INVESTIGADORES
CERUTTI Estela soledad
artículos
Título:
Factorial design optimization of experimental variables in the on-line separation/preconcentration of copper in water samples using solid phase extraction and ICP-OES determination
Autor/es:
ESCUDERO, L.A., CERUTTI, S., OLSINA, R.A., SALONIA, J.A., GASQUEZ, J.A.
Revista:
JOURNAL OF HAZARDOUS MATERIALS.
Editorial:
ELSEVIER SCIENCE BV
Referencias:
Año: 2010 vol. 183 p. 218 - 223
ISSN:
0304-3894
Resumen:
An
on-line preconcentration procedure using solid phase extraction (SPE)
for the determination of copper in different water samples by
inductively coupled plasma optical emission spectrometry (ICP-OES) is
proposed. The copper was retained on a minicolumn filled with ethyl
vinyl acetate (EVA) at pH 8.0 without using any complexing reagent. The
experimental optimization step was performed using a two-level full
factorial design. The results showed that pH, sample loading flow rate,
and their interaction (at the tested levels) were statistically
significant. In order to determine the best conditions for
preconcentration and determination of copper, a final optimization of
the significant factors was carried out using a central composite design
(CCD). The calibration graph was linear with a regression coefficient
of 0.995 at levels near the detection limit up to at least 300 μg L−1. An enrichment factor (EF) of 54 with a preconcentration time of 187.5 s was obtained. The limit of detection (3σ) was 0.26 μg L−1.
The sampling frequency for the developed methodology was about
15 samples/h. The relative standard deviation (RSD) for six replicates
containing 50 μg L−1 of copper was 3.76%. The methodology was
successfully applied to the determination of Cu in tap, mineral, river
water samples, and in a certified VKI standard reference material.