Factorial designs for Cd, Cr, Hg, Pb and Se ultrasound-assisted acid leaching from human hair followed by atomic absorption spectrometric determination
P. Bermejo-barrera et al., Factorial designs for Cd, Cr, Hg, Pb and Se ultrasound-assisted acid leaching from human hair followed by atomic absorption spectrometric determination, J ANAL ATOM, 15(2), 2000, pp. 121-130
An acid leaching procedure, for use as a sample pre-treatment, was develope
d for Cd, Cr, Hg, Pb and Se determination in human hair. A Plackett-Burman
experimental design was used as a multivariate strategy for the evaluation
of the effects of varying several variables at once. The effects on acid le
aching of metals of nitric acid, hydrochloric acid and hydrogen peroxide co
ncentrations, acid solution volume, exposure time to ultrasound, temperatur
e of the ultrasonic bath, and hair particle size, have been investigated. F
rom these studies, certain variables showed up as significant, and they wer
e optimised by a 2(3) + star central composite design, which involved 16 ex
periments. Optimum values of the variables were selected for the developmen
t of acid leaching procedures to extract trace metals from human hair. Elec
trothermal atomic absorption spectrometry (ETAAS) was used to determine Cd,
Cr, Pb and Se, while cold vapour-atomic absorption spectrometry (CVAAS) wa
s used for Hg measurements. An acid digestion induced by microwave energy w
as used to obtain the total metal concentration and also for comparative pu
rposes. IAEA-085 and NIES No. 13 certified reference materials, which offer
certified values for some elements, were used in order to verify the accur
acy of the methods.