TY - JOUR AU - Ipolyi, I AU - Massanisso, P AU - Sposato, S AU - Fodor, Péter AU - Morabito, R TI - Concentration levels of total and methylmercury in mussel samples collected along the coasts of Sardinia Islands (Italy) JF - ANALYTICA CHIMICA ACTA J2 - ANAL CHIM ACTA VL - 505 PY - 2004 IS - 1 SP - 145 EP - 151 PG - 7 SN - 0003-2670 DO - 10.1016/S0003-2670(03)00174-0 UR - https://m2.mtmt.hu/api/publication/1719946 ID - 1719946 LA - English DB - MTMT ER - TY - JOUR AU - Grinberg, P. AU - Campos, R.C. AU - Mester, Zoltán AU - Sturgeon, R.E. TI - A comparison of alkyl derivatization methods for speciation of mercury based on solid phase microextraction gas chromatography with furnace atomization plasma emission spectrometry detection JF - JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY J2 - J ANAL ATOM SPECTROM VL - 18 PY - 2003 IS - 8 SP - 902 EP - 909 PG - 8 SN - 0267-9477 DO - 10.1039/b212545e UR - https://m2.mtmt.hu/api/publication/30393739 ID - 30393739 N1 - Institute for National Measurements Standards, National Research Council of Canada, Ottawa, Ont. K1A 0R6, Canada Department of Chemistry, Pontificia Universidade Católica do Rio de Janeiro, Rua Marques de Sao Vicente, 225, 22453-900 Rio de Janeiro-RJ, Brazil Cited By :50 Export Date: 15 January 2019 Correspondence Address: Sturgeon, R.E.; Institute for National Measurements Standards, National Research Council of Canada, Ottawa, Ont. K1A 0R6, Canada; email: ralph.sturgeon@nrc.ca AB - Several derivatizing agents were evaluated for use in speciating mercury in biological samples using solid phase microextraction in conjunction with tandem gas chromatography-furnace atomization plasma emission spectrometry (SPME-GC-FAPES). Following digestion with methanolic potassium hydroxide, the pH of the samples was adjusted and NaCl added when necessary. The mercury species were then derivatized with sodium tetraphenylborate or sodium tetrapropylbqrate and extracted by SPME using a 100 um PDMS coated fiber. The derivatized species were then separated by GC and detected by FAPES. All experimental parameters were optimized for best separation and analytical response. Propylation proved to be more sensitive, robust and faster than ethylation or phenylation, leading to procedural detection limits of 0.55 ng g-1 for methylmercury, 0.34 ng g-1 for ethylmercury and 0.23 ng g-1 for inorganic mercury. An intra-day and intra-fiber precision of typically 2.2% was achieved whereas long-term (4 months) and inter-fiber reproducibility precision was typically 4.4%. The accuracy of the method was validated by the analysis of Certified Reference Materials (DORM-2, DOLT-2 and TORT-2) from the National Research Council of Canada. © The Royal Society of Chemistry 2003. LA - English DB - MTMT ER - TY - JOUR AU - Yang, L. AU - Mester, Zoltán AU - Sturgeon, R.E. TI - Determination of methylmercury in fish tissues by isotope dilution SPME-GC-ICP-MS JF - JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY J2 - J ANAL ATOM SPECTROM VL - 18 PY - 2003 IS - 5 SP - 431 EP - 436 PG - 6 SN - 0267-9477 DO - 10.1039/b301299a UR - https://m2.mtmt.hu/api/publication/30393740 ID - 30393740 N1 - Cited By :73 Export Date: 15 January 2019 Correspondence Address: Yang, L.; Institute for National Measurement Standards, National Research Council Canada, Ottawa, Ont. K1A 0R6, Canada; email: Lu.Yang@nrc.ca AB - A method is described for the accurate and precise determination of monomethylmercury (MMHg) by species specific isotope dilution (ID) calibration using solid phase microextraction (SPME) in combination with gas Chromatographic (GC) separation and inductively coupled plasma mass spectrometric (ICP-MS) detection. Samples were digested with methanolic potassium hydroxide, derivatized in aqueous solution with sodium tetrapropylborate and headspace sampled with a polydimethylsiloxane coated SPME fused silica fiber. The analyte was then directly transferred from the fiber to the head of the GC column for desorption by insertion of the fiber through the heated injection port. Reverse spike ID analysis was performed to determine the accurate concentration of an in-house synthesized 198Hg-enriched monomethylmercury (MM 198Hg) spike [candidate Certified Reference Material (CRM) EOM-1] using two natural abundance MMHg standards. Concentrations of 0.719 ± 0.015 and 4.484 ± 0.029 μg g-1 (one standard deviation, n = 4) as Hg were obtained for MMHg in NRCC CRMs DOLT-2 and DORM-2, respectively, using the present method. These are in good agreement with the certified values of 0.693 ± 0.053 and 4.47 ± 0.32 μg g-1 (as 95% confidence interval). A MMHg concentration of 4.69 ± 0.12 μg g -1 (one standard deviation, n = 4) as Hg in DORM-2 was subsequently determined by standard additions calibration using ethylmercury (EtHg) as an internal standard. A nearly. 4-fold improvement in the precision of determination using ID was obtained, clearly demonstrating its superiority in providing more precise results compared to the method of standard additions. The method was applied to the determination of MMHg in a new biological CRM DOLT-3 and a concentration of 1.540 ± 0.025 μg g-1 (one standard deviation, n = 6) as Hg was obtained. A method detection limit (3σ) of 2.1. ng g-1 was estimated for a 0.25 g of subsample, sufficiently low for the routine determination of MMHg in most biological samples. © The Royal Society of Chemistry 2003. LA - English DB - MTMT ER -