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321 Pages·2017·25.799 MB·English
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Biochar A GUIDE TO ANALYTICAL METHODS Editors: Balwant Singh, Marta Camps-Arbestain and Johannes Lehmann Biochar A GUIDE TO ANALYTICAL METHODS Editors: Balwant Singh, Marta Camps-Arbestain and Johannes Lehmann © Balwant Singh, Marta Camps-Arbestain and Johannes Lehmann 2017 All rights reserved. Except under the conditions described in the Australian Copyright Act 1968 and subsequent amendments, no part of this publication may be reproduced, stored in a retrieval system or transmitted in any form or by any means, electronic, mechanical, pho- tocopying, recording, duplicating or otherwise, without the prior permission of the copyright owner. Contact CSIRO Publishing for all permission requests. The moral rights of the authors have been asserted. National Library of Australia Cataloguing-in-Publication entry Biochar : a guide to analytical methods / Balwant Singh, Marta Camps-Arbestain and Johannes Lehmann, editors. 9781486305094 (paperback) 9781486305100 (epdf) 9781486305117 (epub) Includes bibliographical references and index. Biochar – Analysis. Biochar – Composition. Charcoal – Analysis. Charcoal – Composition. Singh, Balwant, editor. Camps-Arbestain, Marta, editor. Lehmann, Johannes, Dr., editor. 662.74 Published exclusively in Australia and New Zealand by CSIRO Publishing Locked Bag 10 Clayton South VIC 3169 Australia Telephone: +61 3 9545 8400 Email: [email protected] Website: www.publish.csiro.au Published exclusively throughout the world (excluding Australia and New Zealand) by CRC Press/Taylor and Francis Group, LLC, with 978-1-4987-6553-4 CRC Press/Taylor and Francis Group, LLC 6000 Broken Sound Parkway, NW, Suite 300 Boca Raton, FL 33487 Tel: 561.994.0555 Website: www.crcpress.com Front cover: Biochar SEM image © Manawatu Microscopy and Imaging Centre, Massey University Set in 10/13 Minion & Stone Sans Edited by Adrienne de Kretser, Righting Writing Cover design by Andrew Weatherill Typeset by Thomson Digital Index by Bruce Gillespie Printed in China by 1010 Printing International Ltd CSIRO Publishing publishes and distributes scientific, technical and health science books, magazines and journals from Australia to a worldwide audience and conducts these activities autonomously from the research activities of the Commonwealth Scientific and Indus- trial Research Organisation (CSIRO). The views expressed in this publication are those of the author(s) and do not necessarily represent those of, and should not be attributed to, the publisher or CSIRO. The copyright owner shall not be liable for technical or other errors or omissions contained herein. The reader/user accepts all risks and responsibility for losses, damages, costs and other consequences result- ing directly or indirectly from using this information. Original print edition: The paper this book is printed on is in accordance with the rules of the Forest Stewardship Council®. The FSC® promotes environmentally responsible, socially beneficial and economically viable management of the world’s forests. Contents Preface and acknowledgements v List of contributors vii 1 Sampling, storage and preparation of biochar for laboratory analysis 1 Isabel Hilber, Hans-Peter Schmidt and Thomas D. Bucheli 2 Proximate analyses for characterising biochars 9 Akio Enders and Johannes Lehmann 3 Biochar pH, electrical conductivity and liming potential 23 Balwant Singh, Michaela Mei Dolk, Qinhua Shen and Marta Camps-Arbestain 4 Analysis of biochars for C, H, N, O and S by elemental analyser 39 Michael Bird, Claudia Keitel and Will Meredith 5 Inorganic carbon 51 Roberto Calvelo Pereira, Marta Camps-Arbestain, Tao Wang and Akio Enders 6 Dissolved carbon and LC-OCD of biochar 64 Khorshed Chinu, Christopher E. Marjo, Stephen D. Joseph and Balwant Singh 7 Determination of cation exchange capacity in biochar 74 Ellen R. Graber, Balwant Singh, Kelly Hanley and Johannes Lehmann 8 Determining acidic groups at biochar surfaces via the Boehm titration 85 Ellen R. Graber, Ludmila Tsechansky, Rivka B. Fidel, Michael L. Thompson and David A. Laird 9 Total elemental analysis of metals and nutrients in biochars 95 Akio Enders, Saran Sohi, Johannes Lehmann and Balwant Singh 10 Available nutrients in biochar 109 Marta Camps-Arbestain, Qinhua Shen, Tao Wang, Lukas van Zwieten and Jeff Novak 11 Polycyclic aromatic hydrocarbons in biochar 126 Gerard Cornelissen and Sarah E. Hale 12 Analysis of biochar porosity by pycnometry 132 Xiaodong Gao and Caroline A. Masiello 13 Guiding principles for measuring sorption of organic compounds on biochars 141 Rai S. Kookana, Ellen R. Graber and Ronald J. Smernik iv Biochar 14 Analysis of biochars by 13C nuclear magnetic resonance spectroscopy 151 Ronald J. Smernik 15 Analysis of biochars using benzene polycarboxylic acids 162 Michael W.I. Schmidt, Michael D. Hilf and Guido L.B. Wiesenberg 16 Pyrolysis-GC-MS of biochar 170 Joeri Kaal and Roberto Calvelo Pereira 17 Analysis of biochars by hydropyrolysis 187 Will Meredith, Anna McBeath, Philippa Ascough and Michael Bird 18 Biochar analysis by Fourier-transform infra-red spectroscopy 199 Cliff T. Johnston 19 Carbon near-edge absorption fine structure as a tool for understanding chemical differences in biochars 214 Peter S. Nico, Thomas Z. Regier, Adam W. Gillespie and Anca Cristina Cismasu 20 X-ray photoelectron spectroscopy analysis of biochar 229 Graham C. Smith 21 X-ray diffraction analysis of biochar 245 Balwant Singh and Mark D. Raven 22 Stable isotope analysis of biochars 253 Claudia Keitel, Philippa Ascough, Chris Wurster and Michael Bird 23 Application of scanning electron microscopy to the analysis of biochar-related materials 272 Stephen D. Joseph and Paul R. Munroe 24 Thermal analysis for biochar characterisation 283 Ondrˇej Mašek and Cliff T. Johnston Appendix 1. Biochar samples and their preparation for laboratory analysis 295 Balwant Singh, Qinhua Shen and Marta Camps-Arbestain Appendix 2. Specific surface area and porosity measurements 297 Scott Donne Index 300 Preface and acknowledgements Biochar is perhaps one of the topics with the greatest for the workshop in 2014. The reference biochars used increase in research activity among soil and environ- for the analyses were kindly provided by the UK Bio- ment researchers over the last decade. The initial char Research Centre, Edinburgh (UK), US Depart- interest in biochar research was mostly focused on its ment of Agriculture (USDA), Florence, (USA), roles in long-term carbon storage in soils, and soil University of Sydney, Pacific Pyrolysis Somersby fertility. However, in recent years biochar research has (Australia), NSW Department of Primary Industries, expanded into environmental, water science, mining, Wollongbar (Australia), Fraunhofer-Institute for microbial ecology and other fields. While the research Environmental, Safety, and Energy Technology advances for agriculture and environmental applica- (UMSICHT), Sulzbach-Rosenberg (Germany), tions of biochar are well covered in numerous journal Department of Agriculture (Thailand), and Univer- publications and the two editions of Biochar for Envi- sity of Zurich (Switzerland). We are particularly grate- ronmental Management: Science, Technology and ful to Adriana Downie, Andreas Hornung, Jeff Novak, Implementation (Eds J. Lehmann and S. Joseph) the Nattaporn Prakongkep, Michael Schmidt, Saran Sohi, analytical aspects of biochar have remained largely Fabian Stenzel and Lukas van Zwieten for their efforts neglected. This book aims to fill that gap. It provides in the provision of biochar samples. We are grateful to procedures and guidelines for routine and advanced several other colleagues for their help in the analysis characterisation of biochar to the biochar community of biochar and the review of manuscripts, in particu- including researchers, industry and users. lar Jim Amonette, Feike Dijkstra, Tim Filley, Arthur There have been discussions at various scientific Gessler, Robert Gilkes, Bill Gong, Stefan Hill, Bill meetings and conferences about the procedures used Koskinen, Felipe Macías, David Mitchell, Klaas in the laboratory analysis of biochars. Work on this Nierop, Juan Carlos Novoa-Muñoz, Alain Plante, book was initiated after the 20th World Congress of Malcolm Possell, Alessandro Girolamo Rombolà, Soil Science in Jeju, Korea in June 2014. Following the Hilary Stuart-Williams, Michael Turner, Sophie conference, reference biochars were assembled and Uchimiya and John Watts. We also thankful to subsamples were distributed to researchers for various Qinhua Shen for her help in formatting the chapters. analyses. The intention was to include a wide range of Our sincere thanks to CSIRO Publishing, particu- the measurements and techniques that are employed larly Lauren Webb for her friendly reminders and set- for biochar characterisation for various applications. ting firm but realistic time-lines for finalising the We contacted several research groups with experience chapters and guiding us through the publication pro- in specialised techniques. Analytical results of the cess. We also thank Julia Stuthe, who enthusiastically reference biochars were discussed at an international approved the book proposal. Finally, we are immensely workshop at the University of Sydney in December grateful to our respective families for their kind sup- 2014, and a framework for the book was prepared at port during the time we indulged in writing and edit- the workshop. This resulted in the preparation of 24 ing the book. chapters and two appendices – this book. We antici- pate that the procedures and analytical data presented Balwant Singh, Marta Camps-Arbestain and Johannes here will not only be an important resource for Lehmann researchers, but also have utility for practitioners and regulatory agencies. We are grateful to Professor Mark Adams, former Dean of the Faculty of Agriculture and Environment, University of Sydney for providing generous funding This page intentionally left blank List of contributors Philippa Ascough, Scottish Universities Environ- Michaela Mei Dolk, Centre for Carbon, Water and mental Research Centre, Scottish Enterprise Techno- Food, Faculty of Agriculture and Environment, Uni- logy Park, Rankine Avenue, East Kilbride G75 0QF, versity of Sydney, Sydney NSW 2006, Australia. UK. [email protected] [email protected] Michael Bird, College of Science, Technology and Scott Donne, PRC for Energy, Discipline of Chemis- Engineering and Centre for Tropical Environmental try, University of Newcastle, Callaghan NSW 2308, and Sustainability Science, James Cook University, Australia. [email protected] PO Box 6811, Cairns Qld 4870, Australia. michael. [email protected] Akio Enders, Department of Soil and Crop Sciences, Cornell University, Ithaca NY 14853, USA. ae55@cor- Thomas D. Bucheli, Agroscope Institute for Sustain- nell.edu ability Sciences, Reckenholzstrasse 191, 8046 Zurich, Switzerland. [email protected]. R.B. Fidel, Department of Agronomy, Iowa State Uni- versity, Ames IA 50011, USA. [email protected] Roberto Calvelo Pereira, New Zealand Biochar Research Centre, Institute of Agriculture and Envi- Xiaodong Gao, Department of Earth Science, Rice ronment, Private Bag 11222, Massey University, 4442 University, Houston TX 77005, USA. [email protected] Palmerston North, New Zealand. R.CalveloPereira@ massey.ac.nz Adam W. Gillespie, Ministry of Agriculture, Food and Rural Affairs, Guelph, Ontario, Canada. Marta Camps-Arbestain, New Zealand Biochar [email protected] Research Centre, Institute of Agriculture and Envi- ronment, Private Bag 11222, Massey University, 4442 Ellen R. Graber, Institute of Soil, Water and Environ- Palmerston North, New Zealand. M.Camps@massey. mental Sciences, Volcani Center, ARO, Bet Dagan ac.nz 50250, Israel. [email protected] Khorshed Chinu, Mark Wainwright Analytical Cen- Sarah E. Hale, Norwegian University of Life Sciences, tre, University of New South Wales, Sydney NSW NMBU, Ås, Norway. [email protected] 2052, Australia. [email protected] Kelly Hanley, Department of Soil and Crop Sciences, Gerard Cornelissen, Norwegian Geotechnical Insti- Cornell University, Ithaca NY 14853, USA. klh54@ tute, Oslo, Norway, and Norwegian University of Life cornell.edu Sciences, NMBU, Ås, Norway. Gerard.Cornelissen@ ngi.no Isabel Hilber, Agroscope Institute for Sustainability Sciences, Reckenholzstrasse 191, 8046 Zurich, Swit- Anca Cristina Cismasu, Earth and Environmental zerland. [email protected] Sciences Area, Lawrence Berkeley National Labora- tory, Berkeley, California. cristina.cismasu@gmail. Michael D. Hilf, Department of Geography, Univer- com sity of Zurich, 8057 Zürich, Switzerland. michael. [email protected] viii Biochar Cliff T. Johnston, Crop, Soil and Environmental Sci- Caroline A. Masiello, Department of Earth Science, ences, Department of Agronomy, 915 W. State St, Rice University, Houston TX 77005, USA. masiello@ Purdue University, West Lafayette IN, USA. cliffjohn- rice.edu [email protected] Anna McBeath, College of Science, Technology and Stephen D. Joseph, School of Materials Science and Engineering, and Centre for Tropical Environmental Engineering, University of New South Wales, Sydney and Sustainability Science, James Cook University, NSW 2052, Australia, and Discipline of Chemistry, PO Box 6811, Cairns Qld 4870, Australia. anna. University of Newcastle, Callaghan NSW 2308, [email protected] Australia. [email protected] Will Meredith, Department of Chemical and Envi- ronmental Engineering, Jubilee Campus, University Joeri Kaal, Institute for Heritage Sciences, Spanish of Nottingham, Nottingham, NG7 2TU, UK. william. National Research Council, Universidade de Santiago [email protected] de Compostela, Dep. Edafoloxía e Química Agrícola, 15704 Santiago de Compostela, Spain. joeri@samage. Paul R. Munroe, School of Materials Science and net Engineering, University of New South Wales, Sydney NSW 2052, Australia. [email protected] Claudia Keitel, Centre for Carbon, Water and Food, Faculty of Agriculture and Environment, University Peter S. Nico, Earth and Environmental Sciences of Sydney, 380 Werombi Rd, Brownlow Hill NSW Area, Lawrence Berkeley National Laboratory, Berke- 2570, Australia. [email protected] ley, California. [email protected] Rai S. Kookana, CSIRO Land and Water, PMB 2, Jeff Novak, USDA-ARS, Coastal Plain Soil, Water and Glen Osmond SA 5064, Australia, and School of Agri- Plant Research Center, 2611 West Lucas St, Florence culture, Food and Wine, University of Adelaide, PMB SC 29501, USA. [email protected] 1, Glen Osmond SA 5064, Australia. Rai.Kookana@ csiro.au Mark D. Raven, CSIRO Land and Water, Waite Rd, Urrbrae SA 5064, Australia. [email protected] D.A. Laird, Department of Agronomy, Iowa State University, Ames IA 50011, USA. [email protected] Thomas Z. Regier, Canadian Light Source Inc., Sas- katoon, Saskatchewan, Canada. tom.regier@light- Johannes Lehmann, Department of Soil and Crop source.ca Sciences, Cornell University, Ithaca NY 14853, USA. [email protected] Hans-Peter Schmidt, Ithaka Institute, Ancienne Eglise 9, 1974 Arbaz, Switzerland. schmidt@ithaka- Christopher E. Marjo, Mark Wainwright Analytical institut.org Centre, University of New South Wales, Sydney NSW 2052, Australia. [email protected] Michael W.I. Schmidt, Department of Geography, University of Zurich, 8057 Zürich, Switzerland. Ondřej Mašek, UK Biochar Research Centre, School [email protected] of GeoSciences, University of Edinburgh, Crew Build- ing, The Kings Building, Edinburgh EH92JN, UK. Qinhua Shen, New Zealand Biochar Research Centre, [email protected] Institute of Agriculture and Environment, Private Bag List of contributors ix 11222, Massey University, 4442 Palmerston North, L. Tsechansky, Institute of Soil, Water and Environ- New Zealand. [email protected] mental Sciences, Volcani Center, Agricultural Research Organization, POB 6, Bet Dagan, 50250, Balwant Singh, Centre for Carbon, Water and Food, Israel. [email protected] Faculty of Agriculture and Environment, University of Sydney, Sydney NSW 2006, Australia. balwant. Lukas van Zwieten, NSW Department of Primary [email protected] Industries, 1243 Bruxner Hwy, Wollongbar NSW 2477, Australia. [email protected] Ronald J. Smernik, School of Agriculture, Food and Wine, and Waite Research Institute, University of Tao Wang, Department of Biology, Microbial Ecology Adelaide, Waite Campus, Urrbrae SA 5064, Australia. Group, Lund University, SE-223 62 Lund, Sweden. [email protected] [email protected] Graham C. Smith, Department of Natural Sciences, Guido L.B. Wiesenberg, Department of Geography, University of Chester, Thornton Science Park, Chester University of Zurich, 8057 Zürich, Switzerland. guido. CH2 4NU, UK. [email protected] [email protected] Saran Sohi, UK Biochar Research Centre, School of Chris Wurster, College of Science, Technology and GeoSciences, University of Edinburgh, Crew Build- Engineering, and Centre for Tropical Environmental ing, The Kings Building, Edinburgh EH92JN, UK. and Sustainability Science, James Cook University, [email protected] PO Box 6811, Cairns Qld 4870, Australia. christopher. [email protected] M.L. Thompson, Department of Agronomy, Iowa State University, Ames, Iowa 50011, USA. mlthomps@ iastate.edu

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