Acoplamento de cela de difusão gasosa a sistema de análise por injeção seqüencial visando a determinação espectrofotométrica de sulfeto

A new configuration for coupling a gas diffusion cell to a sequential injection system is presented. The matrix exchange is made without the need for additional rotary injection valves or peristaltic pumps, keeping the original mechanical components of the sequential injection apparatus: one syringe pump (or peristaltic pump) and one selection valve. The system was tested constructing analytical curves for sulfide exploring the formation of the methylene blue dye. The proposed method has a detection limit of 60 µg L-1 S2-, with a linear dynamic range between 0.10 and 4.0 mg L-1 S2- concentrations, with a sampling frequency of 20 h-1.

Determinação de arsênio em águas contaminadas usando fluorescência de raios-X por energia dispersiva

This work proposes a simple, fast and inexpensive method to determine As in natural waters, using X-ray fluorescence. 50 µL of each sample containing 100 mg L-1 of yttrium as internal standard were deposited over a 2.5 µm thickness MylarTM film. The samples were dried at 50 °C for 2 h. X-ray spectra were obtained using an EDXRF apparatus. The accuracy was determined by analyte addition/recovery and by comparison with Hydride Generation Atomic Absorption Spectrometry (HG AAS). A recovery of about 100% was obtained and the results were in good agreement with HG AAS. The method showed a relative standard deviation of 6.8% and a detection limit of 10.5 µg L-1 of As.

Espectroscopia de fotoelétrons de limiares de átomos e moléculas

A threshold photoelectron spectrometer applied to the study of atomic and molecular threshold photoionization processes is described. The spectrometer has been used in conjunction with a toroidal grating monochromator at the National Synchrotron Radiation Laboratory (LNLS), Brazil. It can be tuned to accept threshold electrons (< 20 meV) and work with a power resolution of 716 (~18 meV at 12 eV) with a high signal/noise ratio. The performance of this apparatus and some characteristics of the TGM (Toroidal Grating Monochromator) beam line of LNLS are described and discussed by means of argon, O2 and N2 threshold photoelectron spectra.

A convenient method for the determination of moisture in aromatic plants

A method is proposed for the determination of the moisture content of aromatic plants. This method is based on the co-distillation of the starting material in a modified Clevenger apparatus with four organic solvents (toluene, cyclohexane, dichloromethane and carbon tetrachloride). The results were compared with those obtained by oven drying at 105 ºC and steam distillation of the essential oil. The efficiencies of the methods were shown to be equivalent. The solvent distillation method was more practical, especially with respect to operating time (2 h).

Um aparato para monitorar reações rápidas: um "stopped-flow" artesanal de baixo custo

The modern stopped-flow reaction analyzer has shown high efficiency and flexibility, which provides outstanding sample economy with a dead-time of less than 1 ms. However the cost of the equipment imposes a serious restriction to many Brazilian scientists and teachers. In this work we describe the construction of a low-cost stopped-flow system coupled to a UV-Vis spectrophotometer. The performance of the system was checked by monitoring the kinetics of two reactions: the fading of phenolphthalein in aqueous alkaline solution and the chlorophyll a demetallation in acid medium. The apparatus showed reasonable efficiency with a dead-time of 0.3 to 0.5 s. The very good results obtained in these two illustrative processes show that the system is satisfactory for determining rate constants with mean reaction times ranging from seconds to minutes.

A technique for high recoveries from vacuum distillations

The design and use of a novel apparatus for a variant of vacuum distillation is described. Relative to a conventional device, the apparatus/technique described permits superior recovery of multigram quantities of moderately volatile liquids from vacuum distillations.

Um sistema simples para preparação de microesferas de quitosana

This article describes the construction and optimization of an inexpensive apparatus for the production of uniform and porous chitosan microspheres. It also describes the control of the main operational parameters and strategies for the production of uniform chitosan microspheres.

Construção de um espectrógrafo de projeção e sua utilização em demonstrações de espectroscopia óptica

This article describes a projection spectrograph for use in optical spectroscopy classrooms demonstrations. The apparatus is based on an overhead projector and permits the visualization of several phenomena such as, light dispersion by diffraction gratings, diffraction order, optical fluorescence, continuous and discrete optical emission spectra, and light absorption by liquids and solids. A historical survey about the optical spectroscopy development is also presented.

Distinção entre cachaças destiladas em alambiques e em colunas usando quimiometria

One hundred fifteen cachaça samples derived from distillation in copper stills (73) or in stainless steels (42) were analyzed for thirty five itens by chromatography and inductively coupled plasma optical emission spectrometry. The analytical data were treated through Factor Analysis (FA), Partial Least Square Discriminant Analysis (PLS-DA) and Quadratic Discriminant Analysis (QDA). The FA explained 66.0% of the database variance. PLS-DA showed that it is possible to distinguish between the two groups of cachaças with 52.8% of the database variance. QDA was used to build up a classification model using acetaldehyde, ethyl carbamate, isobutyl alcohol, benzaldehyde, acetic acid and formaldehyde as chemical descriptors. The model presented 91.7% of accuracy on predicting the apparatus in which unknown samples were distilled.

Un sistema para la deteccion de antioxidantes volatiles comunmente emitidos desde especias y hierbas medicinales

An apparatus which allows the direct measurement of the antioxidant capacity of volatiles compounds emitted from some herbs and culinary spices is described. The device comprises: a sample chamber, a mixing chamber, a pump and, a detection system. Volatiles from Clove (Syzygium aromaticum (L.) Merr. & L.M. Perry) were purged and captured into a DPPH-containing solution and changes in the absorbance were recorded on-line. Linear response was observed when temperature was set between 30-53 ºC; nitrogen flow was 15 mL min-1 during 60 min; DPPH concentration was 20 µmol L-1 and a sample size (powdered Clove) ranged between 200-1000 mg.

Development and validation of a dissolution test for telithromycin in coated tablets

A dissolution test for telithromycin tablets was validated and developed. In order to choose the most discriminatory one, the conditions to carry out are 900 mL of sodium phosphate buffer at pH 7.5, paddles at 50 rpm stirring speed, time test set to 60 min and using USP apparatus 2 with paddles. The UV spectrophotometric method for determination of telithromycin released was developed and validated. The method presents linearity (r = 1) in the concentration range of 20-60 µg/mL. Precision and recoveries were good, 100.62 and 97.06%, respectively. The method was successfully used for the dissolution test of telithromycin tablets.

Development of dissolution method for benznidazole tablets

The aim of this work was the development of a dissolution method for benznidazole (BNZ) tablets. Three different types of dissolution media, two stirring speeds and apparatus 2 (paddle) were used. The accomplishment of the drug dissolution profiles was compared through the dissolution efficiency. The assay was performed by spectrophotometry at 324 nm. The better conditions were: sodium chloride\hydrochloride acid buffer pH 1.2 with stirring speed of 75 rpm, volume of 900 mL and paddle as apparatus. Ahead of the results it can be concluded that the method developed consists in an efficient alternative for assays of dissolution for benznidazole tablets.

Composição química dos componentes voláteis de Capsicodendron dinisii Schwancke (Canellaceae)

The volatile components of the stem bark of Capsicodendron dinisii were obtained by hydrodistillation using a modified Clevenger-type apparatus. The chemical compounds were identified using the arithmetic index and confirmed by GC-MS. Twenty-three compounds suggest the identified representing almost 90% of the total oil composition. Limonene (68.5%) was the major compound found. The stereochemistry of limonene was determined and was found to be represented by (+)-limonene (94%) and (-)-limonene (6%). The presence of drimenol (0.7%), a drimane sesquiterpenoid, confirmed the volatile components characteristics of the Canellaceae family.

Sistema limpo em linha para extração em fase sólida de contaminantes emergentes em águas naturais

A solid-phase in-line extraction system for water samples containing low levels of emerging contaminants is described. The system was specially developed for large volume samples (up to 4 L) using commercial solid-phase extraction (SPE) cartridges. Four sets containing PTFE-made connectors, brass adapters and ball valves were used to fit SPE cartridges and sample bottles to a 4-port manifold attached to a 20 L carboy. A lab-made vacuum device was connected to the manifold cap. The apparatus is robust and less expensive than the typical available system. Its also provides less experimental handling, avoiding cross contamination and sample losses.

Losartan potassium dissolution test for drug release evaluation in pharmaceutical capsules using HPLC and UV spectrophotometry

This work describes the development and validation of a dissolution test for 50 mg losartan potassium capsules using HPLC and UV spectrophotometry. A 2(4) full factorial design was carried out to optimize dissolution conditions and potassium phosphate buffer, pH 6.8 as dissolution medium, basket as apparatus at the stirring speed of 50 rpm and time of 30 min were considered adequate. Both dissolution procedure and analytical methods were validated and a statistical analysis showed that there are no significant differences between HPLC and spectrophotometry. Since there is no official monograph, this dissolution test could be applied for quality control routine.