Simultaneous preconcentration of copper, zinc, cadmium, and nickel in water samples by cloud point extraction using 4-(2-pyridylazo)-resorcinol and their determination by inductively coupled plasma optic emission spectrometry.

A procedure for simultaneous separation/preconcentration of copper, zinc, cadmium, and nickel in water samples, based on cloud point extraction (CPE) as a prior step to their determination by inductively coupled plasma optic emission spectrometry (ICP-OES), has been developed. The analytes reacted with 4-(2-pyridylazo)-resorcinol (PAR) at pH 5 to form hydrophobic chelates, which were separated and preconcentrated in a surfactant-rich phase of octylphenoxypolyethoxyethanol (Triton X-114). The parameters affecting the extraction efficiency of the proposed method, such as sample pH, complexing agent concentration, buffer amount, surfactant concentration, temperature, kinetics of complexation reaction, and incubation time were optimized and their respective values were 5, 0.6 mmol L(-1), 0.3 mL, 0.15% (w/v), 50 degrees C, 40 min, and 10 min for 15 mL of preconcentrated solution. The method presented precision (R.S.D.) between 1.3% and 2.6% (n=9). The concentration factors with and without dilution of the surfactant-rich phase for the analytes ranged from 9.4 to 10.1 and from 94.0 to 100.1, respectively. The limits of detection (L.O.D.) obtained for copper, zinc, cadmium, and nickel were 1.2, 1.1, 1.0, and 6.3 microg L(-1), respectively. The accuracy of the procedure was evaluated through recovery experiments on aqueous samples.

Monitoring trace metals in urban aerosols from Buenos Aires city. Determination by plasma-based techniques.

A study was undertaken, within the framework of a 3 years national project, to assess the content of 13 elements in airborne particulate matter collected in representative zones of the metropolitan area of Buenos Aires. The sampling strategy followed consisted in collecting simultaneously 67 samples of PM10 particulate matter in 9 sampling sites covering an area of about 30 km2 during one week. The collection was performed on ash-free fibre-glass filters using high volume samplers. A combination of aqua regia and perchloric acid was used for leaching metals from filters. Key elements, namely Al, Ca, Cu, Fe, Mn, Mo, Ni, Pb, S, Sb, Sn, Zn and Zr, were determined by inductively coupled plasma-optical emission spectrometry (ICP-OES) and inductively coupled plasma-mass spectrometry (ICP-MS) at micro g g(-1) and ng g(-1) levels. Analyte concentration varied from 130 ng g(-1)(Mo) to over 30%(Ca). Multivariate statistical analysis was performed on the data set including the measured elemental compositions for the monitored period. The atmospheric concentration found for Pb confirms the decreasing levels of this element since the introduction of unleaded gasoline in 1995: 88 ng m(-3)(2001) < 220 ng m(-3)(1997) < 3900 ng m(-3)(1994). The average S concentration above 3 microg m(-3) is somehow unexpectedly high for Buenos Aires since the relatively low S content of liquid fuels and the massive usage of natural gas imply low emissions of this element from combustion activities. To the best of our knowledge, S concentrations are reported for the first time for this city.

Identification of a metallothionein in Synechococcus by capillary electrophoresis hyphenated with inductively coupled plasma mass spectrometry.

A home-made system hyphenating capillary electrophoresis with an inductively coupled plasma mass spectrometer (CE-ICP-MS) for cadmium speciation of protein-binding and free cadmium ions in solution is presented. The CE-ICP-MS interface consisted of an acrylic block with an internal volume ca. 20 microL in which a platinum electrode, a capillary column, and a connection to an ICP nebulizer were inserted. A make-up electrolyte solution containing 50 mmol L(-1) Tris-HCl buffer solution (pH 9.0) was continuously flowed through the interface to the ICP nebulizer. The separation of free Cd ions, Cd-cysteine, and Cd bounded to metallothionein (MT) isoforms from rabbit liver was carried out by capillary electrophoresis, and the analytes were detected by ICP-MS. The feasibility to isolate metallothionein compounds extracted from the cyanobacterium Synechococcus PCC7942 was demonstrated. The Cd binding proteins were induced in Synechococcus PCC7942 and further analyzed by CE ICP-MS.