Journal of the Brazilian Chemical Society
On-line version ISSN 1678-4790
ANDRADE, Frank P.; NASCENTES, Clésia C. and COSTA, Letícia M.. Cadmium and lead cloud point preconcentration and determination in tobacco samples by thermospray flame furnace atomic absorption spectrometry. J. Braz. Chem. Soc. [online]. 2009, vol.20, n.8, pp. 1460-1466. ISSN 1678-4790. http://dx.doi.org/10.1590/S0103-50532009000800011.
A thermospray flame furnace atomic absorption spectrometer (TS-FF-AAS) was employed to determine Cd and Pb in different Brazilian tobacco samples. Sample pretreatment consisted of acid decomposition and cloud point (CP) preconcentration optimized by Doehlert design. To promote phase separation in the cloud point procedure, polyoxyethylene(8) isooctylphenyl ether (Triton® X-114) and 2-(bromo-2-pyridylazo)-5-diethyl-amino-phenol (Br-PADAP) were used as a nonionic surfactant and a complexing agent, respectively. The variables of the cloud point preconcentration procedure optimized by Doehlert design were: complexing agent volume, Triton X-114 volume, and pH. A response surface maximum point was obtained for Cd and Pb. For TS-FF-AAS, a sample volume of 50 µL was introduced into the hot Ni tube using air carrier at a flow rate of 0.4 mL min-1. The limits of detection and relative standard deviations obtained for Cd and Pb when CP and TS-FF-AAS were associated were 4.0 and 13 µg kg-1, and 3.1 and 0.7%, respectively. Accuracy was checked by addition-recovery experiments, as well as by using two certified reference materials (tea and peach leaves). Cadmium and lead recoveries ranged from 93 to 103 and 93 to 107%, respectively. All results obtained for reference materials were in agreement with certified values at 95 or 99% confidence levels by t-Student test.
Keywords : tobacco; acid digestion; cloud point preconcentration; Doehlert design; TS-FF-AAS.