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Anal Chem

Title:		Development of the detection threshold concept from a close look at sorption occurrence inside a glass vial based on the in-vial vaporization of semivolatile fatty acids
Author(s):		Kim YH; Kim KH; Szulejko JE; Parker D;
Address:		"Department of Civil and Environmental Engineering, Hanyang University , 222 Wangsimni-Ro, Seoul 133-791, Republic of Korea"
Journal Title:		Anal Chem
Year:		2014
Volume:		20140611
Issue:		13
Page Number:		6640 - 6647
DOI:		10.1021/ac501382e
ISSN/ISBN:		1520-6882 (Electronic) 0003-2700 (Linking)
Abstract:		"Headspace (HS) analysis has been recommended as one of the most optimal methods for extracting and analyzing volatile organic compounds from samples in diverse media such as soil and water. Short-chain volatile fatty acids (VFA, C3-C7) with strong adsorptivity were selected as the target compounds to assess the basic characteristics of the HS analysis through simulation of HS conditions by in-vial vaporization of liquid-phase standards (VL) in 25 mL glass vials. The reliability of the VL approach was assessed by apportioning the in-vial VFA mass into three classes: (1) vaporized fraction, (2) dynamic adsorption on the vial walls (intermediate stage between vaporization and irreversible absorption), and (3) irreversible absorptive loss (on the vial wall). The dynamic adsorption partitioning inside the vial increased with n-VFA carbon number, e.g., 43% (C2: acetic acid, extrapolated value), 65% (C3: propanoic acid), and 98% (C7: heptanoic acid). The maximum irreversible losses for the studied n-VFAs exhibited a quadratic relationship with carbon number. If the detection threshold limit (DTL: the onset of mass detection after attaining the maximum irreversible loss) is estimated, the DTL values for target VFAs were in the range of 101 ng for i-valeric acid to 616 ng for propionic acid, which are larger than the method detection limit by about 3 orders of magnitude. Consequently, quantitation of VFAs using the VL approach should be critically assessed by simultaneously considering the DTL criterion and the initial VFA masses loaded into the vial"
Keywords:		"Adsorption Chemical Fractionation/*instrumentation Equipment Design Fatty Acids, Volatile/*analysis Flow Injection Analysis/instrumentation Gas Chromatography-Mass Spectrometry/*instrumentation Glass/*chemistry Limit of Detection Volatilization;"
Notes:		"MedlineKim, Yong-Hyun Kim, Ki-Hyun Szulejko, Jan E Parker, David eng Evaluation Study Research Support, Non-U.S. Gov't 2014/06/03 Anal Chem. 2014 Jul 1; 86(13):6640-7. doi: 10.1021/ac501382e. Epub 2014 Jun 11"