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Determination of 252-302 Da and tentative identification of 316-376 Da polycyclic aromatic hydrocarbons in Standard Reference Materials 1649a Urban Dust and 1650b and 2975 Diesel Particulate Matter by accelerated solvent extraction-HPLC-GC-MS.
Stockholm University, Faculty of Science, Department of Analytical Chemistry.
Stockholm University, Faculty of Science, Department of Analytical Chemistry.
2008 (English)In: Analytical and Bioanalytical Chemistry, ISSN 1618-2642, E-ISSN 1618-2650, Vol. 391, no 6, 2235-2248 p.Article in journal (Refereed) Published
Abstract [en]

We have assessed and compared the extraction recoveries of polycyclic aromatic hydrocarbons (PAHs) with molecular weights of 252, 276, 278, 300 and 302 from diesel particulate matter (PM) and urban air particles using ultrasonically-assisted extraction and accelerated solvent extraction methods, and evaluated the effects of sample and treatment parameters. The results show that accelerated solvent extraction can extract PAHs more efficiently from diesel PM than ultrasonically assisted extraction. They also show that PAHs are more difficult to extract from diesel PM than from urban air particles. Using toluene and maximum instrumental settings (200 ºC, 3000 psi and five extraction cycles) with 30 min static extraction times > 85 % of the analytes were estimated to be extracted from the diesel particles, but four extraction cycles with just 5 min static extraction times under these conditions seems to be sufficient to extract > 95 % of the analytes from the urban air particles. The accelerated solvent extraction method was validated using Standard Reference Materials (SRM) 1649a, Urban Dust, SRM 2975 and SRM 1650a, Diesel Particulate Matter, from the US National Institute of Standards and Technology (NIST). PAH concentrations determined by on-line high performance liquid chromatography-gas chromatography-mass spectrometry following the developed accelerated solvent extraction method were generally higher than the certified and reference NIST values and concentrations reported in the literature (e.g. the estimated concentration of benzo(a)pyrene in SRM 2975 was 15-fold higher than the NIST-certified value), probably because the extraction recoveries were higher than in previous studies. The developed accelerated solvent extraction method was used to analyze high molecular weight PAHs (Mw>302) in the investigated SRMs, and more than 170 (SRM 1649a), 80 (SRM 1650b) and 60 (SRM 2975) potential high molecular weight PAHs were tentatively identified in them, with molecular weights (depending on the SRM sample analysed) of 316, 326, 328, 340, 342, 350, 352, 366, 374 and 376. This is, to our knowledge, the first study to tentatively report PAHs with molecular weights of 316, 326, 328, 342, 350, 352, 366 and 374 in diesel particulate matter. GC-MS chromatograms obtained in selected ion monitoring mode (extracted ions for the above mentioned m/z) and full-scan mass spectra of tentatively identified high molecular weight PAHs are shown in the electronical supplementary material.

Place, publisher, year, edition, pages
Heidelberg, Germany: Springer-Verlag , 2008. Vol. 391, no 6, 2235-2248 p.
Keyword [en]
ASE, PAH, Dibenzopyrene, HMW PAH, SRM 1649a, SRM 1650b, SRM 2975
National Category
Chemical Sciences
Research subject
Analytical Chemistry
Identifiers
URN: urn:nbn:se:su:diva-29584DOI: 10.1007/s00216-008-2182-xISI: 000257200200029OAI: oai:DiVA.org:su-29584DiVA: diva2:234327
Available from: 2009-09-09 Created: 2009-09-07 Last updated: 2017-12-13Bibliographically approved
In thesis
1. Methods for Determination of Benzo(a)pyrene and High Molecular Weight (>300 Da) Polycyclic Aromatic Hydrocarbons in Particulate Matter from Ambient Air and Vehicle Exhausts
Open this publication in new window or tab >>Methods for Determination of Benzo(a)pyrene and High Molecular Weight (>300 Da) Polycyclic Aromatic Hydrocarbons in Particulate Matter from Ambient Air and Vehicle Exhausts
2009 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Air pollution with particulate matter (PM) raises considerable concern because of its adverse effects on human health. For this reason, and because the mechanisms of PM toxicity are not fully known, there is an urgent need to determine the chemical constituents of atmospheric PM, especially PM emanating from traffic - a major source of urban PM.

This thesis describes analytical methods that have been developed for determining polycyclic aromatic hydrocarbons (PAHs) in ambient air and vehicle exhaust PM, focusing particularly on benzo(a)pyrene (B(a)P) and the dibenzopyrenes: dibenzo(a,l)pyrene, dibenzo(a,e)pyrene, dibenzo(a,i)pyrene and dibenzo(a,h)pyrene. Trace amounts in complex matrices have been met by coupling parts or the entire clean-up step using liquid chromatography on-line with the analysis step using gas chromatography-mass spectrometry into one automated system.

Application of the methodology, using either ultrasonic assisted extraction (USE) or accelerated solvent extraction (ASE), to a National Institute of Standards and Technology (NIST) urban air standard reference material (SRM) yielded comparable or higher concentrations than the assigned NIST values, validating the approach. However, ASE provided higher extraction yields from diesel particulate SRMs than USE, and ASE of diesel SRMs generally yielded higher concentrations than the corresponding NIST values.

Concentrations of dibenzopyrenes in Stockholm air PM, and gasoline- and diesel-fuelled vehicle emissions (ng/km), are reported for the first time. When adjusted in terms of their relative carcinogenic potencies, the dibenzopyrenes were found to pose greater carcinogenic hazards than B(a)P, indicating that the current use of B(a)P as a marker probably leads to underestimates of the carcinogenicity of PAHs in ambient air.

The developed methods also worked well for analyzing larger molecular weight PAHs: more than 60 and 170 potential PAHs were detected in ambient air PM and diesel PM, respectively.

Place, publisher, year, edition, pages
Stockholm: Department of Analytical Chemistry, Stockholm, 2009. 97 p.
Keyword
PAH, dibenzopyrene, benzo(a)pyrene, standard reference material, air particulate matter, diesel particulate matter, toxic equivalence factor, ultrasonic assisted extraction, accelerated solvent extraction, automation, online coupling, GC/MC, LC/GC/MS
National Category
Analytical Chemistry
Research subject
Analytical Chemistry
Identifiers
urn:nbn:se:su:diva-29749 (URN)978-91-7155-920-3 (ISBN)
Public defence
2009-10-16, Magnélisalen, Kemiska övningslaboratoriet, Svante Arrhenius väg 16 B, Stockholm, 13:00 (English)
Opponent
Supervisors
Available from: 2009-09-24 Created: 2009-09-11 Last updated: 2009-09-22Bibliographically approved

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