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Automated high-capacity sorption probe for extraction of organic compounds in aqueous samples followed by gas chromatographic analysis
KTH, Superseded Departments, Chemistry.
KTH, Superseded Departments, Chemistry.
KTH, Superseded Departments, Chemistry.
KTH, Superseded Departments, Chemistry.
2004 (English)In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1033, no 2, 339-347 p.Article in journal (Refereed) Published
Abstract [en]

An automated high-capacity sorption device for GC analysis of ultra trace components has been developed. The scope of the presented technique was to combine the simplicity of solid-phase microextraction (SPME) with the high extraction efficiency of the stir bar sorptive extraction technology. Sorptive extractions of water samples were performed using polydimethylsiloxane (PDMS) rubber tubing (120 μl) mounted onto a glass rod. The sampling procedure was carried out by a robotic autoinjector. Since the setup is fully automated, unattended and precise time-controlled extraction of samples is possible and makes quantitation with non-equilibrium extractions feasible. The sorption probes are easy to exchange, which facilitates off-line/in-field sampling. The system was evaluated with a test mixture of 44 environmentally hazardous compounds. Detection limits were found to be in the sub-ppt region. The performance of the system was demonstrated with the analysis of polycyclic aromatic hydrocarbons in urban snow.

Place, publisher, year, edition, pages
2004. Vol. 1033, no 2, 339-347 p.
Keyword [en]
Automation, Environmental analysis, Extraction methods, Polynuclear aromatic hydrocarbons, Sorption, Water analysis
National Category
Chemical Sciences
Identifiers
URN: urn:nbn:se:kth:diva-4910DOI: 10.1016/j.chroma.2004.01.056ISI: 000220398900018Scopus ID: 2-s2.0-1542298904OAI: oai:DiVA.org:kth-4910DiVA: diva2:6846
Note
QC 20100831Available from: 2008-12-23 Created: 2008-12-23 Last updated: 2017-12-06Bibliographically approved
In thesis
1. New concepts and techniques for quantification and trace analysis by gas chromatography
Open this publication in new window or tab >>New concepts and techniques for quantification and trace analysis by gas chromatography
2004 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

In the first part of this thesis, strategies for avoiding systematic errors when quantifying the main components in mixtures of solvents has been developed (paper I). It is shown that variations in density caused by variations in sample composition and/or volume contraction need to be taken into account. In this way, quantification can be improved.

The second part (paper II-V) describes a number of new methods for the analysis of organic trace components present in gaseous or aqueous samples, after an overview of the most commonly applied sample enrichment techniques has been given.

For the enrichment of volatile trace compounds from gaseous samples, the concept of open tubular trapping has been further developed. A simplified procedure for preparing ultra-thick film, sorptive open tubular traps (OTTs) is described (paper III). The traps are coated with an irregular film of PDMS, and it is shown that the performance in terms of breakthrough volume is only marginally affected by the use of such traps. In paper IV, it is shown both experimentally and with a theoretical model that the enrichment capacity of OTTs can be significantly increased by increasing the inner diameter of the traps.

A fully automated procedure for high-capacity sorption enrichment of trace organic analytes present in water is also reported (paper II). Time-based non-equilibrium extractions are feasible, enabling fast extractions that still allow sub-ppt limits of detection. The high flexibility of the automated system makes it possible to sample from process streams or off-line sources.

Finally, the development of a new 2-dimensional precolumn-backflush method for the analysis of polar volatile trace analytes in water is described (paper V). This concept is based on the action of a hygroscopic salt which has a strong affinity for water, in a precolumn. Organic trace compounds, such as volatile alcohols or ketones show little retention on the precolumn and are eluted ahead of the bulk amount of the water onto a capillary column for subsequent high resolution separation. The residual water is removed from the system by backflushing the precolumn. The procedure allows the direct injection of aqueous sample volumes of at least 100 µl, and the pre-fractionation is accomplished within only a few minutes. Quantification limits for selected polar trace components were in the low ppb-region.

Place, publisher, year, edition, pages
Kemi, 2004. x, 77 p.
Keyword
Chemistry, quantitative accuracy, calibration, extenal standards, valume contraction, molar excess volume, Kemi
National Category
Chemical Sciences
Identifiers
urn:nbn:se:kth:diva-44 (URN)91-7283-827-2 (ISBN)
Public defence
2004-11-12, Kollegiesalen, KTH, Valhallavägen 79, Stockholm, 10:00 (English)
Opponent
Supervisors
Available from: 2008-10-10 Created: 2008-10-10 Last updated: 2012-03-21Bibliographically approved

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