A pirólise como técnica analítica

In this paper historical aspects of analytical pyrolysis, the equipment used, the fundamentals and the mechanisms of pyrolysis of different polymeric materials are discussed. The latest work on analytical pyrolysis applied to various types of synthetic and natural samples is reviewed. Current applications of this technique that are discussed include identification of microorganisms, analysis of trace compounds by forensic laboratories, investigation of food and agricultural products, study of the chemical composition of wood, authentication and conservation of artworks, and the study of environmental and geochemical samples.

Integración de visualización científica molecular en el salón de clases

For some years, Chemistry teachers have used scientific visualization software of molecular models in computing rooms and chemistry laboratories for educational purposes. However, its application in classrooms has been limited. This article describes the integration and use of computer programs for scientific molecular visualization in a traditional classroom. We consider that the improvement of technical aspects of their application and use (usability) has a direct effect on students' understanding of molecular structures (including students' extrinsic motivation), among other factors. Consequently, we developed a guide for the integration of hardware and software of molecular visualization for its use in the classroom.

Estrategias en el desarrollo de métodos analíticos para la determinación simultánea de compuestos orgánicos por espectrofotometría derivada

In this work is proposed, a simple experiment for the simultaneous determination of losartan (L) and hydrochlorothiazide (H) in synthetic and real samples by derivative spectrophotometry technique. For the students it is relevant to know this technique for simultaneous determinations of drugs, allowing that the students recognize that this technique is simple, rapid and applicable to quality control. This experimental work, it is proposed in order to being applied to undergraduates into laboratories of analytical chemistry. Furthermore, it is given the integration of the theoretical knowledge with the experimental work; this correlation is of interest for the students.

Construção artesanal de um eletrodo íon seletivo a chumbo(II): uma alternativa para disciplinas experimentais

This works proposes a homemade construction of a lead(II) ISE of solid membrane (Ag2S/PbS) to determine Pb2+ ions in potentiometric titrations, using damaged combined glass electrodes. This electrode can be constructed in teaching laboratories, using it as a learning tool related to the theoretical principle of ISE. The analytical curve obtained (y = 27.056x + 337.58; R = 0.996) was linear on the range of 1 x 10-5 to 1 mol L-1 and has presented a very close behavior of the Nernstian. The homemade ISE has presented a similar selectivity to the commercial electrodes, showing to be a good alternative to the experimental activities on teaching laboratories.

Desempenho analítico de laboratórios prestadores de serviço na determinação de metais em águas

Analytical laboratories are expected to produce reliable results. Decision makers are guided in their actions (financial, legal and environmental) using analytical data provided by numerous laboratories. This work aimed to evaluate the analytical performance of Brazilian laboratories on producing trustworthy results. Nineteen laboratories, accredited and non-accredited ones, were contracted to analyze a USGS (United States Geological Survey) certified water sample for 17 chemical elements (mostly metals) without knowing the origin of the sample. Considering all the results produced, only 35% of them were valid. Three laboratories present satisfactory performances, whereas the majority showed a very poor overall performance. The outcomes of this work show the need for a more effective analytical quality program to Brazilian laboratories.

Validação de metodologia para a caracterização química de bagaço de cana-de-açúcar

In this work, a methodology for the characterization of sugar cane bagasse was validated. Bagasse pre-treated with steam in a 5000 L reactor at a pressure of 15.3 kgf/cm², during 7 min, was used to test the methodology. The methodology consisted of the hydrolysis of the material with H2SO4 at 72% v/v, for the quantification of carbohydrates, organic acid, furfural and hydroxymethylfurfural by HPLC; insoluble lignin and ash by gravimetry; and soluble lignin by spectrophotometry. Linearity, repeatability, reproducibility and accuracy of the results obtained in two Research Laboratories were determined, and were considered to be suitable for the validation of the methodology.

Parâmetros r e R obtidos de programa interlaboratorial: como usá-los

Intralaboratorial and interlaboratorial variabilities can be obtained by conducting an specially designed interlaboratory program. Using the analysis of variance technique one can calculate the r (repeatability) and R (reproducibility) indexes that can help participant laboratories to monitor their routine quality control procedures. An example is described using data obtained from an interlaboratory program where twelve laboratories determined total iron content in silicon metal sample by using flame atomic absorption spectrometry.

Identificação química da clorofenilpiperazina (CPP) em comprimidos apreendidos

Designer drug is a term used to describe psychoactive drugs of abuse which are usually synthesized by modifying the molecular structures of existing drugs of abuse. The term gained widespread popularity when MDMA (ecstasy) experienced a popularity boom in the mid 1980´s. In Brazil, designer drugs seizures have increased in the last few years, and actually tablets with unknown psychoactive compounds began to be forwarded to the Forensic Laboratories. This work describes the analytical assays that were performed to identify the chlorophenylpiperazine, a psychoactive substance first time identified in seized tablets in Sao Paulo state.

Uma métrica gráfica para avaliação holística da verdura de reacções laboratoriais - "Estrela Verde"

A new semi-quantitative metrics, Green Star (GS), for evaluation of the global greenishness of chemical reactions used in teaching laboratories has been developed. Its aim is to help choosing the more acceptable reactions for implementing Green Chemistry (GC) and to identify suitable modifications of reaction protocols to improve the greenishness of chemistry. GS considers globally all the Twelve Principles of GC. To illustrate its construction, the tetraamminecopper(II) sulfate monohydrate laboratory synthesis, performed under several sets of conditions to pursue greenishness, is presented. A comparative study with other GC metrics showed the advantages of GS and that it accomplishes its purpose.

Produção científica e formação de recursos humanos na área de bioquímica em instituições federais do Rio Grande do Sul: fomento estadual

Brazilian scientific production in Biochemistry is growing impressively fast, and Rio Grande do Sul is outstanding in that context. This study aims to outline the state's scientific research profile, given its prominent position in the national scenario. Hence, researchers, laboratories, development of human resources and investments by Foundation for the Support to Research in the State of Rio Grande do Sul (FAPERGS) were identified and mapped. We observed that amount of financial support by FAPERGS decreases in last years. Therefore, there is the necessity to reestablish some of FAPERGS's programs, as well as to increase financial support to Biochemistry departments.

Comparação interlaboratorial para análise de dureza total e cloreto em água

Interlaboratorial comparison of the determination of hardness and chloride in water had been performed by 38 and 37 laboratories, respectively. In all cases the participating laboratories used its routine methods. Homogeneity and stability testing were performed on the samples sent to the laboratories. The codified results are graphically reported and compared to assigned value, determined by the consensus of the laboratories. Satisfactory results were obtained for 71 and 73% of the laboratories, considering hardness and chloride determination, respectively.

Síntese de fotoprotetores e sua imobilização em poli(metacrilato de metilo): um projeto integrado de química orgânica, química de polímeros e fotoquímica

Dibenzalacetone and other aldol condensation products are known sunscreens commonly used in cosmetics. This type of compounds can easily be prepared in an Organic Chemistry Lab by reaction of aldehydes with ketones in basic medium. These compounds can be incorporated in poly(methyl methacrylate) and used as UV light absorbers, for example in sunglasses. This project has the advantage of using inexpensive reagents which are readily available in Chemistry Laboratories. This experiment can also be a base starting point for discussions of organic, polymer and photochemistry topics.

Eletrização de dielétricos: novas propostas para resolver velhos problemas

Electrostatic phenomena were discovered long ago but their interpretation according to well-established atomic-molecular theory is still lacking. As a result, electrostatic phenomena are often irreproducible and uncontrolled, causing serious practical problems. Highly reproducible recent experimental results on electrostatic charging from this and other laboratories are reviewed in this work, together with a description of the relevant but not so usual Kelvin probe and Faraday cup techniques. These results support a new model for electrostatic charging of dielectrics and insulated metals, based on the role of moist atmosphere as a charge reservoir.

Spectrophotometric and spectrofluorimetric determination of some drugs containing secondary amino group in bulk drug and dosage forms via derivatization with 7-Chloro-4-Nitrobenzofurazon

Sensitive and selective spectrophotometric and spectrofluorimetric methods have been developed for determination of some drugs such as Pramipexole, Nebivolol, Carvedilol, and Eletriptan, which commonly contain secondary amino group. The subject methods were developed via derivatization of the secondary amino groups with 7-Chloro-4-Nitrobenzofurazon in borate buffer where a yellow colored reaction product was obtained and measured spectrophotometrically or spectrofluorimetrically. Concentration ranges were found as 2.0 to 250 μg mL-1 and 0.1 to 3.0 μg mL-1, for spectrophotometric and spectrofluorimetric study, respectively. The described methods can be easily applied by the quality control laboratories in routine analyses of these drugs in pharmaceutical preparations.

Estatística aplicada à química: dez dúvidas comuns

Ten common doubts of chemistry students and professionals about their statistical applications are discussed. The use of the N-1 denominator instead of N is described for the standard deviation. The statistical meaning of the denominators of the root mean square error of calibration (RMSEC) and root mean square error of validation (RMSEV) are given for researchers using multivariate calibration methods. The reason why scientists and engineers use the average instead of the median is explained. Several problematic aspects about regression and correlation are treated. The popular use of triplicate experiments in teaching and research laboratories is seen to have its origin in statistical confidence intervals. Nonparametric statistics and bootstrapping methods round out the discussion.