Institution: | aFaculty of Chemistry, University of Sofia, 1 James Bourchier Blvd., Sofia 1164, Bulgaria bFood Institute, Faculty of Veterinary Medicine, Sts. Cyril and Methodius University, P.O. Box 95, MK-1000, Skopje, Macedonia cInstitute of Chemistry, Faculty of Science, Sts. Cyril and Methodius University, P.O. Box 162, MK-1000, Skopje, Macedonia |
Abstract: | Analytical procedure for the determination of toxicologically relevant arsenic (the sum of arsenite, arsenate, monomethylarsonate and dimethylarsinate) in urine by flow injection hydride generation and collection of generated inorganic and methylated hydrides on an integrated platform of a transverse-heated graphite atomizer for electrothermal atomic absorption spectrometric determination (ETAAS) is elaborated. Platforms are pre-treated with 2.7 μmol of zirconium and then with 0.10 μmol of iridium which serve both as an efficient hydride sequestration medium and permanent chemical modifier. Arsine, monomethylarsine and dimethylarsine are generated from diluted urine samples (10–25-fold) in the presence of 50 mmol L?1 hydrochloric acid and 70 mmol L?1 l-cysteine. Collection, pyrolysis and atomization temperatures are 450, 500, 2100 and 2150 °C, respectively. The characteristic mass, characteristic concentration and limit of detection (3σ) are 39 pg, 0.078 μg L?1 and 0.038 μg L?1 As, respectively. The limits of detection in urine are ca. 0.4 and 1 μg L?1 with 10- and 25-fold dilutions. The sample throughput rate is 25 h?1. Applications to several urine CRMs are given. |