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Determination of the flame retardant tetrabromobisphenol A in air samples by liquid chromatography-mass spectrometry.
Stockholm University, Faculty of Science, Department of Analytical Chemistry.
Stockholm University, Faculty of Science, Department of Analytical Chemistry.
2006 (English)In: Journal of Chromatography A, ISSN 0021-9673, Vol. 1104, no 1-2, 106-12 p.Article in journal (Refereed) Published
Abstract [en]

An original method based on LC-MS for determination of the flame retardant tetrabromobisphenol A (TBBPA) in air is presented, as an alternative to the traditionally used GC-MS. The soft ionization in LC-MS makes it possible to monitor the intact molecule and to use 13C-labelled TBBPA as an internal surrogate standard, two features that improve both accuracy and precision of the analyses. Comparison of different acquisition modes in electrospray ionization showed that the lowest detections limit, 3.1 pg TBBPA injected, was obtained in SIM monitoring the molecular ions 542.7/544.7. A fragmentation pathway of TBBPA in LC-ESI-MS is suggested. The only sample clean-up steps required are solvent reduction and filtration of the sample extract. Recoveries were 93% at a 30 ng level and 75% at 3 ng. The new method was tested by analyses of air samples collected at a recycling plant for electronic equipment. The amount of TBBPA found was 13.8 ng/m3 with an RSD of 5.9%. Furthermore, it was found that TBBPA in a standard solution could be partially debrominated, if not carefully protected from light during storage.

Place, publisher, year, edition, pages
2006. Vol. 1104, no 1-2, 106-12 p.
National Category
Analytical Chemistry
Research subject
Analytical Chemistry
Identifiers
URN: urn:nbn:se:su:diva-26592DOI: 10.1016/j.chroma.2005.11.067PubMedID: 16337636OAI: oai:DiVA.org:su-26592DiVA: diva2:211073
Available from: 2009-04-07 Created: 2009-04-02 Last updated: 2009-04-08Bibliographically approved
In thesis
1. New methods for determination of airborne pollutants: Focus on tetrabromobisphenol A, organophosphate triesters and polycyclic aromatic hydrocarbons
Open this publication in new window or tab >>New methods for determination of airborne pollutants: Focus on tetrabromobisphenol A, organophosphate triesters and polycyclic aromatic hydrocarbons
2009 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

The work presented in this thesis concerns the development and evaluation of new methods of sampling and analysis of organic pollutants in the indoor and outdoor environment.

In Paper I, the development of a new method was reported for the determination of the brominated flame retardant tetrabromobisphenol A (TBBPA) in air using sampling with glass fiber filter and polyurethane foam (PUF), ultrasonic solvent extraction and liquid chromatography coupled to electrospray ionisation mass spectrometry (LC-ESI/MS). The MS fragmentation mechanism of TBBPA was thoroughly investigated and different acquisition modes were evaluated to achieve the most sensitive and selective detection.

In Papers II and III, the potential use of Empore SPE membranes was evaluated for air sampling of volatile, semi-volatile and particle-associated organic compounds. Breakthrough studies conducted for 24h at air flows of 10- 20 L/min showed that the SPE membranes efficiently retains volatile and semi-volatile organophosphate esters and particles >10 nm. Effort was invested in the development of fast and environmental friendly methods, with low cost, for sample clean up and analysis.

In Paper II, the sample preparation technique was dynamic solvent extraction with methanol coupled to LC-ESI/MS. The total run time per sample, including both extraction and separation, was less than 34 min, consuming only 1.6mL methanol. In Paper III, efficiency of selective extraction of polycyclic aromatic hydrocarbons from particulate matter sampled with Empore SPE membranes, using dynamic subcritical water extraction (DSWE) was investigated. Acceptable recoveries of the investigated compounds from reference material (SRM 1649a) were achieved. In Paper IV, the application of dynamic solid phase micro-extraction (SPME) air sampling was evaluated using, gas chromatography/positive ion chemical ionisation (GC/PICI) and tandem-MS detection for the determination of organophosphate esters in work environment.

Place, publisher, year, edition, pages
Stockholm: Department of Analytical Chemistry, Stockholm University, 2009. 80 p.
Keyword
Air sampling, sampling methods, indoor air, SPE, SPME, extraction, dynamic extraction, online coupling, SWE, subcritical water extraction, GC/MS, LC/MS, organophosphate triesters, PAH, tetrabromobisphenol A
National Category
Analytical Chemistry
Research subject
Analytical Chemistry
Identifiers
urn:nbn:se:su:diva-26700 (URN)978-91-7155-843-5 (ISBN)
Public defence
2009-05-14, Magnélisalen, Kemiska Övningslaboratoriet, Svante Arrhenius väg 12 A, Stockholm, 13:00 (Swedish)
Opponent
Supervisors
Available from: 2009-04-23 Created: 2009-04-07 Last updated: 2010-12-14Bibliographically approved

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