Sample treatment with focused ultrasound and bath sonication as a powerful tool for the evaluation of cadmium pollution in estuarine waters

A new sample treatment was developed for the determination of dissolved cadmium in Tagus estuarine waters, based on focused ultrasound in conjunction with small volumes in the extraction steps for Cd pre-concentration. Cadmium was first pre-concentrated using a classical approach (APDC as the complexing agent and MIBK as the organic phase) and then back-extracted into HNO ₃ with the aid of focused ultrasound, which reduced the acid concentration by more than one order of magnitude (from 4 to 0.1 mol L ^{- 3} ). This sample treatment was accomplished in less than 5 min, using low sample volume (20 mL), and low-volume, low-concentration reagents. The pre-concentration factor used in this work was 25, but different sample/organic volume ratios may be used in order to increase that value. The limit of detection and the limit of quantification in Tagus water samples were 0.03 nmol L ^{- 1} and 0.1 nmol L ^{- 3} , respectively. Recoveries from spiked Tagus water were higher than 90%. The procedure was validated using the reference estuarine water NRC-SLEW-3. In the solubilization of Cd particulate, bath ultrasonication was used in conjunction with HNO ₃ + HCl, followed by H ₂ O ₂ , which took about 2 instead of the usual 12 h (cooling included) when high-pressure microwave digestion is used.