title: Fiber-based solid phase microextraction using fused silica lined bottles to collect, store, and stabilize a multianalyte headspace gas sample for offline analyses.
abstract: We have developed a solid phase microextraction (SPME) sampling method using fused silica lined bottles (400 ml) to collect, store, and stabilize a headspace subsample from the source for subsequent offline, repetitive analyses of the gas using fiber-based SPME. The method enables long-term stability for repeated offline analysis of the organic species collected from the source headspace and retains all the advantages of fiber SPME sampling (e.g. rapid extraction, solvent free, simple and inexpensive) while providing additional advantages. Typically, the analytes collected on the SPME fiber must be desorbed and analyzed immediately to mitigate analyte loss or contamination. The new SPME sampling method, conducted offline using carboxen/polydimethylsiloxane (carboxen/PDMS - 85 μm) coated fibers, has been shown to be identical to in situ SPME sampling of a headspace acquired from an 80 component organic matrix with reproducibility demonstrated to be less than %RSD=7.0% for replicate samples measured over a 30-day period. In addition, repetitive samplings from one headspace aliquot are possible using one or more fibers and fiber types as well as quantitative options such as internal standard addition as demonstrated in a feasibility study using a benzene/toluene/xylene (BTX; 1 ppmv) certified gas standard, in which the SPME measurement precision (%RSD) was improved by a factor of 1.5-1.9 compared to the use of an external standard.
authors.affiliation: Lawrence Livermore National Laboratory, 7000 East Ave., Livermore, CA 94550, United States. Electronic address: harvey11@llnl.gov.
authors.forename: Chris A
authors.initials: CA
authors.lastname: Harvey
authors.affiliation: Lawrence Livermore National Laboratory, 7000 East Ave., Livermore, CA 94550, United States.
authors.forename: J Chance
authors.initials: JC
authors.lastname: Carter
authors.affiliation: Lawrence Livermore National Laboratory, 7000 East Ave., Livermore, CA 94550, United States.
authors.forename: John R
authors.initials: JR
authors.lastname: Ertel
authors.affiliation: Lawrence Livermore National Laboratory, 7000 East Ave., Livermore, CA 94550, United States.
authors.forename: Cindy T
authors.initials: CT
authors.lastname: Alviso
authors.affiliation: Lawrence Livermore National Laboratory, 7000 East Ave., Livermore, CA 94550, United States.
authors.forename: Sarah C
authors.initials: SC
authors.lastname: Chinn
authors.affiliation: Lawrence Livermore National Laboratory, 7000 East Ave., Livermore, CA 94550, United States.
authors.forename: Robert S
authors.initials: RS
authors.lastname: Maxwell
mesh_terms: D001554:Benzene / Q000032:analysis; D002623:Chemistry Techniques, Analytical / Q000295:instrumentation / Q000379:methods*; D005740:Gases / Q000737:chemistry*; D015203:Reproducibility of Results; D012822:Silicon Dioxide / Q000737:chemistry*; D052617:Solid Phase Microextraction / Q000295:instrumentation*; D014050:Toluene / Q000032:analysis; D014992:Xylenes / Q000032:analysis
chemical_list: D005740:Gases; D014992:Xylenes; D014050:Toluene; D012822:Silicon Dioxide; D001554:Benzene
keywords: External standard; Fiber SPME; Fused silica lined bottle; GC–MS; Gas chromatography; Headspace gas analysis; In situ HS-SPME; Internal standard; Magnetic translation; Material outgassing