Classificação periódica: um exemplo didático para ensinar análise de componentes principais

A dataset of chemical properties of the elements is used herein to introduce principal components analysis (PCA). The focus in this article is to verify the classification of the elements within the periodic table. The reclassification of the semimetals as metals or nonmetals emerges naturally from PCA and agrees with the current SBQ/IUPAC periodic table. Dataset construction, basic preprocessing, loading and score plots, and interpretation have been emphasized. This activity can be carried out even when students with distinct levels of formation are together in the same learning environment.

Análise térmica aplicada à caracterização da sinvastatina em formulações farmacêuticas

Thermogravimetry (TG) and differential scanning calorimetry (DSC) are used in pharmaceutical studies for drugs characterization, purity, formulations compatibility, polymorphism identification, stability evaluation, and thermal decomposition of drugs and pharmaceutical formulations. Simvastatin showed fusion at 138.5 ºC and thermal stability up to 248 ºC. Simvastatin was incompatible with preservative excipient butylhydroxyanisole (BHA) performing a process of crystal amorphization. The drug showed morphological polymorphism, where it has the same unit cell but with different crystal habits according to the recrystallization solvent.

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.

A análise por injeção sequencial (SIA): vinte anos em uma perspectiva brasileira

The year of 2010 marks the 20th anniversary of the development of Sequential Injection Analysis (SIA) by Ruzicka and Marshall. Considered the second generation of the flow injection methods, this article briefly describes the history, the basic principles of the technique and reviews all papers developed by Brazilian scientists aiming the divulgation of this automation technique in Analytical Chemistry.

Validação e estimativa da incerteza de método para análise de licopeno e β-caroteno em polpa de tomate por cromatografia líquida de alta eficiência

A method to quantify lycopene and β-carotene in freeze dried tomato pulp by high performance liquid chromatography (HLPC) was validated according to the criteria of selectivity, sensitivity, precision and accuracy, and uncertainty estimation of measurement was determined with data obtained in the validation. The validated method presented is selective in terms of analysis, and it had a good precision and accuracy. Detection limit for lycopene and β-carotene was 4.2 and 0.23 mg 100 g-1, respectively. The estimation of expanded uncertainty (K = 2) for lycopene was 104 ± 21 mg 100 g-1 and for β-carotene was 6.4 ± 1.5 mg 100 g-1.

Aplicação de métodos quimiométricos na caracterização de charutos utilizando extração por dispersão da matriz em fase sólida e análise por cromatografia gasosa acoplada à espectrometria de massas

In this work, the organic compounds of cigar samples from different brands were analyzed. The compound extraction was made using the matrix solid-phase dispersion (MSPD) technique, followed by gas chromatography and identification by mass spectrometry (GC-MS) and standards, when available. Thirty eight organic compounds were found in seven different brands. Finally, with the objective of characterizing and discriminating the cigar samples, multivariate statistical analyses were applied to data, e.g.; principal component analysis (PCA) and hierarchical cluster analysis (HCA). With such analyses, it was possible to discriminate three main groups of three quality levels.

Desenvolvimento de métodos de análise por CLAE-UV para os antimicrobianos tetraciclina, sulfametoxazol e trimetoprima utilizando materiais à base de sílica como sistemas de pré-concentração

This paper evaluates the adsorption capacity of zirconocene-based silica materials in the pre-concentration of antimicrobians (tetracycline, sulfamethoxazole and trimethoprim) in aqueous medium. These materials were prepared by grafting the zirconocene onto silicas pre-treated at different temperatures. The retention capacity of these materials was evaluated by off line SPE and HPLC-UV and the proposed methodology was validated in ultrapure, tap and river water. The recovery for tetracycline was 72% (in the solid phase A) and, for sulfamethoxazole and trimethoprim was 68 and 95% in the commercial C18, respectively. The target antimicrobians were not detected in the Arroio Dilúvio (Porto Alegre - RS).

Voltametria de Pulso Diferencial (VPD) em estado sólido de manchas de Cromatografia de Camada Delgada (CCD): um novo método de análise para fitoativos antioxidantes

A new electroanalytical method coupling TLC-DPV in solid state was developed for quantitative determination of phytoantioxidants with medicinal purpose, e.g. rosmarinic acid (RA) in samples of phytopharmaceuticals, e.g. rosemary (Rosmarinus officinalis L.). The method showed to be feasible, presenting linearity in concentrations ranging from 0.694 x 10-3 to 9.526 x 10-3 mol L-1 (r = 0.9945), good sensibility, selectivity, reproducibility, repeatability, agility and affordable cost. The concentrations of RA in different extracts of rosemary ranged from 0.05 to 0.52 (% w/w), presenting high recovery levels when compared to HPLC.

Otimização de método para análise de folatos em hortaliças folhosas por cromatografia líquida de alta eficiência com detecção por fluorescência

We optimized a method for the determination of three main folate isoforms in leafy vegetables. Analysis was carried out by HPLC, using gradient of elution and fluorescence detection. Limits of quantification were 2 ng/mL; 2 ng/mL and 28 ng/mL for tetrahydrofolate (THF), 5-methyltetrahydrofolate (5-MTHF) and 5-formyltetrahydrofolate (5-FTHF), respectively. Recovery rates of THF, 5-MTHF and 5-FTHF varied from 87.86 to 100.64%; 88.12-94.22% and 89.82-106.69%, respectively. Test of repeatability showed relative standard deviation for peak areas lower than 10%. Tests for linearity showed high coefficients of determination. The results showed advances in folates extraction and analysis in raw and cooked leafy vegetables.

Pré-concentração de Cr(III) e análise de especiação de cromo empregando montmorilonita saturada com íons potássio

The clay mineral montmorillonite-K10 (MT), treated under acidic medium and saturated with potassium ions (MTK), was employed in sorption and desorption studies aiming the preconcentration of Cr(III) and the speciation analysis of chromium. The sorption process of Cr(III) was close to 100%, suggesting that MTK was a good material for Cr(III) preconcentration, although, the maximum recovery in HNO3 solution was near 89%. On the other hand, Cr(VI) practically was not retained in MTK, suggesting this material as an appropriate mineral phase to be used in speciation analysis of chromium in aqueous medium.

Estudo das condições de estocagem do bagaço de cana-de-açúcar por análise térmica

An evaluation was made of the properties of sugarcane bagasse during the storage process for subsequent burning in a boiler. Samples of bagasse were collected over a period of 150 days from the Caeté sugar mill (MG) at various points of the stockpile soon after the sugarcane was pressed to extract its juice, as well as from natural bagasse, dry and damp. Thermal analyses of the samples were carried out and the results indicated that, during the storage of bagasse, dry or damp, the biomass loses up to 32% of its calorific power, due to decomposition of the hemicellulose.

Adsorção do corante azul de metileno em partículas de argilominerais: análise dos tamanhos das partículas

Interactions of cationic dye methylene blue (MB) with clay particles in aqueous suspension have been extensively studied. As already known, the number of natural negative charges on the clay modifies significantly the particle sizes dispersed in water and therefore the nature of the interaction with the dye. This work evaluated with UV-Vis spectroscopy method how the clay particle sizes weighted on the adsorption and rearrangement of the dye molecules in aqueous system. The results obtained from light-scattering measurements confirmed that larger particles are found in suspensions containing the high-charged clays as the visible absorption band related to the MB aggregates (570 nm) on these suspensions prevailed.

Identificação de adulteração de biocombustível por adição de óleo residual ao diesel por espectrofluorimetria total 3D e análise das componentes principais

Total spectrofluorimetry associated to Principal Components Analysis (PCA) were used to classify into different groups the samples of diesel oil, biodiesel, vegetal oil and residual oil, as well as, to identify addition of non-transesterified residual vegetable oil, instead of biodiesel, to the diesel oil. Using this method, the samples of diesel oil, mixtures of biodiesel in diesel and mixtures of residual oil in diesel were separated into well-defined groups.

Discriminação entre estádios de maturação e tipos de processamento de pós-colheita de cafés arábica por microextração em fase sólida e análise de componentes principais

A fruit chemical composition reflects its maturation stage. For coffee, it is also the reflex of the post-harvesting processing type, dry, semi-wet and wet. The object of this work was to verify if headspace solid phase microextraction coupled to gas chromatography (HS-SPME-GC) could be used to discriminate between samples harvested in different maturation stages and treated by different processes. With application of principal component analysis to the area of 117 compounds extracted by SPME, using divinylbenzene/Carboxen/polydimethylsiloxane fiber, it was possible to discriminate, in the roasted and ground coffee, the maturity stage and processing type used .

Construção de uma célula de gás de baixo custo para análise no infravermelho

Infrared spectroscopy is a versatile technique used for qualitative and quantitative determination of all types of molecular species. As far as analysis of confined or flowing gases is concerned, different types of cell can be found in the market, but they are often very expensive. This study describes the construction of a very efficient gas cell with good reproducibility for qualitative infrared analysis of confined or flowing gases, using easily available and low-cost materials.