Abstract This paper presents a brief description of the prevailing ideas and hypothesis about the nature of matter from antiquity to the end of XIX century. It shows how gradually, since the Hauy proposal of the existence of the unit cell, the crystal lattice and symmetry and subsequent derivation of the 14 crystal classes by the French Physicist A. Bravais, the 32 point groups by the German mathematician A. Shoenfliess and the 230 space groups independently deduced by the Russian mathematician E. S. Fedorov and A. Shoenflies confirmed the atomic theory suggested by the Greek philosopher Democritus. These empirical and theoretical findings, conducted by several scientists, are one of the most brilliant theoretical predictions of all time in Science, fully confirmed after von Laue discovery of X-ray diffraction by crystals in 1912 and its application on the determination of molecular and crystalline structure by the English physicists W. H. Bragg (1862-1942) and his son W. L. Bragg (1890-1971).
Corundum, sapphire or α-Al2O3 is an important technological material in many optical and electronic applications such as solid-state lasers, optical windows and, more recently, as a radiation detector. Landauer (Glenwood, IL, USA) accumulated large number of archived and stored Luxel™ dosemeters composed of Al2O3:C, which were subjected to a recovery process. Due to the importance of this advanced crystalline material in OSL dosimetry, a recovery process was developed based on the dosemeters calcination and Al2O3:C has been reused in manufacturing of new dosemeters. This paper does not aim to optimize the recovery process, but provides an opportunity to study the involved process parameters and to recover this valuable crystalline material from used dosemeters. To the best of our knowledge no other recovery process involving this dosimetric material was described in scientific literature. Fourier Transform Infrared Spectrometry (FTIR), Thermogravimetry/Differential Thermoanalysis (TG/DTA), Differential Scanning Calorimetry (DSC), X-ray Diffraction (XRD), Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES), Optically Stimulated Luminescence (OSL) and Rietveld Refinement were used to characterize the recovered material and to check for the stability of its structural and dosimetric properties.
In this work, the synthetic hydroxyapatite (HAP) was studied using different preparation routes to decrease the crystal size and to study the temperature effect on the HAP nano-sized hydroxyapatite crystallization. X-ray diffraction (XRD) analysis indicated that all samples were composed by crystalline and amorphous phases . The sample with greater quantity of amorphous phase (40% of total mass) was studied. The nano-sized hydroxyapatite powder was heated and studied at 300, 500, 700, 900 and 1150 °C. All samples were characterized by XRD and their XRD patterns refined using the Rietveld method. The crystallites presented an anisotropic form, being larger in the  direction. It was observed that the crystallite size increased continuously with the heating temperature and the eccentricity of the ellipsoidal shape changed from 2.75 at 300 °C to 1.94, 1.43, 1.04 and 1.00 respectively at 500, 700, 900 and 1150 °C. In order to better characterize the morphology of the HAP the samples were also examined using atomic force microscopy (AFM), infrared spectrometry (IR) and thermogravimetric analysis (TGA).
The mineralogical characterization through mineral quantification of Brazilian soils by X-ray diffraction data using the Rietveld Method is not common. A mineralogical quantification of an Acric Ferralsol from the Ponta Grossa region, state of Paraná, Brazil, was carried out using this Method with X-Ray Diffraction data to verify if this method was suitable for mineral quantification of a highly-weathered soil. The A, AB and B3 horizons were fractioned to separate the different particle sizes: clay, silt, fine sand (by Stokes Law) and coarse sand fractions (by sieving), with the procedure free of chemical treatments. X-ray Fluorescence, Inductively Coupled Plasma Atomic Emission Spectrometry, Infrared Spectroscopy and Mössbauer Spectroscopy were used in order to assist the mineral identification and quantification. The Rietveld Method enabled the quantification of the present minerals. In a general way, the quantitative mineralogical characterization by the Rietveld Method revealed that quartz, gibbsite, rutile, hematite, goethite, kaolinite and halloysite were present in the clay and silt fractions of all horizons. The silt fractions of the deeper horizons were different from the more superficial ones due to the presence of large amounts of quartz. The fine and the coarse sand fractions are constituted mainly by quartz. Therefore, a mineralogical quantification of the finer fraction (clay and silt) by the Rietveld Method was successful.
A caracterização mineralógica por meio da quantificação dos minerais presentes em solos brasileiros por difração de raios X usando o Método de Rietveld é, ainda, pouco comum. Neste trabalho foi realizada a quantificação mineralógica de um Latossolo Vermelho ácrico da região de Ponta Grossa, Paraná, Brasil, utilizando o Método de Rietveld com dados de Difração de Raios X e também verificado se o método foi adequado na quantificação mineral de um solo altamente intemperizado. Os horizontes A, AB e B3 foram separados fisicamente nas frações: argila, silte, areia fina (por meio da Lei de Stokes) e areia grossa (por peneiramento) sem qualquer tratamento químico. As técnicas de Fluorescência de raios X, Espectroscopia de Emissão Atômica com Fonte de Plasma Induzido, Espectroscopia de Infravermelho e Espectroscopia Mössbauer foram utilizadas para auxiliar na identificação e quantificação dos minerais. O Método de Rietveld possibilitou a quantificação dos minerais presentes nas frações argila e silte de todos os horizontes: quartzo, gibbsita, rutílio, hematita, goethita, caulinita e haloisita. Na fração silte os horizontes mais profundos são diferentes do mais superficial devido à presença de grandes quantidades de quartzo. As frações areia fina e grossa são constituídas principalmente de quartzo. Portanto, o Método de Rietveld foi adequado para quantificação dos minerais, principalmente, das frações mais finas (argila e silte).
The accurate determination of the clay component contents of Latosols can contribute for the improvement of both use and management of such soils. In this research, the kaolinite and gibbsite contents of iron-free clay in Latosols were determined by differential scanning calorimetry (DSC) and with the application of the Rietveld method to X-ray diffraction data for comparison with mineral contents calculated by the allocation method. It is likely that crystallographic differences between kaolinite and gibbsite used in the DSC calibrations and the kaolinites and gibbsites in the samples were responsible for the inaccuracy of the mineral contents evaluated by this thermal method. The Rietveld method determined gibbsite contents almost identical to those calculated by the allocation method and kaolinite contents with acceptable similarity to the ones calculated by the allocation of total SiO2 iron-free clay contents.
A acurada determinação dos teores dos minerais que constituem a fração argila dos Latossolos pode contribuir para o aprimoramento de seu uso e manejo. Neste trabalho, teores de caulinita e gibbsita da fração argila desferrificada de Latossolos foram determinados por calorimetria exploratória diferencial (CED) e pela aplicação do método de Rietveld a dados de difratometria de raios X (DRX), e comparados com seus respectivos teores calculados pelo método da alocação. Possivelmente, diferenças cristalográficas entre a caulinita e a gibbsita utilizadas na calibração da CED e suas respectivas contrapartidas encontradas nas amostras analisadas tenham contribuído para a menor exatidão dos teores de caulinita e de gibbsita determinados pelo referido método térmico. Os teores de gibbsita das argilas desferrificadas quantificados com a abordagem DRX-Rietveld foram praticamente idênticos aos calculados por alocação, ao passo que os de caulinita foram similares aos respectivos teores determinados com o método de Rietveld.
A new lactonic triterpene isolated from the heartwood of Austroplenckia populnea (Celastraceae) was characterized as 3alpha-hydroxyolean-12-en-29,22alpha-olide (the gamma-lactone of the 3alpha,22alpha-dihydroxyolean-12-en-29alpha-oic acid), the 3-epimer of the abruslactone A, on the basis of its spectral data, chemical transformations, and single crystal X-ray analysis.
Um triterpeno lactônico inédito isolado do cerne de Austroplenckia populnea (Celastraceae) foi caracterizado como 3alfa-hidroxiolean-12-en-29,22alfa-olídeo (a gama-lactona do ácido 3alfa,22alfa-diidroxiolean-12-en-29alfa-óico), o epímero em C-3 da abruslactona A, com base em dados espectrais, oxidação e análise cristalográfica.