Study of parameters associated with the determination of cadmium in lake sediments by slurry sampling electrothermal atomic absorption spectrometry

摘要

Cadmium concentration in lake sediments is determined by suspending the solid samples in a solution containing 5% (v/v) concentrated nitric acid and 0.1% (v/v) Triton X-100.Three modifiers were tested for the direct determination.The furnace temperature programmes and appropriate amount for each modifier were optimised to get the highest signal and the best separation between the atomic and background signals.The drying stage is performed by programming a 400 deg C temperature,a ramp time of 25s and hold time of 10s on the power supply of the atomiser.No ashing step is used and platform atomisation is carried out at 2200 C.W-Rh permanent modifier combined with conventional modifier by delivering 10 mul of 0.50% (w/v) NH_4H_2PO_4 solution was the best chemical modifier for cadmium determination.This modifier also acts as a liquid medium for the slurry,thus simplifying the procedure.Calibration is performed using aqueous standards in the 1-5 mug l~(-1) range.The optimised method gave a limit of detection of 0.56 ng ml~(-1),characteristic mass of 10.1 +- O.Spg for aqueous standard,9.6 +-0.7 pg for slurry samples containing different Cd concentrations and good precision (7.6-5.2%).The method was validated by analysing four certified reference lake sediment materials: LKSD-1,LKSD-2,LKSD-3 and LKSD-4; satisfactory recoveries were obtained (90.0-96.3%) and no statistical differences were observed between the experimental and the certified cadmium concentration.The developed methodology was used to determine cadmium in three 'real' sediment samples from lakes in the area of Wielkopolski National Park,Poland.