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Determination of Organotin Compounds in Coastal Sediment Pore-Water by Diffusive Gradients in Thin-Films (DGT) Technique

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Determination of Organotin Compounds in Coastal Sediment Pore-Water by Diffusive Gradients in Thin-Films (DGT) Technique Determination of organotin compounds in coastal sediment pore-water by diffusive gradients in thin-films (DGT) technique by Russell Francis Cole Submitted in partial fulfilment of a degree of Doctor of Philosophy in the Faculty of Science September 2016 University of Portsmouth School of Earth and Environmental Sciences Burnaby Building Burnaby Road Portsmouth PO1 3QL Abstract Organotin compounds still present a high risk to biota in the aquatic environment. Measuring the behaviour of the freely dissolved fractions of these compounds in sediment compartments is challenging, with costly and sensitive analytical techniques required for their measurement. Diffusive gradients in thin-films (DGT) allow for the uptake and pre-concentration of analytes in a binding gel and is used to measure dissolved metals and some organic compounds. The utility of novel silica-bound sorbents (C8, C18, mixed phases) as DGT binding gels for the sequestration of organotins in the marine environment was the primary focus of work in this project. The C8 sorbent showed the optimum performance in the uptake and recovery of organotins across pH, ionic strength and in filtered sea water. It was used subsequently as the binding layer in DGT sediment devices (160 mm × 34 mm) overlaid with a mixed-cellulose ester membrane (0.45 µm) as the single diffusion layer. These were used to investigate pore water mobilisation and concentrations of organotins in coastal sediment cores collected from a contaminated site. Organotins demonstrated a non-sustained uptake scenario, with DGT flux and freely dissolved concentrations in pore water measured to decline at 1 cm depth intervals over deployments of 2-28 days. Using time series, concentrations in pore water at t = 0 were calculated providing empirical pore water depletion curves for sediment cores. Using standard laboratory instrumentation (i.e. gas chromatography-mass spectrometry) low limits of detection were achieved (TBT = 0.4 ng L-1 after 2 weeks of sampling). ii Contents 1.1. Organotin compounds in the environment .............................................. 1 1.1.1. Chemistry and application of organotin compounds ................... 1 1.1.2. Behaviour, fate and degradation ................................................ 6 1.1.3. Partitioning behaviour ................................................................. 8 1.1.4. Sediment profiling and the mobilisation of organotins to sediment pore waters ............................................................... 11 1.1.5. Degradation of organotin compounds ...................................... 13 1.1.5.1. Butyltin degradation index (BDI) and phenyltin degradation index (PhDI) ............................................................................. 14 1.1.6. Toxicity ..................................................................................... 15 1.2. The analysis of organotin compounds ................................................... 22 1.2.1. Extraction ................................................................................. 22 1.2.1.1. Reagents ........................................................................... 22 1.2.1.2. Techniques ........................................................................ 23 1.2.2. Derivatisation ........................................................................... 31 1.2.3. Separation ................................................................................ 32 1.2.3.1. Gas chromatography ......................................................... 32 1.2.3.2. Liquid chromatography ...................................................... 32 1.2.4. Detection .................................................................................. 33 1.2.5. Quantification ........................................................................... 35 1.3. Monitoring techniques for organotin compounds in water ......... 36 1.3.1. Discrete sampling ..................................................................... 36 1.3.2. Biological monitoring ................................................................ 36 iii 1.3.3. Electrochemical ........................................................................ 38 1.3.4. Passive sampling techniques for monitoring organotin compounds in water ................................................................. 39 1.3.4.1. Chemcatcher® .................................................................... 42 1.3.4.2. Silicone rubber sheets ....................................................... 43 1.3.4.3. SPMDs .............................................................................. 44 1.4. Monitoring techniques for organotin compounds in sediments and in sediment pore-waters ............................................................... 45 1.4.1. Discrete sampling ..................................................................... 45 1.4.2. Passive sampling techniques for monitoring organotin compounds in sediment ........................................................... 46 1.5. Regulation and management of organotin compounds in the aquatic environment ................................................................................................. 48 1.5.1. International regulations and quality guideline standards ......... 48 1.5.2. Management of contaminated dredged sediments within England and Wales .................................................................. 50 1.5.2.1. Sea disposal ...................................................................... 53 1.5.2.2. Inland disposal ................................................................... 55 1.5.2.3. Monitoring by Cefas ........................................................... 57 1.6. Aims and objectives of research project ...................................................... 59 2.1. Introduction ........................................................................................... 61 2.2. Instrument ............................................................................................. 62 2.3. Chemicals and Reagents ...................................................................... 64 2.3.1. Safety Protocols ....................................................................... 64 2.3.2. Standards ................................................................................. 65 2.3.3. Reagents .................................................................................. 66 2.3.3.1. 1% Sodium tetraethyl borate (1 % NaBEt4 (w/v)) ............... 67 2.3.3.2. 1 M Acetate buffer (1 L) ..................................................... 67 2.3.3.3. 13 M methanolic acetic acid (1 L) ...................................... 68 2.3.3.4. 20% (approximate) sodium hydroxide (NaOH) solution ........ (~ 1 L) ............................................................................... 69 2.3.4. Preparation of glassware/FEP centrifuge tubes ....................... 69 2.4. Simultaneous extraction and derivatisation of sea water ...................... 69 iv 2.4.1. Sampling of sea water .............................................................. 69 2.4.2. Sampling of sediment ............................................................... 70 2.4.3. Extraction and derivatisation .................................................... 70 2.5. Extraction and derivatisation of sediment samples ................... 71 2.5.1. Extraction and derivatisation .................................................... 71 2.6. Calibration ................................................................................. 75 2.6.1. Calibration for water analysis ................................................... 75 2.6.2. Calibration for sediment analysis.............................................. 75 2.6.3. Summary of calibration parameters.......................................... 76 2.7. Development of a cold programmed temperature vaporisation-large volume injection (PTV-LVI) technique for organotin compounds ................. 79 2.7.1. Background .............................................................................. 79 2.7.1.1. Inlet and injection parameters ............................................ 80 2.7.1.2. Limits of detection for splitless injection/PTV-LVI .............. 85 2.8. Validation of methods .................................................................................. 87 2.8.1. Organotins in water .................................................................. 87 2.8.2. Organotins in sediment ............................................................ 88 2.8.3. Field samples ........................................................................... 90 2.8.3.1. Sea water........................................................................... 90 2.8.3.2. Further developmental work .............................................. 91 2.8.3.3. Sediment............................................................................ 92 2.9. Summary ...................................................................................................... 92 3.1. Introduction ................................................................................................... 95 3.1.1. Theory ...................................................................................... 95 3.1.2. Considerations for DGT ............................................................ 97 3.1.2.1. pH and ionic strength ......................................................... 97 3.1.2.2. Biofouling ..........................................................................
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