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Analysis of nitroaromatic compounds in complex samples using solid-phase microextraction and isotope dilution quantification gas chromatography-electron-capture negative ionisation mass spectrometry
Örebro University, Department of Natural Sciences.
Örebro University, Department of Natural Sciences.
Örebro University, Department of Natural Sciences.ORCID iD: 0000-0001-6217-8857
2007 (English)In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1164, no 1-2, p. 65-73Article in journal (Refereed) Published
Abstract [en]

A solid-phase microextraction (SPME) method using gas chromatography–electron-capture negative ionisation mass spectrometry (GC–ECNI-MS) and isotope dilution quantification for the analysis of nitroaromatic compounds in complex, water based samples has been optimised. For ionisation, ECNI was the most sensitive and selective method. SPME was compared to solid-phase extraction (SPE) and found to be more sensitive for these small volume samples. LODs were in the range 0.02–38 ng L−1 for SPME and 6–184 ng L−1 for SPE, respectively. The SPME method was applied on samples in the ng L−1 level from artificial reed beds treated with sludge containing residues from explosives and pharmaceuticals.

Place, publisher, year, edition, pages
Amsterdam: Elsevier , 2007. Vol. 1164, no 1-2, p. 65-73
National Category
Natural Sciences Chemical Sciences
Research subject
Chemistry
Identifiers
URN: urn:nbn:se:oru:diva-2905DOI: 10.1016/j.chroma.2007.07.023OAI: oai:DiVA.org:oru-2905DiVA, id: diva2:135472
Available from: 2008-02-15 Created: 2008-02-15 Last updated: 2017-12-14Bibliographically approved
In thesis
1. Microextraction for usage in environmental monitoring and modelling of nitroaromatic compounds and haloanisoles
Open this publication in new window or tab >>Microextraction for usage in environmental monitoring and modelling of nitroaromatic compounds and haloanisoles
2008 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Processes in the environment are often complex and the description and prediction of the behaviour of environmental pollutants requires sophisticated methodology including multidimensional technology. Multivariate statistical methods including principal component analysis (PCA) and partial least squares projection to latent structures (PLS) were used to characterise several nitroaromatic compounds according to a large number of chemical and physical properties. These descriptors were derived from databases and semi-empirical, empirical and quantum-chemical calculations. A model was calculated and used for prediction of experimentally determined relevant environmental parameters, including volatility through gas chromatographic retention times and the distribution between air and water phase using solid-phase microextraction measurements. Analytical microextraction techniques are very well suited for both monitoring and measuring relevant environmental properties. Two such methods, solid-phase microextraction (SPME) and microextraction by packed syringe (MEPS), which are both faster and less resource demanding than traditional methodology, were used to improve the analysis of nitroaromatic compound and haloanisoles. Both techniques showed few interfering compounds and good reproducibility in combination with GC-MS detection. The reproducibility for SPME and MEPS was further enhanced by the usage of isotopically labelled internal standards (nitroaromatic compounds) or internal standards with similar chemical properties as the analytes (haloanisoles).

The SPME method for nitroaromatic compounds was tested using industrial wastewater from a wastewater treatment facility receiving input from several nitrogen based industries. Using gas chromatography-negative chemical ionisation-mass spectrometry(GC-NCI-MS) as the final detection, limits of detection (LODs) in the range 0.02–38 ng L−1 were achieved. Results for the 2,4,6-TCA (TCA) and 2,4,6-TBA (TBA) using high resolution GC-MS were even more impressive obtaining LODs in the range 0.02-0.03 ng L-1, which are currently the lowest reported in the international literature. Although the newly developed MEPS technology is generally faster than SPME, similar LODs as for SPME could not yet be achieved. Both methods were found to be so sensitive that TCA and TBA could be detected in wine before it could be sensorically noticed as cork tainted.

Place, publisher, year, edition, pages
Örebro: Örebro universitet, 2008. p. 58
Series
Örebro Studies in Chemistry, ISSN 1651-4270 ; 9
Keywords
PCA, PLS, QSPR, SPME, MEPS, nitroaromatic compounds, TCA, TBA
National Category
Chemical Sciences
Research subject
Chemistry
Identifiers
urn:nbn:se:oru:diva-1786 (URN)978-91-7668-582-2 (ISBN)
Public defence
2008-03-07, Bion, Forumhuset, Örebro universitet, Örebro, 10:00
Opponent
Supervisors
Available from: 2008-02-15 Created: 2008-02-15 Last updated: 2017-10-18Bibliographically approved

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Jönsson, SofieGustavsson, Lillemorvan Bavel, Bert

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