Determination of cadmium in water by ICP-AES with on-line adsorption preconcentration using DPTH-gel and TS-gel microcolumns

Two flow injection inductively coupled plasma atomic emission spectrometric methods for the preconcentration and determination of trace amounts of cadmium in sea-water and waste-water samples are described based on the adsorption of the metal ion on a micro-column placed in the injection valve of the FI manifold and packed with silica gel funtionalised with 1,5-bis(di-2-pyridyl) methylene thiocarbohydrazide (DPTH-gel) and silica gel functionalised with methylthiosalicylate (TS-gel), respectively. Various parameters and chemical variables affecting the preconcentration and determination of this metal by ICP-AES are evaluated. The DPTH-gel preconcentration method has a linear calibration range from 5 to at least 100 ng ml −1 of cadmium, with a R.S.D. of 1.1% for ten independent analyses of 100 ng ml −1, a detection limit of 1.1 ng ml −1 and a throughput of 40 samples per hour using a 60 s preconcentration time. The TS-gel preconcentration method shows a linear range between 10 and 100 ng ml −1, with a R.S.D. of 2.5% for ten independent analyses of 100 ng ml −1, a detection limit of 4.3 ng ml −1 and a sample throughput of 24 samples per hour for a preconcentration time of 120 s. Validation was carried out against a certified reference water sample and by determining the analyte content in spiked synthetic sea-water, sea-water and waste-water.