Preparo de amostras de combustíveis fósseis por piroidrólise para a determinação de flúor e cloro

Pyrohydrolysis is proposed for fossil fuels sample preparation for further fluorine and chlorine determination. Samples were heated during 10 min at temperatures up to 1000 °C. Water vapor was passed through the reactor and the volatile products were condensed and collected in NH4OH solution. Fluoride was determined by potentiometry using an ion selective electrode (ISE) and Cl by ICP OES and DRC-ICP-MS. The results are in good agreement with certified values and the precision is better than 10% (n = 4). Sample preparation by means of pyrohydrolysis is relatively simple, whereas chlorine and fluorine can be determined at low concentrations.

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.

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.

Capacidade de oxidação como índice de estabilidade da matéria orgânica de sedimentos de acordo com gradiente fluvial-estuarino do rio Paraíba do Sul

The hummus composition and it redox properties have been used to evaluate the organic matter quality from natural systems. The objectives of this study were the fractionation of the organic matter and the determination of the oxidation capacity of humic acids to evaluate the organic matter quality of sediments from a gradient fluvial-estuarine in the Brazilian Southeast. The carbon/nitrogen and humic acid/fulvic acid relationships of the organic matter and of the oxidation capacity of humic acids were positively correlated and followed the order: estuarine bordered mangroves ≅ fluvial bordered urban center and pasture > estuarine bordered pasture ≅ marine.

Análise térmica aplicada a fármacos e formulações farmacêuticas na indústria farmacêutica

Several matters of the pharmaceutical demonstrate the great importance of thermal analysis application, especially TG and DSC for the pharmaceutical industry future, namely: characterization of the drugs with the thermal events definition, in studies of drug purity, in the polymorphs identification, in compatibility studies of solid dosage pharmaceutical formulations, in drugs and pharmaceutical formulations thermal stability, and in determination of shelf life for isothermal degradation kinetics by extrapolation using the Arrhenius equation. Thus, the test results obtained from thermal analysis are directly related to the quality of a pharmaceutical product, whether the stability or bioavailability of the pharmaceutical product.

Estudo por espectrometria de massas de soluções de hidróxi(tosilóxi)iodobenzeno: propostas para mecanismos de desproporção

Solutions of [hydroxy(tosyloxy)iodo]benzene (HTIB or Koser's reagent) in acetonitrile were analyzed using high resolution electrospray ionization mass spectrometry (ESI-MS) and electrospray ionization tandem mass spectrometry (ESI-MS/MS) under different conditions. Several species were characterized in these analyses. Based on these data, mechanisms were proposed for the disproportionation of the iodine(III) compounds in iodine(V) and iodine(I) species.

Extração/pré-concentração de íons cobre no ponto nuvem explorando a formação de complexos com DMIT [4,5-dimercapto-1,3-ditiol-2-tionato]

The present study proposes a method for cloud point preconcentration of copper ions at pH 2.0 based on complexes formed with [4,5-dimercapto-1,3-dithyol-2-thionate] and subsequent determination by flame atomic absorption spectrometry (FAAS). Under optimal analytical conditions, the method provided limits of detection of 0.84 and 0.45 µg L-1, by preconcentrating 12.0 and 24.0 mL of sample, respectively. The method was applied for copper determination in water samples, synthetic saliva, guarana powder, tea samples and soft drinks and the accuracy was assessed by analyzing the certified reference materials Dogfish Liver (DOLT-4) and Lobster Hepatopancreas (TORT-2).

A Importância da determinação analítica de intermediários reativos e de seus produtos de reações com biomacromoléculas: uma mini revisão

Metabolic reactive intermediates can react with biomolecules such as DNA and proteins to produce adducts. Recently, research has shown that such adducts can act as precursors of some chronic diseases (cancer, Parkinson's, immunologic system diseases, etc.), and their determination is important because they are biomarkers of undesirable health effects. These compounds are produced at very low concentrations, but the development and dissemination of sensitive new analytical tools, especially those based on chromatography coupled to other analytical instruments, make such determinations possible. This mini review is focused on the formation of reactive intermediates, their reaction with biomolecules, and the importance of their determination.

EXTRAÇÃO ASSISTIDA POR ULTRASSOM PARA DETERMINAÇÃO COLORIMÉTRICA DE FERRO EM SOLO: UMA COMPARAÇÃO COM ESPECTROMETRIA DE MASSA COM PLASMA INDUTIVAMENTE ACOPLADO

A simple procedure for ultrasound-assisted extraction and colorimetric determination of iron in soil samples was developed. The iron concentration in the analyzed samples was determined by the colorimetric method and the results compared with inductively coupled plasma mass spectrometry (ICP-MS). Fifteen soil samples were analyzed and the iron concentration results compared with those obtained by ICP-MS using microwave-assisted sample digestion. The proposed procedure showed good efficiency for iron extraction and the results obtained by colorimetric determination exhibited good agreement with ICP-MS. Moreover, ultrasound-assisted extraction and colorimetric determination is a simple, fast and low-cost procedure for application in routine analysis.

Product costing model for laser welded hollow core steel panels

The aim of the study was to create an easily upgradable product costing model for laser welded hollow core steel panels to help in pricing decisions. The theory section includes a literature review to identify traditional and modern cost accounting methodologies, which are used by manufacturing companies. The theory section also presents the basics of steel panel structures and their manufacturing methods and manufacturing costs based on previous research. Activity-Based costing turned out to be the most appropriate methodology for the costing model because of wide product variations. Activity analysis and the determination of cost drivers based on observations and interviews were the key steps in the creation of the model. The created model was used to test how panel parameters affect the costs caused by the main manufacturing stages and materials. By comparing cost structures, it was possible to find the panel types that are the most economic and uneconomic to manufacture. A sensitivity analysis proved that the model gives sufficiently reliable cost information to support pricing decisions. More reliable cost information could be achieved by determining the cost drivers more accurately. Alternative methods for manufacturing the cores were compared with the model. The comparison proved that roll forming can be more advantageous and flexible than press brake bending. However, more extensive research showed that roll forming is possible only when the cores are designed to be manufactured by roll forming. Due to that fact, when new panels are designed consideration should be given to the possibility of using roll forming.

MODELING A COMPUTER APPLICATION FOR MANAGEMENT OF MAINTENANCE ACTIVITIES OF UNPAVED ROADS

ABSTRACTThis study presents a contribution to the modeling of a computer application employing a method of serviceability performance for unpaved roads, aiming the management of maintenance/restoration activities of the primary surface layer. The proposed methodology consisted of field inspections during dry (April to September) and rainy (October to March) periods, during which objective evaluations were performed to survey of defects and their densities and degrees of severity. To aid the functional classification of analyzed road sections and the determination of the defect with major influence on the serviceability of these roads, the method of serviceability performance proposed by Silva (2009)was implemented in the Visual Basic for Applications (VBA) language in Microsoft Excel software. With the use of the computer application proposed it was possible to identify among the defects analyzed in field, through the index of serviceability of the sampling unit per defect type (ISUdef), which one had the greatest influence on determining the relative serviceability index per road section (IST). The results allow us to conclude that the computer application Road achieved satisfactory results, since the objective evaluation criteria applied to road sections denotes consistency regarding their serviceability.

The position effect of structural Eucalyptus round timber on the flexural modulus of elasticity

Round timber has great use in civil construction, performing the function of beams, columns, foundations, poles for power distribution among others, with the advantage of not being processed, such as lumber. The structural design of round timber requires determining the elastic properties, mainly the modulus of elasticity. The Brazilian standards responsible for the stiffness and strength determination of round timber are in effect for over twenty years with no technical review. Round timber, for generally present an axis with non-zero curvature according to the position of the element in the bending test, may exhibit different values of modulus of elasticity. This study aims to analyze the position effect of Eucalyptus grandis round timber on the flexural modulus of elasticity. The three-point bending test was evaluated in two different positions based on the longitudinal rotation of the round timber element. The results revealed that at least two different positions of the round timber element are desired to obtain significant modulus of elasticity.

Fetal heart rate responses during maternal resistance exercise: a pilot study

PURPOSE: To determine fetal heart rate (FHR) responses to maternal resistance exercise for the upper and lower body at two different volumes, and after 25 minutes post-exercise.METHODS: Ten pregnant women (22-24 weeks gestation, 25.2±4.4 years of age, 69.8±9.5 kg, 161.6±5.2 cm tall) performed, at 22-24, 28-32 and 34-36 weeks, the following experimental sessions: Session 1 was a familiarization with the equipment and the determination of one estimated maximum repetition. For sessions 2, 3, 4 and 5,FHR was determined during the execution of resistance exercise on bilateral leg extension and pec-deck fly machines, with 1 and 3 sets of 15 repetitions; 50% of the weight load and an estimated repetition maximum. FHR was assessed with a portable digital cardiotocograph. Results were analyzed using Student's ttest, ANOVA with repeated measures and Bonferroni (α=0.05; SPSS 17.0).RESULTS: FHR showed no significant differences between the exercises at 22-24 weeks (bilateral leg extension=143.8±9.4 bpm, pec-deck fly=140.2±10.2 bpm, p=0.34), 28-30 weeks (bilateral leg extension=138.4±12.2 bpm, pec-deck fly=137.6±14.0 bpm, p=0.75) and 34-36 weeks (bilateral leg extension=135.7±5.8 bpm, pec-deck fly=139.7±13.3 bpm, p=0.38), between the volumes(bilateral leg extension at 22-24 weeks: p=0.36, at 28-30 weeks: p=0.19 and at 34-36 weeks: p=0.87; pec-deck fly at 22-24 weeks: p=0.43, at 28-30 weeks: p=0.61 and at 34-36 weeks: p=0.49) and after 25 minutes post-exercise.CONCLUSION: Results of this pilot study would suggest that maternal resistance exercise is safe for the fetus.

Estimating Attractor Dimension on the Nonlinear Pendulum Time Series

Chaotic dynamical systems exhibit trajectories in their phase space that converges to a strange attractor. The strangeness of the chaotic attractor is associated with its dimension in which instance it is described by a noninteger dimension. This contribution presents an overview of the main definitions of dimension discussing their evaluation from time series employing the correlation and the generalized dimension. The investigation is applied to the nonlinear pendulum where signals are generated by numerical integration of the mathematical model, selecting a single variable of the system as a time series. In order to simulate experimental data sets, a random noise is introduced in the time series. State space reconstruction and the determination of attractor dimensions are carried out regarding periodic and chaotic signals. Results obtained from time series analyses are compared with a reference value obtained from the analysis of mathematical model, estimating noise sensitivity. This procedure allows one to identify the best techniques to be applied in the analysis of experimental data.

Ion mobility spectrometry in liquid analysis

Ion mobility spectrometry (IMS) is a straightforward, low cost method for fast and sensitive determination of organic and inorganic analytes. Originally this portable technique was applied to the determination of gas phase compounds in security and military use. Nowadays, IMS has received increasing attention in environmental and biological analysis, and in food quality determination. This thesis consists of literature review of suitable sample preparation and introduction methods for liquid matrices applicable to IMS from its early development stages to date. Thermal desorption, solid phase microextraction (SPME) and membrane extraction were examined in experimental investigations of hazardous aquatic pollutants and potential pollutants. Also the effect of different natural waters on the extraction efficiency was studied, and the utilised IMS data processing methods are discussed. Parameters such as extraction and desorption temperatures, extraction time, SPME fibre depth, SPME fibre type and salt addition were examined for the studied sample preparation and introduction methods. The observed critical parameters were extracting material and temperature. The extraction methods showed time and cost effectiveness because sampling could be performed in single step procedures and from different natural water matrices within a few minutes. Based on these experimental and theoretical studies, the most suitable method to test in the automated monitoring system is membrane extraction. In future an IMS based early warning system for monitoring water pollutants could ensure the safe supply of drinking water. IMS can also be utilised for monitoring natural waters in cases of environmental leakage or chemical accidents. When combined with sophisticated sample introduction methods, IMS possesses the potential for both on-line and on-site identification of analytes in different water matrices.