Reversible intermittent flow-injection determination of mercury in sediments and vinasses by cold vapor atomic absorption spectrometry

A reversible intermittent pow-injection procedure is proposed for the automated determination of mercury in sediments and vinasses by cold vapor atomic absorption spectrometry, CVAAS. Solutions of sample and stannous chloride are carried by two air streams and sequentially injected into the generator/separator chamber in a segmented asynchronous merging zone configuration. The intermittent flow in the forward direction carries the mercury vapor through the flow cell, and in the backward direction, if aspirates the the remaining solution from the vessel to waste. We investigated composition and concentration of reagents, pow rates, commutation times, reactor configuration, and conditions for mercury release. The accuracy was checked by mercury determination in a certified sediment and spiked vinasses and river waters. The system handles about 100 samples per hour (0.50-5.00 mu g L-1), consuming ca. 2.5 mL of sample and 50 mg of SnCl2 per determination; Good recoveries (92-103%) were obtained with spiked samples. Results are precise (RSD <3% for 2.5 mu g Hg L-1, n = 12) and in agreement with values for certified reference material at 95% confidence level. (C) 1999 John Wiley & Sons, Inc.

Determination of mercury in agroindustrial samples by flow-injection cold vapor atomic absorption spectrometry using ion exchange and reductive elution

A flow-injection system with a Chelite-S® cationic resin packed minicolumn is proposed for the determination of trace levels of mercury in agroindustrial samples by cold vapor atomic absorption spectrometry. Improved sensitivity and selectivity are attained since mercuric ions are on-line concentrated whereas other potential interferents are discarded. With on-line reductive elution procedure, concentrated hydrochloric acid could be replaced by 10% w/v SnCl2, in 6 M HCl as eluent. The reversed-intermittent stream either carries the atomic mercury, to the flow cell in the forward direction or removes the residue from reactor/gas liquid separator to a discarding flask in the opposite direction. Concentration and volume of reagent, acidity, flow rates, commutation times and potential interfering species were investigated. For 120 s preconcentration time, the proposed system handles about 25 samples h-1 (50.0 500 ng l-1), consuming about 10 ml sample and 5 mg SnCl2 per determination. The detection limit is 0.8 ng l-1 and the relative standard deviation (RSD) (n = 12) of a 76.7 ng l-1 sample is about 5%. Results are in agreement with certified value of standard materials at 95% confidence level and good recoveries (97-128%) of spiked samples were found. (C) 2000 Elsevier Science B.V.

Determination of mercury in river water by diffusive gradients in thin films using P81 membrane as binding layer

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

Determination of Hg in water by CVAAS using 2-aminothiazole modified silica

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

Reduction of mercury(II) by tropical river humic substances (Rio Negro) - A possible process of the mercury cycle in Brazil

The evolution of elemental Hg from its environmental compounds has already been supposed to be an important process within the global mercury cycle. The present study characterizes the abiotic reduction of Hg(II) ions by typical river humic substances (HS) conventionally pre-isolated by the adsorbent XAD 8 from the Rio Negro near Manaus, Brazil. For the investigation of this reduction process a special reaction and Hg(0) trapping unit combined with cold-vapor atomic absorption spectrometry (CVAAS) was developed. Preconcentration of traces of mercury(II), if required, was obtained by a home-made FIA system using microcolumns filled with the Hg(II)-selective collector CheliteS(R) (Serva Company). The effect of environmentally relevant parameters such as the pH value, the Hg(II)/HS ratio and the HS concentration on the I-IE;(II) reduction process was studied as a function of the time. The Hg(0) production was highest at pH 8.0 and in the case of decreasing HS amounts (0.5 mg) when about 65% of initially 1.0 mug Hg(H) was reduced within 50 h. Moreover, the reduction efficiency of HS towards HE;(II) strongly depended on the HS concentration but hardly on the Hg(II)/HS ratio. The reduction kinetics followed a relatively slow two-step first-order mechanism with formal rate constants of about 0.1 and 0.02 h(-1), respectively. Based on these findings the possible relevance of the abiotic evolution of mercury in humic-rich aquatic environments is considered. (C) 2000 Elsevier B.V. B.V. All rights reserved.

Estudo metalômico do mercúrio em leite materno coletado da população ribeirinha da área de influência do Ahe Jirau-bacia do rio Madeira

Pós-graduação em Biologia Geral e Aplicada - IBB

Redução de mercúrio iônico por substâncias húmicas aquáticas

Pós-graduação em Química - IQ

Cádmio, chumbo, cromo, mercúrio e níquel nos rios do estado de São Paulo e em peixes do Rio Sorocaba (São Paulo, Brasil)

To verify the levels of concentration of some heavy metals in fishes from Sorocaba river (São Paulo, Brazil) and evaluate if this contamination offers health risks to the fishermen, 63 samples of fishes collected from four points along the river were studied for cadmium, lead, chromium, nickel and mercury, with emphasis in this last, since it is the most toxic and most probable as a fish contaminant. Analyzing muscle samples by cold vapor atomic absorption spectrometry it was shown that the fishes are not contaminated. None of the five metals studied were present in prohibitive level and the fishes could be judged secure for human consume. It was also analyzed data from four years of cadmium, lead, chromium, nickel and mercury monitoring made by CETESB, from 1997 to 2000, in water from the main rivers of the State of São Paulo. The study pointed out that the majority of the monitored rivers still present contamination by those metals in a level that requires an improvement of the pollution control actions.

In situ selective determination of methylmercury in river water by diffusive gradient in thin films technique (DGT) using baker's yeast (Saccharomyces cerevisiae) immobilized in agarose gel as binding phase

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

A metalloproteomics study on the association of mercury with breast milk in samples from lactating women in the Amazon region of Brazil

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

Direct determination of Cu, Cd, Ni and Pb in aquatic humic substances by graphite furnace atomic absorption spectrometry

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

Tungsten permanent chemical modifier for fast estimation of Se contents in soil by graphite furnace atomic absorption spectrometry

A tungsten carbide coating on the integrated platform of a transversely heated graphite atomizer was used as a modifier for the direct determination of Se in soil extracts by graphite furnace atomic absorption spectrometry. Diethylenetriaminepentaacetic acid (0.0050 mol L-1) plus ammonium hydrogencarbonate (1.0 mol L-1) extracted predominantly available inorganic selenate from soil. The formation of a large amount of carbonaceous residue inside the atomizer was avoided with a first pyrolysis step at 600 degreesC assisted by air during 30 s. For 20 muL of soil extracts delivered to the atomizer and calibration by matrix matching, an analytical curve (10.0-100 mug of L-1) with good linear correlation (r = 0.999) between integrated absorbance and analyte concentration was established. The characteristic mass was similar to63 pg of Se, and the lifetime of the tube was similar to750 firings. The limit of detection was 1.6 mug L-1, and the relative standard deviations (n = 12) were typically <4% for a soil extract containing 50 mug of L-1. The accuracy of the determination of Se was checked for soil samples by means of addition/recovery tests. Recovery data of Se added to four enriched soil samples varied from 80 to 90% and indicated an accurate method.

Development of a method to determine Ni and Cd in biodiesel by graphite furnace atomic absorption spectrometry

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

Analytical procedure based on slurry sampling for determining selenium in organic vegetable samples by graphite furnace atomic absorption spectrometry

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

Application of cellulose modified with p-aminobenzoic groups in preconcentration system for determination of Cu, Fe, Ni, and Zn in fuel ethanol samples by flame atomic absorption spectrometry

Cellulose chemically modified with p-aminobenzoic groups, abbreviated as Cel-PAB, was used for preconcentration of copper, iron, nickel, and zinc from ethanol fuel, normally used in Brazil as engine fuel. The surface characteristics and the surface area of the cellulose were obtained before and after chemical modification using FT-IR, elemental analysis, and surface area analysis (B.E.T.). The retention and recovery of the analyte elements were studied by applying batch and column techniques.