Triple sorbent thermal desorption/gas chromatography/mass spectrometry determination of vapor phase organic contaminants

Book · Sat Dec 31 04:00:00 EST 1994

OSTI ID:197317

Ma, C Y; Skeen, J T; Dindal, A B; Higgins, C E; Jenkins, R A ^[1]

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1. Oak Ridge National Lab., TN (United States). Chemical and Analytical Sciences Div.

A thermal desorption/gas chromatography/mass spectrometry (TD/GC/MS) method has been evaluated for the determination of volatile organic compounds (VOCs) in vapor phase samples using Carbosieve S-III/Carbotrap/Carbotrap C triple sorbent traps (TST), similar to those available from a commercial source. The analysis was carried out with a Hewlett-Packard 5985A or 5995 GC/MS system with a modified injector to adapt an in-house manufactured short-path desorber for transferring desorbate directly onto a cryofocusing loop for subsequent GC/MS analysis. Vapor phase standards generated from 26 compounds were used for method validation, including alkanes, alkyl alcohols, alkyl ketones, and alkyl nitriles, a group of representative compounds that have previously been identified in a target airborne matrix. The method was validated based on the satisfactory results in terms of reproducibility, recovery rate, stability, and linearity. A relative standard deviation of 0.55 to 24.3% was obtained for the entire TD process (generation of gas phase standards, spiking the standards on and desorbing from TST) over a concentration range of 20 to 500 ng/trap. Linear correlation coefficients for the calibration curves as determined ranged from 0.81 to 0.99 and limits of detection ranged from 3 to 76 ng. For a majority of standards, recoveries of greater than 90% were observed. For three selected standards spiked on TSTs, minimal loss (10 to 22%) was observed after storing the spiked traps in a 4 C refrigerator for 29 days. The only chromatographic artifact observed was a 5% conversion of isopropanol to acetone. The validated method has been successfully applied to the determination of VOCs collected from various emission sources in a diversified concentration range.

• DOE Contract Number: AC05-84OR21400
• OSTI ID: 197317
• Report Number(s): CONF-9405167--
• Country of Publication: United States
• Language: English

Related Subjects

54 ENVIRONMENTAL SCIENCES
ALCOHOLS
ALKANES
CHEMICAL ANALYSIS
EXPERIMENTAL DATA
KETONES
MASS SPECTROSCOPY
NITRILES
VAPORS
VOLATILE MATTER