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Novel Passive Sampling Materials for the Determination of Priority Pollutants in Surface Waters

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Novel Passive Sampling Materials for the Determination of Priority Pollutants in Surface Waters Novel passive sampling materials for the determination of priority pollutants in surface waters. by Rachel NicArdgháil 53345505 Thesis submitted for the Degree of Doctor of Philosophy Supervisor: Prof. Fiona Regan Dublin City University December 2011 Declaration I hereby certify that this material, which I now submit for assessment on the programme of study leading to the award of PhD is entirely my own work, that I have exercised reasonable care to ensure that the work is original, and does not to the best of my knowledge breach any law of copyright, and has not been taken from the work of others save and to the extent that such work has been cited and acknowledged within the text of my work. Signed: _____________________________________________________ (Candidate) ID No.: ___________________ Date: ____________________ ii Rachel NicArdgháil Index ACKNOWLEDGEMENTS Firstly I’d like to thank Prof. Fiona Regan for giving me the opportunity to work within her research group in Dublin City University and for all her help within this project. I would also like to thank all the friends I have made along the way both in my undergraduate degree who joined me in the undertaking of a PhD and also to the friends I made during my time as a postgraduate researcher. I want to make special mention of the friends I made within the group, both past and present; Lisa, Aga, James, Louise, Tim, Ciprian, Imogene and Li Li. They were there for me both with cups of tea and a friendly ear to chat to but also to help me when I needed it. Thanks should be given to two fourth year students that I worked with, Helen Flynn and Niamh Nolan and also an exchange student Constance Balliet who worked with me over the summer of 2011 and was invaluable in the work carried out for the tuning of my passive sampling devices. Both Lorna Fitzsimons and Nina Hanzlikova deserve recognition for the help they provided me in determining the diffusion coefficients. Finally, thanks to my parents, family and loved ones who have supported me not only through out the years but have been extremely helpful in the last few months helping to look after me and encouraging me during my worst moments. This Project (Grant-aid Agreement No. 2007-PhD-ET-1) was carried out with the support of the EPA under the Science, Technology, Research & Innovation (STRIVE) Programme 2007 – 2013. iii Rachel NicArdgháil Index CONTENTS Acknowledgements ....................................................................................................... iii List of Figures ............................................................................................................... xii List of tables ................................................................................................................xxv Abstract ..................................................................................................................... xxxii Abbriviations ............................................................................................................ xxxiii CHAPTER 1: INTRODUCTION 1.1 Introduction ............................................................................................................. 2 1.1.1 Aims and Objectives .......................................................................................... 2 1.2 Legislation ................................................................................................................ 4 1.2.1 Water Framework Directive .............................................................................. 6 1.3 Priority Pollutants .................................................................................................. 10 1.3.1 Pesticides ......................................................................................................... 13 1.3.2 Polycyclic Aromatic Hydrocarbons .................................................................. 18 1.4 Passive Sampling .................................................................................................... 19 1.4.1 Historical Perspective ...................................................................................... 19 1.4.2 Theory ............................................................................................................. 20 1.4.3 Passive sampling vs. Active sampling .............................................................. 26 1.4.4 Sampling Devices ............................................................................................. 28 1.4.4.1 Semi-permeable membrane devices (SPMDs) ......................................... 28 1.4.4.2 Polar Organic Chemical Integrative Sampler (POCIS) ............................... 29 1.4.4.3 Passive In-Situ Concentration Extraction Sampler (PISCES) ..................... 31 1.4.4.4 Chemcatcher (passive sampler using Empore Disk) ................................. 32 1.4.5 Factors Influencing Passive Sampler Performance ......................................... 33 -iv- Rachel NicArdgháil Index 1.4.5.1 Sampler Design ......................................................................................... 34 1.4.5.2 Temperature ............................................................................................. 34 1.4.5.3 Hydrodynamics ......................................................................................... 35 1.4.5.4 Bio-fouling ................................................................................................ 35 1.4.6 Latest Trends in Passive sampling ................................................................... 36 1.4.6.1 Combination of passive sampling devices ................................................ 36 1.4.6.2 Use of passive samplers in lieu of bio-organisms for analyte uptake ...... 37 1.4.6.3 Accuracy in TWA concentrations .............................................................. 38 1.5 Conclusions ............................................................................................................ 39 1.6 References ............................................................................................................. 40 CHAPTER 2: DEVELOPMENT OF ANALYTICAL METHODS FOR TESTING PASSIVE SAMPLING MATERIAL PERFORMANCE 2.1 Introduction ........................................................................................................... 50 2.1.1 Target analytes ................................................................................................ 50 2.1.2 Solid Phase Extraction (SPE) ............................................................................ 52 2.1.3 Gas Chromatography Mass Spectrometry (GC-MS) ....................................... 54 2.1.4 High Performance Liquid Chromatography (HPLC) ......................................... 56 2.1.5 Aims and Objectives ........................................................................................ 59 2.2 Materials and Methods .......................................................................................... 60 2.2.1 Reagents .......................................................................................................... 60 2.2.2 Instrumentation .............................................................................................. 60 2.2.2.1 Solid Phase Extraction (SPE) .................................................................... 60 2.2.2.2 Gas Chromatography (GC) ........................................................................ 60 2.2.2.3 High Performance Liquid Chromatography (HPLC) .................................. 62 2.3 Results and Discussion ........................................................................................... 63 -v- Rachel NicArdgháil Index 2.3.1 Solid Phase Extraction ..................................................................................... 63 2.3.1.1 Cartridge selection.................................................................................... 63 2.3.1.2 Elution solvent selection ........................................................................... 70 2.3.1.3 Optimisation of Elution Solvent ................................................................ 73 2.3.1.4 Breakthrough Studies ................................................................................ 74 2.3.1.4.1 Breakthrough volume analysis .......................................................... 75 2.3.1.4.2 Breakthrough concentration analysis ............................................... 76 2.3.5 SPE of pesticide standard ................................................................................ 77 2.3.2 Gas Chromatography – Mass Spectrometry ................................................... 79 2.3.2.1 Instrumentation ........................................................................................ 79 2.3.2.2 Solution Preparation ................................................................................. 79 2.3.2.3 Initial Method Development .................................................................... 82 2.3.2.4 Second Test Method ................................................................................. 86 2.3.2.5 Method Validation .................................................................................... 89 2.3.2.6 Analysis of environmental samples on GC-MS ......................................... 99 2.3.3 High Performance Liquid Chromatography .................................................. 102 2.3.3.1 Instrumentation .....................................................................................
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