Simultaneous determination of zinc, copper, lead, and cadmium in fuel ethanol by anodic stripping voltammetry using a glassy carbon-mercury-film electrode

A new, versatile, and simple method for quantitative analysis of zinc, copper, lead, and cadmium in fuel ethanol by anodic stripping voltammetry is described. These metals can be quantified by direct dissolution of fuel ethanol in water and subsequent voltammetric measurement after the accumulation step. A maximum limit of 20% (v/v) ethanol in water solution was obtained for voltammetric measurements without loss of sensitivity for metal species. Chemical and operational optimum conditions were analyzed in this study; the values obtained were pH 2.9, a 4.7-mum thickness mercury film, a 1,000-rpm rotation frequency of the working electrode, and a 600-s pre-concentration time. Voltammetric measurements were obtained using linear scan (LSV), differential pulse (DPV), and square wave (SWV) modes and detection limits were in the range 10(-9)-10(-8) mol L-1 for these metal species. The proposed method was compared with a traditional analytical technique, flame atomic absorption spectrometry (FAAS), for quantification of these metal species in commercial fuel ethanol samples.

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.

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.

Synthesis, characterization and thermal behaviour of solid-state compounds of folates with some bivalent transition metals ions

Solid-state M-L compounds, where M stands for bivalent Mn, Co, Ni, Cu and Zn and L is folate (C19H17N7O6), have been synthesized. Simultaneous thermogravimetry and differential scanning calorimetry (TG-DSC), X-ray powder diffractometry, infrared spectroscopy (FTIR), TG-DSC coupled to FTIR, elemental analysis and high-resolution continuum source flame atomic absorption spectrometry technique (HR-CS FAAS) were used to characterize and to study the thermal behaviour of these compounds. The results provided information concerning the composition, dehydration, thermal stability and thermal decomposition. © 2013 Akadémiai Kiadó, Budapest, Hungary.

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.

Biogeoquímica de metais em sedimentos dos rios da Bacia Hidrográfica do Turvo/Grande

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

Otimização de procedimentos para a determinação de maganês em amplo intervalo de concentração por espectrometria de absorção atômica em chama

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Estratégias analíticas para determinação de fósforo por espectrometria de absorção atômica com fonte contínua de alta resolução

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Determinação de boro, enxofre e fósforo em plantas medicinais por espectrometria de absorção atômica de alta resolução com fonte contínua

Pós-graduação em Química - IQ

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

Pós-graduação em Química - IQ