Needle microextraction trap for on‐site analysis of airborne volatile compounds at ultra‐trace levels in gaseous samples

Abstract

Different capillary needle trap (NT) configurations are studied and compared to evaluate the suitability of this methodology for screening in the analysis of volatile organic compounds (VOCs) in air samples at ultra-trace levels. Totally, 22 gauge needles with side holes give the best performance and results, resulting in good sampling flow reproducibility as well as fast and complete NT conditioning and cleaning. Two different types of sorbent are evaluated: a graphitized carbon (Carbopack X) and a polymeric sorbent (Tenax TA). Optimized experimental conditions were desorption in the GC injector at 300°C, no make-up gas to help the transport of the desorbed compounds to the GC column, 1 min splitless time for injection/desorption, and leaving the NT in the hot injector for about 20 min. Cross-contamination is avoided when samples containing high VOC levels (above likely breakthrough values) are evaluated. Neither carryover nor contamination is detected for storage times up to 48 h at 4°C. The method developed is applied for the analysis of indoor air, outdoor air and breath samples. The results obtained are equivalent to those obtained with other thermal desorption devices but have the advantage of using small sample volumes, being simpler, more economical and more robust than conventional methodologies used for VOC analysis in air samples.