Análise por meio de espectroscopia de emissão óptica das espécies ativas em nitretação iônica e gaiola catódica

Plasma process like ionic nitriding and cathodic cage plasma nitriding are utilized in order to become hard surface of steels. The ionic nitriding is already accepted in the industry while cathodic cage plasma nitriding process is in industrial implementation stage. Those process depend of plasma parameters like electronic and ionic temperature (Te, Ti), species density (ne, ni) and of distribution function of these species. In the present work, the plasma used to those two processes has been observed through Optical Emission Spectroscopy OES technique in order to identify presents species in the treatment ambient and relatively quantify them. So plasma of typical mixtures like N2 H2 has been monitored through in order to study evolution of those species during the process. Moreover, it has been realized a systematic study about leaks, also thought OES, that accomplish the evolution of contaminant species arising because there is flux of atmosphere to inside nitriding chamber and in what conditions the species are sufficiently reduced. Finally, to describe the physic mechanism that acts on both coating techniques ionic nitriding and cathodic cage plasma nitriding

Diagnóstico de descarga de cátodo oco de ar e pós-descarga Ar N2 por espectroscopia de emissão óptica e espectrometria de massa

Many applications require that the plasma discharge is produced apart from the surface to be processed, thus preventing damage caused by bombardment and/or plasma radiation. In the post-discharge regime in various applications thermally sensitive materials can be used. In this work, active species produced by discharge and post-discharge hollow cathode were diagnosed by optical emission spectroscopy and mass spectrometry. The discharge was produced with the gases Ar and Ar - N2 gas flow ranging from 1 to 6 cm3/min and electric current between 150 to 600 mA. It was estimated that the ion density inside the hollow cathode, with 2 mm diameter ranged between 7.71 and 14.1 x 1015 cm-3. It was observed that the gas flow and the electric current changes the emission intensity of Ar and N2 species. The major ionic species detected by quadrupole mass spectrometry were Ar+ and N2+. The ratio of optical emission intensities of N2(1 +)/Ar(811 nm) was related to the partial pressure of N2 after the hollow cathode discharge at low pressure

Análise por meio de espectroscopia de emissão óptica das espécies ativas em nitretação iônica e gaiola catódica

Plasma process like ionic nitriding and cathodic cage plasma nitriding are utilized in order to become hard surface of steels. The ionic nitriding is already accepted in the industry while cathodic cage plasma nitriding process is in industrial implementation stage. Those process depend of plasma parameters like electronic and ionic temperature (Te, Ti), species density (ne, ni) and of distribution function of these species. In the present work, the plasma used to those two processes has been observed through Optical Emission Spectroscopy OES technique in order to identify presents species in the treatment ambient and relatively quantify them. So plasma of typical mixtures like N2 H2 has been monitored through in order to study evolution of those species during the process. Moreover, it has been realized a systematic study about leaks, also thought OES, that accomplish the evolution of contaminant species arising because there is flux of atmosphere to inside nitriding chamber and in what conditions the species are sufficiently reduced. Finally, to describe the physic mechanism that acts on both coating techniques ionic nitriding and cathodic cage plasma nitriding

Pré-concentração de cádmio com Saccharomyces cerevisiae e determinação em águas fluviais usando espectrometria de emissão óptica com plasma indutivamente acoplado

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

Espectrometria de emissão óptica com plasma indutivamente acoplado aliada à quimiometria na determinação de íons metálicos no molusco Mytella falcata para discriminação de estuários potiguares

This work examined the possibility of using mussel Mytella falcata as bioindicator sample to detect metal ions in several estuaries potiguares, since species substances that accumulate in their tissues due to its characteristics filter feeders have been used for environmental monitoring. The chemometrics by principal components analysis was used to reduce the size of the original data in order to establish a pattern of distribution of metal ion. Samples were collected at three different points in the estuaries Curimataú, Guaraíra-Papeba, Potengi, Galinhos-Guamaré and Piranhas-Assu having been marked with the location using GPS (Global Positioning System). The determination of humidity content and digestion of the samples were performed using methods described in the Compendium of analytical standards of the Institute Adofo Lutz (2005) and the determination of metal ions of the elements Al, Ba, Cd, Cr, Cu, Mn, Ni, Pb, Sn and Zn were performed by optical emission spectrometry with inductively coupled plasma as described by USEPA method 6010C. The results show that it is possible to use this molluscum Mytella falcata in the estuaries of Rio Grande do Norte for the determination of metal ions. The data were subjected to principal components analysis (PCA) which enabled us to verify the distribution pattern of the metal ions studied in several estuaries potiguares and group them according to the metal ions in common with and relate them to the activities in each region

Decomposição de argilas em forno de microondas e determinação simultânea dos seus constituintes principais por espectrometria de emissão óptica em plasma indutivamente acoplado

ANALYSIS OF CLAYS BY INDUCTIVELY COUPLED PLASMA OPTICAL EMISSION SPECTROMETRY AFTER CLOSED-VESSEL MICROWAVE-ASSISTED ACID DECOMPOSITION. In this work a closed-vessel microwave-assisted acid decomposition procedure for clays was developed. Aluminum, Ca, Fe, K, Mg, Na, Si, and Ti were determined in clay digestates by inductively coupled plasma optical emission spectrometry. The most critical parameter for total decomposition of clays was the composition of the reagent mixture. The applied power and the heating time exerted a less critical influence. Best decomposition conditions were attained using a reagent mixture containing 4 mL aqua regia plus 3 mL HF and the heating program was implemented in 12 min. The accuracy of the results was demonstrated using two standard reference materials and a paired t-test showed a good agreement between determined and certified values at a 95% confidence level.

Metodologia para determinação de arsênio, antimônio e bismuto por espectrometria de emissão óptica com fonte de plasma acoplado indutivamente (ICPOES) e geração de hidretos aplicada à rochas

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

DETERMINAÇÃO DE ARSÊNIO, ANTIMÔNIO E BISMUTO EM ROCHAS POR ESPECTROMETRIA DE EMISSÃO ÓPTICA COM FONTE DE PLASMA ACOPLADO INDUTIVAMENTE (ICP-OES) E GERAÇÃO DE HIDRETOS

No presente trabalho descreve-se o método para determinação de arsênio, antimônio e bismuto em materiais geológicos, utilizando a geração de hidretos acoplado ao ICP-OES, que proporciona a determinação, com exatidão, dos elementos de interesse em concentrações abaixo de 1 ppm. O método é sensível e, por isso, está sujeito a interferências, como as causadas por elementos presentes na matriz. Desenvolveu-se uma técnica de dissolução eficiente e foram realizados diversos tratamentos com dopagens de soluções-padrão e testes com o uso de tiouréia e iodeto de potássio com ácido ascórbico em diferentes concentrações, com o objetivo de minimizar possíveis interferências presentes na matriz. Os resultados finais, mediante a dissolução de material geológico de referência internacional na determinação de arsênio, bismuto e antimônio, mostraram recuperações superiores à 97% em amostras com concentrações abaixo de 1 ppm.

Estudo de temperatura de plasma de álcool através de espectroscopia de emissão natural radical C2*

Non-intrusive methods of diagnosis, such as spectral analysis of the radiation emitted by the system, have been used as a viable alternative for determining the temperature of combustion systems. Among them, the determination of temperature by natural emission spectroscopy has the advantage of requiring relatively simple experimental devices. Once Chemiluminescent species are formed directly in the excited state, the collection and recording of radiation emission spectrum is enough to determine the temperature (CARINHANA, 2008). In this study we used the process of making direct comparisons between the experimental spectra obtained in the laboratory from the plasma of alcohol, and the theoretical spectra plotted from a computer program developed at the IEAv. The objective was to establish a fast and reliable method to measure the rotational temperature of the radical C2*. The results showed that the temperature of the plasma, which in turn can be taken as the rotational temperature of the system, is proportional to the pressure. The temperature values ranged from ca. 2300 ~ 2500 K at a pressure of 19 mmHg to 3100 ~ 3500 K for the pressure of 46 mmHg. The temperature values are somewhat smaller when we consider the theoretical spectrum as a Lorentzian curve. The overlap of the spectra was better when using the profile curve, but still were not exactly superimposed. The solution to improve the overlap of the theoretical with the experimental spectra is the use of a curve that has the convolution of two profiles analyzed: Lorentzian and Gaussian. This curve is called the Voigt profile, which will also be implemented by programmers and studied in a next work

Determinação de metais em óleos lubrificantes utilizando a técnica de espectrometria de emissão óptica com plasma induzido por laser

IPEN/D

Pré-concentração de cádmio com Saccharomyces cerevisiae e determinação em águas fluviais usando espectrometria de emissão óptica com plasma indutivamente acoplado

A preconcentration method based on the use of Saccharomyces cerevisiae as sorbent material is proposed for the determination of Cd(II) in river water. The solid phase extraction was performed in batch mode and the determination of the analyte in the solid phase was easily carried out by introducing a slurry of the yeast (0.0625 g / 2.5 mL) directly into the ICP OES. A limit of detection of 0.11 µg L-1 and a sample throughput in the range of 4 - 54 sample h-1 were obtained. Determinations of cadmium in a certified sample and in real river water samples were in excellent agreement with the expected values.

Determinação de As, Sb e Se em material agronômico por espectrometria de emissão óptica acoplada a plasma induzido com geração de hidretos (HG-ICP OES).

2005

Tratamento termoquímico do titânio auxiliado por plasma de ar - N2 - O2

Discs were grade II cp Ti oxynitride by plasma of Ar - N2 - O2 using different proportions of individual gases. These ratios were established from analysis of optical emission spectroscopy (OES) of plasma species. The proportions that resulted in species whose spectra showed an abrupt change of light intensity were chosen for this study. Nanohardness tests revealed that there was a correlation between the intensity of N2 + species with the hardness, because the treatments where they had a higher intensity, obtained a higher value nanohardness, although the crystalline phases have remained unchanged. With respect to topography, it was observed that in general, the surface roughness is related to the intensities of plasma species, because they may have different values depending on the behavior of the species. Images obtained by optical microscopy revealed a surface with grains of different colors to optical reflectance showed a peak of reflection in the red area. Measures the contact angle and surface tension showed hydrophilic properties and hydrophilic with little variation of polar and dispersive components of surface tension

Influência das espécies ativas na absorção de intersticiais durante a carbonitretação a plasma do TI

Physical-chemical properties of Ti are sensible to the presence of interstitial elements. In the case of thermochemical treatments plasma assisted, the influence of different active species is not still understood. In order to contribute for such knowledge, this work purposes a study of the role played by the active species atmosphere into the Ar N2 CH4 carbonitriding plasma. It was carried out a plasma diagnostic by OES (Optical Emission Spectroscopy) in the z Ar y N2 x CH4 plasma mixture, in which z, y and x indexes represent gas flow variable from 0 to 4 sccm (cm3/min). The diagnostic presents abrupt variations of emission intensities associated to the species in determined conditions. Therefore, they were selected in order to carry out the chemical treatment and then to investigate their influences. Commercial pure Ti disks were submitted to plasma carbonitriding process using pre-established conditions from the OES measurements while some parameters such as pressure and temperature were maintained constant. The concentration profiles of interstitial elements (C and N atoms) were determined by Resonant Nuclear Reaction Analysis (NRA) resulting in a depth profile plots. The reactions used were 15N(ρ,αγ)12C and 12C(α,α)12C. GIXRD (Grazing Incidence X-Ray Diffraction) analysis was used in order to identify the presence of phases on the surface. Micro-Raman spectroscopy was used in order to qualitatively study the carbon into the TiCxN1 structure. It has been verified which the density species effectively influences more the diffusion of particles into the Ti lattice and characteristics of the layer formed than the gas concentration. High intensity of N2 + (391,4 nm) and CH (387,1 nm) species promotes more diffusion of C and N. It was observed that Hα (656,3 nm) species acts like a catalyzer allowing a deeper diffusion of nitrogen and carbon into the titanium lattice.

Influência dos parâmetros de processo na deposição de nitreto de titânio por plasma em gaiola catódica

Titanium nitride films were grown on glass using the Cathodic Cage Plasma Deposition technique in order to verify the influence of process parameters in optical and structural properties of the films. The plasma atmosphere used was a mixture of Ar, N2 and H2, setting the Ar and N2 gas flows at 4 and 3 sccm, respectively and H2 gas flow varied from 0, 1 to 2 sccm. The deposition process was monitored by Optical Emission Spectroscopy (OES) to investigate the influence of the active species in plasma. It was observed that increasing the H2 gas flow into the plasma the luminescent intensities associated to the species changed. In this case, the luminescence of N2 (391,4nm) species was not proportional to the increasing of the H2 gas into the reactor. Other parameters investigated were diameter and number of holes in the cage. The analysis by Grazing Incidence X-Ray Diffraction (GIXRD) confirmed that the obtained films are composed by TiN and they may have variations in the nitrogen amount into the crystal and in the crystallite size. The optical microscopy images provided information about the homogeneity of the films. The atomic force microscopy (AFM) results revealed some microstructural characteristics and surface roughness. The thickness was measured by ellipsometry. The optical properties such as transmittance and reflectance (they were measured by spectrophotometry) are very sensitive to changes in the crystal lattice of the material, chemical composition and film thicknesses. Therefore, such properties are appropriate tools for verification of this process control. In general, films obtained at 0 sccm of H2 gas flow present a higher transmittance. It can be attributed to the smaller crystalline size due to a higher amount of nitrogen in the TiN lattice. The films obtained at 1 and 2 sccm of H2 gas flow have a golden appearance and XRD pattern showed peaks characteristics of TiN with higher intensity and smaller FWHM (Full Width at Half Maximum) parameter. It suggests that the hydrogen presence in the plasma makes the films more stoichiometric and becomes it more crystalline. It was observed that with higher number of holes in the lid of the cage, close to the region between the lid and the sample and the smaller diameter of the hole, the deposited film is thicker, which is justified by the most probability of plasma species reach effectively the sample and it promotes the growth of the film