Method and apparatus for pyrolysis—Porous layer open tubular column—Cryoadsorption headspace sampling and analysis

In previous work, dynamic headspace vapor collection on short, porous layer open tubular (PLOT) capillary columns maintained at low temperature was introduced. In this paper, that metrology is extended with the introduction of a small in situ pyrolysis platform that provides for rapid heating and rapid vapor capture for a wide variety of samples. The new approach is referred to as pyro-PLOT-cryo. The pyrolysis platform is made from two small copper lead wires that hold a basket formed from small diameter, high resistance stainless steel or NiCr wire. The basket is formed to accept a small sample, the mass of which can typically range from 0.2 to 0.05 mg. The pyrolysis is performed by use of a resistor capacitor circuit of the type used in spot welders. We have provided examples of the application of this technique with the analysis of facial cosmetics, plastic explosives, organometallic gasoline additives, polymers, and in micro scale chemical reactions. Additional modifications and future work are also discussed.

► New method consists of a combination of PLOT-cryoadsorption for headspace collection and pyrolysis, called pyro-PLOT-cryo.
► Pyro-PLOT-cryo is a headspace sampling method that makes its own headspace.
► Headspace collections can be done in a fraction of the time it took for previous methods.
► Headspace collections can be done with a fraction of the material that was required for previous methods.