111 resultados para ICP-menetelmät

em Scielo Saúde Pública - SP


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As indicações para intervenção coronária percutânea (ICP) continuam a evoluir devido ao contínuo desenvolvimento da tecnologia, critérios de seleção mais amplos para pacientes e lesões e novas evidências advindas de testes clínicos. Uma controvérsia considerável foi gerada pelos resultados principais do estudo COURAGE (Clinical Outcomes Utilizing Revascularization and Aggressive Drug Evaluation), o qual não demonstrou diferenças no resultado em longo prazo para pacientes estáveis com doença coronariana, randomizados para uma estratégia inicial de ICP mais tratamento médico otimizado versus tratamento médico otimizado isolado. Em pacientes com angina estável crônica, o tratamento médico permanece sendo a pedra fundamental e deveria ser otimizado em todos os pacientes, enquanto os maiores objetivos alcançáveis da ICP são ter efeito sobre os sintomas, através de sua diminuição ou prevenção, reduzir a necessidade de procedimentos subsequentes e aliviar a isquemia. Em pacientes com doença arterial coronariana (DAC) estável, entretanto, nenhuma redução na incidência de morte ou infarto do miocárdio foi observada e essas limitações da ICP nesse cenário clínico precisam ser enfatizadas. A mensagem do estudo COURAGE pode ser refinada com base nos recentes sub-estudos nuclear e angiográfico, de forma que os pacientes com isquemia residual significante, submetidos a tratamento médico otimizado, deveriam ser considerados para tratamento com ICP, já que estão associados com maior probabilidade de morte e infarto do miocárdio. Entretanto, esses achados precisam ser confirmados por avaliação prospectiva antes de sua mais ampla aceitação pela comunidade intervencionista.

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The amounts of macro (P, K, Ca and Mg) and micronutrients (Cu and Zn) extracted with the Mehlich-1 (M1) solution, by the 1.0 mol L-1 KCl (KCl) and with the 0.1 mol L-1 HCl (HCl) for representative soil types of the Rio Grande do Sul state (Brazil) were compared with those extracted with the Mehlich-1 solution determined with the inductively coupled plasma optical emission spectroscopy (ICP). The amounts of nutrients extracted by the different methods showed high correlation coefficients. On average, the Mehlich-1 solution extracted similar amounts of P, determined with colorimetric and ICP methods, and, K determined with emission and ICP. The amounts of Ca and Mg extracted with the Mehlich-1 solution, determined by ICP, were similar to those extracted with the KCl solution determined by the atomic absorption spectrophotometry. The amounts of Cu and Zn extracted with the Mehlich-1 solution, determined by the ICP, were higher than those extracted with the 0.1 mol L-1 HCl determined by the atomic absorption spectrophotometry. The results indicate that the Mehlich-1 solution and ICP can be used for simultaneous multielement extraction and determination for Southern Brazilian soils. However, a conversion factor for values interpretation is needed. The use of the conversion factor to determine the K availability index in soils is adequate and does not affect the K recommendations for crops in southern Brazilian soils.

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A adoção do ICP para análise de fósforo tem apresentado controvérsias, pois o valor determinado por essa técnica, muitas vezes, não é comparável com o obtido por colorimetria. Nos EUA, alguns laboratórios apresentam restrições à adoção dessa técnica, pelas seguintes razões: as recomendações de adubação em uso foram desenvolvidas empregando-se o método colorimétrico para a determinação do P; e as diferenças significativas têm sido obtidas entre os teores determinados por colorimetria e por ICP, pois, devido à alta temperatura do plasma, o ICP mede outras formas de P além do ortofosfato, atribuída ao P orgânico na solução. Este estudo teve por objetivo comparar os teores de P extraído do solo pela solução de Mehlich-1, determinado por colorimetria (COL) e por ICP, em 595 amostras de solos do Estado do Rio Grande do Sul, com amplas variações nas características físicas, químicas e mineralógicas. Os teores de P extraído, determinado por ICP e por COL, não diferiram estatisticamente (r = 0,94; p < 0,001). Não foi observada diferença estatística entre os teores de P determinado pelas duas técnicas em solos com teores de P menores do que 30 mg dm-3. A diferença relativa (ICP/COL) não foi alterada pela textura, pelo teor de matéria orgânica, pelo pH e pelo índice SMP das amostras. As quantidades de P2O5 recomendadas para o milho tiveram alto grau de associação, e as doses não diferiram entre as técnicas de determinação. Com base nos resultados, pode-se concluir que a determinação do P disponível no solo, extraído pela solução de Mehlich-1, pode ser feita por ICP sem alterações nas tabelas de interpretação dos teores estabelecidos para o método colorimétrico, em solos do Estado do Rio Grande do Sul.

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O crescente interesse dos laboratórios brasileiros de análise de fertilidade de solos pela espectrometria de emissão óptica com plasma indutivamente acoplado (ICP OES) em detrimento da técnica de titrimetria deve-se à possibilidade da determinação simultânea de diferentes metais em uma ampla faixa de concentrações em extratos de interesse agronômico. Este estudo compara a precisão, reprodutibilidade e exatidão das duas técnicas de determinação de Ca, Mg e Al trocáveis extraídos com KCl 1 mol L-1 em amostras de solos. Foram analisadas 15 amostras de solos de referência, sendo três deles selecionados para avaliar a precisão e a reprodutibilidade das técnicas de determinação. A titrimetria e o ICP OES forneceram resultados mais reprodutíveis e precisos para a determinação de Ca, Mg e Al quando o extrato foi analisado sem diluição. As técnicas de determinação diferiram estatisticamente (p < 0,05) pelo teste de identidade aplicado para comparação dos resultados de Ca, Mg e Al. Nas condições testadas, não se recomenda o uso de ICP OES para as determinações de Ca, Mg e Al trocáveis em amostras de solos.

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An automatic dispenser based on a flow-injection system used to introduce sample and analytical solution into an inductively coupled plasma mass spectrometer through a spray chamber is proposed. Analytical curves were constructed after the injection of 20 to 750 µL aliquots of a multielement standard solution (20.0 µg L-1 in Li, Be, Al, V, Cr, Mn, Ni, Co, Cu, Zn, As, Se, Sr, Ag, Cd, Ba, Tl, Pb) and the acquisition of the integrated transient signals. The linear concentration range could be extended to ca. five decades. The performance of the system was checked by analyzing a NIST 1643d reference material. Accuracy could be improved by the proper selection of the injected volume. Besides good precision (r.s.d. < 2%), the results obtained with the proposed procedure were closer to the certified values of the reference material than those obtained by direct aspiration or by injecting 125 µL of several analytical solutions and samples.

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The multi-element determination of Al, Cr, Mn, Ni, Cu, Zn, Cd, Ba, Pb, SO4= and Cl- in riverine water samples was accomplished by inductively coupled plasma mass spectrometry (ICP-MS). The sample passed through a column containing the anionic resin AG1-X8 and the metals were determined directly. The retained anionic species were eluted and SO4= and Cl- were determined at m/z 48 and 35 correspondent to the ions SO+ and Cl+ formed at the plasma. Accuracy for metals was assessed by analysing the certified reference TM-26 (National Water Research Institute of Canada). Results for SO4= and Cl- were in agreement with those obtained by turbidimetry and spectrophotometry. LOD's of 0.1 µg l-1 for Cd, Ba and Pb; 0.2 µg l-1 for Al, Mn and Cu; 0.5 µg l-1 for Cr; 0.9 for Zn; 2.0 µg l-1for Ni , 60 µg l-1 for S and 200 µg l-1 Cl were attained.

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Results on the optimization of analytical methods for the determination of phosphorus in phosphino-polycarboxylate (PPCA), used frequently as scale inhibitor during oil production, by ICP-AES and ICP-MS are presented. Due to the complex matrix of production waters (brines) and their high concentration in inorganic phosphorus, the separation of organic phosphorus prior to its determination is necessary. In this work, minicolumns of silica immobilized C18 were used. Optimization of the separation step resulted in the following working conditions: (1) prewashing of the column with methanol (80% v/v); (2) use of a flow rate of 5 mL/min and 10 mL/min, respectively, for the preconditioning step and for percolation of the water sample; (3) final elution of organic phosphorus with 7 mL of buffer of H3BO3/NaOH (0.05 M, pH 9) with a flow rate of 1 mL/min. Sample detection limits (3s) for different combinations of nebulizers and spectrometric methods, based on 10 mL water aliquots, are: ICP-AES -Cross flow (47 mg/L) and Ultrasonic (18 mug/L); ICP-MS -Cross flow (1.2 mug/L), Cyclonic (0.7 mug/L) and Ultrasonic (0.5 mug/L). Typical recoveries of organic phosphorus are between 90 and 95% and the repeatability of the whole procedure is better than 10%. The developed methodology was applied successfully to samples from the oil-well NA 46, platform PNA 2, Campos basin, Brazil. Assessment of the PPCA inhibitor was possible at lower concentrations than achieved by current analytical methods, resulting in benefits such as reduced cost of chemicals, postponed oil production and lower environmental impacts.

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An on-line electrodissolution procedure implemented in a flow injection system for determination of copper, zinc and lead in brasses alloys by ICP-AES is described. Sample dissolution procedure was carried out by using a PTFE chamber and a DC power supply with constant current. Solid sample was attached to chamber as anode and a gold tubing coupled in the chamber was used as cathode. An electrolytic solution flowing through the gold tubing closed the electric circuit with sample, in order to provide condition for electric dissolution when the DC power supply was switched on. The best results were achieved by using a 1.5 mol l-1 nitric acid solution as electrolyte and a 2.5 A current intensity. The procedure presented a good performance characterized by a relative standard deviation better than < 5% (n=5) and a sample throughput of 180 determinations per hour for Cu, Zn and Pb. Results were in agreement with those obtained by conventional acid dissolution (99% confidence level).

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The salt accumulation process in some reservoirs of regular and irregular use (from 10 to 50 years of constrution), located in the Southeast of Bahia State was evaluated. Inductively coupled plasma atomic emission spectrometry was used to evaluate the concentrations of Na, K, Ca and Mg in water samples from inside and upstream of the reservoirs. The results showed that for reservoirs of irregular use, the salt accumulation, indicated by the tracer Na, increases with the age of the reservoirs, however for the reservoirs of regular use the hydraulic retention time is the main parameter.

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Different methods have been applied to solve special problems of metal analysis. First, the solid samples of tool steels were analyzed by X-ray fluorescence. Alternatively, an on-line electrodissolution implemented in a flow injection system and conventional dissolution procedure for determination of W, Mo, V and Cr in tool steels by ICP-AES is described. The resulting analyte solutions were compared with conventional dissolution procedure and determination by ICP-AES. The electrolytic procedure presented a good performance characterized by a sample throughput of 164 determinations per hour. Results were in agreement with those obtained by conventional acid dissolution.

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Inductively Coupled Plasma Optical Emission Spectrometry was used to determine Ca, Mg, Mn, Fe, Zn and Cu in samples of processed and natural coconut water. The sample preparation consisted in a filtration step followed by a dilution. The analysis was made employing optimized instrumental parameters and the results were evaluated using methods of Pattern Recognition. The data showed common concentration values for the analytes present in processed and natural samples. Principal Component Analysis (PCA) and Hierarchical Cluster Analysis (HCA) indicated that the samples of different kinds were statistically different when the concentrations of all the analytes were considered simultaneously.

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The levels of several chemical elements were determined simultaneously in ten different beers of the Venezuelan market by ICP-OES. With the exception of chromium, beer does not provide important amounts of nutritional oligoelements. The average chromium content found (33 µg/L) is higher than one reported for USA's beer (10 µg/L) but smaller than another reported for Brazilian beer (66 µg/L). The average percentage of chromium RDA by beer consumption found for Venezuela (6.3%) is similar to that reported for Belgium (5%). Regarding toxic elements, one of the samples contained an elevated amount of aluminium, probably dissolved from the aluminium can.

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A method for selective determination of tributyltin in the presence of Sn(IV) by combining hydride generation inductively coupled plasma optical emission spectrometry (HG-ICP OES) and solid phase extraction (SPE) using baker's yeast is proposed. The procedure is based on selective retention of TBT by the yeast at pH = 6. Detection limit of 1.9 µg L-1 and quantification limit of 6.3 µg L-1 were obtained. TBT and San(IV) were determined in the range of 0-25 µg L-1 and the proposed approach was applied to analyze river water, sea water and biological extracts, with recoveries of 114, 101 and 86%, respectively.

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A study of the partial USEPA 3050B and total ISO 14869-1:2001 digestion methods of sediments was performed. USEPA 3050B was recommended as the simpler method with less operational risk. However, the extraction ability of the method should be taken in account for the best environmental interpretation of the results. FAAS was used to quantify metal concentrations in sediment solutions. The alternative use of ICP-OES quantification should be conditioned by a previous detailed investigation and eventual correction of the matrix effect. For the first time, the EID method was employed for the detection and correction of the matrix effect in sediment ICP-OES analysis. Finally, some considerations were made about the level of metal contamination in the area under study.

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The performance of inductively-coupled plasma optical emission spectrometers with axial and radial views for determination of iodine in table salt was evaluated. Interference and memory effects in nitric acid and water-soluble tertiary amines (CFA-C) media were studied. Based on a factorial experiment, one optimum instrument operational condition for axial configuration, and two optima conditions for radial configuration was established. The ICP OES with axial view was 5-fold more sensitive than the radial view. Both matrix matching and standard addition methods were used for iodine quantification and for most samples, both strategies of calibration led to similar results. Recoveries ranged from 104 to 114%.