Evaluation and Application of TS-FF-AAS System Using Ceramic Tube as Atomization Cell for Tin Determination in Canned Foods

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

Comparison of metallic and ceramic tubes as atomization cells for tin determination by TS-FF-AAS

This work describes the development of an analytical procedure for on-line tin determination using thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS). Two tubes were evaluated as atomization cells: a metallic tube (Ni-Cr, principal components composition: 73.95% Ni and 16.05% Cr) and a ceramic tube (99.8% Al2O3). The use of air as the carrier was made by employing a Rheodyne valve to inject the samples, allowing an analytical frequency of 90 h(-1) and avoiding sample dispersion. The carrier flow rate (air), sample volume injected, and acid concentration (HCl) were evaluated for the optimization of the TS-FF-AAS system. The sensitivity for 50 mL of analytical solution with TS-FF-AAS was 2 and 5 times higher (to metallic and ceramic tube, respectively) than using an acetylene-nitrous oxide flame with pneumatic aspiration (requiring a sample volume of approximately 20 times higher.

Selenium determination in tissue samples of Nile tilapia using ultrasound-assisted extraction

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

Comparison of the univariate and multivariate methods in the optimization of experimental conditions for determining Cu, Pb, Ni and Cd in biodiesel by GFAAS

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

Evaluation of Cu, Mn, and Se in Vegetables Using Ultrasonic Extraction and GFAAS Quantification

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

Rugged, Portable Tungsten Coil Atomic Emission Spectrometer

Tungsten coil atomic emission spectrometry is an ideal technique for field applications because of its simplicity, low cost, low power requirement, and independence from cooling systems. A new, portable, compact design is reported here. The tungsten coil is extracted from an inexpensive 24 V, 250 W commercial light bulb. The coil is housed in a small, aluminum cell. The emission signal exits from a small aperture in the cell, while the bulk of the blackbody emission from the tungsten coil is blocked. The resulting spectra exhibit extremely low background signals. The atomization cell, a single lens, and a hand-held charge coupled device (CCD) spectrometer are fixed on a 1 x 6 x 30 cm ceramic base. The resulting system is robust and easily transported. A programmable, miniature 400 W solid-state constant current power supply controls the temperature of the coil. Fifteen elements are determined with the system (Ba, Cs, Li, Rb, Cr, Sr, Eu, Yb, Mn, Fe, Cu, Mg, V, Al, and Ga). The precision ranges from 4.3% to 8.4% relative standard deviation for repetitive measurements of the same solution. Detection limits are in the 0.04 to 1500 mu g/L range. Accuracy is tested using standard reference materials for polluted water, peach leaves, and tomato leaves. For those elements present above the detection limit, recoveries range from 72% to 147%.

Simultaneous Determination of Cadmium and Lead in Medicinal Plants Using Graphite Furnace Atomic Absorption Spectrometry and Direct Slurry Sampling

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

Evaluation of solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for direct determination of chromium in medicinal plants

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

Simultaneous determination of Cu and Pb in fuel ethanol by graphite furnace AAS using tungsten permanent modifier with co-injection of Ir

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Influência de nitrato de paládio, nitrato de magnésio e nitrato de níquel no comportamento térmico de arsênio em açúcares por espectrometria de absorção atômica em forno de grafite

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

Determinação direta e simultânea de Al, As, Fe, Mn e Ni em cachaça por espectrometria de absorção atômica em forno de grafite

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

Silver as internal standard for simultaneous determination of Cd and Pb in whole blood by electrothermal atomic absorption spectrometry

The use of internal standardization for simultaneous atomic absorption spectrometry (SIMAAS) was investigated for Cd and Pb determination in whole blood. The comparison of thermochemical and physicochemical parameters allowed the selection of Ag, Bi, and Tl as internal standard candidates. Correlation graphs, plotted from the normalized absorbance signals (n = 20) of internal standard (axis y) versus analyte ( axis x), precision and accuracy were used to select Ag as the most appropriate internal standard. Blood samples were diluted (1 + 9) with 0.11% (m/v) Triton X-100 + 1.1% (v/v) HNO3 + 0.28% (m/v) NH4H2PO4 + 10 mug L-1 Ag+. Pyrolysis and atomization temperatures for the optimized heating program were 550 and 1700 degreesC, respectively. Characteristic masses based on integrated absorbance were 1.68 +/- 0.01 pg for Cd and 30.3 +/- 0.1 pg for Pb. The detection limits (DL) were 0.095 +/- 0.001 mug L-1 and 0.86 +/- 0.01 mug L-1 for Cd and Pb, respectively. The mean RSD for all determinations was the same for Cd (13 +/- 9%) with or without Ag as internal standard ( IS). on the other hand, the use of Ag as IS improved the RSD for Pb from 3.6 +/- 4.0% to 2.2 +/- 2.0%. An effective contribution of the internal standard Ag was verified in the recoveries of spiked samples (0.5 mug L-1 Cd2+ and 5.0 mug L-1 Pb2+). The mean recoveries were 81 +/- 8% and 91 +/- 4% for Cd, and 80 +/- 11% and 93 +/- 6% for Pb without and with IS correction, respectively. This is the first application of IS for a simultaneous determination by SIMAAS.

Tungsten permanent chemical modifier with co-injection of Pd(NO3)(2)+Mg(NO3)(2) for direct determination of Pb in vinegar by graphite furnace atomic absorption spectrometry

A tungsten carbide coating on the integrated platform of a transversely heated graphite atomizer (THGA((R))) used together with Pd(NO3)(2) + Mg(NO3)(2) as modifier is proposed for the direct determination of lead in vinegar by graphite furnace atomic absorption spectrometry. The optimized heating program (temperature, ramp time, hold time) of atomizer involved drying stage (110 degrees C, 5 s, 30 s; 130 degrees C, 5 s, 30 s), pyrolysis stage (1000 degrees C, 15 s, 30 s), atomization stage (1800 degrees C, 0 s, 5 s) and clean-out stage (2450 degrees C, I s, 3 s). For 10 mu L of vinegar delivered into the atomizer and calibration using working standard solutions (2.5-20.0 mu g L-1 Pb) in 0.2% (v/v) HNO3, analytical curve with good linear correlation (r = 0.9992) was established. The characteristic mass was 40 pg Pb and the lifetime of the tube was around 730 firings. The limit of detection (LOD) was 0.4 mu g L-1 and the relative standard deviations (n = 12) were typically <8% for a sample containing 25 pg L-1 Pb. Accuracy of the proposed method was checked after direct analysis of 23 vinegar samples. A paired t-test showed that results were in agreement at 95% confidence level with those obtained for acid-digested vinegar samples. The Pb levels varied from 2.8 to 32.4 pg L-1. Accuracy was also checked by means of addition/recovery tests and recovered values varied from 90% to 110%. Additionally, two certified reference materials were analyzed and results were in agreement with certified values at a 95% confidence level. (C) 2006 Elsevier Ltd. All rights reserved.

Effect of modifiers on thermal behaviour of Se in acid digestates and slurries of vegetables by graphite furnace atomic absorption spectrometry

The influence of sample preparation strategy of vegetables on the electrothermal behaviour of Se without and with chemical modifiers such as Pd(NO3)(2), Pd(NO3)(2) + Mg(NO3)(2), Pd(NO3)(2) + Cd(NO3)(2), pre-reduced Pd, Mg(NO3)(2), and Ni(NO3)(2) was investigated. Acid digestates and slurries of vegetables (0.1% m/v in 1% m/v HNO3 + 0.005% v/v of Triton X-100) were used to prepare reference solutions or slurries. For 10 mul of each modifier tested, pyrolysis and atomization temperatures were evaluated using pyrolysis and atomization curves, respectively. Best conditions, such as thermal stability, signal profile, repeatability and sensitivity were attained using Pd(NO3)(2) as chemical modifier. The following heating program (temperature, ramp/hold time) of the graphite tube of the Varian SpectrAA-800Z atomic absorption spectrometer was used: dry step (85 degreesC, 5/0 s; 95 degreesC, 40/0 s; 120 degreesC, 10/.5 s); pyrolysis step (1400 degreesC, 10/3s); atomization step (2200 degreesC, 1/2 s); clean step (2600 degreesC, 2/0 s). This pyrolysis temperature is 800 degreesC higher than when measuring without any modifier. For 20 muL sample volume and 10 mug Pd(NO3)(2), analytical curves in the 3.0-30 mug Se 1(-1) range were obtained. The method was applied for Se determination in acid digestates and slurries of 10 vegetable samples and one standard reference material (rice flower) and results were in agreement at 95% confidence level. Recoveries varied from 89 to 95% for spiked samples. The lifetime of the graphite tube was ca. 250 firings and the relative standard deviations (n = 12) for a typical acid digestate and slurry containing 20 mug Se 1(-1) were 3.8% and 8.3%, respectively. The limits of detection were 2.0 mug Se 1(-1) and 0.6 mug Se 1(-1) Se for digestates and slurries, respectively. (C) 2002 Elsevier B.V. Ltd. All rights reserved.

Simultaneous determination of As, Cu, Mn, Sb, and Se in drinking water by GRAS with transversely heated graphite atomizer and longitudinal Zeeman-effect background correction

A method has been developed for the direct and simultaneous determination of As, Cu, Mn, Sb, and Se in drinking water by electrothermal atomic absorption spectrometry (ETAAS) using a transversely heated graphite tube atomizer (THGA) with longitudinal Zeeman-effect back- ground correction. The thermal behavior of analytes during the pyrolysis and atomization stages was investigated in 0.028 mol L-1 HNO3, 0.14 mol L-1 HNO3 and 1 + 1 (v/v) diluted water using mixtures of Pd(NO3)(2) + Mg(NO3)(2) as the chemical modifier, With 5 mug Pd + 3 mug Mg as the modifier, the pyrolysis and atomization temperatures of the heating program of the atomizer were fixed at 1400degreesC and 2100degreesC, respectively, and 20 muL of the water sample (sample + 0.28 mol L-1 HNO3, 1 + 1, v/v), dispensed into the graphite tube, analytical curves were established ranging from 5.00 - 50.0 mug L-1 for As, Sb, Se; 10.0 - 100 mug L-1 for Cu; and 20.0 - 200 mug L-1 for Mn. The characteristic masses were around 39 pg As, 17 pg Cu, 60 pg Mn, 43 pg Sb, and 45 pg Se, and the lifetime of the tube was around 500 firings. The limits of detection (LOD) based on integrated absorbance (0.7 mug L-1 As, 0.2 mug L-1 Cu, 0.6 mug L-1 Mn, 0.3 mug L-1 Sb, 0.9 mug L-1 Se) exceeded the requirements of the Brazilian Food Regulations (decree # 310-ANVS from the Health Department), which established the maximum permissible level for As, Cu, Mn, Sb, and Se at 50 mug L-1, 1000 mug L-1, 2000 mug L-1, 5 mug L-1, and 50 mug L-1, respectively. The relative standard deviations (n = 12) were typically < 5.3% for As, < 0.5% for Cu, < 2.1% for Mn, < 11.7% for Sb, and < 9.2% for Se. The recoveries of As, Cu, Mn, Sb, and Se added to the mineral water samples varied from 102-111%, 91-107%, 92-109%, 89-97%, and 101-109%, respectively. Accuracy for the determination of As, Cu, Mu Sb and Se was checked using standard reference materials NIST SRM 1640 - Trace Elements in Natural Water, NIST SRM 1643d - Trace Elements in Water, and 10 mineral water samples. A paired t-test showed that the results were in agreement with the certified values of the standard reference materials at the 95% confidence level.