Simultaneous Element-Selective Detection of C,F, Cl,Br, and I by Capillary Gas Chromatography Coupled with Microplasma Mass Spectrometry

Simultaneous element-selective detection of the halogens and carbon was accomplished with capillary gas chromatography coupled with microplasma mass spectrometry. The microplasma ion source was a radio frequency plasma contained inside the last 4–5 cm of the 0.32 mm i.d. fused silica capillary column. The ion source was located inside the high vacuum housing of the MS, and only the GC carrier gas (2.3 mL min⁻¹ of helium) was used for plasma generation. Atomic ions were detected in the positive mode. Detection limits were in the low picogram area, and the selectivity to carbon ranged from 8×10² for fluorine to higher than 10⁴ for the other halogens. By introduction of both hydrogen and oxygen as reagent gases, peak tailing was avoided by suppression of analyte reactions with the silica walls of the ion source. Special attention was given to the fluorine-selective detection due to an interfering background species at m/z 19, assumed to be H₃O⁺ originating from the reagent gases. The background signal was minimized by careful control of the power level.