Este trabalho descreve um procedimento automático em fluxo monossegmentado para titulação potenciométrica aplicado à determinação de cloreto em leite e vinho. O sistema de fluxo foi desenvolvido com base em uma válvula solenóide de 6 vias, controlada por um microcomputador através de um programa escrito em VisualBasic 3.0. Um eletrodo indicador tubular de Ag 2 S seletivo a Cl -e um eletrodo de referência convencional de Ag/AgCl foram empregados. Um algoritmo baseado na diferença de potencial entre duas adições subsequentes de titulante foi desenvolvido, possibilitando a determinação do ponto final da titulação em, no máximo, 10 tentativas, com uma precisão melhor que 1,0%. O sistema proposto foi avaliado pela determinação de cloreto em leite e vinho, usando uma solução padrão de AgNO 3 como titulante. A exatidão foi avaliada comparando-se os resultados com aqueles obtidos pelo método da AOAC, não sendo encontradas diferenças significativas ao nível de confiança de 95%.An automated flow potentiometric titration procedure for the determination of chloride in milk and wine exploiting the monosegmented flow approach is described. The flow network was designed based on a six-way solenoid valve, controlled by a microcomputer running software written in VisualBasic 3.0, allowing selection of the titration conditions. An Ag 2 S tubular electrode selective for Cl -and a conventional Ag/AgCl electrode were employed as indicator and reference, respectively. An algorithm based on the potential difference between two subsequent titrant additions was developed, allowing to reach the end point in less than 10 attempts, with a precision better than 1.0%. The proposed system was evaluated by determining chloride in milk and wine, using a standard AgNO 3 solution as titrant. Accuracy was ascertained by comparing the results with those obtained using the AOAC procedure. No significant difference at a 95% confidence level was observed.Keywords: potentiometric titration, monossegmented flow, multicommutation, ion selective electrode, chloride in milk, chloride in wine
IntroductionThe mechanisation of the potentiometric titration procedure was first described in 1914 1 and the introduction of flow injection analysis in 1975 2 improved this mechanisation, including for potentiometric and spectrophotometric titrations. [3][4][5] Flow injection titration usually employs a calibration step, in which the peak width (instead of height) is taken as the analytical parameter. The simplest approach, which was first proposed by Ruzicka et al. 6 in 1977, employs a single line manifold and is still being employed nowadays. 7,8 Different alternatives have been proposed to determine the stoichiometric point in a flow titration procedure. Continuous flow systems based on the ratio of sample and titrant flow rates have been exploited to achieve the end point. 9,10 In order to vary the flow rates of the solutions independently, two peristaltic pumps are necessary, which 260 Vieira et al. J. Braz. Chem. Soc. represents the main drawback of these...