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.

O modelamento estatístico de misturas: experimento tutorial usando voltametria de redissolução anódica

This work illustrates the modeling procedure for a solvent mixture using the simplex- centroid approach. The selected experiment was the optimization of the peak current observed in the direct determination of nickel by anodic stripping voltammetry (ASV) in a solvent mixture composed of N,N-dimethylformamide, ethanol and water. The text is presented in a tutorial way, showing in detail the several steps which must be followed in such a process. Since not all possible mixtures lead to a measurable instrumental response, pseudocomponents had to be used to rescale the experimental design. This also allows to show how to apply this tool, usually troublesome for non-specialists in mixture modeling procedures.

Constituição de professores universitários de disciplinas sobre ensino de Química

This paper focuses on the teaching development practice in the field of chemistry covering such disciplines as chemistry teaching practice, chemistry teaching instrumentation and chemistry teaching methodology and/or didactics, thereby describing and analysing the logics of the development practice and the role of teachers as well as the epistemological identity configurations (knowledges which are proper to said identity) within this discipline field.

Classificação de água de coco processada e natural por meio de HCA, PCA e teores de íons metálicos determinados por ICP OES

Inductively Coupled Plasma Optical Emission Spectrometry was used to determine Ca, Mg, Mn, Fe, Zn and Cu in samples of processed and natural coconut water. The sample preparation consisted in a filtration step followed by a dilution. The analysis was made employing optimized instrumental parameters and the results were evaluated using methods of Pattern Recognition. The data showed common concentration values for the analytes present in processed and natural samples. Principal Component Analysis (PCA) and Hierarchical Cluster Analysis (HCA) indicated that the samples of different kinds were statistically different when the concentrations of all the analytes were considered simultaneously.

Determinação de nitrito em águas utilizando extrato de flores

Aspects of visible spectrophotometry can be presented to students using simple experiments in which the color of the crude extract of Macroptilium lathyroides (L.) Urb. is bleached in the presence of nitrite ions in acidic medium. The dependence of the absorption intensity with time, the reaction completeness and the Beer law can be demonstrated. Quantitative results for mineral water samples "contaminated" with nitrite ions were obtained from a method based on the Griess reaction and a procedure based on the bleaching reaction between the crude extract and NO2- ions. Both the Griess and the bleaching reactions were found to be time dependent. Recoveries of about 100 - 104% were obtained with these procedures. The use of natural dyes attracted students' interest enhancing the teaching process. Experiments performed by the teaching staff suggested that the proposed methodology can be performed in a 4 h class, with relative errors ranging from 0.19 to 1.86% in relation to the Griess method.

Reconhecimento de padrões por métodos não supervisionados: explorando procedimentos quimiométricos para tratamento de dados analíticos

An activity for introducing hierarchical cluster analysis (HCA) and principal component analysis (PCA) during the Instrumental Analytical Chemistry course is presented. The posed problem involves the discrimination of mineral water samples according to their geographical origin. Thirty-seven samples of 9 different brands were considered and the results from the determination of Na, K, Mg, Ca, Sr and Ba were taken into account. Non-supervised methods for pattern recognition were explored to construct a dendrogram, score and loading plots. The devised activity can be adopted for introducing Chemometrics devoted to data handling, stressing its importance in the context of modern Analytical Chemistry.

Titulações espectrofotométricas de sistemas ácido-base utilizando extrato de flores contendo antocianinas

Considering the attraction of the students' attention by the changes in the colors of vegetable crude extracts caused by the variation of the pH of the medium, the use of these different colors in order to demonstrate principles of spectrophotometric acid-base titrations using the crude extracts as indicators is proposed. The experimental setup consisted of a simple spectrophotometer, a homemade flow cell and a pump to propel the fluids along the system. Students should be stimulated to choose the best wavelength to monitor the changes in color during the titration. Since the pH of the equivalence point depends on the system titrated, the wavelength must be properly chosen to follow these changes, demonstrating the importance of the correct choice of the indicator. When compared with the potentiometric results, errors as low as 2% could be found using Rhododendron simsii (azalea) or Tibouchina granulosa (Glory tree, quaresmeira) as sources of the crude extracts.

O estado da arte da cromatografia associada à espectrometria de massas acoplada à espectrometria de massas na análise de compostos tóxicos em alimentos

Chromatography combined with several different detection systems is one of the more used and better performing analytical tools. Chromatography with tandem mass spectrometric detection gives highly selective and sensitive analyses and permits obtaining structural information about the analites and about their molar masses. Due to these characteristics, this analytical technique is very efficient when used to detect substances at trace levels in complex matrices. In this paper we review instrumental and technical aspects of chromatography-tandem mass spectrometry and the state of the art of the technique as it is applied to analysis of toxic substances in food.

Determinação não destrutiva do nitrogênio total em plantas por espectroscopia de reflectância difusa no infravermelho próximo

Diffuse reflectance near-infrared (DR-NIR) spectroscopy associated with partial least squares (PLS) multivariate calibration is proposed for a direct, non-destructive, determination of total nitrogen in wheat leaves. The procedure was developed for an Analytical Instrumental Analysis course, carried out at the Institute of Chemistry of the State University of Campinas. The DR-NIR results are in good agreement with those obtained by the Kjeldhal standard procedure, with a relative error of less than ± 3% and the method may be used for teaching purposes as well as for routine analysis.

Determinação de paládio em amostras biológicas aplicando técnicas analíticas nucleares

This study presents Pd determinations in bovine tissue samples containing palladium prepared in the laboratory, and CCQM-P63 automotive catalyst materials of the Proficiency Test, using instrumental thermal and epithermal neutron activation analysis and energy dispersive X-ray fluorescence techniques. Solvent extraction and solid phase extraction procedures were also applied to separate Pd from interfering elements before the irradiation in the nuclear reactor. The results obtained by different techniques were compared against each other to examine sensitivity, precision and accuracy.

Uso de scanner em espectrofotometria de absorção molecular: aplicação em experimento didático enfocando a determinação de ácido ascórbico

Quantitative analysis of colored substances is generally performed using a spectrophotometer for detection of radiation. However, the combination of digital images and mathematical conversion of colors is an alternative for quantitative procedures based on colored chemical reactions. This work proposes a didactic experiment using a scanner for determination of ascorbic acid in medicines based on the formation of the Prussian blue complex. Results were in good agreement with a conventional spectrophotometer method and the procedure is attractive for instrumental analysis undergraduate courses.

Espectrometria de absorção atômica: o caminho para determinações multi-elementares

This paper present an overview of way covered for the spectrometry of atomic absorption (AAS), tracing a line of the historical events in its development and its establishment as a multielement technique. Additionally, the efforts carried by through several researchers in the search for the instrumental evolution, the advances, advantages, limitations, and trends of this approach are related. Several works focusing its analytical applications are cited employing simultaneous multielement determination by flame (FAAS) and/or graphite furnace (GF AAS), and fast sequential multielement determination using FAAS are reported in the present review.

Experimento didático sobre cromatografia gasosa: uma abordagem analítica e ambiental

This paper describes an experiment to teach the principles of gas chromatography exploring the boiling points and polarities to explain the elution order of a series of alcohols, benzene and n-propanone, as well as to teach the response factor concept and the internal standard addition method. Retention times and response factors are used for qualitative identification and quantitative analysis of a hypothetical contamination source in a simulated water sample. The internal standard n-propanol is further used for quantification of benzene and n-butanol in the water sample. This experiment has been taught in the instrumental analysis course offered to chemistry and oceanography students.

Eletrocromatografia capilar: contextualização, estado da arte e perspectivas

Capillary electrochromatography (CEC) is a separation technique in which the mobile phase flow is based on the application of a voltage across a packed capillary, which generates an electroosmotic flow that transports the analytes along the capillary toward the detector. As it combines the separation mechanisms of high-performance liquid chromatography (HPLC) and of capillary electrophoresis (CE), CEC can be considered a hybrid of HPLC and CE. This review presents some fundamental aspects of CEC and is focused on the instrumental advances of the technique, such as column technology, operation modes and detection systems, presenting recent papers on these topics and some applications and perspectives about CEC.

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.