2 resultados para High-resolution continuum source graphite furnace atomic absorption spectrometry

em Universidade Federal do Rio Grande do Norte(UFRN)


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The determination and monitoring of metallic contaminants in water is a task that must be continuous, leading to the importance of the development, modification and optimization of analytical methodologies capab le of determining the various metal contaminants in natural environments, because, in many cases, the ava ilable instrumentation does not provide enough sensibility for the determination of trace values . In this study, a method of extraction and pre- concentration using a microemulsion system with in the Winsor II equilibrium was tested and optimized for the determination of Co, Cd, P b, Tl, Cu and Ni through the technique of high- resolution atomic absorption spectrometry using a continuum source (HR-CS AAS). The optimization of the temperature program for the graphite furnace (HR-CS AAS GF) was performed through the pyrolysis and atomization curves for the analytes Cd, Pb, Co and Tl with and without the use of different chemical modifiers. Cu and Ni we re analyzed by flame atomization (HR-CS F AAS) after pre-concentr ation, having the sample introduction system optimized for the realization of discrete sampling. Salinity and pH levels were also analyzed as influencing factors in the efficiency of the extraction. As final numbers, 6 g L -1 of Na (as NaCl) and 1% of HNO 3 (v/v) were defined. For the determination of the optimum extraction point, a centroid-simplex statistical plan was a pplied, having chosen as the optimum points of extraction for all of the analytes, the follo wing proportions: 70% aqueous phase, 10% oil phase and 20% co-surfactant/surfactant (C/S = 4). After extraction, the metals were determined and the merit figures obtained for the proposed method were: LOD 0,09, 0,01, 0,06, 0,05, 0,6 and 1,5 μg L -1 for Pb, Cd, Tl, Co, Cu and Ni, re spectively. Line ar ranges of ,1- 2,0 μg L -1 for Pb, 0,01-2,0 μg L -1 for Cd, 1,0 - 20 μg L -1 for Tl, 0,1-5,0 μg L -1 for Co, 2-200 μg L -1 and for Cu e Ni 5-200 μg L -1 were obtained. The enrichment factors obtained ranged between 6 and 19. Recovery testing with the certified sample show ed recovery values (n = 3, certified values) after extraction of 105 and 101, 100 and 104% for Pb, Cd, Cu and Ni respectively. Samples of sweet waters of lake Jiqui, saline water from Potengi river and water produced from the oil industry (PETROBRAS) were spiked and the recovery (n = 3) for the analytes were between 80 and 112% confirming th at the proposed method can be used in the extraction. The proposed method enabled the sepa ration of metals from complex matrices, and with good pre-concentration factor, consistent with the MPV (allowed limits) compared to CONAMA Resolution No. 357/2005 which regulat es the quality of fresh surface water, brackish and saline water in Brazil.

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The accelerated growth of urban regions have produced relevant effects on water resources. Urban regions need an adequate institutional structure that can be able to face environmental demands and the adverse effects of land use on water resources. This study aims at analysing land use effects on heavy metals concentration in sediments and water, as well as making a comparative analysis involving water physical-chemical parameters. Applied methodology included both in loco water parameters measurement and water and bed sediment sampling at 8 sections along the fluvial system. Sample analysis was performed in laboratory in order to measure heavy metal concentrations. It was measured metal concentrations of Al, Cu, Pb, Cd, Fe, Ni and Zn. Once the samples were subjected to acid digestion (method 3050B), concentration values were measured by using atomic absorption spectrometry by flame (ICP-FLAA). The analysis results were compared with normative reference, these standards is intended to assess the risks of toxic substances in sediment and water management programs. The normative reference used in this work were: a) Ontario Ministry of the Environment and Energy (OMEE, 1993) b) Normative Netherlands (VROM, 2000); c) Normative Canadian (CCME, 1999); d) United States Environmental Protection Agency (USEPA, 1977), e) CONAMA Resolution No. 344/2004; f) CONAMA Resolution No. 357/2005. The high concentrations of iron (38,750 mg.g-1), Lead (1100 mg.g-1), Nickel (100 μg.g-1) and zinc (180 μg.g-1) detected sediments confirm the state of degradation of the aquatic system. Iron concentrations (1.08 mg.L-1), Aluminum (0.6 mg.L-1) and phosphorus (0.05 mg.L-1) present in the water are outside the established standards for human consumption