title: Application of Doehlert designs for optimisation of an on-line preconcentration system for copper determination by flame atomic absorption spectrometry.
abstract: In the present paper, a system for on-line preconcentration and determination of copper by flame atomic absorption spectrometry (FAAS) was developed. It was based on solid phase extraction of copper(II) ions on a minicolumn of Amberlite XAD-2 loaded with 2-(2-thiazolylazo)-5-dimethylaminophenol (TAM). The optimisation process was carried out using Doehlert designs. Four variables (sampling flow rate, SR; elution flow rate, buffer concentration, BC; and pH) were regarded as factors in the optimisation. The parameter "sensitivity efficiency (SE)" proposed in this paper, and defined as the analytical signal obtained for an on-line enrichment system for a preconcentration time of 1 min was used as analytical response in the optimisation process. Using the established experimental conditions, the proposed on-line system allowed determination of copper with detection limit (3sigma/S) of 0.23 mug l(-1), and a precision (repeatability), calculated as relative standard deviation (R.S.D.) of 3.9 and 3.7% for copper concentration of 5.00 and 20.00 mug l(-1), respectively. The preconcentration factor obtained is 62. The recovery achieved for copper determination in presence of several cations demonstrated that this has enough selectivity for analysis of food samples. The robustness of the proposed system was also evaluated. The accuracy was confirmed by analysis of the following certified reference materials (CRMs): Rice flour NIES 10a, Spinach leaves NIST 1570a, Apples leaves NIST 1515 and Orchard leaves NBS 1571. This procedure was applied for copper determination in natural food samples.
authors.affiliation: Grupo de Pesquisa em Qui&#x0301;mica Anali&#x0301;tica, Instituto de Qui&#x0301;mica, Universidade Federal da Bahia, Campus Universitário de Ondina, Salvador, Bahia 40170-290, Brazil.
authors.forename: Sérgio L C
authors.initials: SL
authors.lastname: Ferreira
authors.forename: Marcos A
authors.initials: MA
authors.lastname: Bezerra
authors.forename: Walter N L
authors.initials: WN
authors.lastname: Dos Santos
authors.forename: Benı X0301 Cio B
authors.initials: BX
authors.lastname: Neto