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Determination of aromatic hydrocarbons in asphalt release agents using headspace solid-phase microextraction and gas chromatography-mass spectrometry
KTH, School of Architecture and the Built Environment (ABE), Civil and Architectural Engineering, Highway and Railway Engineering.
KTH, School of Architecture and the Built Environment (ABE), Civil and Architectural Engineering, Highway and Railway Engineering.
2005 (English)In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1069, no 2, 235-244 p.Article in journal (Refereed) Published
Abstract [en]

The possibility of quantitative analysis of aromatic hydrocarbons in oil-based asphalt release agents was investigated using headspace solid-phase microextraction (HS-SPME) followed by gas chromatography-mass spectrometry (GC-MS). The target analytes studied were benzene, toluene, ethylbenzene, p-, m-, and o-xylene (BTEX) and 1,3,5-trimethylbenzene and 1,2,4-trimethylbenzene. Experimental parameters influencing HS-SPME efficiency were studied (equilibration time between sample and headspace and between headspace and SPME fiber, sample amount and sample matrice effects). A HS-SPME method using hexadecane as a surrogate matrice was developed. The detection limit was estimated as 0.03-0.08 ppm (w/w) for the target analytes investigated. Good linearity was observed (R-2 > 0.999) for all calibration curves at high, medium and low concentration level. The repeatability of the method (RSD, relative standard deviation) was found to be less than 10 % (generally less than 5 %) in triplicate samples and approximately 2 % at eight consecutive tests on one and the same sample. The accuracy of the method given by recovery of spiked samples was between 85 and 106 % (generally between 95 and 105 %). The HS-SPME method developed was applied to four commercially available asphalt release agents. External calibration and standard addition approaches were investigated regarding accuracy. The results showed that standard addition generates higher accuracy than external calibration. The contents of target aromatic hydrocarbons in the asphalt release agents studied varied greatly from approximately 0.1-700 ppm. The method described looks promising. and could be a valuable too] for determination of aromatic hydrocarbons in different types of organic matrices.

Place, publisher, year, edition, pages
2005. Vol. 1069, no 2, 235-244 p.
Keyword [en]
headspace, solid-phase microextraction, asphalt release agents, aromatic hydrocarbons, BTEX
National Category
Building Technologies
Identifiers
URN: urn:nbn:se:kth:diva-7986DOI: 10.1016/j.chroma.2005.02.011ISI: 000227995500011Scopus ID: 2-s2.0-15244353942OAI: oai:DiVA.org:kth-7986DiVA: diva2:13184
Note
QC 20100913Available from: 2008-02-13 Created: 2008-02-13 Last updated: 2017-12-14Bibliographically approved
In thesis
1. Applications of Solid-Phase Microextraction to Chemical Characterization of Materials Used in Road Construction
Open this publication in new window or tab >>Applications of Solid-Phase Microextraction to Chemical Characterization of Materials Used in Road Construction
2008 (English)Doctoral thesis, comprehensive summary (Other scientific)
Abstract [en]

Environmental and health aspects of road materials have been discussed for a long time, mostly regarding bitumen and bitumen fumes. However, just a few studies on other types of road materials have been reported. In this doctoral study, two types of materials, asphalt release agents and bituminous sealants, were investigated with regard to chemical characterization and emission profiles. Besides conventional test methods, solid-phase microextraction (SPME) technique was applied for emissions profiles screening and quantitative analysis.

General description of main characteristics of asphalt release agents and bituminous sealants is given, and a comprehensive state-of-the-art on SPME technique is presented, especially on methodologies for analyzing mono- and polycyclic aromatic hydrocarbons (MAHs and PAHs) in different sample matrices.

In the experimental study, chemical characterization of the two material types was performed using conventional methods, including fourier transform infrared spectroscopy - attenuated total reflectance (FTIR-ATR), gel permeation chromatography (GPC), mass spectrometry (MS) and gas chromatography – mass spectrometry (GC-MS). General patterns regarding functional groups and molecular weight distribution were studied. In the case of asphalt release agents, more detailed information on chemical compositions, especially the contents of MAHs and PAHs, was obtained.

General information on emission proneness of asphalt release agents was obtained using thermogravimetric analysis (TGA) and MS. Using headspace(HS)-SPME and GC-MS, emission profiles of asphalt release agents were characterized at different temperatures, whereas the profiles of bituminous sealants were obtained solely at room temperature. The results presented were used for ranking the materials with regard to degree of total emission as well as emission of hazardous substances.

The applicability of HS-SPME for quantitative analysis of MAHs in asphalt release agents and emulsion-based bituminous sealants was investigated. The use of a surrogate sample matrix was concerned, and experimental parameters influencing the HS-SPME procedure, such as equilibration and extraction time, as well as effects of sample amount and matrices, were studied. The methods were evaluated with regard to detection limit, accuracy as well as precision. Different calibration approaches including external calibration, internal calibration and standard addition were investigated. The determination of MAHs in asphalt release agents and emulsion-based bituminous sealants using HS-SPME-GC-MS was conducted.

Place, publisher, year, edition, pages
Stockholm: KTH, 2008. vi, 54 p.
Series
Trita-VT. FR, ISSN 1650-867X ; 08:01
Keyword
Asphalt release agents, Petroleum oils, Vegetable oils, Bituminous sealants, Bitumen, Emissions, Monocyclic aromatic hydrocarbons, Polycyclic aromatic hydrocarbons, Fourier Transform Infrared Spectroscopy - Attenuated Total Reflectance, Gel Permeation Chromatography, Mass Spectrometry, Gas Chromatography - Mass Spectrometry, Thermogravimetric Analysis, Headspace, Solid-phase microextraction, Calibration.
National Category
Building Technologies
Identifiers
urn:nbn:se:kth:diva-4637 (URN)
Public defence
2008-03-10, Sal F3, Lindstedtsvägen 26, KTH, Stockholm, 10:00
Opponent
Supervisors
Note
QC 20100913Available from: 2008-02-13 Created: 2008-02-13 Last updated: 2010-09-13Bibliographically approved

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