RESUMEN

In this work a construction procedure for tubular fluoride electrode to be used in flow systems is outlined. The electrode was constructed from a commercially available, LaF3 single crystal. Principal advantages of the flow detector presented include simplicity of construction, robustness, durability, low cost and easy coupling into any point of a flow manifold. Evaluation of the intrinsic working characteristics of the potentiometric detector in a low dispersion manifold is presented with respect to analytical and dynamic parameters. The constructed detector has similar working characteristics to those of the conventional fluoride electrodes, namely the detection limit, lower limit of linear response and operational pH range. The analytical usefulness of the constructed device was assessed in a flow system developed for fluoride determination in toothpaste, tablet, collutory and water samples for which the reference procedures suggest the determination of fluoride ion with a conventional ion selective electrode.

Asunto(s)

Técnicas de Química Analítica/instrumentación , Técnicas de Química Analítica/métodos , Fluoruros/análisis , Electrodos , Análisis de Inyección de Flujo/instrumentación , Análisis de Inyección de Flujo/métodos , Potenciometría/instrumentación , Potenciometría/métodos

RESUMEN

In this paper, the construction and evaluation of an electrode selective to nitrate with improved sensitivity, constructed like a conventional electrode (ISE) but using an operational amplifier to sum the potentials supplied by four membranes (ESOA) is described. The two types of electrodes, without an inner reference solution, were constructed using tetraoctylammonium bromide as sensor, dibutylphthalate as solvent mediator and PVC as plastic matrix, the membranes obtained directly applied onto a conductive epoxy resin support. After the comparative evaluation of their working characteristics they were used in the determination of nitrate in different types of tobacco. The limit of detection of the direct potentiometric method developed was found to be 0.18 g kg(-1) and the precision and accuracy of the method, when applied to eight different samples of tobacco, expressed in terms of mean R.S.D. and average percentage of spike recovery was 0.6 and 100.3%, respectively. The comparison of variances showed, on all ocassions, that the results obtained by the ESOA were similar to those obtained by the conventional ISE, but with higher precision. Linear regression analysis showed good agreement (r=0.9994) between the results obtained by the developed potentiometric method and those of a spectrophotometric method based on brucine, adopted as reference method, when applied simultaneously to 32 samples of different types of tobacco.

RESUMEN

A low inner volume (ca. 64 ml) probe was built up in an injector-commutator in order to behave as a photometric leaping detector in flow analysis. It comprises a bicolour light-emitting diode (BLED), as a source of pulsed radiation in the red and green visible region, and two phototransistors as transducers. Sample injection, detector relocation, analytical signal recording, data treatment and definition of the spectral working range were computer-controlled. The feasibility of the system was initially demonstrated in the flow-injection speciation of iron, and the overall standard deviation of results was estimated as +/- 1.6 and +/- 1.4% for 1.6-4.0 mg l(-1) Fe(II) or total iron after eightfold processing of synthetic samples. The system was further applied to drug analysis: the mean deviations of results for typical samples were estimated as +/- 5.2 and +/- 3.3%, and the relative standard deviation as +/- 1.6 and +/- 1.3% for Fe(II) and total iron, respectively. Results were compared with those obtained by a conventional spectrophotometric procedure and no statistic differences at the 95% confidence level were found. In relation to an earlier system with multi-site detection, the proposed system is more stable, presenting low drift with a relative standard deviation of 0.026% and 0.039% for measurements (n=120 during 4 h of observation) with green and red emission. It is also faster with a sampling rate of 133 h(-1) and carryover problems are not found. The possibility of compensating the Schlieren noise by dual-wavelength spectrophotometry is discussed.

RESUMEN

The construction of a microcomputer-controlled electrode switch for use in potentiometric determinations is described. This can be coupled to most of the analytical equipment usually found in laboratories, to enable a setting up of automatic systems capable of performing sequential determinations with several ion-selective electrodes. The assessment of its analytical usage and behaviour are discussed.