Estimativa do fluxo de amônia na interface ar-mar na Baía de Guanabara: estudo preliminar

In the begining of April 2004, concentrations of NHx (NH3 + NH4+) were measured in surface waters of the Guanabara Bay. Concentrations varied from 2 to 143 mmol L-1. Ammonia exchange at the air-sea interface was quantified using a numerical model. No measurement of NH3 concentration in air (c air) was performed. Thus, calculations of NH3 flux were based on the assumptions of c air = 1 and 5 µg m-3. Fluxes were predominantly from the water to the atmosphere and varied from -20 to almost 3500 µg N m-2 h-1.

Determinação turbidimétrica de metilbrometo de homatropina em formulações farmacêuticas empregando um sistema de análise por injeção em fluxo

A flow injection turbidimetric procedure exploiting merging zones is proposed for determining homatropine methylbromide (HMB) in pharmaceutical preparations. The determination is based on the precipitation reaction of homatropine methylbromide with AgNO3 solution to form a precipitate, which was measured at 410 nm. The analytical curve was linear in the HMB concentration range from 8.0x10-4 to 1.7x10-3 mol L-1, with a detection limit of 9.5x10-5 mol L-1. The recoveries ranged from 94.9 to 104 %, the sampling frequency was 75 h-1 and relative standard deviations were smaller than 2.0 % for solutions containing 1.2x10-3 and 1.5x10-3 mol L-1 HMB (n=10). The results obtained for commercial formulations using the FIA procedure were in good agreement with those obtained by using a comparative method (r= 0.9983).

Controle da biossíntese de poli-hidroxialcanoatos bacterianos através do fluxo de substratos

Manipulation of the flux of substrates was utilized to control the amount of 3-hydroxyvalerate and 3-hydroxy-4-pentenoate produced by Burkohlderia sp. The 3HV production rate was directly proportional to the propionic acid uptake rate with the last one completely directed to 3HV biosynthesis. The 3HPE production rate was inversely proportional to the sucrose uptake rate probably due to operation of the glyoxylate cycle.

Adsorção de íons cobre(II) pela quitosana usando coluna em sistema sob fluxo hidrodinâmico

The adsorption of Cu(II) ions from aqueous solution by chitosan using a column in a closed hydrodynamic flow system is described. The adsorption capacities as a function of contact time of copper(II) ions and chitosan were determined by varying the ionic strength, temperature and the flow of the metal solution. The Langmuir model reproduced the adsorption isothermal data better than the Freundlich model. The experimental kinetic data correlate properly with the second-order kinetic reaction for the whole set of experimental adsorption conditions. The rate constants exercise great influence on the time taken for equilibrium to be established by complexation or electrostatic interaction between the amino groups of chitosan and the metal.

Uso da pressão gerada por uma coluna de água para controle da vazão em sistemas de análises em fluxo

This work presents a new approach to control the flow rate in hydrodynamic flow experiments. The combination of air pressure generated by an aquarium air pump and the pressure generated by a water column were used for this purpose. This device supports a stable flow rate without pulsation for a long period of time. Furthermore, the flow rate can be easily controlled at various values in one or more streams. The performance of this approach was investigated using Fe(CN)6(4-) solutions in flowing systems using amperometric and voltammetric detection in wall-jet configuration. The results showed that the performance of the proposed device was better than a commercial peristaltic pump. It suggests that this approach can be used successfully in flow analysis systems.

Construção de uma cela de fluxo de longo caminho óptico para medidas espectrofotométricas

A simple and low-cost flow cell with 30 cm optical path for spectrophotometric measurements is described. It presents desirable characteristics such as low attenuation of the radiation beam and internal volume (75 µL) comparable to that of a 1-cm conventional cell (80 µL). Despite the increase in optical path, the effect on sample dispersion was also similar to that attained in the commercial cell. The performance of the cell was assessed by the determination of phosphate based on the molybdenum blue method, yielding a linear response range between 0.05 and 0.8 mg L-1 phosphorus (r=0.999). The increase in sensitivity (30.4-fold) in comparison with that obtained with a conventional 1-cm flow cell agreed with that estimated by the Lambert-Beer law.

Implementação computacional do modelo carga-fluxo de carga-fluxo de dipolo para cálculo e interpretação das intensidades do espectro infravermelho

The first computational implementation that automates the procedures involved in the calculation of infrared intensities using the charge-charge flux-dipole flux model is presented. The atomic charges and dipoles from the Quantum Theory of Atoms in Molecules (QTAIM) model was programmed for Morphy98, Gaussian98 and Gaussian03 programs outputs, but for the ChelpG parameters only the Gaussian programs are supported. Results of illustrative but new calculations for the water, ammonia and methane molecules at the MP2/6-311++G(3d,3p) theoretical level, using the ChelpG and QTAIM/Morphy charges and dipoles are presented. These results showed excellent agreement with analytical results obtained directly at the MP2/6-311++G(3d,3p) level of theory.

Determinação espectrofotométrica em fluxo de cloro em água usando célula de longo caminho óptico e multicomutação

A multicommuted method for determination of chlorine in water samples using a 100-cm cell was developed. In this method, orto-Tolidine reacts with chlorine and the product was monitored at 438 nm. The analytical curve for chlorine was linear in concentration range from 1.34x10-6 to 2.01x10-5 mol L-1 with a detection limit of 9.40x10-8 mol L-1. A sampling rate of 45 h-1and a RSD of 1.0 % (n = 15) were obtained. The method was applied with success for chlorine determination in six water samples.

Sistema multicomutado de análise em fluxo para determinação de amônio e monocloramina em águas residuais e produtos de desinfecção

A binary sampling flow analysis system equipped with gas diffusion cell was developed for NH4+ and/or NH2Cl determination in wastewater and disinfection products samples based on the Berthelot reaction of the NH2Cl diffused through the semi-permeable PTFE membrane. The effect of the analytical conditions related to the reaction and flow parameters were evaluated and N-NH4+ and N-NH2Cl were determined in concentration ranges from 0.17 to 5 mg L-1 and from 0.5 to 14.5 mg L-1, respectively. Limits of detection (3σ) of 50 and 140 µg L-1 for N-NH4+ and N-NH2Cl were calculated, respectively, and RSD of 5 and 2% were calculated for 10 consecutive determinations of N-NH4+ (1 and 3 mg L-1) and N-NH2Cl (3 and 9 mg L-1), respectively with 30 determinations h-1.

Autoamostrador de baixo custo para análise por injeção em fluxo

This paper describes a homemade autosampler for flow injection analysis (FIA), constructed with two step motors from old floppy disk drives (5¼-inch). The autosampler was connected to a computer through the parallel port and the sampling process was controlled by software in Quick Basic. The performance of the system was assessed by the determination of ammonium, based on the gaseous diffusion into a bromocresol purple solution, following the spectrophotometric determination of change in absorbance. The easy and simple construction is the main characteristics of this equipment and analytical results with RSD lower than 1% were obtained.

Determinação de paracetamol pela inibição da reação quimiluminescente do luminol-hipoclorito de sódio em um sistema de análise em fluxo empregando o conceito de multicomutação

A flow injection chemiluminescence method for the determination of paracetamol in pharmaceutical formulations is described. It is based on the consumption of the sodium hypochlorite by paracetamol and decreases of the analytical signal. The analytical curve was linear in the paracetamol concentration range from 5.0 x 10-6 to 5.0 x 10-5 mol L-1, with a detection limit of 1.8 x 10-6 mol L-1. The RSDs were 2.0 and 1.2% respectively for 2.0 x 10-5 and 4.0 x 10-5 mol L-1 paracetamol solutions (n = 10) and a sampling frequency of 180 h-1 was obtained.

Determinação turbidimétrica em fluxo de cloridrato de fluoxetina em formulações farmacêuticas

A simple, accurate and precise flow-injection turbidimetric procedure for the determination of fluoxetine hydrochloride in pharmaceutical formulations is reported. The procedure is based on the precipitation of chloride of fluoxetine hydrochloride with silver nitrate solution and the yielded insoluble AgCl(s) was monitored at 420 nm. The analytical curve was linear in the fluoxetine hydrochloride concentration range 3.0 x 10-5 - 5.0 x 10-4 mol L-1 with a detection limit of 10 µmol L-1 and, a sample throughout of 60 h-1.

Construção e caracterização de um detector eletroquímico para análises em fluxo

The present work describes a low-cost electrochemical "wall-jet" detector for flow analysis. The electrolytic solution enters into the cell through a tube of stainless steel (200 to 300 µm i.d), reaching to the center of the working electrode perpendicularly and then being mixed to the remaining solution in the cell, which flows under atmospheric pressure into a waste reservoir. The proposed electrochemical detector can be used with any type of working electrode, from commercial to home-made, such as glassy carbon and metallic electrodes (modified or unmodified), which enlarge the applications of the electrochemical detector.

Análise screening de vinhos empregando um analisador fluxo-batelada, espectroscopia UV-VIS e quimiometria

A simple, robust, versatile, high analytical frequency method was proposed to check if a sample of wine is within the range of standards set by the manufacturer, using the UV-VIS spectroscopy, multivariate analysis and a flow-batch analyzer. Two hundred and fifty-two samples of wines were analyzed. The results from the application of Hierachical Cluster Analysis (HCA) to the matrix of the data involving all samples show the formation of fifteen types of wine. A Soft Independent Modelling of Class Analogy (SIMCA) model was constructed and used to classify the samples of the overall forecast. As a result, it is observed that the prediction was performed with a success rate of 99.2% for a confidence level of 95%. This shows that the proposed methodology can be used as an effective tool for classifying of samples of wines.

Degradação eletroquímica do cloranfenicol em reator de fluxo

This paper reports a study of electrochemical degradation of the chloramphenicol antibiotic in aqueous medium using a flow-by reactor with DSA® anode. The process efficiency was monitored by chloramphenicol concentration analysis with liquid chromatography (HPLC) during the experiments. Analysis of Total Organic Carbon (TOC) was performed to estimate the degradation degree and Ion Chromatography (IC) was performed to determinate inorganic ions formed during the eletrochemical degradation process. In electrochemical flow-by reactor, 52% of chloramphenicol was degraded, with 12% TOC reduction. IC analysis showed the production of chloride ions (25 mg L-1), nitrate ions (6 mg L-1) and nitrite ions (4.5 mg L-1).