title: Validation of a digestion system using a digester block/cold finger system for the determination of lead in vegetable foods by electrothermal atomic absorption spectrometry.
abstract: This paper presents the validation of a system for sample digestion using a digester block/cold finger to determine the lead content in vegetables by electrothermal atomic absorption spectrometry (ETAAS). After mineralization, lead contents were determined by ETAAS using a calibration curve based on aqueous standards prepared in 2.60 M nitric acid solutions containing 5 microg ammonium phosphate as chemical modifier. A pyrolysis temperature of 900 degrees C and atomization temperature of 2000 degrees C were used. This method allowed the determination of lead with a characteristic mass of 35 pg; LOD and LOQ of 0.6 and 2 nglg, respectively, were found. The precision was investigated in terms of reproducibility and repeatability. Reproducibility was estimated by analysis of nine different portions of a certified reference material (CRM) of spinach leaves, and the repeatability was determined through the analysis of nine aliquots of the same solution. The reproducibility and repeatability were found to be 4.27 and 2.94% RSD, respectively. The accuracy was confirmed by analysis of whole meal flour, spinach leaves, and orchard leaves CRMs, all furnished by the National Institute of Standards and Technology. Lead contents were measured using the newly developed technique in 11 different potato samples. The lead contents ranged from 12.80 to 69.27 ng/g, with an average value of 28.59 ng/g. These values were in agreement with data reported in the literature.
authors.affiliation: Universidade Federal da Bahia, Instituto de Química, CEP-40170-270 Salvador-BA, Brazil.
authors.forename: Robson M
authors.initials: RM
authors.lastname: De Jesus
authors.forename: Mario M S
authors.initials: MM
authors.lastname: Junior
authors.forename: Geraldo D
authors.initials: GD
authors.lastname: Matos
authors.forename: Ana M P
authors.initials: AM
authors.lastname: Dos Santos
authors.forename: Sérgio L C
authors.initials: SL
authors.lastname: Ferreira
mesh_terms: D004785:Environmental Pollutants / Q000737:chemistry; D005504:Food Analysis / Q000379:methods; D005506:Food Contamination; D007854:Lead / Q000737:chemistry*; D015203:Reproducibility of Results; D013054:Spectrophotometry, Atomic / Q000379:methods*; D014675:Vegetables / Q000737:chemistry*
chemical_list: D004785:Environmental Pollutants; D007854:Lead