircônio, Estanho, Manganês e Rubídio. Já nos estudos qualitativos, observa-se a diferença de composição nas amostras extraídas com e sem o estimulante. Com as análises quantitativas, esta observação ganha respaldo numérico e tem-se a confirmação de que a composição da resina exudada naturalmente é diferente da estimulada artificialmente.

A utilização de resíduos de EVA na construção civil vem sendo intensificada na última década. É notório o grande potencial que estes resíduos possuem para emprego como agregados leves, em substituição aos agregados naturais, e na elaboração de compósitos cimentícios alternativos. Neste trabalho são analisados os elementos químicos presentes na composição dos pigmentos em amostras de EVA da empresa Start Impermeabilizantes a partir de uma análise da espectroscopia por fluorescência de Raios X utilizando um micro espectrômetro da AMPTEK em diversas amostras com cores distintas. A avaliação dos elementos presentes no EVA busca viabilizar a utilização dos resíduos deste material como agregado na produção de concreto permeável, que permite que a água das chuvas passe através dele e seja armazenada nas camadas inferiores, base e sub-base. Os resultados foram obtidos para amostras com sete cores diferentes, de modo a aferir os elementos presentes em diferentes tipos de pigmentos. A partir da análise foram encontrados como elementos principais o cálcio (Ca), titânio (Ti), zinco (Zn) e ferro (Fe). Segundo a literatura a presença de tais elementos pode ser atribuída a substâncias largamente utilizadas na indústria de pigmentos como o carbonato de cálcio, dióxido de titânio, óxido de zinco e óxido de ferro II. Por fim, a partir dos resultados obtidos é possível estudar a utilização dos refugos de EVA como agregado através da interação do EVA com o cimento na produção de concreto permeável bem como a avaliação ambiental de modo que, durante a passagem de água, substâncias poluentes não sejam carreadas para o lençol freático, causando o fenômeno conhecido como lixiviação.

Neste trabalho 68 contas de vidro encontradas no sítio arqueológico do Cais do Valongo na zona portuário do Rio de Janeiro foram analisadas usando a técnica de fluorescência de raios de raios X (XRF). Para análise por XRF as contas foram separadas seguindo as suas formas e coloração: nove de cor branca e cilíndricas, quinze de cor vermelha e cilíndricas e quarenta e quatro de cor azul e facetadas. Para a análise das contas foi utilizado um sistema comercial de XRF (ARTAX 200 - Bruker) composto por um tubo de raios X com anodo de Molibdênio e um detector XFlash. As condições operacionais de análise foram: 35 kV, 500 µA e tempo de exposição de 600 s. Foi possível detectar 16 elementos: Si, K, Ca, Ti, Mn, Fe, Co, Ni, Cu, Zn, As, Rb, Sr, Sb, Pb e Bi. Na análise dos resultados utilizou-se a correlação de Pearson, a fim de se observar como as variáveis se comportavam entre si, e a análise de componentes principais (PCA) a fim de investigar possíveis semelhanças ou diferenças entre as contas de acordo com cada conjunto de cores. Associado ao PCA também foi realizada a análise por agrupamento hierárquico (HCA). Os resultados mostraram que o grupo de contas brancas se separou em dois grandes grupos e em duas contas que se separam entre si e dos grupos; uma devido a contribuição maior de Ca e a outra devido as contribuições de Cu e Zn. Apenas nas contas brancas foi detectado o elemento Sb que é normalmente utilizado na formação dos vidros brancos opacos No caso das contas vermelhas, observou-se a separação das contas em três grupos e uma conta que se separou dos grupos (grandes concentrações de Cu e Pb). As contas azuis apresentaram a formação de três grupos e uma conta que se separou bastante das outras contas azuis devido a grande concentração de Pb. Assim, com o uso da técnica de fluorescência de raios X e análises por PCA e HCA foi possível caracterizar as diferenças entre as contas de forma eficaz sem qualquer tipo de alteração física e preservando integralmente o material estudado.

This project intends to develop a remote control to micro X-ray fluorescence (µXRF) system. X-ray microfluorescence represents a relatively specialized form of XRF analysis, it is becoming increasingly adopted in specialized applications because of its unique analytical capabilities and the complementary nature of results in comparison with other microprobe techniques. The system utilized was developed by Laboratório de Instrumentação Eletrônica e Técnicas Analíticas (LIETA) group and named Sistema Integrado de Controle (SIC). The system consists in three main integrated modules: X-ray tube, digital pulse processor and high accurate table. A microcomputer connect all the modules and process the data acquisition. This equipment has a graphic user interface by means of a website. The website control enables the final user to perform µXRF measurment by any device with web browser available. With simple steps, the automated system initiates all computacional commands of the routine and generate photon counts per channel data files. All the generated data is processed at PyMca analysis software.

Cerium oxide (CeO2) nanoparticle (NP) has unique physical and chemical properties. These particular features enable the CeO2 NP to a wide variety of recent application, such as UV absorption, catalysis, solid oxide fuel cells use, and so forth. However, the environmental risks of CeO2 NP have not been extensively studied so far and it has been a matter of currently concern worldwide. In this context, this study aims at the CeO2 NP (20 nm particle size) mobility as well as its conceivable transformation in Typic Hapludox and Rhodic Hapludox soils. For the soil CeO2 NP mobility evaluation, an acrylic column filled with the abovementioned soils top covered with 350 mg CeO2 NP was employed as shown in Figure 1. Breakthrough assays using a volume of synthetic rain water equivalent to average precipitation from Jan-Mar were carried out. The translocation of Br- and CeO2 were investigated for both soils. Benchtop energy dispersive X-ray fluorescence (EDXRF) was used to detect the presence of Br and Ce in the eluate. Br- was highly mobile whereas CeO2 did not leach. Further EDXRF analysis showed that CeO2 remained adsorbed at the first two centimetres of the soil column. Another matter of concern regards possible chemical transformations undergone by CeO2 NP in the soil. To assess CeO2 NP reactivity the NP was incubated in Typic Hapludox and Rhodic Hapludox soils aqueous suspensions for two weeks under stirring. Then, Ce-L3 X-ray absorption spectra were recorded at the XAFAS2 beamline at the Brazilian Synchrotron Light Source (LNLS). Figure 2 shows the near edged fine structure spectra for the NP incubated in Typic Hapludox and the pristine one. The preliminary results indicate that only slight changes have been observed. The whiteline increasing might be related to changes at the electronic structure of the incubated NP. Seemingly, the density of empty states increases, which could be promoted by oxygen vacancies. Anyway, for this short period, i.e. two weeks, under mild environmental conditions we have not find any dramatic changes on CeO2 chemical environment.

In recent decades, it has been a large increase in the use of electronic devices as well as their batteries consumption. However, the improper disposal of these materials can cause soil and groundwater contamination by potentially toxic metals. In this context, the present study aims to evaluate the total elemental content and their leaching from soil exposed to Zn-C and alkaline batteries and electronic components from printed circuit boards. Test soil columns 40 cm in length containing the above mentioned materials were prepared. The soil columns were exposed to artificial rain and the leachate were collected. The leachate samples were analyzed by the synchrotron radiation total reflection X-Ray fluorescence spectrometry (SRTXRF) at the Brazilian Synchrotron Light Laboratory D09-XRF beam line. The Cr, Mn, Fe, Cu, Zn and Pb content in the leachate were lower than the set maximum values CONAMA 369/2008 resolution. The SRTXRF K, Ca, Ti, Cr, Mn, Fe, Cu, Zn and Pb detection limits ranged from 0.22 μg L^(-1) to 4.32 μg L^(-1). The results showed a higher leaching of K, Mn, Zn and Pb in the columns containing batteries. For soil analysis, Al, Si, K, Ca, Ti, Cr, Mn, Fe, Cu, Zn, Zr and Pb were evaluated using a benchtop energy dispersive X-Ray fluorescence spectrometer (EDXRF) and the detection limits ranged from 5390 to 16 mg kg^(-1). For soil columns batteries containing, higher K, Mn and Zn levels were found in the surface soil layer compared to the control. For soil columns printed circuit boards containing, an increase of Ti, Mn and Pb were evident. In addition, the metal concentration variation in soil was evident only in surface soil, up to 10 cm. From 10 to 40 cm the difference soil was minimal compared to the blank. SRTXRF and EDXRF were showed promising techniques for evaluation of metals in the leachate and soil, respectively.

Nowadays men and women spend a lot of time, resources and efforts to the cultivation of personal hygiene and the best possible look, as a result, the cosmetics industry plays an important role in the economy of most developed countries. The raw materials used in cosmetics are classified as active principles or excipients. Excipient is all inert ingredient added to a formulation to give consistency, in order that the product can be applied, handled and packaged appropriately. The active ingredients are substances that effectively work and promote changes on the body regions in which the cosmetics are applied, e.g., skin, eyelids, nails, etc., thus their amounts need to be controlled due to the application acceptable limits, its toxicity, the consequences of excessive doses, possible side effects, and the possibility of sensitization and allergic reactions. The concentration and quality of the raw material used in the manufacture of a cosmetics product can be verified by analytical methods, among them the X-ray fluorescence, since X-ray fluorescence technique is suitable for performing multi-elemental analysis with low cost and fast results. This study, developed in Applied Nuclear Physics Laboratory (LFNA) of the Londrina State University (UEL), had as objective inorganic elements determination in cosmetic samples, as well as its matrix characterization. It was used a portable energy dispersive X-ray fluorescence (EDXRF) system associated with principal components analysis (PCA). For the measurements was used a home-made portable system which consists of a X-ray tube with Ag target and filter (MAGNUM MUHV50, Moxtek); a high voltage source (FTC-200, Moxtek) for control of the voltage and electric current applied to the X-ray tube; the X-123 complete X-ray spectrometer with Si-PIN detector (Amptek) with FWHM@5.9 keV: 153 eV; and a laptop for acquisition, storage and data treatment. A total of 40 eye shadows samples from 4 manufacturers and suppliers in the Brazilian market representing different colors and shades were analyzed. It was possible to identify and quantify the elements Cl, K, Ca, Ti, Cr, Fe, Cu, Zn and Bi. In order to verify tendencies in the classification of the samples, the set of X-ray spectra was evaluated by principal components analysis. The whole X-ray spectrum was considered in the analysis and it was possible to verify a separation of the samples in groups in accordance with manufacturer. From the multi-elemental data obtained by X-ray fluorescence and the information revealed by the principal component analysis it was possible to identify the differences in the composition of each set of samples. Based on these results it can be seen that the combination of X-ray fluorescence technique with the principal component analysis presents a valuable tool for the classification and characterization of cosmetics samples.

A técnica de fluorescência de raios X por dispersão em energia (EDXRF) é amplamente empregada em análises de obras de artes e em objetos de patrimônio histórico por ser uma técnica não invasiva, capaz de fornecer informações sobre a composição química e a concentração dos elementos. Muitos objetos de valor arqueológico são compostos por uma estrutura de duas ou mais camadas de diferentes materiais, sendo uma de substrato e uma ou mais camadas de revestimento. A técnica de EDXRF tem sido avaliada como uma possível ferramenta para determinar a espessura de duas e/ou várias camadas de materiais, podendo auxiliar na conservação e restauração de objetos do patrimônio cultural [1]. O objetivo desse trabalho consiste na avaliação da metodologia de medida de espessura de camadas depositadas sobre uma base usando a razão entre as linhas de fluorescência de raios X (Kα/Kβ ou Lα/Lβ) emitidas por elementos da base. As análises das espessuras foram realizadas em folhas de alumínio de diferentes espessuras (12 μm, 36 μm e 60 μm) depositadas em dois materiais de base: cobre e chumbo. O sistema de XRF utilizado para as medidas de espessura é formado por um mini tubo de raios X de baixa potência com anodo de Ag e um detector SiPIN. Variando a posição do tubo de raios X e do detector foram avaliadas três configurações do sistema de XRF para o cálculo da espessura: tubo de raios X perpendicular a amostra, detector perpendicular a amostra e , por fim, tubo de raios X e detector simétricos a amostra. Em cada geometria variou-se o ângulo entre o feixe incidente e detector. Foi possível determinar as três espessuras das folhas de alumínio nas três geometrias analisadas, tanta na base de cobre quanto na base de chumbo. As medidas de espessura obtidas com a segunda geometria (detector perpendicular a amostra) foram as que apresentaram menores exatidões quando comparadas com o valor esperado das espessuras das folhas de alumínio. Os resultados mostraram que a primeira e a terceira geometrias foram mais eficientes para o cálculo da espessura de camadas. Além disso, os resultados demonstraram que quanto menor o ângulo entre o detector e a amostra mais preciso se torna o cálculo da espessura.

The materials analysis by Energy Dispersive X-ray Fluorescence (EDXRF) depends on the elementary composition and the layer thickness studied. Samples with many layers are common in historical artifacts, with pigments overlapping paintings or metal layers of recoating. In this work, the layer’s thickness measurement method using the intensity of Ka/Kb or La/Lb characteristic X-ray peaks was studied. Using few samples extracted from the baroque sculpture in polychrome wood from Saint João Evangelista, from XVIII century, it was measured the gold layer thickness that overlies gold details of the image. The sculpture was carved to the Jesuits Church's altar built at Castelo's Hill in 1567. After the Hill’s overthrow, in 1922, the artworks were been saved at Saint Inácio School's hall (Rio de Janeiro, Brazil). For the X-ray peaks intensity analysis, was used 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 from the technique using the X-ray peaks were compared to the results obtained using the high resolution optical microscope automated, model Axio Imager M2m from Carl Zeiss. The founded results prove the technique efficiency, it is important when are only available sample’s fragments that do not allow using optical microscope

A radiação espalhada tende a ser uma fonte de problemas em técnicas radiológicas, tanto a para a qualidade da imagem quanto para a radioproteção. Ela pode aumentar o ruído da radiografia, prejudicando a uniformidade e o contraste da imagem, mas também pode aumentar a exposição do operador, pois torna a amostra uma fonte secundária de radiação ionizante. A consciência da existência e do comportamento da radiação espalhada é um importante fator para práticas de proteção radiológica, mas também para a otimização dos parâmetros da técnica, otimizando a imagem. Imagens computacionais representativas deste tipo de radiação são excelentes materiais para a demonstração destes. O processo de interação da radiação ionizante com a matéria, que gera radiação espalhada tem algumas similaridades com o processo de luz visível, mas não acontece apenas na superfície de um determinado corpo. O objetivo deste trabalho é criar um simulador de baixo custo computacional para cálculo e demonstração gráfica do comportamento da radiação espalhada, em função de diversos fatores como energia e intensidade do feixe, material e meio radiografado, assim como os efeitos da mesma na imagem gerada. O simulador será construído na linguagem C e na plataforma de cálculo numérico OCTAVE. Todo o processo será executado dentro do ambiente virtual que fará parte do simulador. Mantendo a possibilidade de mudança e criações de condições diferenciadas e mantendo interatividade com o usuário final. O principal produto do simulador serão imagens do ambiente virtual da radiografia, assim como das radiografias geradas. Estas imagens terão predominantemente viés educativo, mas com capacidade para simular testes reais.

Occupational exposures are important parameters that need to be investigated to evaluate the radiological effects. On this work we used Geant4, version 9.6.p03 and low energy model Livermore, to define the energy correction factor (ECF) to be used on correction of thermoluminescent dosimeters (TLDs) measurements. The simulated TLDs were positioned over Bomb phantoms, representing occupational workers involved in fluoroscopic paediatric procedures. We calculated the ECF to X-ray scattered spectra by different paediatric phantoms (newborn, 1 year old, 5 years old and 10 years old), representing patients of different size undergoing fluoroscopic barium meal procedure at 60 kVp and 75 kVp. The TLDs were fixed over three regions of the occupational workers simulated: eyes (left and right), thyroid (over and under the collar of protection) and hands (left and right). The primary spectrum and scattered spectrum, that interact to each TLD, were recorded and used to calculate the ECF. We used a systematic analyses to observe de significance on influences and tendencies observed. As results we found that: (i) the scattered dimensions (paediatric phantoms simulated) does influence on ECF, in a way that an increase on scatterer size tends to increase the ECF to a fixed position of the TLD; (ii) the incident spectra energy (ripple and peak tension) can change the ECF significantly.

The study in avian neurology has been largely enrichened by the use of CT scans. This methodology presents obvious advantages. Materials usually do not need treatment before entering the scanner, no deterioration occurs during the scan, and the results allow the reconstruction of high-quality 3D models, which represent an essential step in order to perform more complex anatomical and biomechanical studies. The datasets obtained by the scans are longlasting and easily portable, facilitating the comparison and study of the 3D models obtained, which are easily manipulated, sectioned and redescribed. More importantly, this methodology provides data on extant taxa characterized as ‘very rare’ or endangered, andsvn add extinct birds rare in the fossil record. In order to explore brain anatomy in several bird species, X-raysvn add micro-CT data were obtained using an experiemntal micro-CT scanner available at Facultad desvn add Matemática, Astronomía y Física (FaMAF). This equipment allows to obtain 2D and 3D images up to 20svn add cm x 20 cm with resolutions of 194 microns. It is also possible to maximize the quality of the images fromsvn add the control of main parameters involved in the image acquisition: conformation of the X-ray beam (spatialsvn add and spectral distribution), counting statistics, number of projections, relative position of the sample andsvn add detector. Different reconstruction algorithms and filtering algorithms were implemented in order to obtainsvn add highest quality 3D models. This is actually possible thanks to the interdisciplinary work of professionalssvn add from different areas of knowledge.

The novel Cr1-xTixSe compounds have been synthesized for x = 0, 0.05, 0.10 and 0.15. Although both CrSe and TiSe are individually reported as NiAs-type phases, solid solutions in this system have not been previously synthesized. Structural characterization was made using X-Ray Powder Diffraction (XRD) data. All samples belong to the P63/mmc space group and share the nickel arsenide (NiAs) structure type. Chromium and titanium are known to have different oxidation states in selenide compounds, both varying between +2 and +4 oxidation states. In the case of study stoichiometry suggests a +2 oxidation state for the metals. However, the NiAs structure presents a very short cation-cation distance that can lead to some degree of bonding, affecting oxidation states. X-ray Emission Spectroscopy (XES) measurements were carried out in order to study the oxidation state of chromium in these new compounds. A high-resolution Kβ spectrum of a common chromium selenide is shown in Figure 1. By calculating the difference between the Kβ5and Kβ1,3 peak positions (DE) and comparing with appropriate standards, oxidation states can be inferred for each sample. All three substituted samples contain chromium in an average +2 oxidation state within experimental error. Additional sample characterization included resistivity measurements, which will also be discussed and complemented by the conclusions of the structural characterization as a whole.

Para este estudio seleccionamos muestras de cerámicas y adobes del yacimiento de Cerro Cepero localizado en la comarca de Baza, Andalucía (España). Cronológicamente su fase de ocupación abarca desde la época del Bronce Final hasta el siglo VII d.C. Esa región tuvo diversas excavaciones irregulares desde hace muchos años, por diferentes equipos de arqueólogos. Y actualmente el yacimiento es objeto de estudio del Centro de Estudios de Arqueología Bastetana. En este yacimiento fue posible recuperar materiales cerámicos de gran relevancia y estudiar adobes de estructuras ibéricas, siendo la principal de ellas la muralla que aflora en la zona norte. La caracterización de las muestras fue hecha mediante el empleo de Difracción de Rayos X y Fluorescencia de Rayos X, teniendo otras técnicas complementarias como el estudio de Análisis de Imágenes, Análisis Petrográfica y Colorimetria. La Difracción de Rayos X fue utilizada para definir las fases mineralógicas que componen los adobes y las cerámicas, además de estimar su posible temperatura de cocción. El estudio de la composición química fue hecho mediante la Fluorescencia de Rayos X, donde se han discriminado los elementos mayoritarios y los trazas. Los datos obtenidos fueron tratados por el método de Análisis de Componentes Principales (PCA) con el fin de comparar las variables químicas.

O ferro é um importante elemento no transporte respiratório do oxigênio e dióxido de carbono e nas enzimas envolvidas no transporte celular. A anemia ferropriva é um problema de saúde pública no mundo que afeta cerca de dois bilhões de pessoas, especialmente nos países em desenvolvimento. No Brasil os programas de prevenção e tratamento da anemia fazem a reposição do ferro utilizando de forma padronizada o sulfato ferroso devido ao seu baixo custo aliado à sua alta biodisponibilidade. Neste estudo foram preparadas amostras com quantidades conhecidas de F2SO4 em base de celulose e construir uma curva apropriada para identificação rápida de conteúdo deste material em medicamentos adquiridos no comércio. Foram produzidas amostras e com duas granulometrias e com quantidades de F2SO4 entre 80 e 375mg por grama de celulose, de modo a observar a influência da granulometria no resultado. As amostras produzidas foram medidas num sistema de XRF da Amptek com tubo de raios X com anodo de Au (com tensão de 20keV e corrente de 20µA)e espectrômetro 123 (SDD). Os resultados mostraram que para quantidades até 300mg/g a resposta é linear e essa técnica pode ser utilizado neste tipo de amostra. Novas medidas estão sendo feitas com base de lactose, pois são estas as bases mais utilizadas em medicamentos comerciais.

O estudo dos ossos e de suas características histomorfométricas é fundamental para a correta classificação de várias espécias de animais. Estas medidas, em sua maioria, são feitas através da separação dos tecidos ósseos dos demais tecidos biológicos da amostra e posterior medição. É muito comum o uso de técnicas como a diafanização e a maceração no estudo de vertebrados. Estes processos, apesar de amplamente utilizados, são processos destrutivos que em muitos casos não pode ser aplicado devido ao tamanho reduzido dos ossos de alguns exemplares. Para contornar estas limitações o uso de técnicas de diagnósticos por imagens não destrutivas tem sido amplamente utilizado para a obtenção das informações volumétricas internas e externas dos ossos. Neste trabalho utilizamos a microtomografia computadorizada para aquisição destas informações. Agregando a este cenário uma crescente oferta de tecnologias para prototipagem rápidas a custos cada vez mais reduzidos, torna possível com auxílio de software de CAD a construção de modelos biológicos que permitem a reprodução de inúmeras réplicas da estrutura óssea. Estes modelos podem ser reproduzidos em diferentes dimensões, posições e materiais, tanto na parte externa ou interna do osso. No entanto, este é um processo complexo que exige a manipulação das imagens por diversos programas específicos até a obtenção do modelo tridimensional a ser prototipado. Os resultados obtidos em ossos de codornas (Coturnix Coturnix) e em pequenos sapos da espécie Proceratophrys bigibbosa, mostraram o grande potencial de aplicação desta ferramenta computacional na construção de biomodelos para estudos biológicos e didáticos de pequenos animais.

O teor de biodiesel no diesel, em volume, aumentará dos atuais 7 % até 10 % em 2019, podendo chegar a 15 % se os testes e os ensaios com motores validarem essa adição. O Programa de Monitoramento da Qualidade dos Combustíveis da ANP referencia as normas ASTM D5453, ASTM D2622, ASTM D4294, ASTM D7039 e ABNT NBR 14533 para a determinação de enxofre em diesel comercializado no Brasil que, à exceção da primeira, baseiam-se na espectrometria de fluorescência de raios X, cuja acurácia depende da correta correção do efeito matriz. Tendo isso em mente, foram estudados o efeito matriz devido à presença de biodiesel, ou seja, de oxigênio, na intensidade de emissão da radiação S-Kα de amostras de diesel contendo traços de enxofre e algoritmos de correção do efeito matriz por meio de coeficientes de influência empíricos e teóricos. A avaliação da estatística erro relativo mostrou que o algoritmo de De Jongh considerando o oxigênio foi o que melhor corrigiu o efeito do oxigênio na quantificação de enxofre em misturas de diesel S5 e S10, ambos contendo até 10 % de biodiesel em volume.

El análisis y control en tiempo real de un yacimiento sea en un pozo exploratorio o un pozo de producción nos permite reducir el tiempo de respuesta durante las decisiones operacionales de perforación o recobro y obtener una correlación más acertada de la litoestratigrafía del yacimiento. Ante la necesidad de optimizar los procesos de exploración y producción en la industria petrolera, los analizadores portables prometen ser una tecnología de fácil operación en las campañas onsite particulares de esta industria. Esta metodología propuso el uso del análisis por DRX de montajes desorientados tanto a nivel de la roca total como a nivel de la fracción menor de 2 µm mediante el uso de un difractómetro de rayos-x portable marca Olympus modelo Terra-441 bajo condiciones de ensayo de 30 kV de energía y 350 µA de intensidad. La validación de esta metodología se desarrolló con mezclas de referencia y rocas del subsuelo colombiano de yacimientos convencionales y no convencionales.

Métodos de análise multivariada tais como, PLS tem sido amplamente utilizado em conjunto com outras técnicas analíticas para estudos de objetos arqueológicos e do patrimônio cultural. O procedimento de PLS utilizando compreende duas etapas: a validação e calibração. A etapa de calibração é utilizada para o estabelecimento de uma relação entre a matriz de dados X (sinais instrumentais, variáveis independentes) e as propriedades amostras usando amostras de referência (variáveis dependentes) organizadas na matriz Y. A etapa de validação permite a verificação se o modelo é capaz de prever as propriedades das novas amostras. Foi estudado uma moldura dourada da peça intitulada Mulher Enxugando o Braço Esquerdo (Após o Banho) realizada em 1884, de autoria do pintor Degas, Hilaire-Germain Edgar de Gas com dimensões de 58 x 64 cm. Seis pontos foram analisados por PXRF durante 300 segundos. Para obter os padrões (variáveis dependentes) utilizados no modelo PLS folhas de ouro com espessuras conhecidas foram utilizadas correspondendo aos valores 0,094, 0,188, 0,564, 1,128, 2,068 µm, respectivamente. Para a regressão PLS, os dados dos espectros de calibração foram arranjados em uma matriz 5x1024 (X) e uma matriz de 5x1 (Y) com os valores de espessuras. Os dados de validação foram arranjados em uma matriz 6x1024 (X) com os espectros a partir da moldura. Foi usado um filtro de média como um passo de pré-processamento dos dados, e todos os espectros foram normalizados para o mesmo tempo de medição. A metodologia proposta com base em uma abordagem PLS foi capaz de prever as espessuras de Au numa moldura de madeira dourada de uma pintura. A diferença relativa entre os dois métodos permaneceu entre 6 até 16%, e os valores de espessura podem ser consideradas equivalentes, dentro das barras de erro.

Intended primarily for decoration, currently thin films are used as the basis of high technology. Among the physical quantities that characterize it, thickness strongly influences other properties of the film. Thickness measurements are performed using sophisticated and high cost equipment, which often need a proper treatment of the sample to accomplish the desired measurement. Thus, the methodology of X-Ray Fluorescence with portable equipment (PXRF) shows a highly suitable tool to determine these thicknesses. Thus, it was proposed and developed a procedure for the determination of film thickness by PXRF employing K lines attenuation. The thin films were deposited by thermal evaporation from the pellets with 100 mg, 70 mg and 35 mg of V2O5 powder (Sigma-Aldrich, 99.9%). Knowing that Calcium (Ca) is one of the constituents of the glass substrate, it is used the differential attenuation of the K lines of this element after traversing the layer of V2O5. It was employed a Portable X-ray Fluorescence system (PXRF) composed of a Si-Pin detector with a 6 mm2 crystal and 500 μm thickness, a 12.5 μm thickness Beryllium window and a silver anode X-ray tube with silver collimator and filter. Thickness obtained by PXRF was compared with the measurements obtained by scanning electron microscopy. Through the PXRF technique values of 54, 98 and 167 nm for film thicknesses of 35, 70 and 100 mg were obtained. These values are in good agreement with measures by electron microscopy, 50 ± 7, 110 ± 3 and 160 ± 5 nm, respectively. It is observed that the values of the calculated thicknesses are slightly larger than the values measured by the scanning micrographs, due to the fact that a small residual deposits in the boat evaporation. Thus, the PXRF methodology is a highly suitable tool to determine the thickness of nanometric thin.

La técnica de fluorescencia de rayos X (XRF) permite la identificación y cuantificación de elementos en muestras de diversa naturaleza. En particular su aplicación en tejidos biológicos es ventajosa porque no exige una preparación de muestras compleja en comparación con técnicas instrumentales alternativas. Los estudios por XRF permiten realizar un seguimiento de las concentraciones de elementos metálicos contribuyendo de esta manera al entendimiento de diversos procesos fisiológicos de los organismos vivos donde los metales son partícipes esenciales. Sin embargo, las concentraciones de metales en tejidos biológicos se encuentran en niveles traza por lo que su análisis requiere una cuidadosa optimización de la sensitividad del espectrómetro y del proceso de preparación de muestras. En este trabajo se desarrolló un dispositivo compacto que permita modificar el haz de excitación en energía y tamaño, para esto fue utilizado un cristal de silicio (100) y colimadores de láminas paralelas de vidrio tanto en el canal de excitación como en el canal de detección tanto antes como después del cristal. El dispositivo se acopló a un tubo de rayos X de difracción Philips modelo PW2275/20 con ánodo de molibdeno de modo de seleccionar la línea Kα de emisión característica. El haz de rayos x de excitación resultante es altamente monocromatizado (E= 0,8 keV), intenso y con sección transversal de 1mm×3,5mm, permitiendo registrar espectros por XRF con muy baja señal de fondo y alta tasa de conteo, lo cual incrementa considerablemente la sensitividad del espectrómetro. Para alcanzar límites de detección en el orden de las partes por millón, las muestras de tejidos biológicos deben además ser liofilizadas. En el presente trabajo se muestran los resultados de la caracterización del espectrómetro desarrollado (límites de detección, propiedades del haz de excitación) y algunas aplicaciones sobre tejidos biológicos (especialmente tumores malignos de mama).

Se preparó una solución (a temperatura ambiente) de 0,1 mL de trietilamina en 10 mL de tolueno. Posteriormente, se preparó otra solución de 4 mL de DMF con una mezcla de 0,2 g del nitrato de zinc hexahidratado [Zn(NO3)2.6H2O] y 0,08 g del ácido tereftálico diluido en 16 mL de tolueno. Las soluciones anteriores se mezclaron con agitación constante durante 16 horas. Finalmente se filtró al vacío, se secó el producto, obteniendo un sólido blanco con punto de fusión de 211°C. El rendimiento de la reacción fue de 51%. El compuesto fue caracterizado molecularmente por diversas técnicas analíticas y cristalográficamente por difracción de rayos-X obteniendo que cristaliza en el sistema monoclínico con constantes de celda: a = 23.689 (7) Å, b = 5.007 (5) Å, c = 23.349 (9) Å, ß = 115.93° (3) y V = 2491.21 Å3.

A espécie Plagioscion squamosissimus, pertence à família Scianidae, conhecida popularmente como corvina ou pescada branca, sendo originária da bacia amazônica e amplamente comercializada nas regiões norte e nordeste do Brasil. Alimenta-se de peixes menores e camarões. Como peixe ósseo possui três pares de corpos inorgânicos chamados otólitos, cada par tendo um nome especifico. São eles: sagittae, lapillus e asteriscus, sendo o sagittae, em várias espécies, mais notório em dimensão e objeto de vários estudos. Otólitos são concreções calcárias em volta de uma matriz protéica, presentes no ouvido dos peixes ósseos (atrás dos olhos), com funções específicas de equilíbrio, sentido de direção e receptor de vibrações sonoras. Nele está contida informações da idade, crescimento, local de nascimento, padrões migratórios, determinação de eventos importantes no ciclo de vida do peixe. Com a determinação química inorgânica do otólito é possível saber como o peixe está interagindo com o meio, uma vez que biomineraliza os minerais que consome por meio de sua alimentação. Os otólitos utilizados para análise foram retirados de exemplares coletados na região pesqueira de Manacapuru, interior do Amazonas, Baixo Solimões, os mesmos triturados e aglutinados em pastilhas de ácido bórico para análise qualitativa e quantitativa no equipamento de fluorescência de raios-x por dispersão de ondas. Os elementos encontrados nas amostras foram Ca, Na, Al, Si, P, S, Cl, K, Fe, Sr, Ag, Rb e Mo, sendo o cálcio presente em maior quantidade, uma vez que os otólitos são concreções calcárias sob a forma mineral de aragonita.

During the last 20 years the archaeological research in the Oriental Pyrenees, especially in the Cerdanya region (Girona, NE Spain), has evidenced the presence of an important Iron Age population, the Cerretani, mentioned in the ancient literary sources. They occupied the central valleys of the eastern Pyrenees, from the planes (up to 1100 m. asl) to the main hills and the pasture lands (up to 2.000 m. asl). This cerretani were settled in several oppida, the typical Iron age hill forts, of modest dimensions (0,6 Ha.), placed along the course of the Segre river. The main site discovered, the Castellot oppidum (Bolvir), has been excavated in the last ten years, showing the presence of a limited population (about 200-250 people) since the beginning of the 4th c. B.C. The excavations have shown the presence of an Iberian community but with some specificities, like the importance of the livestock strategies or the low presence of imported materials. The recent discovery of several objects in archaeological context in the Oriental Pyrenees (la Cerdanya region, Catalonia) has aroused the question of the Roman presence in this mountain area, and the development of some metallurgical activities in this previously considered marginal zone. . About the middle half of 2nd c. B.C. these cerretani oppida were remodelled, as we have documented: the setting up of a new urbanism, the opening of a fortified gate, and specially the uses of new metallurgical technologies, show the potential impact of the Roman presence, probably in a military context. Coming from different sites, we have collected some metallurgical objects (earring, rings and coins) that use gold and silver in an elaborated technology, and pointed out the question of the use of gold in pre-Roman and Roman times in this Pyrenean area. The use of gold and silver in some objects has to be also connected with the recent identification of a metallurgical workshop in the Castellot site, dating from the 2nd half of 2nd c. B.C. It seems the technology of the Gold earring from the Castellot site, and specially the gilded ring from Baltarga, had to be connected directly with the Roman military presence in the region from the middle 2nd c. B.C. The iron and silver ring found in the archaeological sites evidence also the use of a complex metallurgical technology, characterized by X-ray techniques, by the local communities' long time before the Roman presence, and likely the knowledge and exploitation of silver and gold resources.

Antoni Gaudí was an architect from Catalonia, Spain, who belonged to the Modernist (Art Nouveau) movement and was famous for his unique style and highly individualistic designs. Gaudi is the author of many of the most famous and representative buildings of Barcelona architectural landscape, such as the Sagrada Familia basilique, the Park Guell, Guell Palace, Casa Milá and Casa Batlló. Gaudí studied at the High School of Architecture in Barcelona from 1873 to 1877, obtaining the title of architect in 1878. The newly named architect immediately began to plan and design innovative buildings, and collaborated with the School his entire life. The Modernist movement was prodigious in its use of ceramics not only in Catalonia, but also in other places throughout the Iberian Peninsula or in many other European countries. Ceramics are certainly omnipresent in Gaudí’s work; their use is perhaps one of their most distinctive characteristics. In 1879, Gaudí’s name first appeared on the books of the Pujol I Bausis ceramic factory which mention a shade of yellow called “Gaudí.” This suggests that from his very first projects, Gaudí used ceramic tile overlay as an essential component of his work. All of Gaudí’s works display a notable wealth of ceramic decoration, well represented in one of its first work: Casa Vicens, built between 1883 and 1888. It is significant because it is an outstanding work dominated by ceramic elements with widely contrasting chromaticism. Casa Vicens was named a UNESCO World Heritage Site in 2005 along with a selection of the architect's other works. Nowadays the home is being restored and it is planned to be opened as a museum next year. Casa Vicens suffered several architectural modifications around 1925 and also some restoration ending the 1990's. In each in each of these modifications some of the tiles were replaced with new identical colour but different manufacturing process. The aim of the present work is focussed on identifying the composition of the body ceramic pieces and the characterization the glazes, approaching to their production techniques and the process they were decorated. The complete characterization of the materials used in Cultural Heritage monuments is a crucial step, enabling to make decisions about restoration and preventive conservation methods. We mainly used non-invasive instrumentation, such as "in-situ" and laboratory Energy dispersive X-ray fluorescence, X-ray diffraction, SEM/EDX and optical microscopy.

In interventional procedures using fluoroscopy, the medical staff is exposed to ionizing radiation, often above the limit allowed to occupationally exposed individuals and are only seen at the end of the procedure or after a month when using individual dosimeters. The aim of this study was to develop a system to estimate the equivalent dose of ionizing radiation in real time during the interventional medical procedure using fluoroscopy. The performance of the remote-controlled fluoroscopy system of scattered radiation measurements was operated at 50 kVp and 30 mA and 9DP model ionization chamber Ludlum and phantom PMMA. Dose rates were collected by the ionization chamber for the regions of the gonads, 90 cm, the trunk 128 cm eyes, 166 cm and the distance of the main beam 19, 38, 76 and 152 cm, alternately turning 45.O and 45.O around the fluoroscopy table. The rates above 10μSv/h doses and the reproducibility of the measurements were considered. The criterion of Chauvenet was used to eliminate the discrepant results data, and were calculated the mean and standard deviation for each position. The result of this selection was used to construct isodose curves using interpolation techniques. System linearity tests were conducted by varying the voltage obtaining the correlation coefficient of 0.97 and 0.99 respectively for the interventional physician and nurse positions. For viewing in real time dose rates ionization chamber was set at the top of the fluoroscopy table as a fixed reference point. The collected data were sent to the computer to determine the dose rates estimated indirectly in relation to the predetermined isodose and positioning of the medical staff in interventional procedure. Dose rates and the estimated cumulative dose are shown in real time via a TV monitor located visibly showing the intensities of dose rates with a visual indication of color scale to the doses received by members of the medical team. Student's test was used to validate the system with p < 0.05. The exposure of ionizing radiation was reduced when the medical team changed its position or increasing distance in relation to the main beam during the interventional procedure.

Nowadays, renewable energy resources as well as more efficient energy storage systems have taken a starring role, since more sustainable energy systems are being demanded due mainly to the increasing needs of modern society together with the collateral effects of conventional energy sources. This situation has driven to a search for improved electrochemical storage systems that can safely store energy from sustainable sources, proving the energy needed, for example, for transportation and residential uses. As an example of everyday technology, the use of portable electronic devices has been feasible thanks to the lithium-ion batteries (LIB). The energy storage capacity of the LIB system is 5 times higher than lead-acid batteries, and it shows an average voltage of 3.8 V per cell in comparison with the average 2.0-2.2 V of the lead-acid batteries. In addition, lithium-ion batteries have the advantage of lower weight, higher energy density and faster charge and discharge rates compared to other similar battery technologies. Even though they are the most widely batteries employed in portable electronics, it is important to attend several issues regarding safety, and to improve its energy storage capacity in order to be used at larger scales, in, for example, electric vehicles. Lithium titanate, Li4Ti5O12 (LTO), is a promising candidate for anode material at the moment because of many its advantages. Due to this, a better knowledge regarding the LTO structure and how changes are related with its ulterior performance is of great importance. In this work, Resonant Inelastic X-ray Scattering (RIXS) has been used for studying titanium local environment changes in the LTO molecule when different levels of charge are applied. As complementary technique, XANES spectra of the Ti-K edge were also measured. The measurements were carried out at the Brazilian Synchrotron Light Source (LNLS, Campinas) in the D09B beamline and at ELETTRA Sincrotrone Trieste (Italy) in the IAEA end-station of the XRF-beamline. Several samples with different levels of charge (not charged, partially charged and fully charged) were studied. Reflection geometry was used together with monochromatic photons of 4900 eV (just beneath the K absorption edge of titanium) for the RIXS measurements and XANES spectra were acquired scanning the incident beam energy in the range 4930-5080 eV, i.e., around the Ti-K edge. For data analysis, and in order to discriminate the changes on the titanium chemical state of the LTO molecule, Principal Component Analysis (PCA) was used on both RIXS and XANES spectra. The results show that RIXS allows the detection of minor changes in the structure of the lithium-based compound due to the particular level of charge. In this way, typical chemical studies as the ones performed with conventional absorption techniques (XANES, EXAFS) can be achieved with this technique, with the advantageous characteristics of shorter measuring times and suppressing any energy scan during the analysis, between others.

El compuesto MoO2Cl2-4,7-dimetilfenantrolina se obtuvo a partir de la disolución de 238 mg de MoO2Cl2 ( 1.2 equiv) en 10 mL de diclorometano seco bajo atmósfera de nitrógeno en un schlenk al cual se le adicionaron lentamente 28mg de 4,7-dimetil-1,10-fenantrolina disueltos en 15 mL de diclorometano seco bajo atmósfera de nitrógeno. La reacción se agitó durante 4 horas a temperatura ambiente protegida de la luz. La mezcla de reacción se filtró al vacío y el sólido resultante se lavó varias veces con éter etílico para obtener un sólido gris. Posteriormente se realizó la caracterización cristalográfica por difracción de rayos-X policristalinas, encontrando que el compuesto de interés cristaliza en el sistema monoclínico con constantes de celda celda: a = 12.918 (4) Å, b = 9.768 (2) Å, c = 11.998 (4) Å, ß = 101.68° (2) y V = 14826.61 Å3

Se disolvieron 238,mg de MoO2Cl2 (1.2 equiv) en 10mL diclorometano seco bajo atmosfera de nitrógeno en un schlenk, al cual se le adicionaron lentamente 184 mg de dimetilbipiridina disueltos en 10mL diclorometano seco bajo atmosfera de nitrógeno. La reacción se agitó durante 3 horas a temperatura ambiente protegida de la luz. La mezcla de reacción se filtró al vacío y el sólido resultante (3) se lavó varias veces con éter etílico para obtener un sólido gris. La caracterización molecular se realizó por diversas técnicas instrumentales y la caracterización cristalográfica por difracción de rayos-X de muestras policirstalinas, obteniendo que el compuesto de interés cristaliza en el sistema monoclínico con constantes de celda: a = 22.343 (1) Å, b = 4.923 (3) Å, c =17.176 (1) Å, ß = 99.78° (6) y V = 1861.71 Å3.

A utilização de técnicas não destrutivas na análise de material arqueológico é recomendada a fim de garantir sua preservação. Neste estudo foi analisada uma moeda do Império Romano datada do século IV D.C. do governo de Constantine II. Sua composição química superficial foi obtida de forma qualitativa através da técnica de Fluorescência de Raios X por Energia Dispersiva (EDXRF) e a homogeneidade da liga foi avaliada por Microtomografia Computadorizada (µ-CT). A leitura por EDXRF em três pontos distintos da moeda é apresentado na Tabela 1. É possível perceber um aumento da quantidade de prata e chumbo no ponto b em relação aos outros pontos medidos. A µ-CT revelou uma variação de densidade na superfície da moeda, especialmente na região do ponto b, como pode ser observado na Figura 1. Estes resultados são compatíveis com o processo térmico/mecânico conhecido como enriquecimento superficial de prata, que promove a migração destes metais para a superfície e confere um brilho prateado à moeda.

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.

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.

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]. Posteriormente 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.

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.

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.

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.

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. The 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]. This 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. [1]“Degradation Process of Lead Chromate Yellows in Paintings by Vincent Van Gogh” Letizia Monico. PhD thesis. University of Antwerp and University of Perugia. [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. [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. Acknowledgement: 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.

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.

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.

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. [1] M. Hložek, T. Trojek, Radiat. Phys. Chem. 116 (2015) 332. [2] F. Bilo et al., Appl. Surf. Sci. 359 (2015) 215. [3] X. Li, Z. Yu, Appl. Radiat. Isot. 111 (2016) 45. [4] T. Trojek, D. Trojková, , Radiat. Phys. Chem. 116 (2015) 321. [5] R. M. Rousseau, Rigaku J. 18 (2001) 33 [6] CG Clayton, R. Spackman, Nucl Geophys 1 (1987) 25. [7] S. Steenstrup, J Appl Crystallogr 14 (1981) 226. [8] B. Vekemans et al., X‐Ray Spectrom 23 (1994) 278. [9] P. Bury et al., Nucl Instrum Methods Phys Res Sect A 383 (1996) 572. [10] L. Yi et al., Nuclear Instruments and Methods in Physics Research A 775 (2015) 12.

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.

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.

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.

Polymorphism and particle size distribution can impact the dissolution behaviour and, as a consequence, bioavailability and bioequivalence of poorly soluble drugs, such as Efavirenz (EFV). Nevertheless, these characteristics do not explain some failures occurring in in vitro assays and in in vivo studies. EFV belongs to class II of the biopharmaceutics classification system and the high activity antiretroviral therapy (HAART) is considered the best choice in the treatment of adults and children. In a previous study, Fandaruff et. al. demonstrated the biorrelevance of the microstructure (crystalline domain sizes) in EFV and the correlation between changes in dissolution properties and changes in crystallite size rather than particle size [1]. The microstructure study of these samples was done using synchrotron radiation X-ray diffraction at ELETTRA facility (Italy). The aim of this work is to expand the previous study of the effect of microstructure on different commercial raw materials and crystallized samples of EFV. A further extension of the method of crystallite size analysis to anisotropic crystallite shape and a reproducibility of the results obtained in X-ray diffraction experiments using synchrotron and conventional radiation sources are reported.

The process of proliferation and differentiation of hematopoietic cells is a complex mechanism which depends on the presence of nuclear proteins, cytoplasmic proteins and the action of various genes. These genes can be mutated so that the differentiation program is changed. Changing the program is related to the onset of leukemia which is characterized by disorder of cell proliferation or the production of abnormal cell clone. This differentiation mechanism has been widely studied in relation to normal human cells and leukemic myeloid type. Myeloid Leukemia can be subdivided according to the degree of cellular maturity. Immature forms present an acute evolution and mature forms have a chronic evolution. The Chronic Myeloid Leukemia (CML) is responsible for 20% of all cases of leukemia and about 3% of childhood leukemia. The predominant age group is between 25 and 60 years, with a greater number of patients with males. The Acute Myeloid Leukemia (AML) is the most common type of acute leukemia and more than 80% of cases occurring in adults. This type of leukemia is around 15-20% of acute leukemia in childhood with a peak incidence between 40 and 60 years. AML is more common in men than in women. The determination of multielemental concentrations in physiological fluids is of considerable interest in clinical chemistry. Since it has been established this levels in human serum can be utilized as indicators for several pathological conditions. The multielement composition determination in human serum is important for the investigation of their role in human physiology and metabolism. We studied hundred serum samples from each group of patients (AML and CML) of both sexes with ages ranging from 19 to 70 years and hundred and twenty healthy volunteers aged 19 to 65 years. All the serum samples were collected from people who live in the urban area of Rio de Janeiro City/Brazil. All of them were submitted to medical history. This study was performed with the approval of the ethics committee. The measurements were performed at the X-Ray Fluorescence Beamline at the Brazilian National Synchrotron Light Laboratory (LNLS), in Campinas, São Paulo. It was possible to determine the concentrations of the following six elements: Na, P, S, Cl, K and Ca. In this work we used statistical analysis by principal components (PCA) SPSS for windows version 20.0. For this analysis, it was performed the test of Kaiser-Meyer-Olklin (KMO) and the Test of Sphericity Bartelett (TSB).

O mapeamento da concentração de elementos químicos, através da fluorescência de raios-X é um importante elemento no estudo de amostras superficiais, como pinturas e quadros. Existem sistemas de fluorescência industriais que são fabricados para tal fim, mas, além de serem demasiadamente custosos para o pequeno usuário, são específicos para determinadas faixas de dimensões de amostras e limitam o pesquisador ou usuário a um procedimento padrão, não dando liberdade a variações metodológicas e novos tratamentos dos dados. Os equipamentos portáteis normalmente não são fabricados para tal finalidade, mas podem ser adaptados com os ajustes certos. Ter o controle sobre o procedimento passo a passo tanto do equipamento, quanto do software que faz a reconstrução deste mapa é um passo importante para utilização em casos adversos e a implementação de novidades dentro desta técnica. Desta forma, a criação de algoritmos, que variam do padrão e possibilitam ao usuário improvisar e criar alterações nas rotinas, tanto computacionais quanto experimentais seria um fator interessante para contornar alguns tipos de dificuldades. O presente trabalho pretende criar um algoritmo para a criação de imagens de mapa de concentração a partir de arquivos resultantes de medidas de fluorescências de raios-X pontuais, implementando, quando possível, rotinas de pré e pós-processamento. Este último visando combinar os resultados com outras técnicas de medidas O algoritmo será criado e executado inicialmente na linguagem computacional matemática OCTAVE, que já possui pacotes próprios e simples para trabalhar com aquisição e manipulação de imagens, sendo de código fonte aberto. Os dados experimentais serão extraídos manualmente de um equipamento de fluorescência portátil, e toda a adaptação necessária tenderá a ser minimizada por soluções computacionais. Variações de modos de aquisição, para diferenciar medidas, otimizar tempo de aquisição de dados e até otimizar a qualidade das imagens poderão ser aplicados também para a melhoria dos resultados.

La validación de los métodos analíticos permite al laboratorio asegurar, mediante evidencia objetiva, que los resultados emitidos aplicando dicho método son confiables. Actualmente, está muy difundida la sistemática para validar métodos cuantitativos; sin embargo cuando se intenta aplicar en cualitativos no es fácil definir la metodología a aplicar. La fluorescencia de rayos X por reflexión total permite determinar en forma simultánea la presencia de elementos desde el Na hasta el U, en una mínima muestra liquida o suspensión que es evaporada en un portamuestra, obteniendo un espectro dispersivo en energía característico. El objetivo del trabajo fue establecer una metodología para determinaren forma inequívoca presencia de elementos en una muestra con un tratamiento estadístico de datos. La técnica a validar involucra la determinación simultanea de elementos desde el S (Z=16) al U (Z=92) con excepción de Mo, en muestras acuosas y en suspensiones. El procedimiento para la medición de muestras acuosas o suspensiones incluye la toma de una alícuota de 5ul en soportes adecuados de cuarzo (discos de 3cm de diámetro), los cuales se llevan a sequedad bajo lámpara IR. Luego de la evaporación, el residuo es excitado en el espectrómetro y finalmente, se adquiere un espectro dispersivo en energía característico de la muestra. El tiempo de medición se establece en 300 segundos para todas las muestras. Los parámetros seleccionados para evaluar el método fueron la selectividad y el límite de corte. En cuanto a la selectividad, la fluorescencia de rayos X implica la medición de longitudes de onda específicos para cada elemento. Asimismo, como todo método analítico no cuantitativo, se evalúa mediante un comportamiento dicotómico y como respuesta analítica se obtiene una distribución binaria en el formato de resultados positivos y negativos. La interacción entre ellos y el grado en que influyen en la determinación de una muestra están dados por el límite de corte. Para establecer los valores del límite de corte se trabajó con soluciones estándares de Ni, K, Fe y U en concentraciones cercanas a 0,005 mg/L.v Las verificaciones de los limites para los elementos desde el K hasta el U se realizaron con soluciones multielementales trazables al NIST. Se realizaron ensayos independientes de 20 blancos que permitieron verificar los cálculos de límites de detección emitidos por el equipo y más de 30 muestras con soluciones estándares a concentraciones variables de sólidos disueltos. Las mediciones se realizaron en un espectrómetro fluorescencia de rayos X por reflexión total (TXRF) S2 Picofox (Bruker) con tubo de Mo, con potencia máxima de 50W, detector tipo SDD con área de 10mm2 y resolución de 160 eV. Los portamuestras empleados fueron de cuarzo y el tiempo de medición seleccionado fue de 300 segundos para los blancos, los estándares y las muestras. Este método validado actualmente es empleado en forma rutinaria para muestras acuosas o en suspensión provenientes de distintas áreas de las centrales nucleares e industrias afines (CONUAR, NASA, etc.) donde se requiere la detección temprana de elementos trazas que puedan estar presentes: polvos residuales provenientes de fisuras en tuberías, impurezas en pastillas de uranio, impurezas en efluentes, etc

Our society has an urgent and growing demand for energy. Because of this need, each day new materials and routes that promise to meet this demand emerges. However, many of these strategies require large areas to become effective or are heavily dependent on weather conditions. And, due to global warming, these energy alternatives cannot be sustained, and this impacts negatively on operating costs. One of the possible energy routes use nuclear energy, this route faces strong resistance, especially from environmentalists and it gains strength when there are accidents like Chernobyl and Fukushima. Despite all the controversy, nuclear power has gained more space in our society, including our country. Brazil has, for decades, nuclear power plants in full operation and, as we have no reports of any problems. Our country has also a huge uranium reserves which has a positive impact on the final cost of energy produced by nuclear route. Because of all that, there are negotiations for the installation of a new plant in the northeast of the country. This region is strategic due to its energy demand and also to the proximity of biggest uranium reserves. Two Brazilian states are always highlighted, from the installation of nuclear power plants, Ceará and Sergipe. This possibility, combined with the intrinsic fears of nuclear energy, led us to seek alternative materials that can be used as radiation levels indicators. In this work, we chose to study usual materials of civil construction for the purpose of employing them in retrospective dosimetry, which aims to determine the excessive dose of radiation exposure, either chronological or acute. The materials studied were sand, mortar, tiles, tile, brick and concrete are commonly present everywhere. The samples here studied were collected in Sergipe cities. The characterization of these materials was done by analytical techniques, initially XRF and XRD were used. After the chemical characterization became clear that we would need to resort to chemical extraction strategies specific to be able to extract the quartz grain which is in fact the species susceptible to radiation. Once applied to acid leaching, named by us as Campos method, new aliquots were characterized by microscopy, ICP-MS and EPR. The results obtained by combining these strategies, demonstrated the potential of using these materials as radiation indicators. However, the high iron content combined with the prohibition of using chemical leaching procedureswith that promote the heating of the sample, showed that more studies are needed in order to establish a routine protocol.

O objetivo deste trabalho é classificar padrões em imagens de Raios X. Para isso, foi desenvolvida uma ferramenta computacional: o SDPI - Sistema de Detecção de Padrões em Imagens. A base da metodologia de classificação, utilizado pelo SDPI, são os Descritores de Textura. O SDPI extrai os Descritores de Textura da imagem a ser analisada, e utiliza estas informações para treinar uma Rede Neural Artificial (RNA). Para testar a ferramenta desenvolvida, foram utilizados dois conjuntos distintos de imagens de mamografia. Após a obtenção dos Descritores de Textura nos dois conjuntos de imagens, utilizamos o primeiro conjunto de imagens para treinar uma RNA, e o segundo conjunto de imagens para testes. Após o treinamento, a RNA determina imagens com calcificações, no conjunto de teste, com uma precisão de 87,50%. Os resultados mostram que a classificação das imagens por Descritores de Textura é uma ferramenta poderosa, que independe de análise visual, que pode sofrer subjetividades. Este processo pode ser utilizado em outras aplicações, tais como localizações de desmatamentos em aerofotografias e determinação de padrões em plantações.

The x-ray microtomography is an important non-destructive technique to investigate fossils and other prehistories specimens, because of its capacity of preserve their physics integrity. Currently, is frequent the search for the technique for studies with palaeontology. This study is about the use of X-ray microtomography to survey a fossil compared with actual specimen of blowfish. The aim of this study is identify the changes that occur over the years. This images were obtained through of system SkyScan 1173. The acquisition parameters 130 kV of voltage, 61uA of current, pixel size 26 µm and the rotation degree was 0.5°. After the scanning was realized the reconstruction and it allows to realize a qualitative analysis with 2D and 3D images. This images allowed to observe a change in orientation of jaw. This result showed that the technique is very important to analyse this type of specimens because is a non-destructive technique that provides qualitative and quantitative tools essentials to allow the visualization of the internal structures preserving the integrity of specimens.

O bjetivo deste estudo foi à caracterização química do material particulado em suspensão na atmosfera da região metropolitana de Goiânia (GO). A amostragem foi realizada no inverno e no verão de 2012. Utilizou-se na coleta o amostrador do tipo Stacker, capaz de amostrar simultaneamente partículas finas (partículas com um diâmetro de até 2,5 µm) e grossas (partículas com um diâmetro entre 2,5 e 10 µm). Neste estudo foram utilizados filtros de policarbonato com diâmetro de 47 milímetros, com tamanho de poro de 0,4 e 8,0 µm, para coleta de PM2,5 e PM10 respectivamente. A massa de aerosol nos filtros PM10 e PM2,5 apresentaram os seguintes valores médios e desvios-padrão: PM10 inverno e verão de 15 ± 7 μg/m³e 90 ± 70 μg/m³, respectivamente; Goiânia PM2,5 inverno 27 ± 7 μg/m³ , verão 14 ± 9 μg/m³. A determinação elementar foi realizada pela técnica de Fluorescência de Raios X Dispersiva em Energia excitada com luz sínctrotron (SRXRF). As concentrações elementares médias e desvios-padrão das amostras coletadas em Goiânia são apresentados da seguinte forma: PM10 inverno (Si 1500 ± 400 ng/m³; S 150 ± 30 ng/m³; Ca 600 ± 200 ng/m³; K 240 ± 90 ng/m³; Ti 130 ± 50 ng/m³; Cr 3,7 ± 0,8 ng/m³; Mn 11 ± 3 ng/m³; Fe 1430 ± 400 ng/m³; Cu 13 ± 4 ng/m³; Zn 22 ± 8 ng/m³ e PM2,5 inverno (Si 650 ± 20 ng/m³; S 120 ± 20 ng/m³; Ca 150 ± 180 ng/m³; K 80 ± 70 ng/m³; Ti 40 ± 30 ng/m³; Cr 1,8 ± 0,6 ng/m³; Mn 3 ± 2 ng/m³; Fe 300 ± 300 ng/m³; Cu 5,6 ± 1,7 ng/m³; Zn 8 ± 4 ng/m³. Verão PM10 (Si 1100 ± 300 ng/m³; S 150 ± 50 ng/m³; Ca 430 ± 140 ng/m³; K 150 ± 60 ng/m³; Ti 70 ± 30 ng/m³; Cr 5 ± 3 ng/m³; Mn 7 ± 2 ng/m³; Fe 800 ± 300 ng/m³; Cu 7 ± 3 ng/m³; Zn 21 ± 7 ng/m³ e PM2,5 verão (Si <LQ, S 130 ± 40 ng/m³; Ca 40 ± 40 ng/m³; K 50 ± 30 ng/m³; Ti 8 ± 7 ng/m³; Cr 1,2 ± 0,8 ng/m³; Mn 1,8 ± 0,7 ng/m³; Fe 60 ± 60 ng/m³; Cu 2,8 ± 0,4 ng/m³; Zn 4,5 ± 1,9 ng/m³). A massa total média (μg/m³) do PM2,5 no inverno foi maior que a do PM10, fenômeno causado pela maior emissão de particulado fino ou devido ao menor tePMo de resiliência do PM10 na atmosfera. No verão o PM10 apresentou concentrações (μg/m³) maiores do que no inverno, cerca de seis vezes maior, já para o PM2,5 a concentração média foi maior no inverno. No geral, os elementos determinados apresentaram concentrações médias maiores no particulado grosso que no fino. A campanha de amostragem de inverno apresentou concentrações médias maiores para as duas frações coletadas. Salva exceção do S, elemento normalmente associado ao PM2,5, não apresentou variação significativa entre as frações coletadas e nem entre as épocas de amostragem. A presença de S no PM10 pode ter ocorrido devido à adsorção de dióxido de enxofre na superfície das partículas sólidas, aderido através de reações com oxidantes já presentes nessas partículas (MARTINS C. R., ANDRADE J. B., 2002).

Este trabalho apresenta o desenvolvimento e caracterização de um sistema portátil automatizado de fluorescência de raios X por reflexão total (TXRF) de alta tecnologia e baixo custo para realizar análises não destrutivas, que pode ser empregado para análise de vários tipos de amostras: biológicas, ambientais, engenharia de materiais e na indústria. O sistema é constituído por um tubo de raios X de 50 W, ânodo de Mo, um guia de onda, um detector Si-PIN, refletores de quartzo, posicionadores para os eixos X, Y e Z, movimentados por dois motores de passos controlados usando a plataforma Arduino e um micro computador. O sistema TXRF foi avaliado e caracterizado a partir de testes de repetibilidade, otimização da posição do feixe de raios X, ângulo de reflexão total e curva de sensibilidade. A operação do sistema foi realizada com 40 kV e 0,4 mA, com contagens de 200 segundos. A precisão e exatidão foram realizadas utilizando-se amostras certificadas de fígado bovino (NIST – Bovine liver 1577b). No teste de repetibilidade, o sistema apresentou um coeficiente de variação menor que 3,2 %. Na condição de reflexão total, o ângulo critico foi de 0,10 ± 0,01 graus, valor que está de acordo com a previsão teórica para a energia do feixe incidente (ânodo de Mo) e o refletor de quartzo. As concentrações determinadas com o sistema automatizado portátil de TXRF apresentaram variação no intervalo de 9 -14 % para os elementos majoritários (P, S e K) e de 2-20 % para os elementos traços (Ca, Mn, Fe, Cu, Zn e Rb). O sistema portátil automatizado de TXRF mostrou que é capaz de efetuar analises de fluorescência de raios X por reflexão total com um sistema de alta tecnologia e baixo custo e analisar elementos em um intervalo de Z=15 a Z=38.

Disposal of industrial wastes and application of fertilizers and pesticides in agriculture has contributed to a continuous accumulation of contaminants in certain areas. Release of toxic soluble substances onto the soil as a result of agricultural and industrial activities may pose a serious threat to the environment. One aspect of sustainability is the accumulation of metals in soil which causes problems if certain levels are exceeded. When a liquid comes in contact with soil, some of their constituents will dissolve to a greater or lesser extent. Leaching of chemical substances occurs across the soil by percolation of water solutions. The leaching potential refers to the risk that soluble contaminants could be transferred through the soil to the groundwater reservoir. The degree of dissolution of individual particles in the contact phase (liquid/soil) determines the leachate composition. The mobility of metals in soil depends on their bond strength with the soil surface. Metal ions generally associate with the hydroxides, sulfides or carbonates of the soil organic matter by different mechanisms such as complexation. The most important factors that affect these processes are pH, redox potential, and organic matter concentration in soil. The binding of the metal to the dissolved organic matter can increase their solubility by more than 2 orders of magnitude. In this research, chromium adsorption in soils coming from the Pampean region of Argentina was studied and compared with the same soils amended with food waste compost. This region shows a high industrial activity that includes tanneries and metallurgical industries. Chromium, as CrVI (anion) and CrIII (cation), was chosen as a representative metal to study the adsorption or retention capacities of these soils. Energy Dispersive X-Ray Fluorescence spectrometry (EDXRF) was employed for the characterization of soils samples and Total Reflection X-Ray Fluorescence Spectrometry (TXRF) for the solutions. This research gives an interesting contribution to be extended for other types of soils allowing in this way to estimate the groundwater contamination risk based on the soil quantitative elemental information and the advantages of the mixing with food waste compost.

Pollution from heavy metals is becoming an increasing concern, since pollution can affect different environmental compartments namely, soil, air and water. Groundwater geochemical arsenic contamination is still a serious problem in Argentina. There is an increased necessity to develop processes to eliminate arsenic or at least to minimize their concentration in wastewaters prior to their release into the environment. Research and development of low-cost procedures in order to recover natural resources of water, superficial or groundwater, have become a very important task and a great challenge. Traditionally, the methods used to remove metals from a solution are chemical precipitation, adsorption, cations-exchange, reverse osmosis, electrodialysis, electrochemical reduction, etc. Adsorption process is the most frequently applied in industries due to low cost, easy procedure, versatility and the possibility to re-use the adsorbent. In this sense, many studies having been carried out in this field. Among natural adsorbents, the hydroxyapatites (HA) are known for their ability to retain various metals and metalloids, due to their surface characteristics; these are calcium phosphates that exist in some phosphate rocks, but especially in teeth and bone tissue of animals. Bovine bones represent an option. Bones are primarily composed of calcium phosphate, hydroxyapatite and collagen; HA was reported as an effective heavy metals adsorbent. The aim of this study was to evaluate the ability of bovine hydroxyapatite (HA) to act as adsorbent of arsenic to be used for remediation purposes. The specific surface area and total pore volume was calculated for the HA by developing an adsorption isotherm in nitrogen gas to its boiling temperature at atmospheric pressure. The method used was the conventional Brunauer– Emmett–Teller (BET) in order to measure the specific surface area of a material. The adsorbent was found to be a non-porous material. To develop the adsorption isotherms, batch experiments were carried out with different As solutions with initial concentrations ranging from 3 mg L-1 to 6 mg L-1 of As and different doses of HA (0.2 to 2 g per 50 mL). The amount of pollutant removed was determined from the difference between the initial concentration of arsenic and the remainder. The employed analytical technique was Total Reflection X-ray Fluorescence spectrometry (TXRF). According to the obtained results it can conclude that HA can be a possible low-cost adsorbent forAs showinga removal of 43%.Reactors water treatment, for reducing As concentration in drinking water,at laboratory scale, is presented. The effect of chemical variables as pH, temperature, competitively with other analytes is also considered.

A Fluorescência de Raios X por Dispersão em Energia (EDXRF) é um método que permite fazer análises quantitativas e qualitativas multielementares dos amostras de forma não destrutiva. Neste trabalho o espectrômetro de XRF da Amptek®, composto por um tubo com anodo de ouro e um detector SDD, foi utilizado para caracterizar amostras de ouro, tendo como referência três amostras de ouro padrão de 14, 16 e 18 quilates. Uma tabela foi montada com os resultados obtidos nas amostras padrão, que teve como base a razão Kα Cu / Lα Au. Posteriormente, amostras de joias de ouro foram comparadas com os padrões de medição e foi verificada a quantidade de ouro. Essa metodologia se mostrou adequada para análise de baixo custo da qualidade de objetos de ouro.

Duplex Stainless Steel is widely used in oil & gas, chemical, petrochemical and nuclear power industries because of its combination of good mechanical properties and high corrosion resistance characteristics. Microstructure of duplex stainless steel is an example of composite material with approximately equal amounts of austenite and ferrite phases. Residual stress measurements in ferrite and austenite phases were made in duplex steel plates jointed by the GTAW welding technology. Software for processing of experimental data obtained by X-ray diffraction method was developed especially for stress measurements in duplex stainless steels. Using of this software allows to improve the accuracy and precision of stress measurements in ferrite and austenite phases and to minimize processing time.

The conservation of cultural heritage metal artworks is a major challenge. The main concern is related with corrosion: a physicochemical interaction between the metal and its environment, involving oxidation process trigged by the exposure of the metallic surface to various substances widely found in the air, such as Oxygen, Chloride and Sulfur Dioxide, intensified by moisture and dust, impurities that settle on the surface and act as catalysts in the metal degradation process. Regarding cultural heritage artefacts, corrosion could be related with the loss of some specific values (artistic, historic, scientific, social, etc.) of that object. There are several approaches regarding methods for cleaning surfaces in order to remove impurities and thereby, to preserve the object and maybe to restore it. One of the most common methods involves wet chemical process using hard abrasives. Indeed, these treatments are effective (for some purposes), and they have a low cost. However, details of the morphology of the surface of the samples are lost by such treatments. Taking into account that when it comes to cultural heritage objects, the goal is find a cleaning treatment which provides the lowest possible damage. The purpose of the present work is therefore study the possible effectiveness and also the advantages and disadvantages of the Glow Discharge Cleaning (GDC) method, through the analysis of coins obtained from Mr. Wilson Gennari's personal collection. In other to stablish an adequate procedure for our goal, we performed analyses in coins with corrosion in the surface. The effectiveness of the cleaning process was monitored with an X-Ray Fluorescence (XRF) portable equipment (Ampetk) before and after the cleaning. Also the coins mass also was monitored during the process. The conditions of Glow Discharge used was: pressure 6,0 x 10־¹torr, current 70 - 90mA, voltage 1,0 - 1,4kV and time 9 minutes. Photographic images were also obtained to follow up the cleaning process. Moreover, was possible to suggest that the physical properties of the alloy were not affected by this GDC process, once a very small reduction was observed in only one of the element matrix (Zinc) without any alteration on Copper content. The results obtained in this study suggest that the GDC procedure can be used to clean metallic surface, with clear advantages when compared to chemical cleaning due the fact that, there was no matrix lost (no mass reduction) and no signs of chemical degradation were found.

A sociedade moderna assiste um crescimento exponencial da violência que atinge todo o mundo. O emprego de armas de fogo (AF) está relacionado significativamente com este evento. Diversos são os trabalhos científicos voltados ao desenvolvimento de meios para se reduzir os índices de criminalidade e prestar suporte tecnológico aos meios de investigação criminal. Este trabalho consiste na pesquisa para a identificação de resíduos de disparos de armas de fogo, gunshot residue (GSR), que podem se depositar sobre as mãos de atiradores. Para o experimento foi utilizado um espectrômetro portátil de raios X produzido pela Amptek, com tubo de raios X com anodo de Au. As amostras forma submetidas a um feixe de 25kV de tensão e 25µA de corrente por um intervalo de 600s. Os espectros foram construídos e analisados com auxílio do programa DppMca, também fornecido pela Amptek. Amostras extraídas das mãos de atiradores mostram que com o emprego da técnica de fluorescência de raios X por dispersão de energia (EDXRF) torna possível identificar traços característicos de GSR.