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1.
Anal Chim Acta ; 581(2): 221-31, 2007 Jan 09.
Article in English | MEDLINE | ID: mdl-17386448

ABSTRACT

The aim of this study was to evaluate the performance characteristics of the recently developed super elastic solid-phase microextraction (SPME) fibers. The fiber needle, plunger and fiber core are manufactured with a special type of flexible alloy that exhibits excellent shape memory and tensile strength. This material makes the assemblies more robust, permitting several hundreds of analyses in a sequence, which is one of the ways to improve the robustness and sample throughput of automated SPME methods. The design and size of the needle utilized in the new fiber assemblies is discussed here, as well as the use of a septum-free injector replacement and a low-volume direct injection glass liner placed in the GC inlet. Deionized water and pump oil samples spiked with target volatile compounds (McReynold's probes and toluene) were used for the purposes of the presented study. A fully automated SPME sample preparation technique was combined with the GC-TOFMS system for the chromatographic separation and identification/quantification of the target analytes.

2.
J Chromatogr Sci ; 44(7): 444-50, 2006 Aug.
Article in English | MEDLINE | ID: mdl-16925942

ABSTRACT

In this study, two methods are developed for the extraction of 1,4-dioxane (dioxane) from water using 80-microm carboxen-polydimethylsiloxane solid-phase microextraction fibers followed by either gas chromatography (GC)-flame ionization detection (FID) or GC-mass spectrometry (MS). With GC-FID, the lower limit of detection (LOD) for 1,4-dioxane is 2.5 microg/L (ppb) with a linear range of 5 to 10,000 microg/L, obtained by immersing the fiber in the sample for 20 min with agitation. Using GC-MS, the lower limit of quantitation is 0.5 microg/L, and the LOD is 0.25 microg/L. The upper linear range limit is 100 microg/L. Samples are extracted in 20 min using either heated headspace with agitation or direct immersion with agitation.


Subject(s)
Dioxanes/analysis , Water Pollutants, Chemical/analysis , Gas Chromatography-Mass Spectrometry , Sensitivity and Specificity
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