An electroanalytical application of 2-aminothiazole-modified silica gel after adsorption and separation of Hg(II) from heavy metals in aqueous solution

2-Aminothiazole covalently attached to a silica gel surface was prepared in order to obtain an adsorbent for Hg(II) ions having the following characteristics: good sorption capacity, chemical stability under conditions of use, and, especially, high selectivity. The accumulation voltammetry of mercury(II) was investigated at a carbon paste electrode chemically modified with silica gel functionalized with 2-aminothiazole (SIAMT-CPE). The repetitive cyclic voltammogram of mercury(II) solution in the potential range -0.2 to + 0.6 V versus Ag/AgCl (0.02 mol L-1 KNO3; V = 20 mV s(-1)) show two peaks one at about 0.1 V and other at 0.205 V. The anodic wave peak at 0.205 V is well defined and does not change during the cycles and it was therefore further investigated for analytical purposes using differential pulse anodic stripping voltammetry in differents supporting electrolytes. The mercury response was evaluated with respect to pH, electrode composition, preconcentration time, mercury concentration, cleaning solution, possible interferences and other variables. The precision for six determinations (n = 6) of 0.02 and 0.20 mg L-1 Hg(II) was 4.1 and 3.5% (relative standard deviation), respectively. The detection limit was estimated as 0.10 mu g L-1 mercury(II) by means of 3:1 current-to-noise ratio in connection with the optimization of the various parameters involved and using the highest-possible analyser sensitivity. (c) 2006 Elsevier Ltd. All rights reserved.

Estudos de Durabilidade Frente ao Ataque Ácido de Compósitos Portland-Polímero para Cimentação de Poços de Petróleo

Portland-polymers composites are promising candidates to be used as cementing material in Northeastern oil wells of Brazil containing heavy oils submitted to steam injection. In this way, it is necessary to evaluate its degradation in the commonly acidizind agents. In addition, to identify how aggressive are the different hostile environments it is an important contribution on the decision of the acidic systems to be used in. It was investigated the performance of the Portland-polymer composites using powdered polyurethane, aqueous polyurethane, rubber tire residues and a biopolymer, those were reinforced with polished carbon steel SAE 1045 to make the electrochemical measurements. HCl 15,0 %, HCl 6,0 % + HF 1,5 % (soft mud acid), HCl 12,0 % + HF 3,0 % (regular mud acid) and HAc 10 % + HF 1,5 % were used as degrading environment and electrolytes. The more aggressive acid solution to the plain Portland hardened cement paste was the regular mud acid, that showed loss of weight around 23.0 %, followed by the soft mud acid, the showed 11.0 %, 15.0 % HCl with 7,0 % and, at last the 10.0 % HAc plus HF 1.5 % with just 1.0 %. The powdered polyurethane-composite and the aqueous polyurethane one showed larger durability, with reduction around 87.0 % on the loss of weight in regular mud acid. The acid attack is superficial and it occurs as an action layer, where the degraded layer is responsible for the decrease on the kinetic of the degrading process. This behavior can be seen mainly on the Portland- aqueous polyurethane composite, because the degraded layer is impregnated with chemically modified polymer. The fact of the acid attack does not have influence on the compressive strength or fratography of the samples, in a general way, confirms that theory. The mechanism of the efficiency of the Portland-polymers composites subjected to acid attack is due to decreased porosity and permeability related with the plain Portland paste, minor quantity of Ca+2, element preferentially leached to the acidic solution, wave effect and to substitute part of the degrading bulk for the polymeric one. The electrolyte HAc 10 % + HF 1,5 % was the least aggressive one to the external corrosion of the casing, showing open circuit potentials around +250 mV compared to -130 mV to the simulated pore solution to the first 24 hours immersion. This behavior has been performed for two months at least. Similar corrosion rates were showed between both of the electrolytes, around 0.01 μA.cm-2. Total impedance values, insipient arcs and big polarization resistance capacitive arcs on the Nyquist plots, indicating passivity process, confirm its efficiency. In this way, Portlandpolymers composites are possible solutions to be succeed applied to oilwell cementing concomitant submitted to steam injection and acidizing operation and the HAc 10,0 % + HF 1,5 % is the less aggressive solution to the external corrosion of the casing

Nitretação em plasma com gaiola catódica: investigação do mecanismo e estudo comparativo com a nitretação em plasma de tensão contínua

The ionic plasma nitriding is one of the most important plasma assisted treatment technique for surface modification, but it presents some inherent problems mainly in nitriding pieces with complex geometries. In the last four years has appeared a plasma nitriding technique, named ASPN (Active Screen Plasma Nitriding) in which the samples and the workload are surrounded by a metal screen on which the cathodic potential is applied. This new technique makes possible to obtain a perfect uniform nitrided layer apart from the shape of the samples. The present work is based on the development of a new nitriding plasma technique named CCPN (Cathodic Cage Plasma Nitriding) Patent PI 0603213-3 derived from ASPN, but utilizes the hollow cathode effect to increase the nitriding process efficiency. That technique has shown great improvement on the treatment of several types of steels under different process conditions, producing thicker and harder layers when compared with both, ASPN and ionic plasma nitriding, besides eliminating problems associated with the later technique. The best obtained results are due to the hollow cathode effect on the cage holes. Moreover, characteristic problems of ionic plasma nitriding are eliminated due to the fact that the luminescent discharge acts on the cage wall instead of on the samples surface, which remains under a floating potential. In this work the enhancement of the cathodic cage nitriding layers proprieties, under several conditions for some types of steels was investigated, besides the mechanism for nitrides deposition on glass substrate, concluding that the CCPN is both a diffusion and a deposition process at the same time

New search for the Neutron Electric Dipole Moment using ultracold neutrons at the Spallation Neutron Source

This document introduces the planned new search for the neutron Electric Dipole Moment at the Spallation Neutron Source at the Oak Ridge National Laboratory. A spin precession measurement is to be carried out using Ultracold neutrons diluted in a superfluid Helium bath at T = 0.5 K, where spin polarized 3He atoms act as detector of the neutron spin polarization. This manuscript describes some of the key aspects of the planned experiment with the contributions from Caltech to the development of the project.

Techniques used in the design of magnet coils for Nuclear Magnetic Resonance were adapted to the geometry of the experiment. Described is an initial design approach using a pair of coils tuned to shield outer conductive elements from resistive heat loads, while inducing an oscillating field in the measurement volume. A small prototype was constructed to test the model of the field at room temperature.

A large scale test of the high voltage system was carried out in a collaborative effort at the Los Alamos National Laboratory. The application and amplification of high voltage to polished steel electrodes immersed in a superfluid Helium bath was studied, as well as the electrical breakdown properties of the electrodes at low temperatures. A suite of Monte Carlo simulation software tools to model the interaction of neutrons, 3He atoms, and their spins with the experimental magnetic and electric fields was developed and implemented to further the study of expected systematic effects of the measurement, with particular focus on the false Electric Dipole Moment induced by a Geometric Phase akin to Berry’s phase.

An analysis framework was developed and implemented using unbinned likelihood to fit the time modulated signal expected from the measurement data. A collaborative Monte Carlo data set was used to test the analysis methods.

Avaliação de inibidores verdes microemulsionados na inibição à corrosão do aço carbono AISI 1020

In general, among the corrosion inhibitors surfactants are the most commonly used compounds, because they are significantly effective by forming protective films on anodic and cathodic areas. In this study, microemulsions containing he biodegradable saponified coconut oil as surfactant (SME-OCS) was used as green corrosion inhibitors. With this purpose, methanolic extracts of Ixora coccinea Linn (IC) and a polar fraction rich in alkaloids (FA) obtained from Croton cajucara Benth solubilized in the SME-OCS system were examined in the presence of AISI 1020 carbon steel, in saline solution (NaCl 3,5 %). The efficiency of corrosion inhibition of IC and FA were evaluated in the following microemulsions: SME-OCS-IC and SME-OCS-FA. The microemulsion system SME-OCS in the presence and absence of IC and FA was assessed by measurements of weight loss and the electrochemical method of polarization resistance, with variation in the concentration of IC and FA (50 - 400 ppm), showing significant results of corrosion inhibition (83,6 % SME-OCS; 92,2 % SME-OCS-FA; and 95,3 % SME-OCS-IC)

Utilização de matérias primas vegetais para aplicabilidade como inibidores de corrosão

In the search for products that act as corrosion inhibitors and do not cause environmental, impact the use of plant extracts as corrosion inhibitors is becoming a promising alternative. In this work the efficiency of polar extracts (ethanol extracts) obtained from the plants Anacardium occidentale Linn (AO) and Phyllantus amarus Schum. & Thonn (PA) as corrosion inhibitors were evaluated in different concentrations. For that AO and PA extracts were solubilized in the microemulsion systems (SME) containing saponified coconut oil as surfactant (SME -OCS and SME-OCS-1) in saline (NaCl 3,5 %) solution, which was also used as electrolyte. Both SME-OCS and SME-OCS-1 were characterized by surface tension and viscosity methods showing a Newtonian fluid behavior. The SME-OCS and SME-OCS-1 systems satisfactorily solubilized the polar extracts AO and PA with measurements carried out by ultraviolet spectroscopy. The measurements of corrosion inhibition efficiencies were performed by the electrochemical linear polarization resistance (LPR) technique as well as weight loss, on the surface of AISI 1020 carbon steel. The maximum corrosion inhibition efficiencies were determined by extrapolation of Tafel plots, showing the following values: 95,6 % for the system SME-OCS-AO, 98,9 % for the system SME-OCS-AO-1 and 93,4 % for the system SME-OCS-PA

Avaliação do efeito de particulados sólidos na eficiência de um inibidor de corrosão recomendado para meios salinos com CO2

The main problem on the exploration activity on petroleum industry is the formation water resulted on the fields producing. The aggravating of this problem is correlated with the advancing technologies used on the petroleum extractions and on its secondary approach objecting the reobtainment of this oil. Among the main contaminants of the water formation are corrosives gases such as: O2, CO2 and H2S, some solids in suspension and dissolved salts. Concerning to those gases the CO2 is the one that produce significant damage for carbon steel on corrosion process of the petroleum and gas industries. Corrosion inhibitors for carbon steel in formation water is one of the most used agents in control of those damages. In this context, the poor investigations of carbon steel corrosion proceeding from solids in suspension is an opened field for studies. On this work the inhibitor effect of the commercial CORRTREAT 703 was evaluated on some specific solids in suspension at saline medium containing 10.000 ppm of de-aerated chloride using CO2 until non oxygen atmosphere been present. For that, quartz, calcium carbonate, magnetite and iron sulphide were subjected to this investigation as the selected solids. The effect of this inhibitor on corrosion process correlated with those specific solids, was measured using electrochemical (resistance of linear polarization and galvanic pair) and gravimetrical techniques. During all the experimental work important parameters were monitored such as: pH, dissolved oxygen, temperature, instantaneous corrosion rate and galvanic current. According to the obtained results it was proved that the suspension solids calcium carbonate and iron sulphide decrease the corrosion process in higher pH medium. Meanwhile the quartz and magnetite been hardness increase corrosion by broking of the passive layer for erosion. In the other hand, the tested inhibitor in concentration of 50 ppm, showed to be effective (91%) in this corrosion process

Avaliação da espécie vegetal Croton cajucara Benth como inibidor de biocorrosão em aço carbono Aisi 1020

Actually in the oil industry biotechnological approaches represent a challenge. In that, attention to metal structures affected by electrochemical corrosive processes, as well as by the interference of microorganisms (biocorrosion) which affect the kinetics of the environment / metal interface. Regarding to economical and environmental impacts reduction let to the use of natural products as an alternative to toxic synthetic inhibitors. This study aims the employment of green chemistry by evaluating the stem bark extracts (EHC, hydroalcoholic extract) and leaves (ECF, chloroform extract) of plant species Croton cajucara Benth as a corrosion inhibitor. In addition the effectiveness of corrosion inhibition of bioactive trans-clerodane dehydrocrotonin (DCTN) isolated from the stem bark of this Croton was also evaluated. For this purpose, carbon steel AISI 1020 was immersed in saline media (3,5 % NaCl) in the presence and absence of a microorganism recovered from a pipeline oil sample. Corrosion inhibition efficiency and its mechanisms were investigated by linear sweep voltammetry and electrochemical impedance. Culture-dependent and molecular biology techniques were used to characterize and identify bacterial species present in oil samples. The tested natural products EHC, ECF and DCTN (DMSO as solvent) in abiotic environment presented respectively, corrosion inhibition efficiencies of 57.6% (500 ppm), 86.1% (500 ppm) and 54.5% (62.5 ppm). Adsorption phenomena showed that EHC best fit Frumkin isotherm and ECF to Temkin isotherm. EHC extract (250 ppm) dissolved in a polar microemulsion system (MES-EHC) showed significant maximum inhibition efficiency (93.8%) fitting Langmuir isotherm. In the presence of the isolated Pseudomonas sp, EHC and ECF were able to form eco-compatible organic films with anti-corrosive properties

Sistema de instrumentação mecanizada Hyflex EDM

A Endodontia é uma área em constante evolução. Consideráveis desenvolvimentos nos materiais e técnicas têm sido essenciais para o melhoramento dos resultados nos tratamentos realizados. É exemplo disso mesmo a constituição dos instrumentos Endodônticos primordiais, construídos em cordas de piano, com evolução para aço de carbono, material este que sofria corrosão provocado pelo cloro presente no hipoclorito de sódio. O aço de carbono evoluiu para aço inoxidável e deste as limas endodônticas passaram a ser feitas em níquel-titânio, conferindo-lhes melhor flexibilidade e efeito de memória de forma. Mesmo com todas estas melhorias significativas, fraturas de instrumentos e erros durante a instrumentação continuam a acontecer e com eles veio a necessidade da pesquisa de possíveis melhorias da constituição das limas em NiTi. Como resultado surgiram ligas como o M-wire, fase-R e CM-wire, criadas a partir de tratamentos térmicos, que trouxeram às limas Endodônticas maior flexibilidade e resistência à fratura que os instrumentos feitos em NiTi convencional. A mais recente evolução das limas Ni-Ti, desenvolvida pela Coltene Whaldent (Allstätten, Suiça), são as limas Hyflex EDM, limas para canais radiculares de 5ª geração. O seu processo de fabrico por eletroerosão cria uma superfície única fazendo com que estas limas sejam mais duras e resistam mais à quebra, aliado à sua alta flexibilidade. É possível assim reduzir o número de limas para a limpeza e modelagem dos canais durante os tratamentos endodônticos sem comprometer a preservação da anatomia dos canais. As limas Hyflex EDM possuem, tal como as limas Hyflex CM, o efeito de controle de memória (CM), o que confere propriedades muito similares entre os dois sistemas.

Low temperature synthesis of carbon nanotubes on indium tin oxide electrodes for organic solar cells

The electrical performance of indium tin oxide (ITO) coated glass was improved by including a controlled layer of carbon nanotubes directly on top of the ITO film. Multi-wall carbon nanotubes (MWCNTs) were synthesized by chemical vapor deposition, using ultra-thin Fe layers as catalyst. The process parameters (temperature, gas flow and duration) were carefully refined to obtain the appropriate size and density of MWCNTs with a minimum decrease of the light harvesting in the cell. When used as anodes for organic solar cells based on poly(3-hexylthiophene) (P3HT) and phenyl-C61-butyric acid methyl ester (PCBM), the MWCNT-enhanced electrodes are found to improve the charge carrier extraction from the photoactive blend, thanks to the additional percolation paths provided by the CNTs. The work function of as-modified ITO surfaces was measured by the Kelvin probe method to be 4.95 eV, resulting in an improved matching to the highest occupied molecular orbital level of the P3HT. This is in turn expected to increase the hole transport and collection at the anode, contributing to the significant increase of current density and open circuit voltage observed in test cells created with such MWCNT-enhanced electrodes.

Bond strength of steel hollow sections using carbon fibre reinforced polymer composites

This research was a step forward in developing bond strength of CFRP strengthened steel hollow sections under tension loads. The studies have revealed the ultimate load carrying capacity of the CFRP strengthened steel hollow sections and the stress distribution for different orientations of the CFRP sheet at different layers. This thesis presents a series of experimental and finite element analysis to determine a good understanding of the bond characteristics of CFRP strengthened steel hollow sections.

The large-scale production of graphene flakes using magnetically-enhanced arc discharge between carbon electrodes

A novel approach to large-scale production of high-quality graphene flakes in magnetically-enhanced arc discharges between carbon electrodes is reported. A non-uniform magnetic field is used to control the growth and deposition zones, where the Y-Ni catalyst experiences a transition to the ferromagnetic state, which in turn leads to the graphene deposition in a collection area. The quality of the produced material is characterized by the SEM, TEM, AFM, and Raman techniques. The proposed growth mechanism is supported by the nucleation and growth model.