Desenvolvimento de metodologia de extração e pré-concentração utilizando sistema microemulsionado para determinação de Cd, Co, Cu, Ni, Pb e Tl em águas naturais e produzidas por HR-CS AAS

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.

Lâminas de água salina e doses de adubação orgânica na produção de palma Miúda adensada no semiárido

Cactus pear is an important forage for livestock in semi-arid region of Brazil, due to its adaptation to climate conditions in this region, high productivity and nutritional value. The yield of this cactus has positively responded to techniques such as planting density, fertilization and cutting managements, however, in Rio Grande do Norte State, only certain areas have favorable climate conditions to the development of this crop. Drip irrigation, with a small amount of water, has proven to be an alternative to the viability of cactus pear cultivation in these areas. The research aimed to evaluate the effects of different levels of saline water and manure organic fertilization on the morphological characteristics and production of fresh and dry matter of the prickly-pear cactus cv. Miúda (Nopalea cochenillifera Salm Dick) in a dense planting system. The experiment was conducted at the Experimental Station of Terras Secas (EMPARN), Pedro Avelino, latitude 5°31'21" South and longitude 36°23'14" West. The soil was classified as Typical Cambisol Haplicum Carbonate and the water used in irrigation, C4S1T3 (5,25 dS.m-1), with planting spacing of 2.0 x 0.25 m (20,000 plants ha-1). A completely randomized design in a split plot was used, where water levels (0, 7.5, 15.0 and 30.0 mm month-1) with 10 days intervals, were the main plots and organic fertilization (0 , 25 and 50 Mg ha-1 yr-1) the subplots, with four replicates. The measured morphological characteristics were number of cladodes, height and volume of the plant; length, width, perimeter, thickness, area and cladodes area index, fresh and dry matter production, dry matter content, water use efficiency (WUE) and damage promoted by cochineal pest (Diaspis echinocacti) and soft rot (Erwinia carotovora). There was no influence (P>0.05) of organic fertilization on most variables, particularly in relation to the production of fresh and dry matter. The water levels had a significant influence (P<0.05) on most variables, promoting higher height and volume of the plants, larger and thicker cladodes, and increase on fresh and dry matter production (13.55 Mg DM ha-1 yr-1). The absence of irrigation caused a significant expansion in plant damage caused by the cochineal pest and when irrigated with different water levels there was an increase in damage and stand loss, caused by soft rot, been more intense at the higher water level.