Application of acetylacetone chelation solid-phase extraction to GFAAS measurements of trace amounts of beryllium in marine organisms.

Trace amounts of Be (0.046-2.59 ng) in a dried marine organism sample (10 mg) could be accurately determined by GFAAS after treating with microwave digestion (HNO3/H2O2) at 85 degrees C for 10 min and using acetylacetone as a chelating agent in the presence of an acetate buffer (pH 6.0). The method detection limit (MDL, 3sigma) for Be was found to be 4.6 ng g(-1); the calibration graph was linear up to 259 ng g(-1). Good recoveries (98.5-105.0%) were obtained for eight marine organism samples (including five fish, one lobster, one oyster, and one algae) with a relative standard deviation (RSD, n = 3) < 3.0%. The proposed method could be applied measurements of Be in various marine organisms.

Determination of total mercury and methylmercury in human hair by graphite-furnace atomic absorption spectrophotometry using 2,3-dimercaptopropane-1-sulfonate as a complexing agent.

For the determination of total mercury in hair, an amount (25.0 mg) of hair sample was digested with conc. HNO3 (400 microl) at 90 degrees C for 10 min in a 7-ml teflon microreaction vessel. After digestion, the pH of the acidic hair mixture was adjusted to 5.0-6.0 by NaOH and was then passed through a clean-up Sep-Pak C18 cartridge. To the eluate, 2,3-dimercaptopropane-1-sulfonate (DMPS) and sodium acetate buffer (pH = 6.0) were added to form a mercury-DMPS complex. This complex was preconcentrated on two Sep-Pak C18 cartridges in series, and each cartridge was eluted with methanol and adjusted to 2.00 ml. A portion (50 microl) was introduced into a graphite cuvette and then atomized according to a temperature program. The method detection limit (MDL, 3sigma) was 0.064 (microg g(-1)); the calibration graph was linear up to 7.52 microg g(-1). Good accuracies were obtained when testing two human hair certified reference materials (GBW 09101 and BCR-397). Six real samples were analyzed, and the recoveries were 95.8 - 98.2% with a relative standard deviation (RSD, n = 3) < 2.1%. For the determination of methylmercury (CH3Hg+), 25.0 mg of hair sample was extracted with 2.0 mol dm(-3) HCl (1.0 ml) by ultrasonicating for 1 h. The supernatant solution was used for CH3Hg+ analysis and the hair residue was used for the analysis of inorganic mercury (Hg2+). The MDL of CH3Hg+ was 0.068 microg g(-1); the calibration graph was linear up to 6.00 microg g(-1). Six real samples were analyzed, and the recoveries were 96.0-99.2% with RSD (n = 3) < 2.3%. The sum of the concentrations of CH3Hg+ and Hg2+ was very close to that of the total mercury measured with a relative error within 3.6%. The proposed method can be accurately applied to the measurement of CH3Hg+, Hg2+, and total mercury in hair samples.