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Dynamic non-equilibrium SPME combined with GC, PICI, and ion trap MS for determination of organophosphate esters in air
Stockholm University, Faculty of Science, Department of Analytical Chemistry.
Stockholm University, Faculty of Science, Department of Analytical Chemistry.
Stockholm University, Faculty of Science, Department of Analytical Chemistry.
2010 (English)In: Analytical and Bioanalytical Chemistry, ISSN 1618-2642, E-ISSN 1618-2650, Vol. 396, no 2, 839-844 p.Article in journal (Refereed) Published
Abstract [en]

Methodology for time-weighted average (TWA) air measurements of semivolatile organophosphate triesters, widely used flame-retardants and plasticizers, and common indoor pollutants is presented. Dynamic non-equilibrium solid-phase microextraction (SPME) for air sampling, in combination with GC/PICI and ion trap tandem MS, yields a fast, almost solvent-free method with low detection limits. Methanol was used as reagent gas for PICI, yielding stable protonated molecules and few fragments. A field sampler, in which a pumped airflow over three polydimethylsiloxane (PDMS) 100-μm fibers in series was applied, was constructed, evaluated, and used for the measurements. The method LODs were in the range 2–26 ng m−3 for a sampling period of 2 h. The uptake on the SPME fibers was shown to be about five times faster for triphenyl phosphate compared to the other investigated organophosphate esters, most likely due to more lipophilic properties of the aromatic compound. The boundary layer for triphenyl phosphate when using a 100-µm PDMS sorbent was determined to 0.08 mm at a linear air velocity of 34 cm s−1. Five different organophosphate triesters were detected in air from a laboratory and a lecture hall, at concentrations ranging from 7 ng m−3 up to 2.8 μg m−3.

Place, publisher, year, edition, pages
Berlin: Springer , 2010. Vol. 396, no 2, 839-844 p.
Keyword [en]
Organophosphate triesters, SPME, Non-equilibrium, Dynamic air sampling, PICI, GC/MS/MS
National Category
Natural Sciences
Identifiers
URN: urn:nbn:se:su:diva-34673DOI: 10.1007/s00216-009-3221-yOAI: oai:DiVA.org:su-34673DiVA: diva2:285263
Available from: 2010-01-11 Created: 2010-01-11 Last updated: 2017-12-12Bibliographically 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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