National Research Council of Canada. NRC Institute for National Measurement Standards
Chloride- and hydride-generation headspace solid-phase microextraction (SPME) techniques have been compared for the detection of trace amounts of germanium by inductively coupled plasma time-of-flight mass spectrometry (ICP–TOFMS). The conditions for generation of germanium chloride, including acid type and concentration, effect of sodium chloride and extraction time, were investigated. Detection limits of 20 and 92 pg mL–1 and precisions of 18% (n=11) and 9.7% (n=11) were achieved for chloride and hydride generation, respectively, at a concentration of 10 ng mL–1. The generated germanium chloride and hydride species identities were characterized and confirmed as GeCl4 and GeH4 by use of electron-impact ionization mass spectrometry. Chloride generation coupled with SPME sampling and ICP–TOFMS detection resulted in twofold enhancement of sensitivity compared to GeH4 and detection limits for continuous hydride generation were 20-fold better than reported atomic fluorescence data.
Analytical and Bioanalytical Chemistry373, no. 8: 849–855.