Synthesis and spectroscopic characterization of polymer and oligomers of ortho-phenylenediamine

Poly(ortho-phenylenediamine) and oligomers of ortho-phenylenediamine were chemically synthesized and characterized by UV-vis, (1)H and (13)C NMR, FTIR and resonance Raman spectroscopies. Polymerization of ortho-phenylenediamine in HCl medium with ammonium persulfate only leads the trimer compound, in disagreement with some previous reports. Nevertheless, in acetic acid medium it was possible to prepare a polymer constituted by ladder phenazinic segments with different protonation levels and quinonediimine rings (polyaniline-like). X-ray absorption at N K-edge (N K XANES), X-ray photoelectron (XPS) and Electron paramagnetic resonance (EPR) spectroscopies were used to determine the different kinds of nitrogen presents in this class of polymer. N K XANES spectrum of poly(ortho-phenylenediamine) shows the band of -N=nitrogen of non-protonated phenazinic rings at 398.2 eV. In addition, XPS and N K XANES data confirm the presence of different types of protonated nitrogens in the polymeric poly(ortho-phenylenediamine) chain and the EPR spectrum shows that the polymer has a very weak polaronic signal. (C) 2009 Elsevier Ltd. All rights reserved.

Structure of chemically prepared poly-(para-phenylenediamine) investigated by spectroscopic techniques

The structure of chemically prepared poly-p-phenylenediamine (PpPD) was investigated by Resonance Raman (RR), FTIR, UV-VIS-NIR, X-ray photoelectron (XPS), X-ray Absorption at Nitrogen K edge (N K XANES), and Electron paramagnetic Resonance (EPR) spectroscopies. XPS, EPR and N K XANES data reveal that polymeric structure is formed mainly by radical cations and dication nitrogens. It excludes the possibility that PpPD chains have azo or phenazinic nitrogens, as commonly is supposed in the literature. The RR spectrum of PpPD shows two characteristic bands at 1527 cm(-1) and 1590 cm(-1) that were assigned to nu C=N and nu C=C of dication units, respectively, similar to polyaniline in pernigraniline base form. The presence of radical cations was confirmed by Raman data owing to the presence of bands at 1325/1370 cm(-1), characteristic of nu C-N of polaronic segments. Thus, all results indicate that PpPD has a doped PANT-like structure, with semi-quinoid and quinoid rings, and has no phenazinic rings, as observed for poly-o-phenylenediamine. (C) 2009 Elsevier Ltd. All rights reserved.

The role of cross-linking structures to the formation of one-dimensional nano-organized polyaniline and their Raman fingerprint

In the present work. the resonance Raman. UV-vis-NIR and scanning electron microscopic (SEM) data of nanorods (about similar to 300 rim in diameter) and nanofibers (about similar to 93 nm in diameter) of PANI are presented and compared. The PANI samples were synthesized in aqueous media with dodecybenzenesulfonic acid (DBSA) and beta-naphtalenesulfonic acid (beta-NSA) as dopants, respectively. The presence of hands at 578, 1400 and 1632cm(-1) in the Raman spectra of PANI-NSA and PANI-DBSA shows that the formation of cross-linking structures is a general feature of the PANI chains prepared in micellar media. It is proposed that these structures are responsible for the one-dimensional PANI morphology formation. In addition, the Raman band at 609cm(-1) of PANI fibers is correlated with the extended PANI chain coil formation. (C) 2008 Elsevier B.V. All rights reserved.

Laponite RD/polystyrenesulfonate nanocomposites obtained by photopolymerization

The present paper describes the synthesis and characterization by dynamic light scattering, X-ray diffraction, scanning electron microscopy and atomic force microscopy of Laponite RD/Sodium polystyrenesulfonate nanocomposites obtained by radical photopolymerization initiated by the cationic dye safranine. The presence of the clay mineral does not affect the hydrotropic aggregation of the monomers, but allows a better deaggregation of the initiator molecules, decreasing the quenching of the excited states that leads to the radicals that initiate polymerization. Increasing the amount of clay mineral loading in the polymerization mixture promotes higher monomer conversion and faster polymerization. The size of the nanocomposite particles, measured by light scattering decreases from 400 to 80 nm for clay mineral loadings of 1.0 wt.%. The X-ray diffraction patterns indicate that the clay mineral does not present a regular crystalline structure in the nanocomposite. Atomic force microscopy studies show films of sodium polystyrenesulfonate polymer with embedded Laponite platelets in its structure, forming 1-8 nm height and 25-100 nm diameter aggregates. (C) 2011 Elsevier B.V. All rights reserved.

Maude Object-Oriented Action Tool

MAIDL, André Murbach; CARVILHE, Claudio; MUSICANTE, Martin A. Maude Object-Oriented Action Tool. Electronic Notes in Theoretical Computer Science. [S.l:s.n], 2008.

Adsorção de Pb(II) utilizando adsorvente composto por montmorilonita e dolomita

The destructive impact of improper disposal of heavy metals in the environment increases as a direct result of population explosion, urbanization and industrial expansion and technological developments. Argil are potential materials for adsorption of inorganic and the pelletization of it is required for use in adsorptive columns of fixed bed. The low cost and the possibility of regeneration makes these materials attractive for use in the purification process, capable of removing inorganic compounds in contaminated aquatic environments. In this work was made pellets of a mixture of dolomite and montmorillonite by wet agglomeration, in different percentages. The removal of Pb (II) was investigated through experimental studies, and was modeled by kinetic models and isotherms of adsorption. The materials were characterized using the techniques of XRD, TG / DTA, FT-IR, and surface area by BET method. The results showed the adsorption efficiency of the contaminant by the composite material studied in synthetic solution. The study found that the adsorption follows the Langmuir model, and the kinetics of adsorption follows the model of pseudosecond order

Síntese de zeólitas e argilas ácidas pilarizadas a partir de matérias primas naturais

Structural changes in waste for zeolites synthesis are subject of many studies carried out in the synthesis of molecular sieves. These materials are named molecular sieves because they have well defined pore sizes and they have the capacity of select molecules by its size. In this work, it was studied the synthesis processes of two types of molecular sieves: pillared acid clays using as starting material one natural montmorillonite clay and the synthesis of zeolites from a silico-aluminous residue. This residue is a byproduct of the extraction of lithium -spodumene. The preparation of pillared acid clays was performed in two steps: 1° acid treatment of clay samples (time and temperature studies) and 2°pilarization of them with Al13 (Keggin ion). The temperature and acid concentration affect the removal of cations in the structure and porosity of the material obtained. The analysis of X-ray diffraction (XRD) and infrared spectroscopy (IR), showed that increasing the severity of the acid treatment compromises the structural material. Also the pore size distribution is approximately uniform. Despite presenting a structural disorganization, the samples were pillared. As evidenced by XRD increasing the basal spacing, specific area and uniform porosity by adsorption of N2. Regarding the microporous molecular sieves were synthesized zeolites A and NaP1 from a silico-aluminous residue, a byproduct of extracting lithium. The temperature and time of agitation during the synthesis were the most important factors for obtaining zeolite A. The aging of the gel and the highest crystallization time promoted the formation of zeolite NaP1 using a Si / Al ratio = 3.2

Selective sorption of mercury(II) from aqueous solution with an organically modified clay and its electroanalytical application

The organo-clay used in this work was prepared from a Na-montmorillonite (Wyoming-USA deposit) by treatment with water solution of hexadecyltrimethylammonium cations. As organo-clays exhibit strong sorptive capabilities for organic molecules, 2-mercapto-5-amino-1,3,4-thiadiazole organofunctional groups, with potential usefulness in chemical analysis, were incorporated on its solid surface. The physically adsorbed reagent did not present any restrictions in coordinating with several metal ions on the surface. The resultant organo-clay complex exhibited strong sorptive capability for removing mercury ions from water in which other metals and ions were also present. The purpose of this work is to study the selective separation of mercury(II) from aqueous solution using the organo-clay complex, measured by batch and chromatographic column techniques, and its application as preconcentration agent in a chemically modified carbon paste electrode for determination of mercury(II) in aqueous solution.

Curing depth of composite resin light cured by LED and halogen light-curing units

The purpose of this study was to evaluate the polymerization effectiveness of a composite resin (Z-250) utilizing microhardness testing. In total, 80 samples with thicknesses of 2 and 4 mm were made, which were photoactivated by a conventional halogen light-curing unit, and light-curing units based on LED. The samples were stored in water distilled for 24 h at 37C. The Vickers microhardness was performed by the MMT-3 microhardness tester. The microhardness means obtained were as follows: G1, 72.88; G2, 69.35; G3, 67.66; G4, 69.71; G5, 70.95; G6, 75.19; G7, 72.96; and G8, 71.62. The data were submitted to an analysis of variance (ANOVA's test), adopting a significance level of 5%. The results showed that, in general, there were no statistical differences between the halogen and LED light-curing units used with the same parameters.

Influence of light guide tip used in the photo-activation on degree of conversion and hardness of one nanofilled dental composite

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Estudo espectro eletroquímico de sistemas estruturados argila-corante

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Mineralogia de uma topossequência de solos desenvolvidos de material holocênico da região de Jequitaí, Estado de Minas Gerais

A região da Serra da Onça é localizada no nordeste do Estado de Minas Gerais, no vale formado pelos trabalhos dos rios São Francisco e seus afluentes Jequitaí e Rio das Velhas. Esta região é caracterizada por diversos ciclos erosivos. Uma topossequência representativa da área foi escolhida para este estudo, sendo constituida por 5 perfis de solos desenvolvidos de sedimentos Quaternários. 0 Perfil 1, um Typic Hapleustox, está localizado na superfície mais antiga. Os outros solos estão localizados no sedimento Holocênico, área aluvial do São Francisco. Estes solos são menos intemperizados e classificados como Plíntic Haplustult (Perfil 2), Oxic Plintaquult (Perfil 3); Fluventic Plinthustult (Perfil 4) e Fluventic Argiustol (Perfil 5). Análises mineralógicas foram efetuadas em todas as fraçõs do solo. O Perfil 1 apresenta, em sua fração areia, somente minerais resistentes ao intemperismo, enquanto que nos demais solos, menos intemperizados, ocorrem micas e plagioclásios. Tais minerais aumentam de acordo com a profundidade do solo e também do Perfil 1 ao Perfil 5 menos intemperizado. A caulinita é o mineral de argila dominante na fração argila de todos os solos estudados, com maior concentração no Perfil 1, mais intemperizado. Este mineral tende a decrescer em profundidade e na direção do Perfil 1. Micas, vermiculita e montmorilonita também ocorrem do Perfil 2 ao Perfil 5.

Caracterização e classificação de solos em uma topossequência sobre calcário na serra da Bodoquena, MS

A serra da Bodoquena, localizada no Estado do Mato Grosso do Sul, apresenta particularidades nos seus solos, que diferem de outras regiões do bioma cerrado-pantanal. Este trabalho teve como objetivo ampliar o conhecimento dos solos formados sobre calcário, por meio da caracterização dos seus atributos físicos, químicos, mineralógicos e da matéria orgânica. Foi selecionada uma topossequência sobre calcário, onde foram abertas trincheiras no topo (P1), terço inferior (P2), sopé (P3) e baixada (P4 e P5). Os perfis foram descritos morfologicamente e analisados os atributos físicos, químicos e mineralógicos dos horizontes. de acordo com o Sistema Brasileiro de Classificação de Solos, os solos estudados foram classificados como: (P1) Organossolo Fólico Sáprico lítico - OOs; (P2) Chernossolo Háplico Órtico típico - MXo; (P3) Chernossolo Argilúvico Órtico típico - MTo; (P4) Gleissolo Melânico Carbonático chernossólico - GMk1; e (P5) Gleissolo Melânico Carbonático organossólico - GMk2. Todos os perfis estudados apresentaram cores escuras nos horizontes superficiais e mais avermelhadas ou acinzentadas em profundidade, em razão da drenagem, sempre associados com elevados valores de saturação por bases e tendo o cálcio como cátion predominante no complexo sortivo. Das frações húmicas, a humina representou a maior fração do carbono orgânico em todos os solos. A análise mineralógica constatou a presença de calcita na fração areia nos perfis GMk1 e GMk2 e caulinita, illita e montmorilonita, na fração argila de todos os solos. A ocorrência do Organossolo Fólico em ambiente não altimontano, diferente do relatado pelo Sistema Brasileiro de Classificação de Solos, sugere maior amplitude das condições ambientais para a ocorrência dessa subordem.

Muscle strength assessment among children and adolescents with growing pains and joint hypermobility

OBJETIVO: Avaliar, por meio de teste quantitativo, a força muscular em crianças e adolescentes com dores de crescimento, associada ou não com hipermobilidade articular e comparadas com controles saudáveis. MÉTODO: Quarenta e sete casos de crianças e adolescentes acompanhados por dores de crescimento, sendo 24 com hipermobilidade articular (DC-HA), 23 sem hipermobilidade articular (DC) e 47 controles saudáveis pareados por idade e gênero foram submetidos a dois testes quantitativos para a avaliação da força muscular, o Childhood Myositis Assessment Scale (CMAS) e o Manual Muscle Strength Test (MMT). Os dados antropométricos como altura, peso, índice de massa corporal, prega cutânea tricipital, circunferência média do braço e a área muscular do braço foram comparados entre os três grupos. RESULTADOS: Os três grupos não apresentaram diferença estatística entre as medidas antropométricas. Houve diferença significante entre a mediana da pontuação do CMAS, sendo menores no grupo DC (47, mínimo e máximo 39-52) e DC-HA (46, mínimo e máximo 40-51), comparados com controles (50, mínimo e máximo 45-52; p<0,0001). Dois dos exercícios cronometrados do CMAS, a elevação da cabeça e a duração da elevação das pernas, tiveram menor pontuação nos pacientes comparados aos controles (p<0.0001). A pontuação mediana do MMT no grupo DC (79, mínimo e máximo 73-80) e DC-HA (78, mínimo e máximo 32-80) também apresentou diferença significante, sendo menor nos pacientes que nos controles (80, mínimo e máximo 78-80; p<0,0001). A melhor correlação entre a pontuação do CMAS e MMT foi no grupo DC-HA (Spearman r=0,65; p=0,0007). A aplicação do CMAS e MMT em duas ocasiões apresentou boa concordância e coeficiente de correlação intraclasse de 0,87 (IC 95% 0,64-0,96; p<0,0001) e 0,92 (IC 95% 0,76-0,97; p<0,0001), respectivamente. CONCLUSÃO: Os pacientes com dores de crescimento com ou sem hipermobilidade articular apresentaram fraqueza muscular de leve a moderada quando comparados com controles saudáveis.

Análise genética da concentração de potássio eritrocitário em bovinos

Red-cell potassium concentration was determined in five breeds of cattle: Brown Swiss, Nelore, Pitangueiras, Gir and Girolanda. All the cattle examined for the red cell potassium concentration presented low potassium concentration or LK type. This were divided in the following sub-types: low-low potassium concentration (LLK variation: 7.0 -15.9 m-equiv/l) in 16.9% of the animals; medium-low potassium concentration (MLK variation: 16.0 - 30.9 m-equiv/l) in 77% of animals and high-low potassium concentration (HLK variation: 31.0 - 50.0 m-equiv/l) in 6.1% of the animals. This results may be associated with a tropical environment because animals whith red-cell potassium concentration have advantage in this environment.