A new method for the decomposition of soybean based edible products (soy extract, textured soy pr... more A new method for the decomposition of soybean based edible products (soy extract, textured soy protein, transgenic soybeans, and whole soy flour) was developed to essential (Co, Cr, Cu, Fe, Mn, Ni, Se, V, and Zn) and non-essential (As, Ba, Cd, Pb, and Sr) trace elements determination by ICP OES and ICP-MS respectively. Effects related to the concentration of HNO3 (2.1-14.5molL(-1)) and the use of hydrogen peroxide on the efficiency of decomposition was evaluated based on the residual carbon content (RCC). It was demonstrated that 2.1molL(-1) HNO3 plus 1.0mL H2O2 was suitable for an efficient digestion, since RCC was lower than 18% and the agreement with certified values and spike recoveries were higher than 90% for all analytes. The concentrations of analytes in the samples (minimum-maximum in mgkg(-1)) were: The concentrations of analytes in the samples (minimum-maximum in mgkg(-1)) were: As (<0.007-0.040), Ba (0.064-10.6), Cd (<0.006-0.028), Co (0.012-102), Cr (0.56-5.88), C...
ABSTRACT Propolis is a complex mixture of substances collected by honeybees from buds or exudates... more ABSTRACT Propolis is a complex mixture of substances collected by honeybees from buds or exudates of plants, beeswax, and other constituents, as pollen and sugars. The main purpose of this study was to evaluate two digestion procedures for determination of major, minor, and trace elements (Ba, Ca, Cd, Cr, Co, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, and Zn) in natura propolis samples by inductively coupled plasma optical emission spectrometry (ICP OES). The first procedure studied was an open-vessel digestion using HNO3 + H2SO4 + H2O2 in a heating block and the second one was a microwave-assisted concentrated acid digestion using HNO3 + H2O2. Both digestion procedures led to similar results and quantitative recoveries. The residual carbon contents (RCCs) for propolis sample digests were 0.269 ± 0.012 % when using the first procedure with conventional heating and 0.458 ± 0.023 % by microwave-assisted closed vessel digestion, demonstrating high efficiency of both procedures. Accuracy of the results was demonstrated using a certified reference material and by comparison with a recommended official method. The t test (unpaired) at 95 % confidence level showed that there was no significant difference between determined and certified values of all analytes under investigation, except Ca concentration employing conventional procedure. The optimized microwave-assisted digestion procedure led to recoveries around 89–103 % and precision better than 5 % for most samples. The second procedure was faster, safer, and more accurate than the one based on conductive heating. Additionally, principal component analysis (PCA) was applied for checking if there was correlation between inorganic composition and source of propolis samples collected around Bahia State in the Northeast of Brazil.
The use of ICP/AES for the determination of zinc, in low concentration levels, in matrices contai... more The use of ICP/AES for the determination of zinc, in low concentration levels, in matrices containing high levels of copper is difficult because copper interferes in the zinc main emission wavelength (213.856 nm). In the present work, a separation of zinc from copper matrices was possible, using the reaction of zinc(II) cation with 1-(2-tiazolylazo)-2-naphthol (TAN), in the pH range of 6.5-8.0, resulting in a stable red complex. Copper also reacts with TAN but its interference was avoided by the addition of ascorbic acid and thiosulphate in the reaction medium. In this way, the aqueous solution was passed through a SEP PAK C18 cartridge, in which the zinc(II)-TAN complex was quantitatively retained, but it did not occur with copper which passes through the cartridge, as [Cu(2)(S(2)O(3))(2)](2-), with the aqueous solution. The cartridge was washed with water and the complex eluted with ethanol. Then, the alcohol was evaporated and the complex decomposed by nitric acid. It results in ...
A separation/preconcentration procedure using solid phase extraction has been proposed for the fl... more A separation/preconcentration procedure using solid phase extraction has been proposed for the flame atomic absorption spectrometric determination of copper and nickel at trace level in food samples. The solid phase is Dowex Optipore SD-2 resin contained on a minicolumn, where analyte ions are sorbed as 5-methyl-4-(2-thiazolylazo) resorcinol chelates. After elution using 1 mol L(-1) nitric acid solution, the analytes are determinate employing flame atomic absorption spectrometry. The optimization step was performed using a full two-level factorial design and the variables studied were: pH, reagent concentration (RC) and amount of resin on the column (AR). Under the experimental conditions established in the optimization step, the procedure allows the determination of copper and nickel with limit of detection of 1.03 and 1.90 microg L(-1), respectively and precision of 7 and 8%, for concentrations of copper and nickel of 200 microg L(-1). The effect of matrix ions was also evaluated. The accuracy was confirmed by analyzing of the followings certified reference materials: NIST SRM 1515 Apple leaves and GBW 07603 Aquatic and Terrestrial Biological Products. The developed method was successfully applied for the determination of copper and nickel in real samples including human hair, chicken meat, black tea and canned fish.
Um novo método espectrofotométrico para determinação de zinco(II) é proposto usando um derivado d... more Um novo método espectrofotométrico para determinação de zinco(II) é proposto usando um derivado da 8-hidroxiquinolina, o ácido 7-(4-nitrofenilazo)-8-hidroxiquinolina sulfônico (p-NIAZOXS). A reação entre o p-NIAZOXS eo zinco(II) é rapida em pH 9,2 eo complexo ...
The determination of impurities in titanium dioxide pigments, such as Al, Cd, Cr, Fe, Mn, P, Zn a... more The determination of impurities in titanium dioxide pigments, such as Al, Cd, Cr, Fe, Mn, P, Zn and Zr, is relevant because trace elements affect pigment properties. The critical step in the analysis of this pigment is the conversion of the solid sample to a representative solution. This study compared four acid decomposition procedures for TiO2 for the determination of
DETERMINATION OF Mn, Cu AND Zn IN SALINE MATRICES BY FLAME ATOMIC ABSORPTION SPECTROMETRY AFTER S... more DETERMINATION OF Mn, Cu AND Zn IN SALINE MATRICES BY FLAME ATOMIC ABSORPTION SPECTROMETRY AFTER SEPARATION AND PRECONCENTRATION ON AMBERLITE XAD-7 IMPREGNATED WITH ALIZARIN RED S. The aim of this work was to explore the ...
Visão contextualizada da Cadeia Produtiva do Biodiesel, a partir da bancada do laboratório para a... more Visão contextualizada da Cadeia Produtiva do Biodiesel, a partir da bancada do laboratório para a indústria, com avaliação crítica do estado-da-arte e desenvolvimento tecnológico através de artigos...
Determination of Cr(VI) and Cr(III) in water samples by inductively coupled argon plasma-atomic e... more Determination of Cr(VI) and Cr(III) in water samples by inductively coupled argon plasma-atomic emission spectrometry (ICP-AES) was performed indirectly employing an on-line system. For this purpose a column with copper shavings was used to reduce Cr(VI) to Cr(III) in acidic media, generating Cu(II) ions in the flow path. This process permitted the evaluation of concentrations in the range of 1-50 mg/l. The protocol allowed a throughput of 100 samples per hour with 10% precision in the concentration.
A new method for the decomposition of soybean based edible products (soy extract, textured soy pr... more A new method for the decomposition of soybean based edible products (soy extract, textured soy protein, transgenic soybeans, and whole soy flour) was developed to essential (Co, Cr, Cu, Fe, Mn, Ni, Se, V, and Zn) and non-essential (As, Ba, Cd, Pb, and Sr) trace elements determination by ICP OES and ICP-MS respectively. Effects related to the concentration of HNO3 (2.1-14.5molL(-1)) and the use of hydrogen peroxide on the efficiency of decomposition was evaluated based on the residual carbon content (RCC). It was demonstrated that 2.1molL(-1) HNO3 plus 1.0mL H2O2 was suitable for an efficient digestion, since RCC was lower than 18% and the agreement with certified values and spike recoveries were higher than 90% for all analytes. The concentrations of analytes in the samples (minimum-maximum in mgkg(-1)) were: The concentrations of analytes in the samples (minimum-maximum in mgkg(-1)) were: As (<0.007-0.040), Ba (0.064-10.6), Cd (<0.006-0.028), Co (0.012-102), Cr (0.56-5.88), C...
ABSTRACT Propolis is a complex mixture of substances collected by honeybees from buds or exudates... more ABSTRACT Propolis is a complex mixture of substances collected by honeybees from buds or exudates of plants, beeswax, and other constituents, as pollen and sugars. The main purpose of this study was to evaluate two digestion procedures for determination of major, minor, and trace elements (Ba, Ca, Cd, Cr, Co, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, and Zn) in natura propolis samples by inductively coupled plasma optical emission spectrometry (ICP OES). The first procedure studied was an open-vessel digestion using HNO3 + H2SO4 + H2O2 in a heating block and the second one was a microwave-assisted concentrated acid digestion using HNO3 + H2O2. Both digestion procedures led to similar results and quantitative recoveries. The residual carbon contents (RCCs) for propolis sample digests were 0.269 ± 0.012 % when using the first procedure with conventional heating and 0.458 ± 0.023 % by microwave-assisted closed vessel digestion, demonstrating high efficiency of both procedures. Accuracy of the results was demonstrated using a certified reference material and by comparison with a recommended official method. The t test (unpaired) at 95 % confidence level showed that there was no significant difference between determined and certified values of all analytes under investigation, except Ca concentration employing conventional procedure. The optimized microwave-assisted digestion procedure led to recoveries around 89–103 % and precision better than 5 % for most samples. The second procedure was faster, safer, and more accurate than the one based on conductive heating. Additionally, principal component analysis (PCA) was applied for checking if there was correlation between inorganic composition and source of propolis samples collected around Bahia State in the Northeast of Brazil.
The use of ICP/AES for the determination of zinc, in low concentration levels, in matrices contai... more The use of ICP/AES for the determination of zinc, in low concentration levels, in matrices containing high levels of copper is difficult because copper interferes in the zinc main emission wavelength (213.856 nm). In the present work, a separation of zinc from copper matrices was possible, using the reaction of zinc(II) cation with 1-(2-tiazolylazo)-2-naphthol (TAN), in the pH range of 6.5-8.0, resulting in a stable red complex. Copper also reacts with TAN but its interference was avoided by the addition of ascorbic acid and thiosulphate in the reaction medium. In this way, the aqueous solution was passed through a SEP PAK C18 cartridge, in which the zinc(II)-TAN complex was quantitatively retained, but it did not occur with copper which passes through the cartridge, as [Cu(2)(S(2)O(3))(2)](2-), with the aqueous solution. The cartridge was washed with water and the complex eluted with ethanol. Then, the alcohol was evaporated and the complex decomposed by nitric acid. It results in ...
A separation/preconcentration procedure using solid phase extraction has been proposed for the fl... more A separation/preconcentration procedure using solid phase extraction has been proposed for the flame atomic absorption spectrometric determination of copper and nickel at trace level in food samples. The solid phase is Dowex Optipore SD-2 resin contained on a minicolumn, where analyte ions are sorbed as 5-methyl-4-(2-thiazolylazo) resorcinol chelates. After elution using 1 mol L(-1) nitric acid solution, the analytes are determinate employing flame atomic absorption spectrometry. The optimization step was performed using a full two-level factorial design and the variables studied were: pH, reagent concentration (RC) and amount of resin on the column (AR). Under the experimental conditions established in the optimization step, the procedure allows the determination of copper and nickel with limit of detection of 1.03 and 1.90 microg L(-1), respectively and precision of 7 and 8%, for concentrations of copper and nickel of 200 microg L(-1). The effect of matrix ions was also evaluated. The accuracy was confirmed by analyzing of the followings certified reference materials: NIST SRM 1515 Apple leaves and GBW 07603 Aquatic and Terrestrial Biological Products. The developed method was successfully applied for the determination of copper and nickel in real samples including human hair, chicken meat, black tea and canned fish.
Um novo método espectrofotométrico para determinação de zinco(II) é proposto usando um derivado d... more Um novo método espectrofotométrico para determinação de zinco(II) é proposto usando um derivado da 8-hidroxiquinolina, o ácido 7-(4-nitrofenilazo)-8-hidroxiquinolina sulfônico (p-NIAZOXS). A reação entre o p-NIAZOXS eo zinco(II) é rapida em pH 9,2 eo complexo ...
The determination of impurities in titanium dioxide pigments, such as Al, Cd, Cr, Fe, Mn, P, Zn a... more The determination of impurities in titanium dioxide pigments, such as Al, Cd, Cr, Fe, Mn, P, Zn and Zr, is relevant because trace elements affect pigment properties. The critical step in the analysis of this pigment is the conversion of the solid sample to a representative solution. This study compared four acid decomposition procedures for TiO2 for the determination of
DETERMINATION OF Mn, Cu AND Zn IN SALINE MATRICES BY FLAME ATOMIC ABSORPTION SPECTROMETRY AFTER S... more DETERMINATION OF Mn, Cu AND Zn IN SALINE MATRICES BY FLAME ATOMIC ABSORPTION SPECTROMETRY AFTER SEPARATION AND PRECONCENTRATION ON AMBERLITE XAD-7 IMPREGNATED WITH ALIZARIN RED S. The aim of this work was to explore the ...
Visão contextualizada da Cadeia Produtiva do Biodiesel, a partir da bancada do laboratório para a... more Visão contextualizada da Cadeia Produtiva do Biodiesel, a partir da bancada do laboratório para a indústria, com avaliação crítica do estado-da-arte e desenvolvimento tecnológico através de artigos...
Determination of Cr(VI) and Cr(III) in water samples by inductively coupled argon plasma-atomic e... more Determination of Cr(VI) and Cr(III) in water samples by inductively coupled argon plasma-atomic emission spectrometry (ICP-AES) was performed indirectly employing an on-line system. For this purpose a column with copper shavings was used to reduce Cr(VI) to Cr(III) in acidic media, generating Cu(II) ions in the flow path. This process permitted the evaluation of concentrations in the range of 1-50 mg/l. The protocol allowed a throughput of 100 samples per hour with 10% precision in the concentration.
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