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Determination of dibenzopyrenes in standard reference materials (SRM) 1649a, 1650, and 2975 using ultrasonically assisted extraction and LC-GC-MS
Stockholm University, Faculty of Science, Department of Analytical Chemistry.
2006 (English)In: Analytical and Bioanalytical Chemistry, ISSN 1618-2642, E-ISSN 1618-2650, Vol. 384, no 2, 438-447 p.Article in journal (Refereed) Published
Abstract [en]

A method has been developed for analysis of the highly potent polycyclic aromatic hydrocarbon (PAH) carcinogens dibenzo(a,l)pyrene, dibenzo(a,h)pyrene and dibenzo(a,i)pyrene (molecular weight 302) present in small amounts in diesel and air particulate materials. The method can also be used for analysis of the PAH benzo(a)pyrene, coronene and perylene, for which reference and certified values are available for the Standard Reference Materials used for validation of the method: SRM 1649a (Urban dust) and SRM 2975 (Diesel particulate matter). The only NIST values that have been published for these dibenzopyrene isomers in the analyzed SRMs are reference values for dibenzo(a,i)pyrene and dibenzo(a,h)pyrene in SRM 1649a. The concentrations determined in the SRMs were in good agreement with reported NIST-certified and reference values and other concentrations reported in the literature. The Standard Reference Material 1650 (Diesel particulate matter) was also analyzed. The method could not, however, be validated using this material because certification of SRM 1650 had expired. The method is based on ultrasonically-assisted extraction of the particulate material, then silica SPE pre-separation and isolation, and, separation and detection by hyphenated LC-GC-MS. The method is relatively rapid and requires only approximately 1-5 mg SRM particulate material to identify and quantify the analytes. Low extraction recoveries for the analytes, in particular the dibenzopyrenes, when extracting diesel SRMs 2975 and 1650 resulted, however, in the dibenzopyrenes being present in amounts near their limit of quantifications in these samples. The method’s limit of quantification (LOQ), based on analyses of SRM 1649a, is in the range of 10-77 pg. By use of this method more than 25 potential PAH isomers with a molecular weight of 302 could be separated.

Place, publisher, year, edition, pages
Heidelberg, Germany: Springer-Verlag , 2006. Vol. 384, no 2, 438-447 p.
Keyword [en]
Dibenzopyrenes, LC-GC-MS, PAH, SRM 1649a, SRM 1650, SRM 2975
National Category
Analytical Chemistry
Research subject
Analytical Chemistry
Identifiers
URN: urn:nbn:se:su:diva-29579DOI: 10.1007/s00216-005-0192-5OAI: oai:DiVA.org:su-29579DiVA: diva2:234318
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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