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).

Crescimento de cristais de rubi e safira pelo método do fluxo

This work reports the growth of corundum crystals by the flux method. The main objective was the evaluation of versatility, effectiveness and real possibilities of the flux method to the synthesis and doping of monocrystals with impurities of particular interest. In this work the chosen impurities were i) Cr and ii) Fe and Ti, aiming the synthesis of rubies and sapphires, respectively. The crystals were grown by heating a mixture of Al2O3:Cr or Al2O3:Fe:Ti and flux (MoO3). The maximum crystal size obtained was 1.0 mm, all transparent, presenting well developed faces, bipiramidal hexagonal shape, and showing a typical red (ruby) and/or light blue (sapphire) color. EDX and XPD experiments were performed in order to characterize some of the synthesized crystals. All crystallized specimens presented the α-alumina atomic structure.

Utilização de planejamento fatorial no preparo de amostras de detergente em pó para a determinação de fósforo por análise em fluxo

The decomposition of detergent powder samples in a microwave oven and autoclave was evaluated. To establish the best experimental conditions a 2(5) factorial design was performed, varying the conditions in autoclave and microwave digestion and flow system parameters for the determination of phosphorus. The best composition was: 0.2 mL sulfuric acid; 500 W power and a 2 min time interval; 6 mmol L-1 of ascorbic acid and 16 mmol L-1 of molybdate to flow system. This factor levels use less reagents than the reference method. No statistically significant differences were found between the autoclave and microwave oven responses at the 95% confidence level.

Aumento da resposta analítica por meio da otimização do sistema de injeção sem divisão de fluxo em cromatografia gasosa empregando a lei dos gases ideais

This paper reports the development of an easy, fast and effective procedure for the verification of the ideal gas law in splitless injection systems in order to improve the response. Results of a group of pesticides were used to demonstrate the suitability of the approach. The procedure helps establish experimental parameters through theoretical aspects. The improved instrumental response allowed extraction with lower sample volumes, the minimization of time and costs and the simplification of sample preparation.

Sistema de análises em fluxo polivalente para a determinação espectrofotométrica de fármacos

A flow system based on the sandwich technique is proposed for the sequential determination of ascorbic acid, dipyrone, acetylcysteine, captopril and paracetamol. The procedure is based on the reduction of Cu(II) by the analytes followed by the spectrophotometric measurement of the complex of Cu(I) with 2,2'-biquinoline 4,4'-dicarboxylic acid. Linear responses were achieved in the µmol L-1 range, with coefficients of variation better than 1.7%. Sampling rate was estimated as 60 determinations per hour, consuming 230 µg of BQA and generating 2.5 mL of waste per determination. Results for commercial samples agreed with those obtained by procedures recommended by the American and European pharmacopeias at the 95% confidence level.

Análise por injeção em fluxo com detecção amperométrica de múltiplos pulsos: potencialidades e aplicações

The potentialities and applications of the Multiple Pulse Amperometric detection (MPA) coupled with Flow Injection Analysis (FIA) are evaluated. Important aspects as cleaning and activation of electrode surface, indirect and simultaneous analysis of electroactive compounds and the use of the internal standard method for quantifications utilizing FIA-MPA are presented. The main parameters concerning the detection of electroactive analytes by multiple pulse amperometric detection in flowing solutions were also discussed. In addition, aspects such as flow rate, sample volume, application time of the potential pulses and instrumentation necessary for implementing of the method were also addressed.

Determinação espectrofotométrica por injeção em fluxo de glifosato em formulações comerciais de herbicidas

A flow injection spectrophotometric procedure for the determination of glyphosate in commercial formulations of herbicides is proposed. The determination is based on the reaction of glyphosate and p-dimethylaminocinnamaldehyde, in acid medium, yielding a colored compound (l máx = 495 nm). Under optimal conditions, Beer's law is obeyed in a concentration range 40-640 mg mL-1 with a correlation coefficient of 0.9996. The detection limit was 8.60 mg mL-1 for glyphosate. The method was successfully applied for the determination of glyphosate in commercial formulations of herbicides. Recovery of glyphosate from various commercial samples of herbicides range from 91.0 to 110%.

Determinação simultânea de ácido ascórbico e ácido acetilsalicílico usando análise por injeção em fluxo com detecção amperométrica pulsada

A simple flow system with multiple pulse amperometric detection using a single working electrode is proposed for simultaneous determination of ascorbic (AA) and acetylsalicylic (AAS) acids in pharmaceutical formulations. The procedure is based on application of two potential pulses: 0.90 V/50 ms: oxidation and determination of AA without the interference of AAS; 1.35 V/50 ms: oxidation of both compounds and quantification of AAS by current subtraction using a correction factor. Sampling rate was estimated as 125 injections per hour and the limits of detection were 0.17 and 0.16 µmol L-1 for AA and AAS, respectively. Results for commercial samples agreed with those obtained using HPLC.

Influência de processos antagônicos no desenvolvimento de sistema de análises em fluxo para a determinação espectrofotométrica de propiltiouracil em medicamentos

A multi-commuted flow system was developed to determine propylthiouracil (PTU) based on the reaction of its thiol form with iminoquinone radical generated by the oxidation of N,N-dimethyl-p-phenylenediamine in an alkaline medium. PTU can be found in tautomeric forms and the tautomeric equilibrium was displaced to enhance the thiol form. However, the reaction product is unstable and its residence time in the flow path was carefully investigated. The proposed procedure showed good precision (< 1.5%) and a limit of detection (3s) of 0.11 mg L-1. High recoveries were obtained in the validation test. The procedure was employed for propylthiouracil determination in medications.