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  • Faculty of Bioscience Engineering

    Academic year 2014 – 2015

    Biomonitoring of polycyclic aromatic hydrocarbons

    and derivatives in Belgium

    Zhimiao Zuo

    Promotor: Prof. dr. ir. Herman Van Langenhove

    dr. ir. Christophe Walgraeve

    Master’s dissertation submitted in partial fulfillment of the

    requirements for the degree of

    Master of Environmental Sanitation

  • I

    Acknowledgement

    The dissertation is almost finished, which means the two-year study in the University of

    Ghent and the living in Belgium are going to the end as well. The experience of studying

    abroad is one of the most important parts of my life. The people I met here will not be

    forgotten ever. At the end of my student period, lots of people should be showed of my

    gratitude.

    Professor Herman Van Langenhove is the promoter of my thesis. He is modest and gentle.

    Besides the thesis, several lectures were given by him. The erudite of knowledge, the precise

    on research, the diligent on work, the humorous on speech and the optimistic on living

    impressed me a lot. I learnt not only knowledge from him, but also knew better on how to

    behave correctly. An old saying in Chinese ‘先生之风,山高水长’ describes Professor Herman

    Van Langenhove perfectly. The meaning of the sentence is: ‘The prestige of the master will

    be spread and remembered forever’.

    My tutors Christophe Walgraeve and Dohai Duc guided me pretty well while the thesis

    proceeded. Christophe worked with me from the very beginning of the thesis. He was so

    scrupulous and conscientious. Even though the experiments always went late to dark, he was

    there in the lab until the last moment to give help and guidance. While dissertation

    compiling, Christophe was so nice that he gave up part of his summer vacation to read and

    modify the text.

    My gratitude goes to Professor Kristof Demeestere as well, who always listened to my report

    and gave some constructive suggestions kindly. His professional opinion enlightened me to

    avoid the detour while thesis designing. He was so responsible to all the students in the lab,

    and tried to help the best all the time.

    The staff from The Department of Sustainable Organic Chemistry and Technology, such as

    Wouter De Soete, Joren Bruneel and so on, although I hardly talked to all of them, the smile

    and warm greeting they gave encouraged me every time I arrived at the lab. Especially, my

    special thanks to Patrick De Wispelaere, who supported me on GC-MS operation.

    Professor Peter Goethals, the coordinators of Master of Science in Environmental Sanitation

    (IMENVI) Sylvie Bauwens and Veerle Lambert. Thank you so much for approving my

    application and giving such a wonderful and rare opportunity to study in the best university

    around the world, and to work with so many amiable and brilliant brains.

    I want to show my great thanks to my lovely classmates, we came together from different

    continents. Every one of you gave me lots of help and encouragement while I was

    disoriented. Daniel Paul Odhiambo Ombaka, Audisny Apristiaramitha Teddy and Workineh

    Mengesha Fereja who were working together in the same lab for thesis, gave me lots of

  • II

    suggestion and introduction about lab work as well.

    My parents and grandfather are the inner pillar supported and motivated me to finish this

    program straight. My friends in Beijing are the ones released my pressure in the two-year.

    My girlfriend is the one consoled and accompanied me while I was frustrated. Without them,

    I would never success.

    At last, the great thanks to the committee. Thank you for the time and patience to read my

    dissertation.

  • III

    List of Abbreviations

    ACN Acetonitrile SEC Size Exclusion Chromatography

    AC Adsorption Chromatography SPE Solid Phase Extraction

    ASPEC Automated Solid-Phase Extraction Clean-up USEPA U.S. Environmental Protection Agency

    DCM Dichloromethane VOCs Volatile Organic Compounds

    DNA Deoxyribonucleic Acid WHO World Health Organization

    d.w. Dry Weight

    F-PAHs Mono-fluorinated PAHs

    FW Fresh Weight

    GC Gas Chromatography

    EI Electron Ionization

    GMF Glass Microfiber Filter

    GPC Gel Permeation Chromatography

    HEX Hexane

    HPLC High Performance Liquid Chromatography

    IARC International Agency for Research on Cancer

    IS Internal standard

    LRAT Long-range Atmospheric Transport

    MS Mass Spectrometry

    NF Not Found

    NPAHs Nitro-polycyclic Aromatic Hydrocarbons

    oxy-PAHs Oxygenated Polycyclic Aromatic Hydrocarbons

    PACs Polycyclic Aromatic Compounds

    PAHs Polycyclic Aromatic Hydrocarbon

    PCBs Polychlorinated Biphenyls

    PLE(ASE)

    Pressurized Liquid Extraction (Acceleration

    Solvent Extraction)

    PM Particulate Matter

    POPs Persistent Organic Pollutants

    PTFE Polytetrafluoroethylene

    RPLC Reversed Phase Liquid Chromatography

    RPA Relative Peak Area

    RSRF Relative Sample Response Factor

    S_B Spiked Blank

    S_SAM_A Sample Spiked After

    S_SAM_B Sample Spiked Before

    SAM Sample

  • IV

    Abstract

    The aim of this study was to develop a bio-monitoring method to analyze polycyclic aromatic

    hydrocarbons (PAHs) and oxygenated polycyclic aromatic hydrocarbons (oxy-PAHs). Taxus

    baccata (European Yew) was chosen as the bio-monitor species in this thesis. This is the first

    time Taxus baccata applied on PAHs and oxy-PAHs researches. The 16 PAHs mentioned in

    this thesis are the 16 U.S. Environmental Protection Agency (USEPA) priority PAHs. The

    oxy-PAHs and PAHs in samples were analyzed by Gas Chromatography Mass Spectrometry

    (GC-MS). The approach of sample preparation, extraction solvent choice, and solid phase

    extraction (SPE) clean-up were optimized and developed. PAHs and oxy-PAHs were

    quantified by internal standards calibration with deuterated PAHs. The recovery and matrix

    effects of PAHs and oxy-PAHs were obtained. The concentration of target compounds in

    sample was obtained and expressed as in mass of leaf dry weight.

    Air pollution, PAHs, oxy-PAHs, vegetation, Taxus, bio-monitoring.

  • V

    CONTENT

    Acknowledgement ............................................................................................................................. I

    List of Abbreviations ......................................................................................................................... III

    Abstract ........................................................................................................................................... IV

    CHAPTER 1 Introduction................................................................................................................- 1 -

    CHAPTER 2 Literature Review .......................................................................................................- 9 -

    2.1 Sampling ..........................................................................................................................- 9 -

    2.2 Sample Preparation & Extraction ................................................................................. - 13 -

    2.3 Clean-up ....................................................................................................................... - 19 -

    2.4 PAHs and oxy-PAHs Analysis ......................................................................................... - 24 -

    2.5 Concentration Levels .................................................................................................... - 28 -

    CHAPTER 3 Chemical Materials .................................................................................................. - 32 -

    3.1 Chemicals & Reagents .................................................................................................. - 32 -

    3.2 Standards Solution ....................................................................................................... - 33 -

    CHAPTER 4 Results & Discussion ................................................................................................ - 34 -

    4.1 Selection of Plant Species ............................................................................................ - 35 -

    4.2 Dry Matter Content ...................................................................................................... - 36 -

    4.3 Solvent Selection .......................................................................................................... - 36 -

    4.4 Size of the Sample Determination ................................................................................ - 37 -

    4.5 Extraction ..................................................................................................................... - 39 -

    4.6 Clean-up & Concentration ............................................................................................ - 40 -

    4.6.1 Clean-up & Concentration Procedure ...............

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