A simple, sensitive and rapid method involving dispersive liquid-liquid microextraction was developed for the determination of molybdenum using electrothermal atomic absorption spectrometry. After injection of a ternary mixture containing trichloroethylene (extractor solvent), ethanol (disperser solvent) and ammonium pyrrolidinedithiocarbamate (chelating reagent), the extraction of molybdenum into the aqueous phase occurs. The quantity of the element in the enriched phase was measured using electrothermal atomic absorption spectrometry. Under optimized conditions (pH 2.5, 2.0 mL of disperser solvent, 50 mL of extraction solvent, 50.0 mL of 0.10% m/v chelating solution and centrifugation at 3000 rpm for 2.5 minutes), the method has a detection limit of 0.013 mg L À1 , a quantification limit of 0.044 mg L À1 and an enrichment factor of 75 for a sample volume of 5.0 mL. The certified reference material NIST 2781, Domestic Sludge, was used to assess the accuracy of the method. The proposed procedure was successfully applied to the determination of molybdenum in natural water samples.
Experimental
InstrumentationAbsorbance measurements were performed using an AAnalyst 400 model atomic absorption spectrometer and an HGA 900 model graphite furnace, both supplied by Perkin Elmer (Shelton, USA). A hollow cathode lamp for molybdenum analysis (Perkin Elmer) was also used. The pH measurements were performed using a Quimis Q400AS pH meter (Diadema, Brazil).