Critical role of a pre-purge setup in the thermal desorption analysis of volatile organic compounds by gas chromatography with mass spectrometry

In general, volatile organic compounds in ambient air are quantified by following a well‐defined standard calibration procedure using a gas‐/liquid‐phase standard. If the liquid standard is analyzed by a thermal desorption, the solvent effect is unavoidable through the alteration of breakthrough pro...

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Published inJournal of separation science Vol. 38; no. 14; pp. 2455 - 2462
Main Authors Kim, Yong-Hyun, Kim, Ki-Hyun
Format Journal Article
LanguageEnglish
Published Germany Blackwell Publishing Ltd 01.07.2015
Wiley Subscription Services, Inc
Subjects
air
Calibration
Chromatography
Desorption
Gas chromatography
gas chromatography-mass spectrometry
Mass spectrometry
Methanol
Methyl alcohol
Organic compounds
Pre-purge
Solvent effect
Solvent effects
solvents
Sorbent tubes
Sorbents
Tubes
VOCs
Volatile organic compounds
Pre-purge
Gas chromatography
Sorbent tubes
Methanol
Solvent effects
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Summary:In general, volatile organic compounds in ambient air are quantified by following a well‐defined standard calibration procedure using a gas‐/liquid‐phase standard. If the liquid standard is analyzed by a thermal desorption, the solvent effect is unavoidable through the alteration of breakthrough properties or retention times. To learn more about the variables of the thermal desorption‐based analysis, the effect of pre‐purge conditions was evaluated for 18 volatile organic compounds with different types of sorbent tube materials by fixing standard volume (1 μL) and flow rate (100 mL/min). The gas phase calibration was also carried out as reference for the non‐solvent effect. A single tube filled with Tenax TA exhibited the least solvent effect with the short pre‐purge (1 min), while being subject to the breakthrough at or above 10 min pre‐purge. For a three‐bed sorbent tube with Carboxen 1000, at least 10 min of pre‐purge was needed for the compounds with a retention time close to methanol (e.g., propanal). Another three‐bed tube with Carbopack X reduced the solvent effect efficiently for a short pre‐purge (2 min) without the breakthrough. As such, the solvent effect can be adjusted by the proper control of the sorbent tube application.
Bibliography:National Research Foundation of Korea (NRF)
Table S1. Basic information for the preparation of liquid phase VOC standard for TD-based analysis. Table S2. Experimental scheme for the calibration analysis of liquid-phase VOC standard by the ST-TD-GC-MS. Table S3. Operational conditions for the calibration analysis of 18 target VOCs by the TD-GC-MS system. Fig. S1. A plot of experimental sequence to prepare the liquid working standard (for 3 point system calibration). Fig. S2. Plot of RF values for each individual VOC: sorbent tube type vs. pre-purge time.
istex:E8BD6F679DC8124CD2012983CDCF71E7C638B3F3
Ministry of Education, Science and Technology (MEST) - No. 2009-0093848
ark:/67375/WNG-DL9P0NZ9-G
ArticleID:JSSC4350
ObjectType-Article-1
SourceType-Scholarly Journals-1
ObjectType-Feature-2
content type line 14
content type line 23
ISSN:1615-9306
1615-9314
1615-9314
DOI:10.1002/jssc.201500367