995 resultados para simultaneous graphite furnace atomic absorption spectrometry


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Biological studies and heavy metal (Ni, v, Fe, Pb,Cd) determination in liver, gonad and muscle of Scomberomorus commerson were carried out from Oct 2006 to Sept 2007 in Hormozgan coastal waters. 599 Samples were gutted for reproduction and nutrition studies, fork length and weight were measured to nearest cm and g respectively. Meanwhile 40 samples were also investigated for heavy metal studies. All specimens were collected from two major landing sites (Bandar Lengeh & Bandar Abbas). Minimums & maximum fork length & weight were 29, 128 cm & 235 and 15350 g respectively.Isometric growth was shown according to our study and b was estimated 2.9 (overall), 2.91(male) & 2.89 (female). The average relative gut length was 0.52± 0.007 and it was determined that S. commerson is a carnivorous. More than 99 percent of gut content was different teleost fishes. Gastro somatic index had two peaks in Nov & Jan (before spawning) and with a decreased trend in July, the spawning period. Occurrence of empty stomach was estimated % 65.77. Maximum amount of condition factor was in Dec. Spawning season was started from June. The average of Absolute & relative fecundity (to weight unit) was 1217149±179315 and 178.2±15.58 respectively. Lm50% was estimated 75 cm for females. Sex ratio was 0.97: 1 (male: female). Chi- Square test showed no significant difference (p>0.05). Maximum amount of hepatosomatic index was estimated in March.Metal concentrations were determined using either Flame Atomic Absorption Spectroscopy (for Fe) or Graphite Furnace Atomic Absorption Spectroscopy (for Pb,Cd,Ni and V). The mean concentration (μg/g dry weight)of Pb,Cd,Ni,V and Fe in the liver were 0.0309, 0.0268, 0.0672, 0.0077, 2.5159 in the gonad 0.0440 ,0.0295, 0.1096, 0.0000, 1.4449 and in the muscle 0.0244, 0.0324, 0.0656, 0.0128, 1.6138 respectively. The maximum metal concentrations were below the maximum permissible limits for human consumption recommended by the USEPA, WHO and the UK. The results of Kendall's Tau-b correlation coefficient were as follows: The Liver tissue: There were significant positive linear relationships between accumulation of V, Fe, and Pb with Fork length, Pb and Fe with weight, GSI with Pb, Cd, V and 109 Fe, and a negative linear relationships between HSI with accumulation of V and Fe, Fork length, weight and GSI. The Gonad tissue: There were significant positive linear relationships between GSI with accumulation of Pb, Cd, Fe, Fork length and weight, a negative linear relationship between HSI with Fork length, weight and GSI. The Muscle tissue: There were significant positive linear relationships between accumulations of V, Fe with Fork length and weight factors and as well as GSI with Cd, V, Fe, Pb, Fork length and weight,a negative linear relationship between HSI with Fork length, weight, Cd, Fe and GSI. The results of Mann-Whitney U tests (P≤0.05) show that there were significant differences between summer and autumn from heavy metal contents in the studied tissues point of view. The only exceptions were for Ni in the liver, gonads and muscle and as well as there were significant differences between male and female from heavy metal contents in the studied tissues. The only exceptions were for Pb in muscle, Ni in liver, gonad and muscle, V in muscle, and Cd and Fe in gonads.

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石墨管原位富集氢化物是近年来研究者比较感兴趣的一个问题,本工作建立了自己的氢化物发生石墨炉原位富集系统。结果表明:氢化物发生器的体积和导气管的材料均影响分析灵敏度,氢化物直接富集在石墨管内壁上比在平台上效果好,石墨炉作原子化器,可以大大减小氢化物形成元素的干扰,涂钯石墨管能在较低温度下富集氢化物应与钯的催化性能有关。

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A novel approach of using a gold disc microelectrode to analyze sweat samples for copper ions by anodic square wave stripping voltammetry (SW stripping voltammetry) is described Sweat was collected from the lower back of four subjects after physical exercise and the sample volume required for the determinations was 100 mu L. Under the optimized conditions the calibration plot was linear over the range 1-100 mu mol L(-1) Cu(II) with a limit of detection of 0 25 mu mol L(-1) The precision was evaluated by carrying out five replicate measurements in a 1 mu mol L(-1) Cu(II) solution and the standard deviation was found to be 1 5% Measurements were performed by inserting the microelectrode into sweat drops and Cu(II) concentrations in the analyzed samples ranged from 09 to 28 mu mol L(-1) Values obtained by the proposed voltammetric method agreed well with those found using graphite furnace atomic absorption spectroscopy (GFAAS) (C) 2010 Elsevier B V All rights reserved

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A solid paraffin-based carbon paste electrode modified with 2-aminothiazole organofunctionalized silica (SiAt-SPCPE) was applied to Ni2+ determination in commercial ethanol fuel samples. The proposed method comprised four steps: (1) Ni2+ preconcentration at open circuit potential directly in the ethanol fuel sample, (2) transference of the electrode to an electrochemical cell containing DMG, (3) differential pulse voltammogram registering and (4) surface regeneration by polishing the electrode. The proposed method combines the high Ni2+ adsorption capacity presented by 2-aminothiazole organofunctionalized silica with the electrochemical properties of the Ni(DMG)2 complex, whose electrochemical reduction provides the analytical signal.All experimental parameters involved in the proposed method were optimized. Using a preconcentration time of 20 min, it was obtained a linear range from 7.5 x 10(-9) to 1.0 x 10(-6) mol L-1 with detection limit of 2.0 x 10(-9) mol L-1. Recovery values between 96.5 and 102.4% were obtained for commercial samples spiked with 1.0 mu mol L-1 Ni2+ and the developed electrode was totally stable in ethanolic solutions. The contents of Ni2+ found in the commercial samples using the proposed method were compared to those obtained by graphite furnace atomic absorption spectroscopy by using the F- and t-test. Neither the F- nor t-values exceeded the critical values at 95% confidence level, confirming that there are not statistical differences between the results obtained by both methods. These results indicate that the developed electrode can be successfully employed to reliable Ni2+ determination in commercial ethanol fuel samples without any sample pretreatment or dilution step. (c) 2006 Elsevier B.V. All rights reserved.

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

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

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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.

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A new and fast procedure is proposed for cleaning autosampler cups using acid-vapor steam-cleaning with a miniaturized assembly in a microwave-heated sealed Teflon vessel. A glass cactus-shaped holder was made to support six polyethylene autosampler cups (volume, 2.0 mt) inside a 100 mt microwave vessel. Regent-grade nitric acid was added to the vessels, and the system was heated in a microwave oven for 5 min at 300 W. Chromium was determined by graphite-furnace atomic-absorption spectrophotometry. The blank values were lower with cleaned cups compared to untreated cups (i.e., as received from supplier). The quantification limits, estimated from detection limits established with Milli-Q water, were 0.66 and 0.95 mu g Cr L-1 for cleaned and untreated auto-sampler cups, respectively. (C) 1998 Elsevier B.V. B.V. All rights reserved.

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This study evaluated the effect of daily chromium supplementation at growing doses on serum Cr levels in cattle. Sixty Nellore heifers 2 to 5 years old were randomly assigned to one of four groups (15 heifers/group) fed non-fertilized Brachiaria decumbens pasture. In the control group (Gc), the heifers received a mineral mixture without Cr. In the other groups, heifers received 0.59, 1.19 or 2.38 mg Cr+3/animal/day, groups G8,5, G17 and G34, respectively. Blood samples were collected on days 0, 30 and 60. Serum concentration of chromium was determined by graphite furnace atomic absorption spectrophotometer. The chromium source used was the chromium yeast. The results do not support any significant difference (p>0.05) among serum chromium levels of heifers in groups Gc, G8,5, G17 and G34 at a same observation day. Only effect of supplementation time was detected in group G34. In this group there was significant increase (p<0,05) in the concentration serum chromium 60 days after the beginning of the experiment. Concluded Cr yeast can be used as the source of this mineral element for animals and supplementation with 2.38 mg/ cattle/day was the dose that most increased the serum concentration of Cr in Nellore cattle during the experimental period.

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Determination of chlorine using the molecular absorption of aluminum mono-chloride (AlCl) at the 261.418 nm wavelength was accomplished by high-resolution continuum source molecular absorption spectrometry using a transversely heated graphite tube furnace with an integrated platform. For the analysis. 10 mu L of the sample followed by 10 mu L of a solution containing Al-Ag-Sr modifier, (1 g L-1 each), were directly injected onto the platform. A spectral interference due to the use of Al-Ag-Sr as mixed modifier was easily corrected by the least-squares algorithm present in the spectrometer software. The pyrolysis and vaporization temperatures were 500 degrees C and 2200 degrees C, respectively. To evaluate the feasibility of a simple procedure for the determination of chlorine in food samples present in our daily lives, two different digestion methods were applied, namely (A) an acid digestion method using HNO3 only at room temperature, and (B) a digestion method with Ag, HNO3 and H2O2, where chlorine is precipitated as a low-solubility salt (AgCl), which is then dissolved with ammonia solution. The experimental results obtained with method B were in good agreement with the certified values and demonstrated that the proposed method is more accurate than method A. This is because the formation of silver chloride prevented analyte losses by volatilization. The limit of detection (LOD, 3 sigma/s) for Cl in methods A and B was 18 mu g g(-1) and 9 mu g g(-1), respectively, 1.7 and 3.3 times lower compared to published work using inductively coupled plasma optical emission spectrometry, and absolute LODs were 2.4 and 1.2 ng, respectively. (C) 2012 Elsevier B.V. All rights reserved.

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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.

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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 background 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 μg Pd + 3 μg Mg as the modifier, the pyrolysis and atomization temperatures of the heating program of the atomizer were fixed at 1400°C and 2100°C, respectively, and 20 μL 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 μg L-1 for As, Sb, Se; 10.0 - 100 μg L-1 for Cu; and 20.0 - 200 μg 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 μg L-1 As, 0.2 μg L-1 Cu, 0.6 μg L-1 Mn, 0.3 μg L-1 Sb, 0.9 μg 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 μg L-1, 1000 μg L-1, 2000 μg L-1, 5 μg L-1, and 50 μg 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, Mn, 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.