title: A new functionalized resin and its application in preconcentration system with multivariate optimization for nickel determination in food samples.
abstract: In this work, Amberlite XAD-2 resin functionalized with 4,5-dihydroxy-1,3-benzenedisulfonic acid was synthesized, characterized and applied as a new packing material for an on-line system to nickel preconcentration. The method is based on the sorption of Ni(II) ions in a minicolumn containing the synthesized resin, posterior desorption using an acid solution and measurement of the nickel by spectrophotometry (PAR method). The optimization of the system was performed using factorial design and Doehlert matrix considering five variables: eluent concentration, PAR solution pH, sample flow rate, PAR solution concentration and sample pH. Signals were measured as peak height by using an instrument software. Using the experimental conditions defined in the optimization, the method allowed nickel determination with achieved sampling rate of 25 samples per hour, detection limit (3s) of 2microgl(-1) and precision (assessed as the relative standard deviation) of 8.2-2.6%, for nickel solutions of 10.0-200.0microgl(-1) concentration, respectively. The experimental enrichment factor of the proposed system was 46, for 120s preconcentration time. The proposed procedure was applied for nickel determination in food samples. Recoveries of spike additions (5 or 10microgg(-1)) to food samples were quantitative (94-110%).
authors.affiliation: Núcleo de Química Analítica (NQA), Laboratório de Química Analítica (LQA), Universidade Estadual do Sudoeste da Bahia, Campus de Jequié, Jequié, Brazil.
authors.forename: Valfredo Azevedo
authors.initials: VA
authors.lastname: Lemos
authors.forename: Patrícia Xavier
authors.initials: PX
authors.lastname: Baliza
authors.forename: Juracir Silva
authors.initials: JS
authors.lastname: Santos
authors.forename: Luana Sena
authors.initials: LS
authors.lastname: Nunes
authors.forename: Adriana Alves de
authors.initials: AA
authors.lastname: Jesus
authors.forename: Marcelo Eça
authors.initials: ME
authors.lastname: Rocha