This paper describes a procedure based on multicommutation in flow analysis system for photometric determination of hydroquinone in pharmaceutical gel formulations. The procedure involves oxidation of hydroquinone by Fe (III) and subsequent reaction between the generated Fe (II) species with 1,10-phenanthroline, producing a complex detected at 510 nm. Under optimized conditions, the proposed system showed a linear response in the range between 5 to 120 µmol L-1 (r = 0.9995), a limit of detection (3σ) 0.52 µmol L-1 and a relative standard deviation (RSD) of 1.5% for a 80 µmol L-1 hydroquinone standard solution. Others profitable features such as an analytical frequency of 72 samples per hour; a reagent consumption of 0.432 and 0.117 mg 1-10-phenantroline and FeCl3.6H2O per determination, respectively; and a waste generation of 4.0 ml per determination were also achieved.

No presente trabalho é proposto um procedimento automático para determinação turbidimétrica de sulfato em águas de chuvas, baseado no processo de multicomutação em análise em fluxo. O equipamento fotométrico foi desenvolvido no laboratório, e inclui um LED (λ = 420 nm), uma cela de fluxo com caminho óptico de 100 mm e um fotodiodo. Uma etapa de preconcentração foi incluída para melhorar a sensibilidade. Após estabelecer as condições operacionais adequadas, o procedimento apresentou as seguintes características: resposta linear na faixa de concentração entre 0,1 a 2,0 mg L-1 de sulfato, limite de detecção (critério 3σ) de 0,04 mg L-1 de sulfato, desvio padrão relativo de 1,5% (n = 7) para uma solução com 0,5 mg L-1 de sulfato, consumo de 17,0 mg de cloreto de bário por determinação, volume de efluente de 7.3 mL por determinação e frquência de amostragem de 13 determinações por hora.

In the present work, an automatic procedure for turbidimetric determination of sulfate in rainwater, based on the multicommuted flow analysis approach, is proposed. The photometer set-up was developed at the laboratory, and includes: a LED (λ = 420 nm), a long pathlength flow cell (100 mm), and a photodiode. A preconcentration step is included in order to improve sensitivity. After establishing the adequate operational conditions, the proposed procedure presented the following useful features: a linear response ranging from 0.1 mg L-1 up to 2.0 mg L-1 sulfate, a detection limit (3σ criterion) of 0.04 mg L-1 sulfate, a relative standard deviation of 1.5% for 0.5 mg L-1 sulfate solution (n = 7), barium chloride consumptions of 17.0 mg per determination, and waste generation of 7.3 mL per determination. Accuracy assessment was achieved by applying the paired t-test between results obtained using the proposed procedure and ICP-OES and showed that there is no significant difference at 95% confidence level.

Automatic flow procedures based on the multicommutation concept, dedicated to the determination of 3-hydroxybutyrate, glucose and cholesterol are proposed. The enzymes were immobilized on glass beads and packed into mini-columns that were coupled to a flow system. Sampling throughputs of 55, 40 and 40 determinations per hour, linear response from 10 to 150, 50 to 600, 25 to 125 mg L-1, detection limits of 1.5, 14 and 4 mg L-1 and relative standard deviations of 1, 2 and 2% for 3-hydroxybutyrate, glucose and cholesterol, respectively, were achieved.

An automatic flow injection procedure for spectrophotometric aluminium determination in purified water and solutions containing high salts concentrations used for hemodyalisis treatment was developed. The method was base on reaction of Al3+ with cianine eriochrome R (ECR) after preconcentration using the AG50W-X8 cationic-exchange resin. Elution was carried out using a 1 % (m/v) calcium chloride solution. The manifold comprised an automatic proporcional injector controlled by a computer equipped with an eletronic interface and software written in QuicBASIC 4.5 with facilities to control the injector and perform data acquisition. Samples with concentration ranging from 4.96 to 19.90 µg L-1 Al were analyzed and recoveries between 88 and 113% were obtained by using the standard addition method. Other profitable analytical characteristics such as a relative standard deviation 1.3 % (n = 10) for a typical sample 14.5 µg L-1 Al, a linear response ranging up to 60.0 µg L-1Al, and a sampling throughput of 10 determinations per hour were achieved. A detection limit of 4.2 µg L-1 Al was estimated as suggested by IUPAC.

A concentração de proteína total em plasma é um parâmetro utilizado no controle da saúde e nutrição animal, sendo que a faixa de concentração considerada normal para animais em bom desenvolvimento situa-se entre 60 e 85 g L -1. Os métodos analíticos propostos para esta determinação geralmente apresentam como limitação a excessiva manipulação das amostras. Este trabalho descreve o desenvolvimento de um procedimento de análises em fluxo para a determinação de proteína total em plasma de sangue bovino, empregando o método do Biureto. O sistema em fluxo, constituído por um injetor comutador automático e uma válvula solenóide de três vias controlados por um microcomputador, foi projetado visando permitir diluição em linha das amostras. Um fator de diluição era estimado procedendo-se a diluição em linha de uma solução com concentração conhecida de albumina e este fator era empregado para o cálculo final das concentrações das amostras após diluição em linha. As soluções das amostras eram inseridas através da válvula solenóide, a qual permitia precisas diluições, diminuindo operações manuais. A faixa analítica estabelecida foi entre 2,5 e 20,0 g L-1, e considerando a diluição gerada, amostras de plasma bovino contendo entre 12,5 e 100,0 g L-1 de proteína total puderam ser analisadas. O procedimento apresentou desvio padrão relativo de 2,8 %, e a freqüência analítica alcançada foi de 76 determinações por hora. Os resultados foram comparados com o método tradicional de análises (Biureto) e não foram observadas diferenças estatisticamente significativas a 95%.

Total protein concentration in plasma samples is normally used as a parameter to control animal health and nutritional conditions. Normal concentration levels are in the range of 60 to 85 g L-1 total protein for animals of good development. The methods proposed for its determination generally present as a disadvantage an excessive handling during operation. In this work an automated flow procedure for total protein determination in bovine serum samples, employing the Biuret method, was developed. The system, including an automatic injector commutator and a three way solenoid valve computer controlled, was designed in order to permit on line sample dilution. Since protein standard solutions were introduced with and without dilution. A dilution factor was estimated and used to calculate protein concentration obtained after on-line dilution of the samples. Solutions samples were inserted through a three way solenoid valve that allows precise dilution minimizing hand operations. The analytical range for total protein determination was 2.5 to 20.0 g L-1, and considering the dilution employed, bovine plasma samples with 12.5 to 100.0 g L-1 of total protein were analysed. The procedure presented a 2.8% rsd and analytical frequency of 76 determinations per hour. Results were in good agreement with the traditional method (Biuret) and no significant difference was verified at 95%.

Different methods have been applied to solve special problems of metal analysis. First, the solid samples of tool steels were analyzed by X-ray fluorescence. Alternatively, an on-line electrodissolution implemented in a flow injection system and conventional dissolution procedure for determination of W, Mo, V and Cr in tool steels by ICP-AES is described. The resulting analyte solutions were compared with conventional dissolution procedure and determination by ICP-AES. The electrolytic procedure presented a good performance characterized by a sample throughput of 164 determinations per hour. Results were in agreement with those obtained by conventional acid dissolution.

Didactic experiments are proposed in order to demonstrate the characteristics of flow injection analysis and to extend the applications of FIA to the determination of physical chemistry parameters in undergraduate labs. All experiments can be performed with the same flow manifold by employing usual FIA devices. Analytical characteristics are presented by means of the determination of iron in river water, employing 1,10-phenantroline as chromogenic reagent. Physical chemistry applications were the determination of reaction stoichiometries by continuous variation and mole-ratio methods and the evaluation of the pH and ionic strength effects on the kinetic of the reduction of hexacianoferrate(III) by ascorbic acid.

An on-line electrodissolution procedure implemented in a flow injection system for determination of copper, zinc and lead in brasses alloys by ICP-AES is described. Sample dissolution procedure was carried out by using a PTFE chamber and a DC power supply with constant current. Solid sample was attached to chamber as anode and a gold tubing coupled in the chamber was used as cathode. An electrolytic solution flowing through the gold tubing closed the electric circuit with sample, in order to provide condition for electric dissolution when the DC power supply was switched on. The best results were achieved by using a 1.5 mol l-1 nitric acid solution as electrolyte and a 2.5 A current intensity. The procedure presented a good performance characterized by a relative standard deviation better than < 5% (n=5) and a sample throughput of 180 determinations per hour for Cu, Zn and Pb. Results were in agreement with those obtained by conventional acid dissolution (99% confidence level).

A flow system based on multicommutation and binary sampling process was developed to implement the sample zone trapping technique in order to increase the spectrophotometric analytical range and to improve sensitivity. The flow network was designed with active devices in order to provide facilities to determine sequentialy analyte with a wide concentration range, employing a single pumping channel to propel sample and reagents solutions. The procedure was employed to determine ortophosphate ions in water samples of river and waste. Profitable features such as an analytical throughput of 60 samples determination per hour, relative standard deviation (r.s.d.) of 2% (n = 6) for a typical sample with concentration of 2.78 mg/L were achieved. By applying the paired t-test no significant difference at 95% confidence level was observed between the results obtained with the proposed system and those of the usual flow injection system.