Metodologias gerais empregadas no isolamento e identificação estrutural de feromônios de insetos

A selection of common procedures which are used for the identification and analysis of volatile biologically active compounds from insects are described.

RMN 2D: Detecção inversa e gradiente de campo na determinação estrutural de compostos orgânicos

A view of the general aspects involving the 2D NMR spectroscopy using inverse detection and field gradient techniques is presented through the analysis of a sesquiterpene.

La producció de ceràmica comuna vidriada del taller del carrer de l'Hospital al segle XIII a partir de la seva caracterització arqueomètrica

La descoberta del forn del segle XIII del taller del carrer de l'Hospital ha permès de realitzar un estudi complet de caracterització arqueomètrica de la ceràmica comuna vidriada que s"hi produïa. Les peces estudiades han estat analitzades mitjançant la fluorescència de raigs X (FRX), la difracció de raigs X (DRX) i la microscòpia òptica per làmina prima (MO). Els resultats han permès la identificació de 2 grups químics que corresponen a una producció poc calcària i a una altra de calcària. Igualment, s"ha pogut constatar com l"única olla estudiada, tot i procedir del taller del carrer de l'Hospital, no correspon a la producció d"aquest forn, que sembla que s'havia especialitzat en la producció de ceràmica comuna vidriada. A més, un dels gibrells correspon també a una altra producció diferenciada. La definició d"aquests dos grups de referència ha permès de comparar, amb més garanties, els materials apareguts en el dipòsit del carrer de Sant Honorat, i confirmar la segura producció barcelonina de la vaixella verda i de la pisa arcaica allà identificades.

Arqueometria ceràmica: una arqueologia ceràmica amb més informació

[spa] En el presente artículo se presentan los tres grandes ámbitos en los que se desarrolla la investigación arqueométrica sobre cerámicas: la identificación de los materiales, la proveniencia de los artefactos y la tecnología en la que se inscriben. El artículo hace una incidencia especial en aquello que se entiende por tecnología, indicando que la tecnología de producción es únicamente una parte de la misma, y que el concepto básico es el de diseño, que debe adecuarse a una multiplicidad de características de desempeño, explicadas por la cadena conductual en la cual transcurre la vida de los artefactos. Dado que las culturas se expresan por medio de artefactos, la vertiente material de éstos refleja, aunque sólo sea en parte, los compromisos que dichos artefactos tienen en las culturas en estudio. La arqueometría, con un cuerpo teórico y metodológico adaptado a la investigación de esta vertiente natural de los artefactos, aparece así como una forma complementaria de hacer arqueología y no como un campo de estudio diferenciado.

Noves dades sobre la producció de ceràmica medieval de Barcelona. La caracterització arqueomètrica del taller del Carrer de Carders

Arran de la troballa d'un taller ceràmic al carrer de Carders de Barcelona, datat entre els segles XII i XIII, s'ha dut a terme la caracterització arqueomètrica de 31 individus per tal de definir les característiques químiques i petrogràfiques de la seva producció. A més, s'han contrastat els resultats amb els obtinguts per a l'altre taller del segle XIII conegut a la ciutat, el del carrer de l'Hospital. L'estudi ha permès de definir el grup de referència (GR) del carrer de Carders, com també indicar l'existència d"individus procedents d'aquesta excavació però que es relacionen amb la producció del carrer de l'Hospital. I a la inversa, l'existència d'individus procedents del carrer de l'Hospital que es relacionen amb el carrer de Carders. Finalment, entre els materials procedents del carrer de Carders s'han identificat dues noves produccions no conegudes anteriorment.

Triterpenóides pentacíclicos de Mentha villosa: identificação estrutural e atribuição dos deslocamentos químicos dos átomos de hidrogênio e carbono

The structures of seven oleanene and ursene triterpenoids (1-7) isolated from aerial parts of Mentha villosa were identified. In addition, the complete ¹H and 13C resonance assignments of these triterpenoids were accomplished using 1D and 2D NMR spectroscopic experiments.

Caracterização textural e estrutural de V2O5/TiO2 obtidos via sol-gel: comparação entre secagem convencional e supercrítica

This work describes a modified sol-gel method for the preparation of V2O5/TiO2 catalysts. The samples have been characterized by N2 adsorption at 77K, x-ray diffractometry (XRD) and Fourier Transform Infrared (FT-IR). The surface area increases with the vanadia loading from 24 m² g-1, for pure TiO2, to 87 m² g-1 for 9wt.% of V2O5. The rutile form is predominant for pure TiO2 but became enriched with anatase phase when vanadia loading is increased. No crystalline V2O5 phase was observed in the catalysts diffractograms. Two species of surface vanadium observed by FT-IR spectroscopy a monomeric vanadyl and polymeric vanadates, the vanadyl/vanadate ratio remains practically constant.

Análise estrutural de ciclodextrinas: um estudo comparativo entre métodos teóricos clássicos e quânticos

In the present work, we analyzed the accuracy of distinct theoretical methods to reproduce the solid state structures of cyclodextrins. The a, b and g-cyclodextrins (CD) were considered and also their hydrates with included water molecules: a-CD.2H2O, b-CD.10H2O and g-CD.12H2O. The geometries were fully optimized using Molecular Mechanics (MM2), semiempirical (AM1 and PM3) and ab initio (HF/3-21G) methods and quantitatively compared with experimental data from X ray diffraction. The results obtained from the classical MM2 method were in best agreement with the experiment. The semiempirical and ab initio structures were also in satisfactory accordance with the experimental data. In general, the PM3 method was found to be more suitable than the AM1 to describe the CD geometries, mainly when the intramolecular hydrogen bonds are considered.

Resina de Protium heptaphyllum: isolamento, caracterização estrutural e avaliação das propriedades térmicas

Three mixtures of triterpenes (maniladiol and breine; alpha and beta-amyrin; lupenone, alpha and beta-amyrinone) were isolated from Protium heptaphyllum March resin. The structural identification was based on NMR and mass spectrometry data. Lupenone, and alpha and beta-amyrinone were not reported before as constituents of this resin. The resin was submitted to methylation and acetylation reactions. The pure and derivatized resins and the mixtures (maniladiol and breine; alpha and beta-amyrin) were analyzed by TG and DSC. The TG curves revealed that the derivatization decreases the thermal stability of the resin. The DSC curves showed peaks that can be assigned to evaporation and phase transitions processes.

Arqueologia biomolecular: passos preliminares para interpretações sobre a origem dos resíduos orgânicos preservados em fragmentos de cerâmica pré-colonial no Brasil

Organic residue analysis of archaeological potsherds is a well-established method for determining the uses of European and North American pottery vessels. In the present work we assess if the organic residues identified in Brazilian potsherd extracts are related to commodity processes (e.g. cooking or surface treatment) or to other non-archaeological sources, using as a model potsherds recovered from the Rio do Meio site (Santa Catarina Island). The potsherd extracts are dominated by saturated fatty acids (Ac16:0, with lower abundances of Ac14:0 and Ac18:0). Our studies provide evidence that the organic residues preserved in the Brazilian archeological potsherds are related to foodstuffs and surface treatment processes of the pottery vessels.

Análise arqueométrica de cerâmica Tupiguarani da região central do Estado do Rio Grande do Sul, Brasil, usando fluorescência de raios X por dispersão de energia (EDXRF)

Energy dispersive X-ray fluorescence methodology (EDXRF) was used to determine Al, Ba, Ca, Cr, Fe, K, Mn, Pb, Rb, S, Si, Sr, Ti, V, Zn in pottery sherds from seven archaeological sites in the central region of Rio Grande do Sul State, Brazil. The potteries' chemical fingerprints from Ijuí River, Ibicuí Mirim River, Vacacaí Mirim River and Jacuí River were identified. Interactions between sites from the Jacuí River, Vacacaí Mirim River and Ibicui Mirim River could have occurred because some samples from these sites are overlapping in a principal component analysis (PCA) graphic. The pottery provenance could be the same.

Elucidação estrutural de substâncias orgânicas com auxílio de computador: evoluções recentes

The development of new tools for chemoinformatics, allied to the use of different algorithms and computer programmes for structure elucidation of organic compounds, is growing fast worldwide. Massive efforts in research and development are currently being pursued both by academia and the so-called chemistry software development companies. The demystification of this environment provoked by the availability of software packages and a vast array of publications exert a positive impact on chemistry. In this work, an overview concerning the more classical approaches as well as new strategies on computer-based tools for structure elucidation of organic compounds is presented. Historical background is also taken into account since these techniques began to develop around four decades ago. Attention will be paid to companies which develop, distribute or commercialize software as well as web-based and open access tools which are currently available to chemists.

Síntese da hidroxiapatita e refinamento estrutural por difração de raios-x

A sample of hydroxyapatite was synthesized and its crystalline structure was analyzed by X-ray diffraction by means of the Rietveld method. Two functions were used to fit the peak profiles, modified Voigt (TCHZ) and Pearson VII. The occupational factors and lattice parameters obtained by both models show that the sample does not contain relevant cationic substitutions. The interatomic distances from Ca1 to oxygens O1, O2 and O3 were adequate for a pure hydroxyapatite without defect at site Ca1. Besides, the use of multiple lines in planes (300) and (002) associated with the model Pearson VII resulted in good agreement with the TCHZ model with respect to the size-strain effectswith an ellipsoidal shape of crystallites. In conclusion, the procedures adopted in the synthesis of hydroxyapatite produced a pure and crystalline material. The experimental results of transmission electron microscopy confirmed the predicted shape of crystals.

Métodos simples de formação de monocristal de substância orgânica para estudo estrutural por difração de raios X

This work presents three operationally simple laboratory protocols for monocrystal growth of small-molecule organic compounds, which have been applied with success in the last ten years for the formation of single crystals for X-ray structural studies. In addition, five structure hints were formulated as general guidelines for selecting a small-molecule organic compound as a candidate for monocrystal growth: molecular weight >200 D, melting point >100 ºC, two or more aromatic rings in the structure, at least two sites for intermolecular hydrogen bond formation, and a halogen or other heavy atom in the structure.