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 vanadium in urine by electrothermal atomic absorption spectrometry using hot injection and preconcentration into the graphite tube

In this work it was developed a procedure for the determination of vanadium in urine samples by electrothermal atomic absorption spectrometry using successive injections for preconcentration into a preheated graphite tube. Three 60 μL volumes were sequentially injected into the atomizer preheated to a temperature of 110°C. Drying and pyrolysis steps were carried out after each injection. A chemical modifier, barium difluoride (100 mg L-1), and a surfactant, Triton X-100 (0.3% v v-1), were added to the urine sample. When injecting into a hot graphite tube, the sample flow-rate was 0.5 μL s-1. The limits of detection and quantification were 0.54 and 1.82 without preconcentration, and 0.11 and 0.37 μg L-1 with preconcentration, respectively. The accuracy of the procedure was evaluated by an addition-recovery experiment employing urine samples. Recoveries varied from 96.0 to 103% for additions ranging from 0.8 to 3.5 μg L-1 V. The developed procedure allows the determination of vanadium in urine without any sample pretreatment and with minimal dilution of the sample.

Use of the internal standardization for difficult sampling by graphite furnace atomic absorption spectrometry

This work shows the potentiality of As as internal standard to compensate errors from sampling of sparkling drinking water samples in the determination of selenium by graphite furnace atomic absorption spectrometry. The mixture Pd(NO 3) 2/Mg(NO 3) 2 was used as chemical modifier. All samples and reference solutions were automatically spiked with 500 μg l -1 As and 0.2% (v/v) HNO 3 by the autosampler, eliminating the need for manual dilutions. For 10 μl dispensed sample into the graphite tube, a good correlation (r=0.9996) was obtained between the ratio of analyte absorbance by the internal standard absorbance and the analyte concentrations. The relative standard deviations (R.S.D.) of measurements varied from 0.05 to 2% and from 1.9 to 5% (n=12) with and without internal standardization, respectively. The limit of detection (LD) based on integrated absorbance was 3.0 μg l -1 Se. Recoveries in the 94-109% range for Se spiked samples were obtained. Internal standardization (IS) improved the repeatability of measurements and increased the lifetime of the graphite tube in ca. 15%. © 2004 Elsevier B.V. All rights reserved.

Direct and simultaneous determination of As, Cu, and Pb in Brazilian sugar cane spirits by graphite furnace AAS using tungsten permanent modifier with co-injection of Pd/Mg(N03)2

A method was developed using the multi-element graphite furnace atomic absorption spectrometry technique for the direct and simultaneous determination of As, Cu, and Pb in Brazilian sugar cane spirit (cachaça) samples. Also employed was the end-capped transversely heated graphite atomizer (THGA) with platforms pre-treated with W permanent modifier and co-injection of Pd/Mg(N03)2. Pyrolysis and atomization temperature curves were established in a cachaça medium (1+1; v/v) containing 0.2% (v/v) HN03 and spiked with 20 μg L-1 As and Pb and 200 μg L-1Cu. The effect of the concentration of major elements usually present in cachaça matrices (Ca, Mg, Na, and K) and ethanol on the absorbance of As, Cu, and Pb was investigated. Analytical working solutions of As, Cu, and Pb were prepared in 10% (v/v) ethanol plus 5.0 mg L-1 Ca, Mg, Na, and K. Acidified to 0.2% (v/v) HNO3, these solutions were suitable to build calibration curves by matrix matching. The proposed method was applied to the simultaneous determination of As, Cu, and Pb in commercial sugar cane spirits. The characteristic mass for the simultaneous determination was 16 pg As, 119 pg Cu, and 28 pg Pb. The pretreated tube lifetime was about 450 firings. The limit of detection (LOD) was 0.6 μg L-1As, 9.2 μg L-1 Cu, and 0.3 μg L-1Pb. The found concentrations varied from 0.81 to 4.28 μg L-1As, 0.28 to 382 mg L-1 Cu and 0.82 to 518 μg L-1 Pb. The recoveries of the spiked samples varied from 94-112% (As), 97-111% (Cu), and 95-101% (Pb). The relative standard deviation (n=12) was 6.9%, 7.4%, and 7.7% for As, Cu, and Pb, respectively, present in a sample at 0.87 μgL-1, 0.81 mgL-1, and 38.9 μgL-1concentrations.

Determination of copper at wide range concentrations using instrumental features of high-resolution continuum source flame atomic absorption spectrometry

This work describes a method to determine Cu at wide range concentrations in a single run without need of further dilutions employing high-resolution continuum source flame atomic absorption spectrometry. Different atomic lines for Cu at 324. 754 nm, 327. 396 nm, 222. 570 nm, 249. 215 nm and 224. 426 nm were evaluated and main figures of merit established. Absorbance measurements at 324. 754 nm, 249. 215 nm and 224. 426 nm allows the determination of Cu in the 0. 07-5. 0 mg L -1, 5. 0-100 mg L -1 and 100-800 mg L -1 concentration intervals respectively with linear correlation coefficients better than 0. 998. Limits of detection were 21 μg L -1, 310 μg L -1 and 1400 μg L -1 for 324. 754 nm, 249. 215 nm and 224. 426 nm, respectively and relative standard deviations (n = 12) were ≤ 2. 7%. The proposed method was applied to water samples spiked with Cu and the results were in agreement at a 95% of confidence level (paired t-test) with those obtained by line-source flame atomic absorption spectrometry.

Cross linked Poly (4-Vinylpyridine-Ethylene Glycol Dimethacrylate) Used for Preconcentration of Cd(II) and its Determination by Flow Injection Flame Atomic Absorption Spectrometry

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

A simple and fast method for assessment of the nitrogen-phosphorus-potassium rating of fertilizers using high-resolution continuum source atomic and molecular absorption spectrometry

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

Determination of lead in eye shadow and blush by high-resolution continuum source graphite furnace atomic absorption spectrometry employing directSolid sampling

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

Simultaneous determination of chromium and nickel in medicinal plants by slurry sampling graphite furnace atomic absorption spectrometry

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

Determination of heavy metals and genotoxicity of water from an artesian well in the city of Vazante- MG, Brazil

The city of Vazante-MG is of great socioeconomic and environmental interest because it is the most important zinc producer district of Brazil. The mineral processing and geochemical processes may determine high concentrations of heavy metals in water intended for human consumption. Thus, the present study aimed to quantify and evaluate the heavy metal genotoxicity of artesian water in the city by Atomic absorption spectrophotometer analysis and testing with the Allium cepa test, respectively. This study reveals a chemical contamination in well water in the city, caused by the presence of heavy metals. Therefore, it can be considered that the high levels of heavy metals found in water samples are correlated with the genotoxic events observed in root cells of A. cepa.

Surface modified Mg-doped ZnO QDs for biological imaging

Fundação Amparo à Pesquisa Estado de São Paulo (FAPESP)