Validação de métodos cromatográficos de análise: um experimento de fácil aplicação utilizando cromatografia líquida de alta eficiência (CLAE) e os princípios da "Química Verde" na determinação de metilxantinas em bebidas

The validation of analytical methods is an important step in quality control. The main objective of this study is to propose an HPLC experiment to verify the parameters of validation of chromatographic methods, based on green chemistry principles, which can be used in experimental courses of chemistry and related areas.

Efeito da acidez e de modificadores orgânicos na determinação de metilxantinas: um experimento de cromatografia liquida de alta eficiência (CLAE) empregando otimização uni e multivariada

In this work a new experiment using HPLC is proposed in order to explore the role of acidity and the organic modifiers in the determination of methylxanthines in tea and coffee. Multivariate and univariate optimizations of the experimental conditions were used.

Determinação de ácido acéttico em amostra de vinagre adulterada com ácido clorídrico - um experimento integrado de titulação potenciométrica e condutométrica

The determination of acetic acid in vinegar adulterated sample using simultaneous potentiometric and condutometric titrations was used as an example of integrated experiment in instrumental analysis. An Excel® spreadsheet, which allows the entry of simultaneous data and the construction of the superimposed experimental curves (condutometric, potentiometric, first and second derivative potentiometric curve and, distribution diagrama of the acetic species as function of pH), was used as powerful tool to discuss the fundamental concepts involved in each technique and choose the best of them to quantify, without mutual interference, H3CCOOH and HCl in vinegar adulterated sample.

Adsorção e propriedades de volume de misturas binárias água álcool: um experimento didático com base em medidas de tensão superficial

An undergraduate physical chemistry experiment based on the drop counting method for surface tension measurements is proposed to demonstrate adsorption isotherms of binary aqueous solutions of ethanol, n-propanol, and n-butanol. Excess surface is obtained by the derivative of surface tension taken with respect to alcohol activity, after this activity calculation using van Laar equation. Laboratory class contents are surface tension, excess surface, percolation of hydrogen bonds, micelle, activity, and ideal solution.

O experimento de Clement-Desormes no século XXI

The Clement-Desormes experiment is reviewed. By reason of a finite difference between the pressure within the system and its surroundings, Bertrand and McDonald have criticized the usual consideration of the adiabatic expansion as reversible. Garland, Nibler and Shoemaker oppose, defining regions through virtual boundaries where the surroundings do not operate. For Holden, the use of virtual boundaries is expendable. Experiments cannot support a hypothesis testing due to experiment's intrinsic uncertainty. The role of polytropy in uncertainty is discussed. Both thermodynamic definitions and kinetic model depict the real processes as irreversible phenomena and the reversible ones as a limiting hypothetical case.

Acetatos homo e heterotrinucleares de ferro: um experimento para o laboratório de química de coordenação

Homo and heterotrinuclear acetates are unique compounds having μ3-oxo bridge and many interesting properties of such compounds are derived from this structure. Some undergraduate inorganic textbooks discuss several aspects of these compounds and we present here an undergraduate experiment for the high-yield synthesis of [Fe2MO(CH3CO2)6(H 2O)3], with M = Fe3+, Co2+ and Ni2+, as well as their characterization using infrared spectroscopy and cyclic voltametry. The proposed experiment gives the opportunity to discuss several concepts of coordination chemistry that follow the characterization techniques, such as: types of acetate coordination, reversibility of electrochemical processes, quelate and trans effects and lability.

Eixo quinário: um elemento de simetria presente em moléculas e quasi-cristais - um experimento didático em cristalografia

Axis of quinary symmetry occur in molecular symmetry, as in the case of fullerenes, and in crystalline symmetry, in the quasicrystals. Minerals with pentagonal faces do not have this element of symmetry, as the pyrite (FeS2) which shows a ridge that is different from the other ones, in any face of the crystal. The purpose of this paper is to demonstrate conceptual differences between pyritohedron and regular pentagonal dodecahedron symmetries, discussing students' difficulties to identify them. Also is proposed a didactic experiment with spatial models of the above-mentioned forms and the demonstration of its symmetries in clinographic projections.

Fracionamento de polifosfato de sódio e caracterização por RMN de 31P: um experimento para aulas de físico-química

This text describes an experiment on fractional precipitation of a polymer together with determination of average degree of polymerization by NMR. Commercial sodium polyphosphate was fractionated by precipitation from aqueous solution by adding increasing amounts of acetone. The polydisperse salt and nine fractions obtained from it were analyzed by 31P Nuclear Magnetic Resonance and the degree of polymerization of the salts and of the fractions were calculated. Long-chain sodium polyphosphate was also synthesized and analyzed. This experiment was tested in a PChem lab course but it can be used also to illustrate topics of inorganic polymers and analytical chemistry.

Tratamento de resíduos de corante por eletrofloculação: um experimento para cursos de graduação em química

This paper describes the use of a simple experiment of electroflocculation for classroom in Chemistry. Parameters such as electrode material, current density and temperature direct influence the process efficiency. Due to the process low cost and efficient color removal, the methodology proposed has shown good potential for use in wastewater treatment. In addition, the proposed experiment allows discussion about environmental electrochemistry, introduction to concepts of water contamination by industry and university, and also about different alternatives in wastewater treatment used nowadays. Finally, the very easy operation make possible to easy adapt this experiment for high school and elementary school.

Avaliação do efeito de gases poluentes na corrosão metálica: um experimento para o ensino da corrosão

In this work one proposes a didactic experience to simulate atmospheric corrosion of copper and nickel, due to sulfur dioxide presence. This is an opportunity to understand some basic aspects of atmospheric corrosion, by using fundamental concepts in chemistry, reactions of extraction and characterization of pollutants, as well as their participation in corrosion process. This subject opens a space for discussion about necessity of pollutant gases emissions control for preservation of materials and the environment.

Efeitos da história térmica nas propriedades do polímero pet: um experimento para ensino de análise térmica

Polyethilenetherephtalate (PET) is commonly used in manufacturing of beverage bottles representing a didactic appeal in thermal analysis education due to its presence in the student's day life. Additionally such polymer presents well defined thermal analytical curves and a well known thermal behavior. TGA curve is used to present the thermal stability. The thermal history effects in the thermal properties of a PET sample from a soft drink bottle are used to demonstrate the effect of different heating/cooling conditions on glass transition, melting, crystallization and crystalline degree using DSC curves.

Experimento didático de quimiometria para análise exploratória de óleos vegetais comestíveis por espectroscopia no infravermelho médio e análise de componentes principais: um tutorial, parte I

This manuscript aims to show the basic concepts and practical application of Principal Component Analysis (PCA) as a tutorial, using Matlab or Octave computing environment for beginners, undergraduate and graduate students. As a practical example it is shown the exploratory analysis of edible vegetable oils by mid infrared spectroscopy.

Redução enzimática do 4-(dimetilamino)benzaldeído com pedaços de cenoura (Daucus carota): um experimento simples na compreensão da biocatálise

The present paper describes a simple, low-costly and environmentally friendly procedure for reduction of 4-(dimethylamino)benzaldehyde using carrot bits in water. This interdisciplinary experiment can be used to introduce the concepts of biocatalysis and green chemistry to undergraduate students.

Síntese da Epoxone a partir de D-frutose: um experimento didático em laboratório de Química Orgânica com foco nos princípios da Química Verde

In recent years, the introduction of the Green Chemistry concepts in undergraduate chemistry classes has been intensively pursued. In this regard, the two-step preparation of Epoxone (an organocatalyst developed by Shi & col.) from commercial D-fructose, through ketalization of vicinal diols followed by oxidation of a sterically congested secondary alcohol, involves important topics in Organic Chemistry and employs inexpensive and nontoxic reagents. The reactions are easy to perform and the products from both steps are readily obtained as crystalline solids after simple procedures, thus facilitating their chemical characterization.

Experimento didático de quimiometria para calibração multivariada na determinação de paracetamol em comprimidos comerciais utilizando espectroscopia no infravermelho próximo: um tutorial, parte II

The aim of this manuscript was to show the basic concepts and practical application of Partial Least Squares (PLS) as a tutorial, using the Matlab computing environment for beginners, undergraduate and graduate students. As a practical example, the determination of the drug paracetamol in commercial tablets using Near-Infrared (NIR) spectroscopy and Partial Least Squares (PLS) regression was shown, an experiment that has been successfully carried out at the Chemical Institute of Campinas State University for chemistry undergraduate course students to introduce the basic concepts of multivariate calibration in a practical way.