Direct thermal desorption of semivolatile organic compounds from diffusion denuders and gas chromatographic analysis for trace concentration measurement

Document Type

Article

Publication Date

1-26-2007

Department

Department of Civil, Environmental, and Geospatial Engineering

Abstract

A novel method for collection and analysis of vapor-phase semivolatile organic compounds (SOCs) in ambient air is presented. The method utilizes thermal desorption of SOCs trapped in diffusion denuders coupled with cryogenic preconcentration on Tenax-TA and analysis by high resolution gas chromatography (GC)-electron-capture detection (ECD). The sampling and analysis methods employ custom-fabricated multicapillary diffusion denuders, a hot gas spike (HGS) apparatus to load known quantities of thermally stable standards into diffusion denuders prior to sample collection, a custom-fabricated oven to thermally desorb SOCs from the diffusion denuder, and a programmable temperature vaporization (PTV) inlet containing a liner packed with Tenax-TA for effective preconcentration of the analytes and water management. High flow rates into the PTV inlet of 750 mL min-1during thermal desorption are ca. a factor of ten greater than typically used. To improve resolution and retention time stability, the thermal desorption and PTV inlet programming procedure includes three steps to prevent water from entering the analytic column while effectively transferring the analytes into the GC system. The instrumentation and procedures provide virtually complete and consistent transfer of analytes collected from ambient air into the GC evidenced by recovery of seven replicates of four internal standards of 90.7 ± 4.0-120 ± 23% (mean ± 95% confidence interval, CI). Retention time based compound identification is facilitated by low retention time variability with an average 95% CI of 0.024 min for sixteen replicates of eight standards. Procedure details and performance metrics as well as ambient sampling results are presented.

Publication Title

Journal of Chromatography A

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