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Ion Chromatographic Analysis of Disinfectant By-Products

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Ion Chromatographic Analysis of Disinfectant By-Products DCU Ion Chromatographic Analysis of Disinfectant By-Products For the award of D octor of Philosophy Leon Barron School of Chem ical Sciences Student ID: 97311006 V S > N C S R National Centra for Sansor Raiaireh Table of Contents Declaration 11 List of Figures 12 List of Tables 20 List of Abbreviations 22 List of Publications 23 List of Poster Presentations 24 List of Oral Presentations 25 List of Honours and A wards 2 5 Acknowledgements 26 Abstract 28 Chapter 1.0 Literature Review 30 1.0 Background 31 1.1 Current Water Treatment Methods 32 1.1.1 Ozonation 32 1.1.2 Chlorination 35 1.2 Factors Affecting the Formation of Disinfectant By- 36 Products 1.2.1 pH 36 1.2.2 Contact Time 37 1.2.3 Temperature and Season 37 1.2.4 Concentration and Properties of Natural Organic Matter 37 1.2.5 Concentration of Chlorine and Residual Chlorine 38 1.2.6 Concentration of Bromide 38 2 1.3 The Haloacetic Acids 39 1.3.1 Chlorinated Acetic Acids 39 1.3.1.1 Physical and Chemical Properties 39 1.3.1.2 Effects on Laboratory Animals and/or 39 Humans 1.3.2 Brominated Acetic Acids 40 1.3.2.1 Physical Properties 40 1.3.2.2 Effect on Laboratory Animals and/or 41 Humans 1.4 Chromatographic Determination of Haloacetic Acids 42 1.4.1 Introduction to chromatographic theory 42 1.4.2 Band broadening in chromatography 45 1.4.2.1 Multiple path lengths 45 1.4.2.3 Molecular diffusion 46 1.4.2.4 Mass transfer 47 1.4.2.5 The van Deemter equation 47 1.5 Ion Exchange Chromatography 48 1.5.1 The Ion Exchange Process 49 1.5.1.1 Cation Exchange 49 1.5.1.2 Anion Exchange 49 1.5.2 Ion Exchange Stationary Phases 51 1.5.2.1 Polymeric exchangers 52 1.5.2.2 Dionex micro-bore anion exchangers 53 suited to HA and oxyhalide analysis 1.5.2.3 Acryiic polymer based phases 55 1.6 Ion Chromatography Instrumentation 55 1.6.1 Eluent delivery and pumping systems 56 1.6.2 Injection systems 58 1.6.3 Detection Techniques in Ion Chromatography 58 1.6.3.1 Ultra Violet Detection 58 1.6.3.2 Conductivity Detection 59 1.6.3.2.1 Suppressed conductivity detection in 64 anion exchange chromatography 3 1.6.3.3 Electrospray Ionisation-Mass 67 Spectrometric Detection (ESI-MS) 1.6.3.3.1 Principles of Electrospray Ionisation (ESI) 67 1.6.3.3.2 Negative ion, positive ion and neutral 68 modes 1.6.3.3.3 Considerations for practical hyphenation 69 to ion chromatography 1.6.3.3.4 The Ion trap mass analyser 73 Applications of 1C to DBP Analysis 75 1.7.1 Chloral Hydrate 75 1.7.2 Oxyhalides of Chloride and Bromide 76 1.7.3 Application of 1C to the determination of HAs 84 1.7.3.1 lon-interaction chromatography 84 1.7.3.2 Ion exchange chromatography 85 1.7.3.3 lon-exclusion chromatography 86 1.7.3.4 IC-ESI-MS 87 1.7.3.5 IC-ICP-MS 89 1.7.4 Preconcentration methods for HAs 92 1.7.4.1 Solid phase extraction (SPE) 93 1.7.4.1.1 Problems with SPE 93 1.7.4.1.2 Comparison of stationary phases 94 1.7.4.1.3 Interference elimination 95 References 100 4 3.3.1 Extraction and elution of HAs using LiChrolut EN SPE 147 cartridges 3.3.2 Determination of the eluting agent 148 3.3.3. Sample load rate and recoveries 149 3.3.4 Durability of the LiChrolut EN cartridge 152 3.3.5 Capacity of LiChrolut EN cartridge 154 3.3.6 Analysis of real samples 156 3.3.7 Standard Addition 160 3.4 Conclusion 162 3.5 References 163 Chapter 4.0 Reagentless Ion Exchange 164 Chrom atography of Haloacetates and Separations with an AS16 C o l u m n 4.1 Introduction 165 4.2 Experimental 168 4.2.1 Instrumentation 168 4.2.2 Reagents 168 4.3 Results and Discussion 169 4.3.1. Initial Separations and Comparison of EG40 to 169 Manually Prepared Eluents 4.3.2 Reproducibility of retention time with electrolytically 172 generated eluents 4.3.3 Limits of Detection 175 4.3.4 Analysis of Real Samples with Preconcentration and 177 EG40 System Separation 4.3.5 Separation of inorganic chloride and MBA 181 4.3.6 Effect of Temperature 186 4.3.7 Comparison of Limits of Detection of AS16 and AS11- 189 HC column methods 4.3.8 Repeatability of AS16 Method 192 4.3.9 Linearity of AS16 method 193 6 4.4 Conclusions 194 4.5 References 195 Chapter 5.0 Trace Detection of HAs with 196 Monolithic Cation Exchange Type Suppressor and Investigation into the Effect of LiChrolut EN Sorbent M a s s 5.1 Introduction 197 5.2 Experimental 199 5.2.1 Instrumentation 199 5.2.2 Chemicals 199 5.2.3 Sample collection and treatment 200 5.3 Results and Discussion 201 5.3.1 Improvements in sensitivity with Atlas suppressor 201 5.3.2 Inclusion of DCBA and CDBA 204 5.3.3 Sample pre-treatment and removal of interferent ions 204 5.3.4 Analysis of drinking water samples 209 5.3.4.1 HAs in drinking water without using 209 preconcentration procedure 5.3.4.2 Preconcentration and HA determination in 212 drinking water supplies 5.3.5 Investigation into LiChrolut EN sorbent mass 218 5.4 Conclusions 227 5.5 References 228 7 Chapter 6.0 Alternative Detection Modes to 229 Suppressed Conductivity Detection for HA Analysis 6.1 Introduction 230 6.2 Experimental 232 6.2.1 Instrumentation 232 6.2.2 Chemicals 232 6.3 Results and Discussion 234 6.3.1 UV detection - wavelength optimisation 234 6.3.2 UV detector linearity and low limit sensitivity 237 6.3.3 Direct Infusion - Mass Spectrometry 239 6.3.4 Ion chromatography-mass spectrometry optimisation 249 6.3.4.1 Elimination of background interference 249 6.3.4.2 Optimum parameters for simultaneous 251 detection of nine HAs 6.3.4.3 Addition of volatilising solvent 253 6.3.4.4 Optimisation of % MeOH in total flow 254 6.3.5.5 Improvement in UV chromatogram with 256 manually prepared eluent 6.3.5 Trends in observed ion types for each HA 257 6.3.6 Analysis of a drinking water sample using suppressed 260 ion chromatography with conductivity, UV and ESI-MS detection 6.4 Conclusion 264 6.5 References 265 8 Chapter 7.0 Use of Temperature Programming 267 to Improve Resolution of Inorganic Anions, Haloacetates and Oxyhalides by Suppressed IC-ESI- MS 7.1 Introduction 268 7.2 Experimental 270 7.2.1 Apparatus 270 7.2.2 Reagents 271 7.2.3 Procedure 271 7.3 Results and Discussion 273 7.3.1 Effect of temperature on ion chromatography - 273 theoretical considerations 7.3.1.1 lon-exchanger 274 7.3.1.2 Mobile phase 275 7.3.1.3 Solutes 276 7.3.2 Van’t Hoff plots 276 7.3.3 Alteration of existing 1C gradient method for separation 282 of oxyhalides from HAs 7.3.4 Effect of elevated temperature upon gradient 1C 283 separation 7.3.5 Column oven performance 285 7.3.6 Application of temperature program 288 7.3.7 Optimum method for suppressed ion chromatography 291 with conductivity and electrospray mass spectrometry. 7.3.8 Analytical performance data for suppressed IC-ESI-MS 292 and conductivity detection 7.3.8.1 Retention time reproducibility of dual 292 gradient method 7.3.8.2 Linearity for suppressed conductivity and 294 ESI-MS 7.3.8.3 LOD for conductivity detection 298 7.3.8.4 ESI-MS of oxyhalides and limit of detection 302 7.3.8.5 ESI-MS Reproducibility 305 9 7.3.9 Application to real samples 306 7.3.9.1 Application to HA and oxyhalide 306 determinations in soil 7.3.9.2 Suppressed IC-conductivity-ESI-MS of 309 drinking water sample 7.4 Conclusions 315 7.5 References 316 Chapter 8.0 Final Conclusions and 3 1 8 S u m m a t i o n s Appendix A.1 3 2 2 Appendix A.2 3 2 6 Appendix A.3 3 2 8 Appendix A.4 3 3 3 Appendix A.5 3 3 7 Appendix A.6 3 3 9 Appendix A.7 Poster Presentations 3 4 3 10 I hereby certify that this material, which I now submit for assessment on the programme of study leading to the award of <Doctor of(Pfiitbsopfiy is entirely my own work 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. ID No.: Date: I I List of Figures Fig. 1.1 Bromate formation pathways during ozonation Fig. 1.2 Relative composition of other DBP classifications associated with ozonation as a proportion of assimilable total organic carbon. Note: This does not include the oxyhalides as they are non-carbon containing DBPs. Fig. 1.3 Classification and relative proportion of halogenated DBPs to total organic carbon in chlorinated drinking water. Fig. 1.4 Typical chromatogram for the separation of two species showing retention time and peak asymmetry (As). Fig.
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