Um fotômetro de fluxo para análises clínicas a base de um diodo emissor de luz bicolor

The construction and evaluation of an inexpensive flow photometer for clinical analysis, using a bicolour LED and a phototransistor adapted for tubular flow cell, are described. The instrument presents some new features such as: automatic zero, electronic calibration and peak-hold signal. When compared with a classical photometer, it is simpler and has the advantages of a flow analysis system: lower volumes of reagents and samples, lower levels of contamination, shorter time for analysis and lower analysis costs. The instrument was used in the determination of the constituents in blood samples. The results obtained agree with those obtained by a classical photometer and the precision was better.

Extração líquido-líquido em sistemas de fluxo

This review deals with principles of the liquid-liquid extraction, when performed in flow systems. This approach is frequently used for sample treatment to improve the selectivity and/or sensitivity in analytical measurements. The advances in this area are reported, including the use of monosegmented flow systems to perform metal extraction through both two-phase and single phase processes.

Construção e avaliação de um eletrodo tubular sensível ao íon hidrogênio como detector em sistemas de análise em fluxo

The construction of a tubular hydrogen ion-selective potentiometric electrode without inner reference solution, based on the tridodecylamine (TDDA) ionophore, and its evaluation in a flow system are described. TDDA was dissolved in 2-nitrophenyl octyl ether, dispersed in a PVC membrane and applied directly to a conducting support which consisted of an epoxy resin and graphite mixture. The electrode was designed with a tubular geometry to effort facilities to be coupled as part of a flow injection network. The main working characteristics such as response time, linear pH range, selectivity and life time were evaluated and compared with those obtained which a conventionally shaped electrode based on the same sensor. The electrode showed a slope of 51-52 mV dec-1 within a linear pH range from 4.0 up to 12.0.

Uma célula simples para adaptação de eletrodos seletivos comerciais em sistemas de análises em fluxo

A simple flow cell for potentiometric detection is described. It was assembled by making use of two perspex pieces fixed together by means of four screws, and allow the connection of plane membrane conventional electrodes to flow system. Details about its construction are presented. The device performance was evaluated by making use of a cyanide ion-selective electrode. The relative standard deviation was about 0.5% with a detection limit of 8.0 x 10-6 mol CN- dm-3. Under experimental conditions, the linear range was 10-5 to10-2 mol dm-3.

Titulador potenciométrico automatizado baseado em sistema de fluxo monossegmentado

A new automated system for acid-base flow titrations is proposed. In the operation mode, several sample to titrant volumetric ratios are injected in an air segmented plug. Five three way solenoid valves and three acrilic junctions, assembled in a hidrodynamic injection system, were accountable for the monosegmented reagents plug formation. A turbulent flow reactor was used for a perfect mix of reagents in the plug. The detector system employed a glass combined electrode fitted in an acrilic holder. Titrations of hydrochloric, nitric and acetic acids, in several concentrations, were performed with standard sodium hidroxide, for evaluation of the efficiency of the system. The relative standard deviation of the determinations was about ±0,5% and each titration was carried out in 3-4 minutes. A Quick BASIC 4.5® program was developed for the titrator control.

Sistema de termostatização para aplicação em análise por injeção em fluxo

A on-line thermostatization system that use simples materials, for flow injection and continuous flow analysis is described. The proposed system showed good performance between 10 to 40ºC.

Classificação e definição dos métodos de análises em fluxo (Recomendações - IUPAC 1994)

The aim of this report is to classify analytical methods based on flowing media and to define (standardize) terminology. After the classification and a discussion of terms describing the systems and component parts, a section is devoted to terms describing the performance of flow systems. The list of terms included is restricted to the most relevant ones; especially "self-explanatory" terms are left out. It is emphasised that the usage of terms or expressions that do not adequately describe the processes or procedures involved should be strongly discouraged. Although belonging to the category of methods based on flowing media, chromatographic methods are not comprised in the present document. However, care has been taken that the present text is not in conflict with definitions in that domain. In documents in which flow methods are described, it should be clearly indicated how the sample and/or reagent is introduced and how the sample zone is transported. When introducing new techniques in the field, or variants of existing techniques, it is strongly recommended that descriptive terms rather than trivial or elaborate names are used.

Construção de uma cela de fluxo para medidas por espectrofotometria em fase sólida

A simple and low cost flow cell is proposed for measurements by solid-phase spectrophotometry employing a conventional spectrophotometer. The flow cell geometry allows the employment of a large amount of the solid support without causing both excessive attenuation of the radiation beam and increasing of the back-pressure. The adaptation of the flow cell in the optical path of the spectrophotometer in order to increase the precision is discussed. The flow cell characteristics were demonstrated by measurements of Co(II), employing 1-(2-tiazolylazo)-2-naphthol (TAN) immobilized on C18 bonded silica as solid support. The apparent molar absorptivity and coefficient of variation were estimated as 1.86 x 10(5) L mol-1 cm-1 and 1.4 % (n=15). A sample throughput of 40 determinations per hour and a detection limit of 15 mug L-1 (99.7 % confidence level) were achieved.

Injetor multicanal com válvulas de estrangulamento para análise em fluxo

An important component for the automation of flow injection analysis (FIA) systems is the sample injection valve. A simple and inexpensive commutator with 16 pinch valves (8 normally open and 8 closed) was developed and configured as a multichannel injection valve. It is activated by a single solenoid of 3 Kgf, powered by a pulsed driver circuit, controlled by a microcomputer or a switch. FIA with spectrophometric detection of potassium dichromate solution was used for the evaluation of the new injection valve and its comparison with other valves, for sample loops of 50, 100, 200, 300 and 500 muL. The repeatability was favorable (RSD 1.0% for 15 injections at each loop volume) compared to a manual injector, an electropneumatic injector and an injector configured with three mini solenoid valves (RSD 1.1, 1.3 and 1.0%, respectively, for15 injections at each loop volume).

Propulsor pneumático versátil e isento de pulsação para sistemas de análise em fluxo

Aquarium air pumps are proposed and evaluated as pneumatic liquid propulsion devices for flow injection and continuos flow analysis (FIA and CFA) systems. This kind of pump is widely available at a very low cost and it can sustain a pressure around of 4 psi (0.28 bar) indefinitely. By applying this air pressure onto a solution contained in a reservoir flask, it is possible to reach flow rates of up to 12.5 mL min-1 for circuits comprising reactors, made from 0.8 i.d. tubing with a length of 100 cm. The precise adjustment of flow rate below the maximum one can be made with a simplified needle valve or inserting in series a short length of capillary tube. The absence of flow pulsation is a definite advantage in comparison with peristaltic pumps, especially when amperometric detection is elected, as confirmed experimentally in FIA and CF applications.

Desenvolvimento de um dispositivo de baixo custo para medidas por quimiluminescência

A simple and low cost device (ca. US$ 150) that comprises two photodiodes fixed in lab-made Perspex flow cell is proposed for chemiluminescence measurements. The characteristics of the device (large observation window and reduced thickness) allow maximizing the amount of the emitted radiation detected. A sensitivity improvement of ca. 50 % was observed by employing two photodiodes for signal measurements. The performance of the device was assessed by the oxidation of luminol by hydrogen peroxide, yielding a linear response within the range of 2.50 to 500 µmol L-1 H2O2. The detection limit was estimated as 0.8 µmol L-1 hydrogen peroxide which is comparable with those obtained by using equipments based on photomultipliers.

Um experimento de análise em fluxo envolvendo reações enzimáticas e quimiluminescência

An experiment is proposed to introduce some fundamentals of flow analysis, chemiluminescence and kinetic monitoring of enzymatic reactions in undergraduate courses. Chemiluminescence detection is performed with a simple spectrophotometer equipped with a lab-made spiral flow cell constructed from a polyethylene tube. The hydrogen peroxide produced by the glucose oxidation in the presence of glucose oxidase is continuously monitored by the reaction with luminol in alkaline media in a flow injection system. The exercise allows also the discussion of important analytical features and the comparison with different optical methods of analysis.

Informações essenciais para a caracterização de um sistema de análise em fluxo

Essential aspects for characterization of a flow-based analytical procedure or system are discussed in order to permit the composition of a checklist that will lead to a protocol for reporting results and systems in flow analysis. Aspects more related to chromatographic procedures are not considered. The intent is to present normalized proposals in the field of flow analysis for practitioners and developers.

Uso de membranas de Nafion para a construção de sensores ópticos para medidas de pH

The behaviour of Nafion® polymeric membranes containing acid-base dyes, bromothymol blue (BB) and methyl violet (MV), were studied aiming at constructing an optical sensor for pH measurement. BB revealed to be inadequate for developing sensing phases due to the electrostatic repulsion between negative groups of their molecules and the negative charge of the sulfonate group of the Nafion®, which causes leaching of the dye from the membrane. On the other hand, MV showed to be suitable due to the presence of positive groups in its structure. The membrane prepared from a methanolic solution whose Nafion®/dye molar ratio was 20 presented the best analytical properties, changing its color from green to violet in the pH range from 0.6 to 3.0. The membrane can be prepared with good reproducibility, presenting durability of ca. 6 months and response time of 22 s, making possible its use for pH determination in flow analysis systems.

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.