Low-temp. gas chromatog. (LT-GC) coupled online with inductively coupled plasma mass spectrometry (ICP-MS) was used to identify volatile metal and metalloid compds. in human breath. After cryogenic sampling, the gas sample was sepd. without any clean-up by increasing the temp. (-100 to +200 Deg). Simultaneous detn. of 11 elements with ICP-MS was used for screening anal. The detection limits of volatile compds. in intra-oral air are in the range of ng/m3. Di-Me selenium was detd. in each gas sample from 6 test persons in the range 0.08-0.98 mg/m3.