Determination of lead and manganese in biological samples and sediment using slurry sampling and flame atomic...

A procedure was developed for the determination of lead (Pb) and manganese (Mn) using slurry sampling. The two elements were detected using flame atomic absorption spectrometry with a slotted tube atom trap. Slurries were prepared by adding nitric acid solution (0.30%, w/v) to a powdered sample (0.10 g). After homogenization by ultrasonic bath for 15 min, the slurries were introduced directly into the detection equipment. Some conditions of the procedure were evaluated, such as acid concentration, presence of surfactants, and sonication time. Under optimized conditions, the LODs and LOQs achieved were 0.8 and 2.6 microg/g for Pb and 0.5 and 1.6 microg/g for Mn, respectively. The precision obtained varied between 3.1 and 5.8% (Mn), and 2.6 and 5.4% (Pb) for slurries of shrimp and sediment. The analytical curves were established using aqueous standards in nitric acid solutions. The accuracy of the method was assessed through the determination of Pb and Mn in the following certified reference materials: ERM-CE 278 (mussel tissue), CRM 397 (human hair), and SRM 1646a (estuarine sediment). The proposed procedure was successfully applied to the determination of Pb and Mn in six samples of shrimp powder, seasoning, and river sediment. The levels of Mn detected varied from 2.2 to 71.3 microg/g; Pb was detected in only one sediment sample (4.3 microg/g).