On-line microwave digestion of slurry samples with direct flame atomic absorption spectrometric elemental detection

Abstract

A flow injection (FI) system for on-line microwave digestion of slurried samples with direct elemental determinations by flame atomic absorption spectrometry is described. Organically based elemental reference samples were prepared as slurries in 5% v/v HNO₃ and the system was optimized for slurry mass, acid strength and tube and microwave cavity geometry. Bubble formation during digestion was controlled by post-digestion cooling and pressure regulation. Comparison of direct and FI calibrations indicated no apparent loss in sensitivity. Various samples were examined and elemental recoveries for Ca, Fe, Mg and Zn were typically found to be in the range 94–107% with precisions of less than 4.5% relative standard deviation. The major source of error was found to be in the dispersion of solids (<180 µm) as slurries in dilute HNO₃. The through put of samples in the system developed was found to be 1–2 min per sample.