Determinação de CD, PB, e TL em água produzida por HR-CS GF AAS após extração em ponto nuvem

Produced water is a major problem associated with the crude oil extraction activity. The monitoring of the levels of metals in the waste is constant and requires the use of sensitive analytical techniques. However, the determination of trace elements can often require a pre-concentration step. The objective of this study was to develop a simple and rapid analytical method for the extraction and pre-concentration based on extraction phenomenon cloud point for the determination of Cd, Pb and Tl in produced water samples by spectrometry of high resolution Absorption source continues and atomization graphite furnace. The Box Behnken design was used to obtain the optimal condition of extraction of analytes. The factors were evaluated: concentration of complexing agent (o,o-dietilditilfosfato ammonium, DDTP), the concentration of hydrochloric acid and concentration of surfactant (Triton X -114). The optimal condition obtained through extraction was: 0,6% m v-1 DDTP, HCl 0,3 mol L-1 and 0,2% m v-1 of Triton X - 114 for Pb; 0,7% m v-1 DDTP, HCl 0,8 mol L-1 and 0,2% m v-1 Triton X-114 for Cd. For Tl was evidenced that best extraction condition occurs with no DDTP, the extraction conditions were HCl 1,0 mol L-1 e 1,0% m v-1 de Triton X - 114. The limits of detection for the proposed method were 0,005 µg L-1 , 0,03 µg L-1 and 0,09 µg L-1 to Cd, Pb and Tl, Respectively. Enrichment factors Were greater than 10 times. The method was applied to the water produced in the Potiguar basin, and addition and recovery tests were performed, and values were between 81% and 120%. The precision was expressed with relative standard deviation (RSD) is less than 5%

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.

Quantificação de metais potencialmente tóxicos em mexilhão dourado (Limnoperna fortunei) por espectrometria de absorção atômica com fonte contínua e alta resolução empregando amostragem direta de sólidos

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Determination of lead in medicinal plants by high-resolution continuum source graphite furnace atomic absorption spectrometry using direct solid sampling

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)

Quantificação de metais potencialmente tóxicos em mexilhão dourado (Limnoperna fortunei) por espectrometria de absorção atômica com fonte contínua e alta resolução empregando amostragem direta de sólidos

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Effect of modifiers for As, Cu and Pb determinations in sugar-cane spirits by GF AAS

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

Different lubricating oil treatments for the determination of Cu, Cr, Fe, Ni, Sb, Pb, and Zn by HR-CS FAAS

Microwave-assisted acid decomposition, direct dilution in kerosene, and oil-in-water emulsion were evaluated as lubricating oil pretreatment procedures for Cu, Cr, Fe, Ni, Pb, Sb, and Zn determination by High-Resolution Continuum Source Flame Atomic Absorption Spectrometry (HR-CS FAAS). For wet digestion, results were compared with those obtained by Flame Atomic Absorption Spectrometry (FAAS). The ultrasound probe used in emulsions sonication contaminated samples with Cr, although better results have been observed for the other six elements in this condition. In general, recovery percentages ranging from 81-106%(Cu), 80-107%(Cr), 85-114%(Fe), 82-116%(Ni), 86-117%(Pb), 85-115%(Sb), and 81-114%(Zn) were obtained. The HR-CS FAAS showed to be faster and more sensitive than FAAS.

Exploring potentialities of the HR-CS FAAS technique in the determination of Ni and Pb in mineral waters

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

Evaluation of modifiers for determination of V in parsley by GF AAS

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

A simple method based on HR-CS FAAS for multi-element determination of Cu, Fe, Mn and Zn in medicinal plants

A simple method to determine Cu, Fe, Mn and Zn in single aliquots of medicinal plants by HR-CS FAAS is proposed. The main lines for Cu, Mn and Zn, and the alternate line measured at the wing of the main line for Fe at 248.327 nm allowed calibration within the 0.025 - 2.0 mg L-1 Cu, 1.0 - 20.0 mg L-1 Fe, 0.05 - 2.0 mg L-1 Mn, 0.025 - 0.75 mg L-1 Zn ranges. Nineteen medicinal plants and two certified plant reference materials were analyzed. Results were in agreement at a 95% confidence level (paired t-test) with reference values. Limits of detection were 0.12 μg L-1 Cu, 330 μg L-1 Fe, 1.42 μg L-1 Mn and 8.12 μg L-1 Zn. Relative standard deviations (n=12) were ≤ 3% for all analytes. Recoveries in the 89 - 105% (Cu), 95 - 108% (Fe), 94 - 107% (Mn), and 93 - 110% (Zn) ranges were obtained.

Cooking Effects on Iron and Proteins Content of Beans (Phaseolus Vulgaris L.) by GF AAS and MALDI-TOF MS

The effects of domestic cooking on proteins, organic compounds and Fe distribution in beans (Phaseolus vulgaris L.) were investigated. Sequential extraction with different extractant solutions (mixture of methanol and chloroform 1:2 v/v, water, 0.5 mol L-1 NaCl, 70% v/v ethanol and 0.5 mol L-1 NaOH) were used for extracting lipids, albumins, globulins, prolamins and glutelins, respectively. Iron determination by graphite furnace atomic absorption spectrometry (GF AAS), proteins by Bradford method and organic compounds by matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) were carried out in this work. High concentration of albumins, globulins and glutelins were found in raw beans, while in the cooked beans, albumins and glutelins are main proteins types. The MALDI-TOF MS spectra of raw and cooked beans revealed that the domestic cooking altered the molecular weight of the organic compounds, since that in the cooked beans were found compounds between 2 and 3.5 kDa, which were not presented in the raw beans. Besides this, in cooked beans were also observed the presence of four compounds of high molecular weight (12-16 kDa), being that in the raw grains there is only one (ca. 15.2 kDa). In raw grains is possible to observe that Fe is mainly associated to albumins, globulins and glutelins. For cooked grains, Fe is associated to albumins and globulins.

Cooking effects on iron and proteins content of beans (Phaseolus Vulgaris L.) by GF AAS and MALDI-TOF MS

The effects of domestic cooking on proteins, organic compounds and Fe distribution in beans (Phaseolus vulgaris L.) were investigated. Sequential extraction with different extractant solutions (mixture of methanol and chloroform 1:2 v/v, water, 0.5 mol L-1 NaCl, 70% v/v ethanol and 0.5 mol L-1 NaOH) were used for extracting lipids, albumins, globulins, prolamins and glutelins, respectively. Iron determination by graphite furnace atomic absorption spectrometry (GF AAS), proteins by Bradford method and organic compounds by matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) were carried out in this work. High concentration of albumins, globulins and glutelins were found in raw beans, while in the cooked beans, albumins and glutelins are main proteins types. The MALDI-TOF MS spectra of raw and cooked beans revealed that the domestic cooking altered the molecular weight of the organic compounds, since that in the cooked beans were found compounds between 2 and 3.5 kDa, which were not presented in the raw beans. Besides this, in cooked beans were also observed the presence of four compounds of high molecular weight (12-16 kDa), being that in the raw grains there is only one (ca. 15.2 kDa). In raw grains is possible to observe that Fe is mainly associated to albumins, globulins and glutelins. For cooked grains, Fe is associated to albumins and globulins.

Sequential factorial designs for method development of the determination of Cd and Pb in fish and shrimp by GF AAS after sample freezedrying and tetramethylammonium hydroxide solubilization.

2016