Sorbent material characterization using in‐tube extraction needles as inverse gas chromatography column

Abstract

In-tube extraction is a full automated enrichment technique that consists of a stainless-steel needle, packed with sorbent material for the extraction of volatile and semivolatile compounds. In principle, all particulate sorbents used for enrichment in air or headspace analysis can be used. However, the selection of the sorbents is merely based on empirical considerations rather than on experimental data, which is caused by a lack of knowledge about the relevant physicochemical properties of the sorbent. Especially, the knowledge of hydrostatic, advective, diffusive, and dispersion mechanisms in addition to sorption enthalpies are important for combined transport and sorption models. To provide these missing parameters, we developed and evaluated a method in which an ordinary in-tube extraction needle was employed directly as column for sorbent characterization by inverse gas chromatography. As probe compounds, benzene, ethyl acetate, and 3-methyl-1-butanol were used to determine thermodynamic parameters such as sorption enthalpy, partitioning constant between the solid and gas phase, and kinetic parameters such as the diffusion coefficient, dispersion coefficient, and apparent permeability, exemplarily. As sorbent, three commercially available phases were characterized to demonstrate the applicability of the method.