Synthesis and characterization of Fe(III)-doped ceramic membranes of titanium dioxide and its application in photoelectrocatalysis of a textile dye

Pure and Fe(III)-doped TiO2 suspensions were prepared by the sol gel method with the use of titanium isopropoxide (Ti(OPri)4) as precursor material. The properties of doped materials were compared to TiO2 properties based on the characterization by thermal analysis (TG-DTA and DSC), X-ray powder diffractometry and spectroscopy measurements (FTIR). Both undoped and doped TiO2 suspensions were used to coat metallic substrate as a mean to make thin-film electrodes. Thermal treatment of the precursors at 400ºC for 2 h in air resulted in the formation of nanocrystalline anatase TiO2. The thin-film electrodes were tested with respect to their photocatalytic performance for degradation of a textile dye in aqueous solution. The plain TiO2 remains as the best catalyst at the conditions used in this report.

The ceramic artifacts in archaeological black earth (terra preta) from lower Amazon region, Brazil: mineralogy

Several archaeological black earth (ABE) sites occur in the Amazon region. They contain fragments of ceramic artifacts, which are very important for the archaeological purpose. In order to improve the archaeological study in the region we carried out a detailed mineralogical and chemical study of the fragments of ceramic artifacts found in the two ABE sites of Cachoeira-Porteira, in the Lower Amazon Region. Their ceramics comprise the following tempers: cauixi, cariapé, sand, sand +feldspars, crushed ceramic and so on and are composed of quartz, clay equivalent material (mainly burned kaolinite), feldspars, hematite, goethite, maghemite, phosphates, anatase, and minerals of Mn and Ba. Cauixi and cariapé, siliceous organic compounds, were found too. The mineralogical composition and the morphology of their grains indicate a saprolite (clayey material rich on quartz) derived from fine-grained felsic igneous rocks or sedimentary rocks as source material for ceramic artifacts, where silica-rich components such cauixi, cariapé and/or sand (feldspar and rock fragments) were intentionally added to them. The high content of (Al,Fe)-phosphates, amorphous to low crystalline, must be product of the contact between the clayey matrix of pottery wall and the hot aqueous solution formed during the daily cooking of animal foods (main source of phosphor). The phosphate crystallization took place during the discharge of the potteries put together with waste of organic material from animal and vegetal origin, and leaving to the formation of the ABE-soil profile.

The ceramic artifacts in archaeological black earth (terra preta) from Lower Amazon Region, Brazil: chemistry and geochemical evolution

This paper carried out a chemical investigation of archaeological ceramic artifacts found in archaeological sites with Black Earth (ABE) in the Lower Amazon Region at Cachoeira-Porteira, State of Pará, Brazil. The ceramic artifacts, mostly of daily use, belong to Konduri culture (from 900 to 400 years BP). They are constituted of SiO2, Al2O3, Fe2O3, Na2O and P2O5; SiO2 and Al2O3 together add up to 80 % and indicate influence of acid rocks, transformed into clay minerals basically kaolinite. The relative high contents of P2O5 (2.37 % in average) come out as (Al,Fe)-phosphate, an uncommon fact in primitive red ceramics, but found in some roman and egyptian archaeological sites. The contents of the trace elements are similar or below the Earth's crust average. This chemical composition (except P2O5) detaches saprolite material derived acid igneous rocks or sedimentary ones as the main raw material of the ceramics. The contents of K, Na and Ca represent the feldspars and rock fragments possibly introduced into saprolitic groundmass, indicated by mineralogical studies. The presence of cauixi and cariapé as well as quartz sand was confirmed by optical microscope, SEM analyses and by the high silica contents of ceramic fragments. Phosphorus was possibly incorporated into groundmass during cooking of foods, and ABE soil profile formation developed on yellow Latosols. The raw materials and its tempers (cauixi, or cariapé, feldspar, crushed rocks, old ceramic artifacts and quartz fragments) are found close to the sites and therefore and certainly came from them.

High prevalence and low E6 genetic variability of human papillomavirus 58 in women with cervical cancer and precursor lesions in Southeast Mexico

Infection with some genotypes of human papillomavirus (HPV) is the most important risk factor associated with cervical cancer (CC). Throughout the world, HPV type 58 prevalence varies from one region to another; it is higher in women from certain countries in Asia and Latin America, such as China and Mexico. Although intratypic variants have been reported on a few occasions, our knowledge about HPV 58 genetic variation remains limited. Therefore, this work aims to (i) determine the prevalence of HPV type 58 amongst Mexican women with invasive CC or precursor lesions and (ii) identify HPV 58 sequence variants. One hundred and forty five colposcopy clinic patients were studied. Genotyping of HPV 16, 18 and 58 was determined by specific nested PCR and HPV 58 variants were detected by direct sequencing. The general prevalence of HPV was 51.7% (75/145). HPV 16 was found in 30.6% (23/75) and HPV 58 in 24% (18/75) of the patients. HPV 18 was not identified in patients with cervical intraepithelial neoplasia (CIN) grade I; it was only found in those with CIN II, with a prevalence of 6.8% (3/44). In patients with CC, the prevalence of HPV 16 and 58 was 78.9%. Regarding HPV 58 variants, 94.4% of the HPV 58 sequences were identical to the prototype strain, whereas one sample showed changes at a single nucleotide. This study demonstrates a high prevalence of HPV 58 and a low genetic variability of E6 sequences amongst Mexican colposcopy patients.

Oxochloroalkoxide of the Cerium (IV) and Titanium (IV) as oxides precursor

The Cerium (IV) and Titanium (IV) oxides mixture (CeO2-3TiO2) was prepared by thermal treatment of the oxochloroisopropoxide of Cerium (IV) and Titanium (IV). The chemical route utilizing the Cerium (III) chloride alcoholic complex and Titanium (IV) isopropoxide is presented. The compound Ce5Ti15Cl16O30 (iOPr)4(OH-Et)15 was characterized by elemental analysis, FTIR and TG/DTG. The X-ray diffraction patterns of the oxides resulting from the thermal decomposition of the precursor at 1000 °C for 36 h indicated the formation of cubic cerianite (a = 5.417Å) and tetragonal rutile (a = 4.592Å) and (c = 2.962 Å), with apparent crystallite sizes around 38 and 55nm, respectively.

Enantioselective synthesis of aziridines using asymmetric transfer hydrogenation as a precursor for chiral derivatives used as bonding agent for rocket solid propellants

A rapid, expedient and enantioselective method for the synthesis of beta-hydroxy amines and monosubstituted aziridines in up to 99% e.e., via asymmetric transfer hydrogenation of a-amino ketones and cyclisation through treatment with tosyl chloride and base, is described. (1R,2R)-N-(para-toluenesulfonyl)-1,2-ethylenediamine with formic acid has been utilised as a ligand for the Ruthenium (II) catalysed enantioselective transfer hydrogenation of the ketones.The chiral 2-methyl aziridine, which is a potentially more efficient bonding agent for Rocket Solid Propellant has been successfully achieved.

Síntese, caracterização e estudo das propriedades catalíticas e magnéticas de nanopartículas de Ni dispersas em matriz mesoporosa de SiO2

Nickel nanoparticles supported on amorphous silica ceramic matrix were synthesized by the polymeric precursor method. The nanostructure was characterized by NMR, BET, XRD, SEM, TEM, and flame atomic absorption spectrometry techniques. It was observed a dependence of the crystallite size on the thermal annealing, under a N2 atmosphere. The materials presented a high catalytic activity and selectivity upon the beta-pinene hydrogenation reaction. The magnetic hystereses were also correlated with the morphology of the processed material.

Preparación y caracterización de la zeolita MCM-22 y de su precursor laminar

The layered precursor of MCM-22 was prepared with different Si/Al ratios: 15, 25, 50, 100 and ¥. Upon heat treatment these precursors form MCM-22 zeolite. Both layered precursor and MCM-22 zeolite were characterized by several techniques: Chemical Analysis by Atomic Absorption Spectroscopy (AAS), X-Ray Diffraction (XRD), Thermo-gravimetric Analysis (TGA), Pore Analysis by N2 and Ar adsorption, Scanning Electron Microscopy (SEM), Infrared Spectroscopy (IR) and Temperature Programmed Desorption of ammonium (TPD).

Efecto de la naturaleza del precursor sobre las caracteristicas de las nanoparticulas de SnO2 sintetizadas

Tin oxide (SnO2) is widely used in industry as raw material for electronic devices, plating of different types of materials, for dyes and pigments, for electroplating, heterogeneous catalysis, etc. In this work SnO2 was obtained by a controlled precipitation method with special attention to the effects the tin precursor has on the microstructure of the final product. The most appropriate pH for obtaining SnO2 with the rutile structure as the main phase is 6.25 for SnCl2 and 6.40 for SnSO4. After heat treatment at 600 °C, particles of nanometric order (~10 - 30 nm approx) were obtained. The characterization of the solid phase was made by X-ray diffraction (XRD), thermal analysis (DTA/TG), transmission electron microscopy (TEM) and Fourier transformed infrared spectroscopy (FTIR).

Otimizaçâo das condições de preparação de eletrodos à base de carbono cerâmico utilizando-se planejamento fatorial

Different parameters of carbon ceramic electrodes (CCE) preparation, such as type of precursor, carbon material, catalyst amount, among others, significantly influence the morphological properties and consequently their electrochemical responses. This paper describes a 2³ factorial design (2 factors and 3 levels with central point replicates), which the factors analyzed were catalyst amount (HCl 12 mol L-1), graphite/precursor ratio, and precursor type (TEOS - tetraethoxysilane and MTMOS - methyltrimetoxysilane). The design resulted in a significant third order interaction for peak current values (Ipa) and a second order interaction for potential difference (ΔE), between thefactors studied, which could not be observed when using an univariated study.

Sinterabilidade de pós de precursor vitrocerâmico do sistema LZSA tratados por troca iônica

Ion exchange method was employed by means of surface modification of the glass powders of LZSA (Li2O-ZrO2-SiO2-Al2O3) system submitted to a 70wt% NaNO3/30wt% NaSO4 bath salt followed by a heat treatment. Chemical analysis by X-ray fluorescence was used to evaluate the efficiency of ion exchange, while optical dilatometry was employed to evaluate sintering of compacts. Evaluation of the structure of sintered bodies was made by scanning electron microscopy. Substitution of Li+ ions by Na+ ions on the surface of powders during heat treatments of 450 and 600 ºC for 2-10 h promoted an increase in densification of the sintered bodies.

SYNGAS PRODUCTION FROM CO2-REFORMING OF CH4 OVER SOL-GEL SYNTHESIZED Ni-Co/Al2O3-MgO-ZrO2 NANOCATALYST: EFFECT OF ZrO2 PRECURSOR ON CATALYST PROPERTIES AND PERFORMANCE

Ni-Co/Al2O3-MgO-ZrO2 nanocatalyst with utilization of two different zirconia precursors, namely, zirconyl nitrate hydrate (ZNH) and zirconyl nitrate solution (ZNS), was synthesized via the sol-gel method. The physiochemical properties of nanocatalysts were characterized by XRD, FESEM, EDX, BET and FTIR analyses and employed for syngas production from CO2-reforming of CH4. XRD patterns, exhibiting proper crystalline structure and homogeneous dispersion of active phase for the nanocatalyst ZNS precursor employed (NCAMZ-ZNS). FESEM and BET results of NCAMZ-ZNS presented more uniform morphology and smaller particle size and consequently higher surface areas. In addition, average particle size of NCAMZ-ZNS was 15.7 nm, which is close to the critical size for Ni-Co catalysts to avoid carbon formation. Moreover, FESEM analysis indicated both prepared samples were nanoscale. EDX analysis confirmed the existence of various elements used and also supported the statements made in the XRD and FESEM analyses regarding dispersion. Based on the excellent physiochemical properties, NCAMZ-ZNS exhibited the best reactant conversion across all of the evaluated temperatures, e.g. CH4 and CO2 conversions were 97.2 and 99% at 850 ºC, respectively. Furthermore, NCAMZ-ZNS demonstrated a stable yield with H2/CO close to unit value during the 1440 min stability test.

Estudo da decomposição térmica de oxalato de estrôncio dopado com cério(III) como precursor de materiais luminescentes

Este trabalho trata da obtenção de SrC2O4, Ce2(C2O4)3, e SrC2O4 dopado com diferentes porcentagens de Ce3+ como precursores do luminóforo azul Sr2CeO4. Os precursores preparados foram estudados por TG e DTA. Uma mistura contendo SrC2O4 e Ce2(C2O4)3 na relação 4:1 respectivamente e SrC2O4 dopado com diferentes porcentagens de Ce3+, foram tratadas termicamente à 1100ºC, 12 horas. Os produtos foram analisados por XRD e espectroscopia de luminescência e apresentam mistura das fases SrCeO3, Sr2CeO4 e SrCO3. Os produtos contendo a fase Sr2CeO4 apresentam luminescência azul de banda larga, com exceção daquele obtido a partir de SrC2O4 dopado com 50% de Ce3+. Neste caso a fase predominante é SrCeO3. Pela curva DTA observa-se um pico endotérmico em torno de 1000ºC para todas as amostras, com exceção da amostra dopada em 50%, evidenciando a temperatura de formação da fase Sr2CeO4. A fase luminescente Sr2CeO4 é preferencialmente obtida partindo-se de SrC2O4:Ce3+ 25% e de misturas mecânicas na proporção de 4:1 de oxalatos de estrôncio e de oxalato de cério.

p16INK4 expression in precursor lesions of squamous cell cervical cancer related to the presence of HPV-DNA

The purpose of the present study was to identify the expression of p16INK4 in cervical cancer precursor lesions by immunohistochemistry and to correlate it with lesion grade and presence of human papillomavirus (HPV) infection. Cervical specimens from 144 women seen consecutively at the gynecology outpatient clinic of our institution from December 2003 to May 2005 were analyzed by cytopathology, histopathology, polymerase chain reaction for HPV-DNA, and p16INK4 immunostaining. Histologically normal biopsies, HPV-DNA negative by polymerase chain reaction, were used as control. HPV-DNA prevalence, including the control group, was 68.1% and the prevalence of p16INK4 expression was 55.0%. The percentage of cells stained by p16INK4 ranged from 10 to 100%, both in the group consisting of cervical intraepithelial neoplasia (CIN)1/HPV specimens and in the group of CIN2/CIN3 specimens with P value of 0.0001. p16INK4 expression was 48.3% in the CIN1/HPV group, as opposed to 94.3% in the CIN2/CIN3 group (P = 0.001), showing a statistically significant difference between the two groups. The quantitative method used here is simple and less subjective than the different semiquantitative methods described in the literature. In view of the different definitions of a p16INK4-positive case, it is almost impossible to compare the findings reported by different investigators. This study confirms the association between p16INK4 and CIN2 and CIN3 lesions. Moreover, it shows that some low grade lesions expressed high levels of this protein. This may indicate that such low grade lesions may be predisposed to progress to high grade lesions. This means that p16INK4 may be a strong marker for "neoplastic lesions" induced by HPV and not just an infection marker.