Flow injection AAS determination of Cd, Cu, and Pb at trace levels in wine using solid phase extraction

A comparative study is reported between C-18 bonded silica gel and powdered polyethylene (PE) as sorbent for Cd, Cu, and Pb determination using ammonium diethyldithiophosphate (ADTP) as the complexing agent in a flow injection system. The complexes were formed in 0.14 mol L-1 HNO3 and processed in a simple flow system comprising a peristaltic pump, a manual injector-commutator, and a sorbent-packed minicolumn. Ethanol was selected as the eluent and analytes in the eluate were determined by flame atomic absorption spectrometry. The optimum concentration of the complexing agent was 0.1% (m/v) ADTP for Cu and Pb determination using either C-18 or PE, and 0.25% (m/v) ADTP for Cd determination using PE. The sample loading flow rates were 5.0, 3.6, and 3.0 mL min(-1) for Cu, Pb, and Cd, respectively. The best elution flow rate was 6.5 mL min(-1). For a 60-sec preconcentration time, the sampling rate was 40 h(-1) and the enrichment factors of 33, 36, and 11 times (C-18) or 18, 22, and 23 times (PE) were obtained for Cu, Pb, and Cd, respectively. The limits of detection (LOD) were 1.6 mug L-1 Cu, 11 mug L-1 Pb, and 2.0 mug L-1 Cd using C-18 or 2.9 mug L-1 Cu, 19 mug L-1 Pb, and 1.0 mug L-1 Cd using PE, respectively. The relative standard deviations (n = 12) were typically <2%, <2%, and <6% for Cd, Cu, and Pb, respectively. The recoveries of Cd, Cu, and Pb added to wine samples varied from 96-99%, 97-102%, and 90-99%, respectively, using C-18 or PE. Accuracy was checked for Cd, Cu, and Pb determination in six wine samples digested by block digestor and open-vessel microwave-assisted digestion systems. The results revealed that C-18 was more efficient for Cu and Pb determination, while PE was the best sorbent for Cd.

Determination of Ca, Mg, and Zn in biodiesel microemulsions by FAAS using discrete nebulization

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

Comparative studies of the sample decomposition of green and roasted coffee for determination of nutrients and data exploratory analysis

The contents of some nutrients in 35 Brazilian green and roasted coffee samples were determined by flame atomic absorption spectrometry (Ca, Mg, Fe, Cu, Mn, and Zn), flame atomic emission photometry (Na and K) and Kjeldahl (N) after preparing the samples by wet digestion procedures using i) a digester heating block and ii) a conventional microwave oven system with pressure and temperature control. The accuracy of the procedures was checked using three standard reference materials (National Institute of Standards and Technology, SRM 1573a Tomato Leaves, SRM 1547 Peach Leaves, SRM 1570a Trace Elements in Spinach). Analysis of data after application of t-test showed that results obtained by microwave-assisted digestion were more accurate than those obtained by block digester at 95% confidence level. Additionally to better accuracy, other favorable characteristics found were lower analytical blanks, lower reagent consumption, and shorter digestion time. Exploratory analysis of results using Principal Component Analysis (PCA) and Hierarchical Cluster Analysis (HCA) showed that Na, K, Ca, Cu, Mg, and Fe were the principal elements to discriminate between green and roasted coffee samples. ©2007 Sociedade Brasileira de Química.

Iron determination by FAAS in fish feed and feces after ultrasound-assisted extraction

This paper proposes a method to determine iron in samples of fish feed and feces using ultrasound in the extraction of the analyte and in subsequent quantification by flame atomic absorption spectrometry. Using HCl 0.10 mol L -1 as the extraction solution, the optimal conditions of extraction were found to be: granulometry of the sample <60 μm; a sonication time of five cycles of 10 s and sonication power of 136 W. The method was applied in studies of the availability of iron in four food sources used in the diet of Nile Tilapia. The results obtained with the proposed extraction method allowed us to calculate the coefficients of apparent digestibility of iron in the food sources, which was not possible when using results obtained from samples mineralized by acid digestion. © Springer Science+Business Media, LLC 2008.

Metodologia analítica para extração ultra-sônica de minerais em rações de suínos

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

An alternative method for the simultaneous determination of copper and lead for quality control of sugar cane spirit using a nanotube-based sensor

The development of an electroanalytical method for simultaneous determination of copper and lead ions in sugar cane spirit (cachaça) using carbon paste electrode modified with ascorbic acid and carbon nanotubes (CPE-AaCNT) is described. Squarewave voltammetry (SWV) with anodic stripping was employed, and this technique was optimized with respect to the following parameters: frequency (50 Hz), amplitude (100 mV) and scan increment (9 mV). The analytical curves were linear in the range from 0.0900 to 7.00 mg L - 1 for lead and copper. The limits of detection were 48.5 and 23.9 µg L - 1 for lead and copper, respectively. The developed method was applied to the simultaneous determination of copper and lead in five commercial samples of sugar cane spirit. The results were in good agreement with those obtained by F AAS/GF AAS (flame atomic absorption spectrometry/graphite furnace atomic absorption spectrometry) and showed that CPE-AaCNT can be successfully employed in the simultaneous determination of these metals in real sugar cane spirit samples.

Recuperação e aplicação do dicromato de potássio proveniente do resíduo de sulfocrômica

A simple procedure for recovering potassium dichromate (K2Cr2O7 ) from treatment of residual sulphochromic solution was proposed in the present work by means of cooling crystallization. The decrease of temperature favored the crystallization of K2Cr2O7 due to the decrease of solubility. 5.0 L of sulphochromic wastes containing 48.08 g L-1 of Cr(VI) were treated and the process of crystallization was performed in three steps until crystals were not formed anymore. On each step the content of Crtotal was determined by flame atomic absorption spectrometry and Cr(VI) by colorimetric method with 1,5- diphenylcarbazide, resulting in the removal of 91% and 92% of Crtotal and Cr(VI), respectively. After the last step, the remaining Cr(VI) in the solution was reduced to Cr(III) from the addition of NaHSO3 , recovering via precipitation in pH 8 approximately 36.13 g of Cr(OH)3 . The final supernatant was discarded since chromium content was below the maximum limit established by the Brazilian legislation for effluents discharge, which corresponds to 0.10 and 1.0 mg L-1 of Cr(VI) and Cr(III), respectively. 628.4 g of K2Cr2O7 were recovered and the salt was characterized by X-ray diffraction and differential thermal analysis. Its applicability was compared to the standard K2Cr2O7 when determining the soil organic matter, in which there was no significant difference, thus inferring that the recovered compound may be incorporated on routine analyses. This recovering process allowed the reuse of K2Cr2O7 , thus reducing costs with the acquisition of new reagents and environmental impacts caused by the inadequate discard of sulphochromic solutions.

Síntese, caracterização e aplicação de celulose funcionalizada com o ligante P-aminobenzóico em pré- concentração de íons metálicos

Pós-graduação em Química - IQ

Composição química e valor nutricional para grandes herbívoros das folhas e frutos de aninga (Montrichardia linifera, Araceae)

Montrichardia linifera (Araceae), conhecida popularmente como 'aninga', faz parte dos ecossistemas de várzea da Amazônia e da dieta natural de animais como peixe-boi, tartarugas, peixes, búfalo e gado. Com o objetivo de contribuir para o conhecimento químico e valor nutricional da mesma, folhas e frutos de M. linifera foram coletados às margens dos rios Guamá e Maratauíra, no Estado do Pará, Brasil. Em folhas e frutos foram realizadas análises de umidade, resíduo mineral fixo (cinzas), lipídios, proteínas, fibra bruta, concentração de carboidratos e valor calórico. A composição mineral (Ca, Mg, Cu, Fe, Zn e Mn) foi obtida por espectrometria de absorção atômica de chama. Observou-se que tanto as folhas quanto os frutos da aninga, apesar de calóricos (289,75 kcal e 355,12 kcal, respectivamente), possuem baixo valor protéico (0,44% e 0,24 %, respectivamente). As concentrações de manganês obtidas (folha = 3279,46 mg kg^-1e fruto = 18151,53 mg kg^-1) foram consideradas tóxicas, extrapolando o limite máximo tolerável para ruminantes (1000 mg kg^-1). A M. linifera, tem capacidade de absorver e bioacumular grandes quantidades de Ca, Mg e Mn presentes no solo, o que torna inadequada a sua utilização exclusiva na alimentação de quelônios, bovinos e bubalinos, havendo necessidade de mais estudos para sua aplicação como parte da ração.

Bovinos como bioindicadores da poluição ambiental por chumbo na região de Guarapuava -PR

Pós-graduação em Medicina Veterinária - FMVZ

Classificação multivariada de ervas medicinais da Região Amazônica e suas infusões de acordo com sua composição mineral

ABSTRACT: In this study, the mineral composition of leaves and teas of medicinal plants was evaluated. Ca, Cu, Fe, Mg, Mn e Zn were determined in the samples using flame atomic absorption spectrometry. Principal component analysis was applied to discriminate the samples studied. The samples were divided within the 2 groups according to their mineral composition. Copper and iron were the variables that contributed most to the separation of the samples followed by Ca, Mg, Mn and Zn. The information in the principal component analysis was confirmed by the dendrogram obtained by hierarchical cluster analysis.

Determinação direta de Ca, Mg, Mn e Zn em amostras de leite de búfala da Ilha de Marajó por espectrometria de absorção atômica com chama (FAAS)

ABSTRACT: This work proposes an analytical procedure for direct determination of calcium, magnesium, manganese and zinc in buffalo milk by flame atomic absorption spectrometry (FAAS). Samples were diluted with a solution containing 10% (v/v) of water-soluble tertiary amines (CFA-C) at pH 8. For comparison, buffalo milk samples were digested with HNO₃ and H₂O₂. According to a paired t-test, the results obtained in the determination of Ca, Mg, Mn and Zn in digested samples and in 10% (v/v) CFA-C medium were in agreement at a 95% confidence level. The developed procedure is simple, rapid, decrease the possibility of contamination and can be applied for the routine determination of Ca, Mg, Mn and Zn in buffalo milk samples without any difficulty caused by matrix constituents, such as fat content, and particle size distribution in the milk emulsion

Avaliação da composição mineral do chá da folha senescente de Montrichardia linifera (arruda) schott (araceae) por espectrometria de absorção atômica com chama (FAAS)

Levels of Ca, Mg, Fe, Zn, Cu and Mn were determinated by FAAS in the tea and dry matter from senescent leaf from Montrichardia linifera, plant used in folk medicine Amazon. The content of these metals that are transferred of the leaf to the infusions have presented significant reductions, however, the Mn values in the infusion may exceed the tolerable daily intake (11 mg) if consumption of this tea is greater than 1.0 L per day. So the tea of senescent leaves of M. linifera may be considered as a toxic beverage and thus its use is not advised.

Metal ions bound to the human milk immunoglobulin A: Metalloproteomic approach

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

An Alternative Method for the Simultaneous Determination of Copper and Lead for Quality Control of Sugar Cane Spirit using a Nanotube-Based Sensor

The development of an electroanalytical method for simultaneous determination of copper and lead ions in sugar cane spirit (cachaca) using carbon paste electrode modified with ascorbic acid and carbon nanotubes (CPE-AaCNT) is described. Squarewave voltammetry (SWV) with anodic stripping was employed, and this technique was optimized with respect to the following parameters: frequency (50 Hz), amplitude (100 mV) and scan increment (9 mV). The analytical curves were linear in the range from 0.0900 to 7.00 mg L-1 for lead and copper. The limits of detection were 48.5 and 23.9 mu g L-1 for lead and copper, respectively. The developed method was applied to the simultaneous determination of copper and lead in five commercial samples of sugar cane spirit. The results were in good agreement with those obtained by F AAS/GF AAS (flame atomic absorption spectrometry/graphite furnace atomic absorption spectrometry) and showed that CPE-AaCNT can be successfully employed in the simultaneous determination of these metals in real sugar cane spirit samples.