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PHOSPHORUS SPECIATION in SOIL LEACHATE USING FIELD-FLOW FRACTIONATION and FLOW INJECTION ANALYSIS by LAURA JANE GIMBERT a Thesis

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PHOSPHORUS SPECIATION in SOIL LEACHATE USING FIELD-FLOW FRACTIONATION and FLOW INJECTION ANALYSIS by LAURA JANE GIMBERT a Thesis PHOSPHORUS SPECIATION IN SOIL LEACHATE USING FIELD-FLOW FRACTIONATION AND FLOW INJECTION ANALYSIS by LAURA JANE GIMBERT A thesis submitted to the University of Plymouth in partial fulfilment for the degree of DOCTOR OF PHILOSOPHY School of Earth, Ocean and Environmental Sciences In collaboration with Institute of Grassland and Environmental Research, North Wyke Research Station, Devon. January 2005^ LIBRARY STORE f University of Plymouth Ubrary . Item No. ABSTRACT PHOSPHORUS SPECIATION IN SOIL LEACHATE USING FIELD-FLOW FRACTIONATION AND FLOW INJECTION ANALYSIS Laura Jane Gimbert Colloidal material (0.001 - I \im) in soil leachate and agricultural drainage waters is an important route for the transport of contaminants such as phosphorus from land to catchments. Excessive phosphorus concentrations can result in eutrophication of natural waters. To be able to characterise the colloidal material, in terms of size distribution, a mild and relatively new separation technique field-flow fractionation (FFF) can be used to fractionate complex colloidal samples. By combining FFF and flow injection analysis (FIA) more detailed physico-chemical information on phosphorus species in soil leachates and agricultural runoff waters can be obtained. Chapter 1 describes the methods used to determine phosphorus and also to characterise colloidal material, especially using FFF, and particularly focusing on the Flow FFF (FIFFF) sub-technique. Chapter 2 concentrates on the experimental considerations for FIFFF with recommended procedures for the setup and calibration of the system. In Chapter 3, SdFFF is used to compare the use of centriftigation and filtration for the fractionation of an Australian soil suspension, and demonstrates the uncertainties surrounding the use of conventional membrane filtration. FIFFF is used in Chapter 4 to optimise a sampling, treatment and preparation protocol for two contrasting soil types sampled in the UK. Centrifligation and filtration methods are also compared in a similar approach used in Chapter 3. In Chapter 5 a portable Fl monitor is optimised for the detection of reactive phosphorus. The linear range for the Fl monitor is determined as 0.8 - 8.0 FO4-P with a limit of detection of 0.6 \xM PO4-P. A digestion method is also optimised for the determination of total phosphorus using an acidic peroxydisulphate autoclaving method. In Chapter 6, FIFFF and FIA are combined in an experiment describing the fractionation of a soil suspension and the subsequent determination of phosphorus associated with different size fractions. The results from this combination show great potential and will help improve our understanding of the role of colloids in phosphorus transport from agricultural land to catchments. TABLE OF CONTENTS List of tables vii List of figures viii List of abbreviations and symbols xiii Acknowledgements xvi Author's declaration xvii Chapter 1 Introduction 1. Introduction 1 1.1 Phosphorus I \AA Sources of phosphorus 1 1.1.2 Eutrophication 4 1.2 Phosphorus speciation 6 1.3 Analytical methods for phosphorus 8 1.4 Flow injection analysis 10 1.5 Colloids 14 1.5.1 Analytical techniques for colloidal material 15 1.5.2 Field-flow fractionation 17 1.5.3 FIFFF instrumentation 18 1.5.4 Frit inlet and frit outlet 20 1.5.5 Carrier liquid 21 1.5.6 Detectors 22 1.5.7 The separation process 22 1.5.8 Operating modes in FIFFF 25 1.5.9 Theoretical aspects 27 1.5.10 Applications 30 1.6 Research aims and objectives 35 1.7 References 36 Chapter 2 Practical Considerations for Flow Field-Flow Fractionation 2.1 Introduction 51 2.2 FIFFF instrumental set-up 52 2.3 Balancing flow rates 53 2.4 Operation of FIFFF system during a run 54 2.5 Installation and replacement of the membrane 54 2.5.1 Step-by-step guide to replacing membrane 55 2.6 Determination of void volume and channel thickness 56 2.6.1 Breakthrough method 58 2.6.2 Retention times method 60 2.7 Conversion of fractograms into particle size distributions 62 2.8 Selection of appropriate crossflow rates for particles <1 fim 64 2.9 Application to lower (5190,15200 and 43300 Dalton) molecular weights 67 2.9.1 Optimisation of channel flow and crossflow rates 68 2.9.2 Calibration of FIFFF channel using PSS 69 3. Conclusions and recommendations 72 4. References 73 Chapter 3 Comparison of Centrifugation and Filtration Techniques for the Size Fractionation of Colloidal Material in Soil Suspensions Using Sedimentation Field-Flow Fractionation 3.1 Introduction 74 3.2 Experimental 76 3.2.1 Laboratory ware 76 3.2.2 Sedimentation field-flow fractionation 76 3.2.3 Sample preparation 79 3.2.4 Fractionation of soil sample 80 Filtration 80 Centrifligation 80 Soil particle density 81 3.3 Results and Discussion 82 3.3.1 Data analysis 82 3.3.2 Fractograms of Lilydale soil suspensions 83 3.3.3 Particle size distributions of Lilydale soil suspensions 84 3.4 Conclusions 89 3.5 References 90 Chapter 4 Effects of Sample Preparation on the Performance of Flow Field-Flow Fractionation Using Two Contrasting Soils 4.1 Introduction 94 4.2 Experimental 96 4.2.1 Laboratory ware 96 4.2.2 Flow field-flow fractionation 96 4.2.3 Sample preparation 98 Rowden soil 98 Dartmoor peat 99 4.2.4 Optimisation of settling conditions for soil suspensions 100 1. Effect of settling time 100 2. Settling of replicate samples 101 3. Re-settling of the same sample 102 4.2.5 Comparison of centrifijgation and filtration for two contrasting soils 102 Stability experiment 102 Optimised settling protocol 103 Filtration 103 Centrifijgation 103 4.2.6 Effect of sample dilution 104 4.2.7 Real soil runoff samples 104 4.3 Results and Discussion 105 4.3.1 Data analysis 105 4.3.2 Optimisation of settling conditions 106 1. Effect of settling time 106 2. Settling of replicate samples 108 3. Re-settling of the same sample 109 4.3.3 Comparison of centrifiigation and filtration for two contrasting soils 110 Stability experiment 110 Optimised settling protocol 110 Fractograms for Rowden soil suspensions (1 % m/v) 111 Particle size distributions for Rowden soil suspensions (1 % m/v) 112 Fractograms for Dartmoor peat suspensions (1 % m/v) 114 iii Particle size distributions for Dartmoor peat soil suspensions (1 %m/v) 115 4.3.4 Effect of sample dilution 117 Particle size distributions for Rowden soil suspensions (0.5 % m/v) 118 Particle size distributions for Rowden soil suspensions (0.25 % m/v) 118 4.3.5 Real soil runoff samples 121 4.4 Conclusions 123 4.5. References 123 Chapters A Portable Flow Injection Monitor for the Determination of Phosphorus in Soil Suspensions 5.1 Introduction 128 5.2 Experimental 129 5.2.1 Laboratory ware 129 5.2.2 Reagents and standards 129 5.2.3 Flow injection instrumentation 131 5.2.4 Optimisation of FI monitor for reactive phosphorus 132 Univariate optimisation 135 Simplex optimisation 135 5.2.5 Analytical figures of merit 136 Linear range and limit of detection 136 Reproducibility 136 5.2.6 Silicate interference study 136 5.2.7 Optimisation of an autoclaving method for the determination of total phosphorus 137 Method 1 137 Method 2 137 5.3 Results and Discussion 138 5.3.1 Optimisation of FI monitor for reactive phosphorus 138 Univariate optimisation 138 Simplex optimisation 141 5.3.2 Analytical figures of merit 144 Linear range and limit of detection 144 Reproducibility 145 5.3.3 Silicate interference study 146 iv 5.3.4 Digestion techniques for the determination of total phosphorus 147 Alkaline peroxydisulphate 149 Acid peroxydisulphate 153 Model compounds 153 5.3.5 Optimisation of an autoclaving method for the determination of total phosphorus 159 Method 1 159 Method 2 160 5.4 Conclusions 161 5.5 References 162 Chapter 6 Combining FIFFF and FI Techniques for the Determination of Phosphorus in Soil Suspensions 6.1 Introduction 169 6.2 Experimental 170 6.2.1 Laboratory ware 170 6.2.2 Preparation of Rowden soil suspensions 171 Centrifiigation 171 6.2.3 FIFFF for Rowden soil suspensions 171 6.2.4 Portable Fl monitor for determination of reactive phosphorus and total phosphorus 172 6.3 Results and Discussion 173 6.3.1 Fractograms and particle size distributions for Rowden soil suspensions 173 6.3.2 Portable FI monitor for determination of reactive phosphorus 173 6.3.3 Portable FI Monitor for determination of total phosphorus 175 6.4 Conclusions 177 6.5 References 178 Chapter 7 Conclusions and Future Work 7.1 Conclusions 179 7.1.1 Experimental practicalities of using SdFFF and FIFFF 179 7.1.2 Soil sampling, treatment and preservation 180 7.1.3 Centriftigation and filtration for the further fractionation of <1 ^im samples 181 7.1.4 FFF as a tool for analysing real colloidal samples 181 7.1.5 Determination of phosphorus species with a portable Fl monitor 182 7.1.6 Determination of phosphorus associated with colloidal material 182 7.2 Future Work 183 7.2.1 Different soil types and real samples 183 7.2.2 Effect of soil temperature 183 7.2.3 Improving the detection limit of the portable FI monitor 184 7.2.4 Improving the FI monitor instrumentation 184 7.2.5 Coupling FIFFF off-line and on-line to the portable Fl monitor 185 Published Papers 186 VI LIST OF TABLES Table LL Surfactants used in FIFFF 22 Table 1.2. Environmental applications 31 Table 1.3. Biological applications 32 Table 1.4. Application to polymers 33 Table L5. Application to inorganic colloids 34 Table 2.1. Calculation of void volume and channel thickness from breakthrough time determined from the fractograms shown in Fig.
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