Alexander Ossanes de Souza

Ultrasound-assisted synthesis of aliphatic acid esters at room temperature.

This work describes the ultrasound-assisted synthesis of saturated aliphatic esters from synthetic aliphatic acids and either methanol or ethanol. The products were isolated in good yields after short reaction times under mild conditions.

Acid Decomposition of Yerba Mate (Ilex paraguariensis) Using a Reflux System for the Evaluation of Al, Ca, Cd, Cr, Cu, Fe, K, Mg, Mn, Na, Pb and Zn Contents by Atomic Spectrometric Techniques

In the first part of this paper, two acid decomposition procedures for the determination of Al, Ca, Fe, Mg, Mn and Zn contents in yerba mate samples by inductively coupled plasma optical emission spectrometry (ICP OES) were compared. Using a reflux system, the samples were treated with a mixture of HNO3 and H2O2 for 3 hours at 220 °C in the digester block. The results from five commercial yerba mate samples were compared with the results obtained from microwave digestion. Good agreement between the procedures at a 95% confidence level was obtained with relative standard deviation (RSD) values lower than 10.0%. The accuracy was evaluated using addition and recovery experiments (80.5 to 112.8%). In the second part, Ca, Cd, Cr, Cu, Fe, K, Mg, Na, Pb and Zn concentrations were evaluated in the yerba mate infusion. The results showed that elements such as Na, K, Mg and Zn are easily transferred to the hot water used for the infusion. For Pb and Cd, the concentrations found in the analyzed samples were lower than the values established by Brazilian legislation.

Obtenção de biodiesel por transesterificação em dois estágios e sua caracterização por cromatografia gasosa: óleos e gorduras em laboratório de química orgânica

Methanolic transesterification of oils and fats was carried out in a two steps procedure, under basic and acidic catalysis. Palm, soybean, canola, corn, rice, grapeseed, sunflower, peanut, pequi and olive oils, besides tallow and lard were used as feedstock. Specific gravity, relative viscosity, thin layer chromatography and gas chromatography were used to characterize the biodiesel. Biodiesel was obtained in high yield and purity. Results were used to discuss the following key-concepts: 1 - triglycerides, composition and properties; 2 - nucleophilic acyl substitution under basic and acid conditions, 3 - thin layer chromatography, 4 - gas chromatography and its quantitative methods.

Evaluation of the use of a reflux system for sample preparation of processed fruit juices and subsequent determination of Cr, Cu, K, Mg, Na, Pb and Zn by atomic spectrometry techniques

The acid decomposition method was applied for the sample preparation of processed fruit juice. The decomposition of 15mL of juice sample using HNO3 and H2O2 was performed in a digester block with reflux system and heated at 200°C for 150min. The limits of detection were 0.03; 0.24; 0.8; 0.008; 0.026 and 0.056mgL-1 for Cr, Cu, K, Mg, Na and Zn, respectively and for Pb was 0.99μgL-1. The accuracy was evaluated by spiked experiments (80 to 119%). Four processed fruit juice samples commercialized in Brazil (strawberry, mango, peach, and orange) were analyzed and indicated the absence of Cr, Zn and Cu in the samples, except for Cu in strawberry juice. Pb was found in the mango juice sample (17.8±0.9μgL-1) and the concentration is below the maximum values recommended by Brazilian legislation for juices of citric fruits (0.3mgkg-1).

DETERMINAÇÃO DE Cd E Pb EM AMOSTRAS DE GOMA XANTANA POR GF AAS

This paper describes the evaluation of a method for determination of Cd and Pb in xanthan gum samples by Graphite Furnace Atomic Absorption Spectrometry (GF AAS) using NH4H2PO4 as the chemical modifier. The sample preparation was performed using a reflux system adapted in the digestion tubes. With this system it was possible to increase the temperature of the digester block above the boiling point of the reaction medium, preventing loss of analyte and excessive evaporation of acids during heating. Samples were digested with HNO3 for 3 h in a digester block at 220 oC. The limits of detection for Cd and Pb were 2.2 and 33.8 ng g-1, respectively. The RSDs for both analytes were, on average, lower than 5.0% and accuracy was verified by recovery tests, yielding values in the 83-100% range.

Ultrasound assisted efficient conversion of aromatic aldehydes from oximes

This work describes the ultrasound-assisted regeneration of aldehydes from oximes in ethanol and phosphoric acid as mediator of the reaction. The large scale regeneration of benzaldehyde was shown under similar conditions. The products were isolated in good yields after short reaction times under mild conditions.

Decomposição ácida assistida por ultrassom para a determinação de Cu, Fe, Mg e Zn por F AAS em cerâmicas de uso doméstico

This paper describes a sample preparation method for domestic ceramics, based on the acid decomposition assisted by ultrasound for further determination of Cu, Fe, Mg and Zn by Flame Atomic Absorption Spectrometry technique. The main optimized conditions were: particle size (25 µm); sample mass (25 mg) and the acid volume (0.5 mL of HNO3 and 0.5 mL of HF). The samples were placed in an ultrasonic bath for 2 hours at 40 oC. The method was employed for eight commercial samples of domestic ceramic, which showed different concentrations for all analytes investigated, showing the existing variety of raw materials. The method showed good accuracy and precision, attested by the addition and recovery test, with values of 87 to 112% for all analytes and relative standard deviation lower than 3.0%.

New Design of Mini PTFE Vessels for Sample Preparation in Micro Scale: Determination of Cd, K, Mg and Na in Biological Sample

This paper presents a study involving the development of a new mini polytetrafluoroethylene (PTFE) vessel project for biological sample preparation in micro scale in closed system with microwave radiation for subsequent determination of Cd, K, Mg and Na by atomic spectrometry techniques. All experiments were carried out in micro quantities of samples (up to 20 mg) and reagents (300 μL of HNO3) for 5 min at 350 W. Certified reference materials of biological samples (bovine muscle and liver) were used to evaluate the accuracy of the proposed system and the results obtained were in agreement with the certified value at 95% of confidence (t-test). Relative standard deviations (RSD) were lower than 8.0% for all elements. The proposed method is not only easy and fast, but it is also based on the use of an inexpensive system for sample digestion.