Application of Factorial Designs and Simplex Optimisation in the Development of Flow Injection-Hydride Generation-Graphite Furnace Atomic Absorption Spectrometry Procedures as Demonstrated for the Determination of Trace Levels of Germanium

The optimisation of a volume-based FI-HG-GFAAS procedure is described for the trace determination of Ge, comprising in situ collection of the generated germane in the graphite furnace. The response function is the peak area readout (A*s). Based on a preliminary study, where factorial designs were used to identify significant factors and interactions, the procedure was optimised using both simplex and OVAT (one variable at the time) methods. The characteristics and merits of these methods are discussed. Under optimal experimental conditions, using a sample volume of 100 mu-l, Ge was determined at a sampling frequency of 22 h-1. The sensitivity, in terms of the characteristic mass, m0, was 26 pg/0.0044 A*s, with a detection limit of 0.21 mu-g/L (3 sigma). The precision (relative standard deviation) was 2.0% (n=10) at the 1 mu-g/L level.