Adriana Vitorino Rossi

Síntese de biodiesel: uma proposta contextualizada de experimento para laboratório de química geral

The contextualized understanding of concepts in Chemistry by students from other areas is a challenging task. In this experiment, the synthesis of biodiesel is done by base catalyzed transesterification of refined soy oil with methanol at room temperature and common glassware found in any chemistry laboratory. The proposal permits introducing several concepts, such as that of emulsion, viscosity and catalysis to illustrate an activity based on an actual problem. In this didactic approach, some common problems of biodiesel production, such as soap formation and phase separation, are introduced into the procedure in order to raise questions and motivate the students to participate in the experimental work and stimulate reflections about critical aspects of biodiesel production. This experiment was carried out in the first semester of 2006, in experimental general chemistry taken by physics and agricultural, civil and chemical engineering students of UNICAMP.

Quantitative spot tests of Fe(III), Cr(VI) and Ni(II) by reflectance measurements

ABSTRACT This work shows that diffuse reflectance measurements, using fiber optical devices, can give rapid quantitative results for application with spot tests determination where little sample manipulation is a desirable feature. The experiments were performed with a Hewlett Packard diode array spectrophotometer HP8452A and a Labsphere RSA-HP-84 reflectance accessory. The quantitative reflectance measurements of different complexes such as Fe (III) with thiocyanate, Cr (VI) with diphenylcarbazide and Ni (II) with dimethylglyoxime could be obtained by forming the complexes on filter paper. Calibration curves were obtained for each metal by plotting the optical density of the reflectance signal (AR) vs. the log of the mol/dm3 concentration, from 1.5 × 103 to 3.6 × 102mol/dm3 for Fe (III), from 8.00 × 10−5 to 2.00 × 103 mol/dm3 for Cr (VI) and from 1.00 × 103 to 8.00 × 102 mol dm3 for Ni (II), with correlation coefficients of 0.9986 for Fe (III), 0.9878 for Cr (VI) and 0.9892 for Ni (II). The results obtai...

Molecularly imprinted solid phase extraction of fluconazole from pharmaceutical formulations

This work encompasses a direct and coherent strategy to synthesise a molecularly imprinted polymer (MIP) capable of extracting fluconazole from its sample. The MIP was successfully prepared from methacrylic acid (functional monomer), ethyleneglycoldimethacrylate (crosslinker) and acetonitrile (porogenic solvent) in the presence of fluconazole as the template molecule through a non-covalent approach. The non-imprinted polymer (NIP) was prepared following the same synthetic scheme, but in the absence of the template. The data obtained from scanning electronic microscopy, infrared spectroscopy, thermogravimetric and nitrogen Brunauer-Emmett-Teller plot helped to elucidate the structural as well as the morphological characteristics of the MIP and NIP. The application of MIP as a sorbent was demonstrated by packing it in solid phase extraction cartridges to extract fluconazole from commercial capsule samples through an offline analytical procedure. The quantification of fluconazole was accomplished through UPLC-MS, which resulted in LOD≤1.63×10(-10) mM. Furthermore, a high percentage recovery of 91±10% (n=9) was obtained. The ability of the MIP for selective recognition of fluconazole was evaluated by comparison with the structural analogues, miconazole, tioconazole and secnidazole, resulting in percentage recoveries of 51, 35 and 32%, respectively.

Modeling kinetic spectrophotometric data of aminophenol isomers by PARAFAC2

Abstract This paper describes an application of PARAFAC2 in the modeling of kinetic-spectrophotometric data. The data were obtained by spectrophotometric monitoring of the reaction between aminophenol isomers and NaNO 2 in acid solution. The data set of various samples produces a three-way data array. This reaction has the property that isomers in different proportions produce different kinetic profiles. Due this property, PARAFAC2 is suitable to model the system because it does not assume parallel proportional kinetic profiles. The results with PARAFAC2 were satisfactory, it being possible to recover the spectral and kinetic profiles, as well as the initial isomer concentrations with good accuracy.

Determinação espectrofotométrica indireta de capsaicinoides em pimentas Capsicum a partir da reação com o complexo de Co(II) com 4-(2-piridilazo) resorcinol

92:8v/v solutions, for quantification of total CAPS in Capsicum peppers. The product of the reaction is CoPAR2CAPS2 and its absorption in aquo-ethanolic solution at 510 nm is proportional to the total CAPS concentration from 0.60 to 17.94 mg L-1. The values of limit of detection and limit of quantification were 0.0004 and 0.001 mg of CAPS/g of pepper, respectively, with 4% relative standard deviation. The developed method yielded similar results to those obtained from high performance liquid chromatography, with 95% of confidence.

A quimiluminescência como ferramenta analítica: do mecanismo a aplicações da reação do luminol em métodos cinéticos de análise

Relevant aspects of proposed mechanisms of the chemiluminescent reaction of luminol are presented and commented to emphasize its perspectives for kinetic analysis. A careful search for analytical applications of this reaction is discussed in order to point out new trends of the studies. Kinetic analysis using the luminol reaction is proposed to be a very attractive due to the good performance of the reaction in analytical applications and the positive characteristics of kinetic analysis, such as low cost and sensibility. It is pointed out that kinetic analysis using the chemiluminescent reaction of luminol should be encouraged.

A Simple, Portable and Low Cost Device for a Colorimetric Spot-Test Quantitative Analysis

ABSTRACT This paper describes a very simple device that can be used for colorimetric quantitative determinations, including spot-test analysis. The sensor is a light detector resistor (LDR) placed into a black PTFE cell and coupled to a low cost multimeter (Ohmmeter). The device has been tested and is easy and fast to use. Quantitative studies were performed with KMnO4 solutions and with the vanadium (V)/PAR/H2O2 system. Calibration curves were obtained by plotting the electric resistance of the LDR against the concentration of the colored species from 0 (blank) to 4.0 × 10-3 mol L-1 for permanganate and from 0 (blank) to 5.0 × 10-5 mol L-1 for vanadium. The detection limit (3σ) was found to be about 5.0 × 10-5 mol L-1 for permanganate and 4.0 × 10-6 mol L-1 for vanadium. The device was used to analyze total vanadium, as vanadium (V), in wastes from an adipic acid plant. The results obtained clearly show that the device can be used for accurate, precise, fast, in situ and low cost colorimetric analysis including quantitative spot-test procedures.

Sobre o desenvolvimento da análise volumétrica e algumas aplicações atuais

Classical methods of analysis played a fundamental role in the development of Chemistry and the chemical industry. They have been tools for analytical procedures since the 18th century, remaining useful until today. The technological appeal of the instrumental methods seems to dazzle the incoming generations of chemists who do not recognize the importance of titrimetry. A short description of the development of titrimetry is presented in order to call attention to historical landmarks for teaching and learning activities in Portuguese. A compilation of some current standard analytical methods that employ titrations is presented to illustrate the availability of titrimetry nowadays.

Synthesis of biodiesel: a contextualized experiment proposal for the general chemistry laboratory

The contextualized understanding of concepts in Chemistry by students from other areas is a challenging task. In this experiment, the synthesis of biodiesel is done by base catalyzed transesterification of refined soy oil with methanol at room temperature and common glassware found in any chemistry laboratory. The proposal permits introducing several concepts, such as that of emulsion, viscosity and catalysis to illustrate an activity based on an actual problem. In this didactic approach, some common problems of biodiesel production, such as soap formation and phase separation, are introduced into the procedure in order to raise questions and motivate the students to participate in the experimental work and stimulate reflections about critical aspects of biodiesel production. This experiment was carried out in the first semester of 2006, in experimental general chemistry taken by physics and agricultural, civil and chemical engineering students of UNICAMP.

The determination of the stoichiometry of the mixed complex of vanadium with hydrogen peroxide and with 4-(2-Pyridilazo) Resorcinol

The present study reports details of the stoichiometric characterization of the mixed complex system, V(H2O2)PAR, formed when vanadium adequately reacts with hydrogen peroxide and with 4-(2-Pyridilazo)Resorcinol. Also the presence of polynuclear species was investigated in order to elucidate about unambiguous assignment of the molar absorptivity, stability constant and composition of the complex. Two mathematical treatments methods of the experimental results were employed. From the results it can be concluded that this system corresponds to a mononuclear complex with 1:1:1 stoichiometry.