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Swain 13 (12Mnth).Pdf MOLECULAR CHARACTERIZATION OF TERRESTRIAL ORGANIC CARBON IN SOME ORGANIC-RICH SOILS IN THE NORTHERN LATITUDES Eleanor Yvonne Swain A thesis submitted to Newcastle University in partial fulfilment of the requirements for the degree of Doctor of Philosophy in the Faculty of Science, Agriculture and Engineering School of Civil Engineering and Geosciences Drummond Building Newcastle University United Kingdom February 2013 Declaration I hereby certify that the work presented in this thesis is my original research work, with the exception of the Ryggmossen samples presented in Chapters 4 and 5. The experiment set up and subsequent peat core and litter sampling was carried out by Dr. Lisa Belyea, Dr. Kathryn Allton, Dr. Chris Laing (Queen Mary, University of London), and subsequently extracted by Dr. Aminu Muhammad (Newcastle University). Carbohydrate and elemental analysis of the Ryggmossen samples were performed by Dr. Greg Cowie (University of Edinburgh, UK), however all interpretation of the data is my own. Wherever contributions of others are involved, every effort is made to indicate this clearly, with due reference to the literature, and acknowledgement of collaborative research and discussions. No part of this work has been submitted previously for a degree at this or any other university. Eleanor Yvonne Swain ii Abstract Northern peatlands store around one third of the global soil carbon, however over the past 100 years significant areas of these peats and peaty gley soils have been drained and planted with coniferous forest. Afforestation could accelerate peat decay due to land disturbance causing the peatland to become a net carbon source, alternatively carbon may accumulate due to increased carbon fixation, causing the peatland to remain a net carbon sink. Despite the global importance of these mechanisms, our understanding of the fate of soil carbon stores in afforested carbon-rich soils (i.e. peaty gley and peat soils) remains unclear. Peat and litter were analysed using thermally assisted hydrolysis and methylation (THM) in the presence of 13C-labelled and unlabelled tetramethylammonium hydroxide (TMAH) which revealed the distribution, degradation transformations and turnover rates of vascular plant- and Sphagnum-derived phenols in carbon-rich soil profiles. The studied sites included afforested peaty gley soils under a first- and second-rotation Sitka spruce plantation, unplanted moorland, and self seeded Sitka spruce on unprepared moorland, all of which are located in Kielder Forest, northern England. A pristine peatland in central Sweden was also extensively sampled to assess the carbon related processes occurring in carbon-rich soils prior to afforestation. The effects of afforestation on total carbon stocks were also investigated. The establishment of coniferous forests on peaty gley soils led to a net accumulation of soil carbon during the second rotation, surpassing the moorland carbon capacity. Whilst the encroachment of Sitka spruce on to open moorland via self seeding has resulted in a decreased carbon stock. The phenol composition of soil horizons displayed a maximum lignin content at deep soil across the afforested sites caused primarily by the horizon inversion that occurred prior to planting. Sphagnum acid THM products were identified across the peatland and serve as putative biomarkers for the contribution of Sphagnum-derived organic matter in peats and afforested peatlands, as well as showing potential to provide information on peatland oxic conditions. Sphagnum phenols accumulate preferentially in the anoxic saturated peat, suggesting changes introduced via land-use change or climate change could affect the water table, and thus increase the potential peat decomposition, and the subsequent loss of carbon in peatlands. iii Acknowledgements My first acknowledgement goes to my supervisor, Dr. Geoff Abbott, whom I thank for his support, great advice and encouragement throughout the years of my PhD. I’m highly indebted to Forest Research and NERC, for the funding of my 3 year PhD studentship. I would also like to thank my supervisors in industry; Dr. Mike Perks, and Dr. Elena Vanguelova for all of their help and guidance throughout the course of this project. Thanks to Ian Harrison, Paul Donohoe, Berni Bowler, Phil Green and Yvonne Hall for all of their technical advice and assistance over the last 4 years in the lab and office. Thanks also to Dr. Tim Filley from the Department of Earth & Atmospheric Sciences, Purdue University, USA, for his supply of 13C-TMAH. I am also indebted to Dr. Sharon Mason, who provided me with the assistance I required at the start of my project, providing me with my first set of samples and guiding me through the array of new techniques. Thank you to everyone in the lab and office that has been there throughout my PhD for their help and friendship over the years. I must also acknowledge the late Dr. Elizabeth Sulzman (Oregon State University, USA). For without her passion and enthusiasm in soil science, I may never have ventured further into the complex and intriguing word of soil science as a young undergraduate student. Elizabeth, you are a true inspiration. Many thanks to my parents and sister for both their financial and emotional support throughout my many years at university. Last but by no means least, my partner Paul Reed. You have the patience of a saint, and your support knows no limits. You got me through it! Thank you. iv Contents Declaration ii Abstract iii Acknowledgements iv Contents v List of Figures x List of Tables xx Chapter 1 Introduction & Literature Review 1 1.1 Introduction 2 1.2 Literature Review 4 1.2.1 Soil Organic Carbon 4 1.2.2 Kyoto Protocol 5 1.2.3 Peatland 6 1.2.4 Sphagnum 8 1.2.5 Sphagnum Characterisation 9 1.2.6 Land-Use Change 9 1.2.7 Lignin 11 1.2.8 Lignin Characterisation 15 1.2.9 THM in the presence of TMAH 16 1.2.10 13C-labelled TMAH 18 1.2.11 Tannin 21 1.2.12 Carbohydrates 22 1.3 Aims and Objectives of this Thesis 24 Chapter 2 Methods & Sites 27 2.1 Standard Laboratory Procedures 28 2.2 THM in the Presence of Unlabelled and 13C-Labelled TMAH 28 2.2.1 Aromatic Hydroxyl Contents 30 2.2.2 Mass Yields and Lignin Parameters 31 2.3 THM Reproducibility 32 2.4 Temperature Calibration of Pyroprobe 32 v 2.5 Bulk Density (Db) 34 2.6 Total Organic Carbon and Carbon Storage Determination 34 2.7 Sites and Samples 35 2.7.1 Afforested Ecosystems 35 2.7.2 Coalburn Forest 36 2.7.3 Harwood Forest 39 2.7.4 Wark Forest 40 2.7.5 Pristine Peat Ecosystem 43 2.7.6 Ryggmossen Peatland 43 2.8 Sample Preparation 46 2.9 Statistical Analyses 46 Chapter 3 Carbon Stock and Phenolic Distributions in Peaty Gley 48 Soils Afforested With Sitka Spruce 3.1 Introduction 49 3.2 Overview of Methods and Sites 52 3.2.1 Site Background 52 3.2.2 TMAH Thermochemolysis 53 3.2.3 TOC & Carbon Storage 53 3.2.4 Lignin Proxies 53 3.3 Results and Discussion 54 3.3.1 Soil Organic Carbon 54 3.3.1.1 Total Organic Carbon 54 3.3.1.2 Bulk Density 56 3.3.1.3 Organic Carbon Storage 56 3.3.2 THM 59 3.3.2.1 Lignin Thermochemolysis Products 59 3.3.2.2 Lignin Yield () 66 3.3.2.3 Lignin Source Proxies 71 3.3.2.4 Non-Lignin Phenols 75 3.4 Conclusions 77 vi Chapter 4 Sphagnum Biomarkers from a Typical Northern Latitude 79 Peatland: Ryggmossen, Sweden 4.1 Introduction 80 4.2 Overview of Methods and Sites 83 4.2.1 Sphagnum Acid Standard 83 4.2.2 Taxon Sampling 83 4.2.3 THM in the Presence of Unlabelled and 13C-Labelled TMAH 84 4.3 Results and Discussion 85 4.3.1 THM in the Presence of TMAH of Authentic Sphagnum Acid 85 4.3.2 THM in the Presence of 13C-TMAH of Authentic Sphagnum Acid 88 4.3.3 Sphagnum Acid in Sphagnum Capitula 90 4.3.4 Sphagnum Acid in non-Sphagnum Plants 94 4.3.5 Sphagnum Parameters 97 4.3.6 Sphagnum Markers in Ryggmossen Peat Litter 98 4.4 Conclusions 101 Chapter 5 Geochemical Records of Sphagnum Peat Cores Spanning the 104 Range of Environmental Conditions from Ryggmossen 5.1 Introduction 105 5.2 Overview of Methods and Sites 107 5.2.1 Study Site 107 5.2.2 Sample Collection and Preparation 108 5.2.3 Water Table and Temperature Dynamics 108 5.2.4 THM in the Presence of TMAH 111 5.2.5 Carbohydrates and Elemental Analyses 111 5.2.6 Sphagnum Proxies 111 5.3 Results and Discussion 111 5.3.1 Surface Vegetation 111 5.3.2 Down Core Variation in Elemental and Isotope Parameters 114 5.3.3 Bulk Density and Carbon Storage 117 5.3.4 Carbohydrates 122 5.3.5 THM in the Presence of TMAH 127 5.3.6 Characterisation of Peat Archives 131 vii 5.4 Conclusions 141 Chapter 6 The Edge Effect of a Sitka Spruce Plantation on the Carbon 144 Storage and Phenolic Distribution in an Adjacent Peatland 6.1 Introduction 145 6.2 Overview of Methods and Sites 148 6.2.1 Site Background 148 6.2.2 TOC, Bulk Density & Carbon Storage 149 6.2.3 13C-TMAH Thermochemolysis 149 6.2.5 Lignin & Sphagnum Parameters 149 6.3 Results and Discussion 149 6.3.1 Carbon Storage 149 6.3.2 Thermochemolysis Products 153 6.3.2.1 Green litter 155 6.3.2.2 Brown litter 155 6.3.2.3 Fibric humic material 156 6.3.2.4 Sapric humic material 156 6.3.2.5 Characterisation of peat profiles 156 6.3.3 Aromatic Hydroxyl Content of THM Products of Lignin 162 6.3.3.1 Cinnamyl derivatives 162 6.3.3.2 Guaiacyl derivatives 163 6.3.3.3 Syringyl derivatives 169 6.3.4 Lignin Parameters 171 6.3.4.1 Lambda & [Ad/Al]G 171 6.3.4.2 Lignin proxies (S/G, C/G) 174 6.3.5 Non-Lignin Products 175 6.3.5.1 Tannin input 175 6.3.5.2 Sphagnum biomarkers 177 6.3.5.3 Polytrichum commune 179 6.3.5.4 Relative vegetation input 179 6.4 Conclusions 181 viii Chapter 7 The TMAH Thermochemolysis
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