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Applications of Solid-Phase Microextraction to Chemical Characterization of Materials Used in Road Construction
KTH, School of Architecture and the Built Environment (ABE), Civil and Architectural Engineering, Highway and Railway Engineering.
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 [en]
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: urn:nbn:se:kth:diva-4637OAI: oai:DiVA.org:kth-4637DiVA: diva2:13186
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
List of papers
1. Analysis of mono- and polycyclic aromatic hydrocarbons using solid-phase microextraction: state-of-the-art
Open this publication in new window or tab >>Analysis of mono- and polycyclic aromatic hydrocarbons using solid-phase microextraction: state-of-the-art
2008 (English)In: Energy & Fuels, ISSN 0887-0624, E-ISSN 1520-5029, Vol. 22, no 3, 1425-1438 p.Article in journal (Refereed) Published
Abstract [en]

The contamination of petroleum hydrocarbons, especially mono- and polycyclic aromatic hydrocarbons (MAHs and PAHs), has been discussed for a long time with regard to environmental and health aspects. Solid-phase microextraction (SPME), as a solvent-free sample preparation technique, has been widely used in environmental analysis. This state-of-the-art summarizes current knowledge regarding analysis of MAHs and PAHs using SPME. General aspects of SPME technique are briefly reviewed, including operating principles, methodologies, applications, and possible problems. The methodology of SPME technique in analysis of MAHs and PAHs in gaseous, liquid, and solid matrices is discussed in detail, covering extraction strategy, optimization of experimental parameters, calibration, and validation as well as analytical instruments connected with SPME. The aim of the paper is to give a concise overview together with general guidelines of MAH and PAH analysis using SPME.

Keyword
Aromatic compounds, Contamination, Extraction, Hydrocarbons, Organic compounds, Petroleum chemistry, Polycyclic aromatic hydrocarbons, Solvent extraction, Analytical instruments, Environmental, Environmental analysis, Experimental parameters, General aspects, Long times, Operating principles, Petroleum hydrocarbons, Sample preparation techniques, Solid-phase microextraction
National Category
Building Technologies
Identifiers
urn:nbn:se:kth:diva-7983 (URN)10.1021/ef7007166 (DOI)000256057600004 ()2-s2.0-45449116607 (Scopus ID)
Note
QC 20100913. Uppdaterad från accepted till published (20100913).Available from: 2008-02-13 Created: 2008-02-13 Last updated: 2017-12-14Bibliographically approved
2. Chemical characterization of oil-based asphalt release agents and their emissions
Open this publication in new window or tab >>Chemical characterization of oil-based asphalt release agents and their emissions
2006 (English)In: Fuel, ISSN 0016-2361, E-ISSN 1873-7153, Vol. 85, no 9, 1232-1241 p.Article in journal (Refereed) Published
Abstract [en]

Four commercial asphalt release agents were chemically characterized using different analytical methods. Functional groups and molecular weight distributions were determined by fourier transform infrared spectroscopy-attenuated total reflectance (FTIR-ATR), gel permeation chromatography (GPC) and mass spectrometry (MS). General compositions of the agents were obtained as petroleum hydrocarbons, fatty acid methyl esters (FAMEs), fatty acids and glycerides using gas chromatography-mass spectrometry (GC-MS) and MS probe inlet method. The contents of health related analytes, such as aromatic hydrocarbons and polycyclic aromatic hydrocarbons (PAHs), were determined. Asphalt release agents emission was investigated using thermogravimetric analysis (TGA) and headspace solid-phase microextraction (HS-SPME) The emission proneness as well as emission level of aromatic hydrocarbons from these agents were compared. The results obtained were used for ranking the agents with regard to health hazards.

Keyword
asphalt release agents, petroleum oil, vegetable oil, solid-phase microextraction, aromatic hydrocarbons, PAHs
National Category
Building Technologies
Identifiers
urn:nbn:se:kth:diva-7984 (URN)10.1016/j.fuel.2005.11.002 (DOI)000236816400009 ()2-s2.0-32544439862 (Scopus ID)
Note
QC 20100913Available from: 2008-02-13 Created: 2008-02-13 Last updated: 2017-12-14Bibliographically approved
3. Chemical characterization and screening of emission profiles of bituminous sealants using solid-phase microextraction
Open this publication in new window or tab >>Chemical characterization and screening of emission profiles of bituminous sealants using solid-phase microextraction
2006 (English)In: Energy & Fuels, ISSN 0887-0624, E-ISSN 1520-5029, Vol. 20, no 4, 1528-1535 p.Article in journal (Refereed) Published
Abstract [en]

Seven commercial bituminous sealants and their emissions were characterized with regard to chemical composition. On the basis of the results of the analysis, the sealants were ranked concerning health aspects. Chemical function groups and molecular weight distributions determined using Fourier transform infrared spectroscopy-attenuated total reflectance (FTIR-ATR) and gel permeation chromatography (GPC) indicated that bituminous material was the main component of the sealants studied. Most of the sealants investigated also contained additives originated from petroleum oil or treated vegetable oil. The emission profiles of these sealants at room temperature were obtained using the headspace solid-phase microextraction (HS-SPME) technique. The main groups of compounds found in the emissions were alkanes (C-9-C-12 normal and branched), cycloalkanes (C-1-C-5 alkylated cyclohexane and different hydronaphthalenes), aromatic hydrocarbons (C-1-C-5 alkylated benzene and C-1-C-2 alkylated naphthalene), and fatty acid methyl esters. The rankings of total emission and aromatics emission were compared. The results showed that HS-SPME is a suitable fast screening tool for emission studies, and it facilitates the selection of appropriate bituminous sealants with regard to environmental and health aspects.

Keyword
Bituminous materials, Characterization, Chemical analysis, Particulate emissions, Sealants, Bituminous sealants, Chemical characterization, Solid-phase microextraction
National Category
Building Technologies
Identifiers
urn:nbn:se:kth:diva-7985 (URN)10.1021/ef0600715 (DOI)000239120000026 ()2-s2.0-33746912716 (Scopus ID)
Note
QC 20100913Available from: 2008-02-13 Created: 2008-02-13 Last updated: 2017-12-14Bibliographically approved
4. Determination of aromatic hydrocarbons in asphalt release agents using headspace solid-phase microextraction and gas chromatography-mass spectrometry
Open this publication in new window or tab >>Determination of aromatic hydrocarbons in asphalt release agents using headspace solid-phase microextraction and gas chromatography-mass spectrometry
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.

Keyword
headspace, solid-phase microextraction, asphalt release agents, aromatic hydrocarbons, BTEX
National Category
Building Technologies
Identifiers
urn:nbn:se:kth:diva-7986 (URN)10.1016/j.chroma.2005.02.011 (DOI)000227995500011 ()2-s2.0-15244353942 (Scopus ID)
Note
QC 20100913Available from: 2008-02-13 Created: 2008-02-13 Last updated: 2017-12-14Bibliographically approved
5. Determination of aromatic hydrocarbons in bituminous emulsion sealants using headspace solid-phase microextraction and gas chromatography-mass spectrometry
Open this publication in new window or tab >>Determination of aromatic hydrocarbons in bituminous emulsion sealants using headspace solid-phase microextraction and gas chromatography-mass spectrometry
2006 (English)In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1137, no 1, 15-21 p.Article in journal (Refereed) Published
Abstract [en]

The possibility of quantitative determination of aromatic hydrocarbons in bituminous emulsion sealants 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) as well as 1,3,5- and 1,2,4-trimethylbenzene. Experimental factors influencing HS-SPME efficiency were studied (sample-headspace equilibration time, extraction time and sample matrix effects). A HS-SPME method using surrogate matrix was developed. The detection limit was estimated as approximately 0.1 ppmw for the target analytes investigated. Good linearity was observed (R-2 > 0.997) for all calibration curves obtained. The repeatability of the method (RSD, relative standard deviation) was found less than 10%. The accuracy of the method given by recovery of spiked samples was between 99 and 116%. The HS-SPME method developed was applied to two commercially available bituminous emulsion sealants. External calibration and standard addition approaches were investigated, and statistical paired t-test was performed. The contents of target aromatic hydrocarbons in the sealants studied varied from approximately 0.4 to 150 ppmw. The method developed shows potential as a tool for the determination of aromatic hydrocarbons in emulsified bituminous materials.

Keyword
bituminous emulsion sealants, aromatic hydrocarbons, BTEX, headspace, solid-phase microextraction
National Category
Building Technologies
Identifiers
urn:nbn:se:kth:diva-7987 (URN)10.1016/j.chroma.2006.10.016 (DOI)000242872700003 ()2-s2.0-33751308862 (Scopus ID)
Note
QC 20100913Available from: 2008-02-13 Created: 2008-02-13 Last updated: 2017-12-14Bibliographically approved

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