Development of a flotation method for preconcentration-separation of trace amounts of some metal ions in plant tissues prior to their FAAS determinations

An efficient flotation method based on the combination of flame atomic absorption spectrometry (FAAS) and separation and preconcentration step for determination of Cr3+, Cu 2+, Co2+, Ni2+, Zn2+, Cd 2+, Fe3+ and Pb2+ ions in various real samples by the possibility of applying bis(2-hydroxyacetophenone)-1,4-butanediimine (BHABDI) as a new collector was studied. The influence of pH, amount of BHABDI as collector, sample matrix, type and amount of eluting agent, type and amount of surfactant as floating agent, ionic strength and air flow rates i.e. variables affecting the efficiency of the extraction system was evaluated. It is ascertained that metal ions such as iron can be separated simultaneously from matrix in the presence of 0.012 mM ligand, 0.025% (w/v) of CTAB to a test sample of 750 mL at pH 6.5. These ions can be eluted quantitatively with 6 mL of 1.0 mol L-1 HNO3 in methanol which lead to the enrichment factor of 125. The detection limits for analyte ions were in the range of 1.3-2.4 ng mL-1. The method has been successfully applied for determination of trace amounts of ions in various real samples.

Alternativas analíticas para determinação de ferro e titânio em cimento Portland

In the present work four different analytical methodologies were studied for the determination of iron and titanium in Portland cement. The cement samples were dissolved with hot HCl and HF, being compared Fe and Ti concentrations through four analytical methods: molecular absorption spectrophotometry using the reagents 1,2-hydroxybenzene-3,5-disulfonic acid (Tiron) and the 5-chloro-salicylic acid (CSA), inductively coupled plasma atomic emission spectrometry (ICP-AES) and flame atomic absorption spectrophotometry (FAAS). In the spectrophotometric determinations were studied pH conditions, reagents addition order, interferences, amount of reagents, linear range and stability of the system. In the techniques of ICP-AES and FAAS were studied the best lines, interferences, sensibility and linear range. The obtained results were compared and the agreement was evaluated among the methods for the determination of the metals of interest.

Determinação direta de Ca, Mg, Mn e Zn em amostras de leite de búfala da Ilha de Marajó por espectrometria de absorção atômica com chama (FAAS)

This work proposes an analytical procedure for direct determination of calcium, magnesium, manganese and zinc in buffalo milk by flame atomic absorption spectrometry (FAAS). Samples were diluted with a solution containing 10% (v/v) of water-soluble tertiary amines (CFA-C) at pH 8. For comparison, buffalo milk samples were digested with HNO3 and H2O2. According to a paired t-test, the results obtained in the determination of Ca, Mg, Mn and Zn in digested samples and in 10% (v/v) CFA-C medium were in agreement at a 95% confidence level. The developed procedure is simple, rapid, decrease the possibility of contamination and can be applied for the routine determination of Ca, Mg, Mn and Zn in buffalo milk samples without any difficulty caused by matrix constituents, such as fat content, and particle size distribution in the milk emulsion.

Determinação de metais em óleos lubrificantes, provenientes de motores de ônibus urbano, utilizando a FAAS

This work proposed a procedure to examine ashes produced in burning lubricating oils used in public transportation, in Teresina PI. Sulphanilic acid was added to the oil samples, which were burned at 550 °C for three hours and 650 °C for two hours. The ash solutions were analyzed by FAAS and there were significant differences in the metal contents of the waste oil produced from normal car service. The quantification limits in μg g-1 were 5.9 (Fe), 4.4 (Pb), 1.7 (Ni), 2.1 (Cu), and 1.2 (Zn). The results showed positive accuracy and precision with recoveries between 88 and 108%, and RSD lower than 10%.

Avaliação da composição mineral do chá da folha senescente de Montrichardia linifera (arruda) schott (araceae) por espectrometria de absorção atômica com chama (FAAS)

Levels of Ca, Mg, Fe, Zn, Cu and Mn were determinated by FAAS in the tea and dry matter from senescent leaf from Montrichardia linifera, plant used in folk medicine Amazon. The content of these metals that are transferred of the leaf to the infusions have presented significant reductions, however, the Mn values in the infusion may exceed the tolerable daily intake (11 mg) if consumption of this tea is greater than 1.0 L per day. So the tea of senescent leaves of M. linifera may be considered as a toxic beverage and thus its use is not advised.

Comparison of USEPA 3050B and ISO 14869-1: 2001 digestion methods for sediment analysis by using FAAS and ICP-OES quantification techniques

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.

Avaliação da mineralização de arroz em sistema de refluxo para a determinação de Cu, Fe, Mn e Zn por FAAS

This paper describes the evaluation of a new method of sample preparation using a cold finger system with continuous water flow for rice analysis by flame atomic absorption spectrometry. The limits of detection for Cu, Fe, Mn and Zn for the proposed method were 0.36, 1.84, 2.12 and 0.16 mg kg-1, respectively. The RSDs were lower than 6.0% for all elements and the CRM analyzed showed values with 95% agreement. The proposed method is simple and safe for the proposed objective and does not require the use of mixtures of acid or special equipment for sample preparation.

Synthesis, characterization and application of ion imprinted poly(vinylimidazole) for zinc ion extraction/preconcentration with faas determination

In this paper, we describe the synthesis of an ion imprinted polymer (IIP) by homogeneous polymerization and its use in solid-phase to extract and preconcentrate zinc ions. Under optimal conditions (pH 5.0, preconcentration flow rate of 12.0 mL min-1, and eluted with 1.0 mol L-1 HNO3) this procedure allows the determination of zinc with an enrichment factor of 10.2, and with limits of detection and quantification of 1.5 and 5.0 µg L-1, respectively. The accuracy of our results was confirmed by analysis of tap water and certified reference materials: NIST 1570a (Spinach leaves) and NIST 1515 (Apple leaves).

Avaliação da combinação da nebulização discreta e processos de microextração aplicados à determinação de molibdênio por espectrometria de absorção atômica com chama (FAAS)

Simple and sensitive procedures for the extraction/preconcentration of molybdenum based on vortex-assisted solidified floating organic drop microextraction (VA-SFODME) and cloud point combined with flame absorption atomic spectrometry (FAAS) and discrete nebulization were developed. The influence of the discrete nebulization on the sensitivity of the molybdenum preconcentration processes was studied. An injection volume of 200 µL resulted in a lower relative standard deviation with both preconcentration procedures. Enrichment factors of 31 and 67 and limits of detection of 25 and 5 µg L-1 were obtained for cloud point and VA-SFODME, respectively. The developed procedures were applied to the determination of Mo in mineral water and multivitamin samples.

Preconcentration of copper from natural water samples using ligand-less in situ surfactant-based solid phase extraction prior to FAAS determination

In the present work, a simple and rapid ligand-less, in situ, surfactant-based solid phase extraction for the preconcentration of copper in water samples was developed. In this method, a cationic surfactant (n-dodecyltrimethylammonium bromide) was dissolved in an aqueous sample followed by the addition of an appropriate ion-pairing agent (ClO4-). Due to the interaction between the surfactant and ion-pairing agent, solid particles were formed and subsequently used for the adsorption of Cu(OH)2 and CuI. After centrifugation, the sediment was dissolved in 1.0 mL of 1 mol L-1 HNO3 in ethanol and aspirated directly into the flame atomic absorption spectrometer. In order to obtain the optimum conditions, several parameters affecting the performance of the LL-ISS-SPE, including the volumes of DTAB, KClO4, and KI, pH, and potentially interfering ions, were optimized. It was found that KI and phosphate buffer solution (pH = 9) could extract more than 95% of copper ions. The amount of copper ions in the water samples varied from 3.2 to 4.8 ng mL-1, with relative standard deviations of 98.5%-103%. The determination of copper in water samples was linear over a concentration range of 0.5-200.0 ng mL-1. The limit of detection (3Sb/m) was 0.1 ng mL-1 with an enrichment factor of 38.7. The accuracy of the developed method was verified by the determination of copper in two certified reference materials, producing satisfactory results.

Determinação de Cd por FAAS em meio aquoso após pré-concentração em linha sobre SiAT

Este trabalho descreve a síntese e caracterização da sílica gel modificada com grupos 2-aminotiazol (SiAT), os resultados de um estudo de adsorção e de pré-concentração (em batelada, e em fluxo utilizando-se a técnica de coluna) de íons Cd(II) em meio aquoso. A capacidade máxima de adsorção de íons Cd(II) determinada para SiAT foi de 1,12 mmol g-1 . Os resultados obtidos nos experimentos em fluxo, mostraram uma recuperação de 98% dos íons Cd(II) adsorvidos em coluna empacotada com 1 g de SiAT, utilizando-se 5 mL de HCl 1 mol L-1 como eluente. A metodologia proposta mostrou-se linear na faixa de concentração de 10 - 100 mg L-1, com limite de detecção de 0,80 mg L-1 e desvio padrão relativo de 3%. O fator de enriquecimento determinado foi de 29 vezes (considerando-se a percolação de 150 mL de solução 25 mg L-1 de Cd(II), 5 mL de eluato). A sorção-desorção quantitativa dos íons Cd(II), permitiram a aplicação do método na pré-concentração e posterior quantificação de traços de Cd(II) em amostras de águas naturais por espectrometria de absorção atômica com chama.

Determination of Copper, Iron, Nickel and Zinc in fuel kerosene by FAAS after adsorption and pre-concentration on 2-aminothiazole-modified silica gel

Silica gel chemically modified with 2-Aminotiazole groups, abbreviated as SiAT, was used for preconcentration of copper, zinc, nickel and iron from kerosene, normally used as a engine fuel for airplanes. Surface characteristics and surface area of the silica gel were obtained before and after chemical modification using FT-IR, Kjeldhal and surface area analysis (B.E.T.). The retention and recovery of the analyte elements were studied by applying batch and column techniques. The experimental parameters, such as shaking time in batch technique, flow rate and concentration of the eluent (HCl- 0.25-2.00 mol L-1) and the amount of silica, on retention and elution, have been investigated. Detection limits of the method for copper, iron, nickel and zinc are 0.77, 2.92, 1.73 and 0.097 mg L-1, respectively. The sorption-desorption of the studied metal ions made possible the development of a preconcentration method for metal ions at trace level in kerosene using flame AAS for their quantification.

Sistema TS-FF-AAS com chama acetileno-ar como alternativa em relação à chama acetileno-óxido nitroso em FAAS na determinação de estanho

Este trabalho propõe o desenvolvimento de um procedimento analítico para a determinação em linha de estanho em soluções analíticas empregando a técnica de espectrometria de absorção atômica com nebulização térmica em tubo metálico aquecido na chama (TS-FF-AAS) como alternativa ao uso da chama de óxido nitroso-acetileno em espectrometria de absorção atômica, cujo comburente apresenta um custo elevado frente ao ar comprimido. Foram avaliados parâmetros para a otimização do sistema, tais como: vazão do carregador (ar), volume de amostra injetada e concentração do ácido (HCl). Foi construída curva analítica linear [A= -0,00163 + 0,00319 [Sn], (r= 0,9998)] no intervalo de 10 a 80 mg Sn L-1. O limite de detecção, o desvio padrão relativo (n=12) e a freqüência analítica foram: 1,7 mg L-1 Sn, £ 2,7% and 120 h-1 respectivamente. O sistema TS-FF-AAS é uma alternativa para a determinação de Sn.

Exploring potentialities of the HR-CS FAAS technique in the determination of Ni and Pb in mineral waters

National Health Surveillance Agency (ANVISA) established in the decree number 54 maximum allowed levels for Ni and Pb in mineral and natural waters at 20 µg L-1 and 10 µg L-1, respectively. For screening analysis purposes, the high-resolution continuum source flame atomic absorption spectrometry technique (HR-CS FAAS) was evaluated for the fast-sequential determination of nickel and lead in mineral waters.Two atomic lines for Ni (232.003 nm - main and 341.477 nm - secondary) and Pb (217.0005 nm - main and 283.306 nm - secondary) at different wavelength integrated absorbance (number of pixels) were evaluated. Sensitivity enhanced with the increase of the number of pixels and with the summation of the atomic lines absorbances. The main figures of merit associated to the HR-CS FAAS technique were compared with that obtained by line-source flame atomic absorption spectrometry (LS FAAS). Water samples were pre-concentrated about 5-fold by evaporation before analysis. Recoveries of Pb significantly varied with increased wavelength integrated absorbance. Better recoveries (92-93%) were observed for higher number of pixels at the main line or summating the atomic lines (90-92%). This influence was irrelevant for Ni, and recoveries in the 92-104% range were obtained in all situations.

Hydraulic conductivity in response to exchangeable sodium percentage and solution salt concentration

Hydraulic conductivity is determined in laboratory assays to estimate the flow of water in saturated soils. However, the results of this analysis, when using distilled or deionized water, may not correspond to field conditions in soils with high concentrations of soluble salts. This study therefore set out to determine the hydraulic conductivity in laboratory conditions using solutions of different electrical conductivities in six soils representative of the State of Pernambuco, with the exchangeable sodium percentage adjusted in the range of 5-30%. The results showed an increase in hydraulic conductivity with both decreasing exchangeable sodium percentage and increasing electrical conductivity in the solution. The response to the treatments was more pronounced in soils with higher proportion of more active clays. Determination of hydraulic conductivity in laboratory is routinely performed with deionized or distilled water. However, in salt affected soils, these determinations should be carried out using solutions of electrical conductivity different from 0 dS m-1, with values close to those determined in the saturation extracts.