Tracking Environmental Change Using Lake Sediments.

Volume 2: Physical and Geochemical Methods

Developments in Paleoenvironmental Research

VOLUME 2
Tracking Environmental Change
Using Lake Sediments
Volume 2:
Physical and
Geochemical Methods

Edited by

William M. Last
Department of Geological Sciences,
University of Manitoba

and

John P. Smol
Department of Biology,
Queen’s University

KLUWER ACADEMIC PUBLISHERS

NEW YORK, BOSTON, DORDRECHT, LONDON, MOSCOW
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 DEDICATION

Dedicated to the memory of Dr. Kerry Kelts, who provided much needed leadership and
vision to the science of paleolimnology for the past quarter of a century.
 CONTENTS

Preface xiii
The Editors xiv
Aims & Scope of Developments in Paleoenvironmental Research Book Series xv
Editors and Board of Advisors of Developments in Paleoenvironmental
Research Book Series xvi
Contents of Volumes 1 to 4 of the Series xvii
Safety Considerations and Caution xx
List of Contributors xxi

1. An introduction to physical and geochemical methods used in paleolimnology.

William M. Last & John P. Smol 1

Part I: Physical Lithostratigraphy Techniques

2. Recognition and analysis of bedding and sediment fabric features.
Alan E. S. Kemp, Jean Dean, Richard B. Pearce & Jennifer Pike 7

Introduction
Approach
Photography and imagery of the core surface
Penetrative imaging of the core
Sampling wet, unconsolidated or semi-consolidated sediment
Sediment drying and resin-embedding
Thin section preparation
SEM analysis of laminated sediment
Summary
Acknowledgements
Appendix 1: Fluid displacive low viscosity resin embedding technique
Method
References

3. Image analysis techniques. Timo Saarinen & Gunilla Petterson 23

Introduction
Image analysis in paleolimnology
Material and methods
Future perspectives
Conclusion
Summary
Acknowledgements
References

vii
viii

4. Textural analysis of lake sediments. William M. Last 41

Introduction and importance of texture

Size
Form and fabric
Example of application of textural studies
Summary
Acknowledgments
References

Part II: Mineralogical and Geochemical Indicator Techniques

5. Inorganic geochemical methods in paleolimnology. J. F. Boyle 83

History & scope

Objectives of inorganic geochemical research
Elemental analysis
Identifying, characterizing, and quantifying sediment components
Areas of contention
Uses of inorganic geochemical data in palaeolimnology
Future developments
Summary
Acknowledgements
References

6. Mineralogical analysis of lake sediments. William M. Last 143

Introduction and importance of mineralogy

Mineralogy versus geochemistry
Minerals in lake sediments
A synopsis of methods
X-ray diffraction
Light microscopy
Future developments
Summary
Acknowledgments
References

7. Fluid inclusions in paleolimnological studies of chemical sediments.

Tim Lowenstein & Sean T. Brennan 189

Introduction
Distinguishing primary from secondary features in chemical sediments
Fluid inclusions in ancient chemical sediments
Fluid inclusion liquid-vapor homogenization temperatures:
paleolake temperatures
 ix

Fluid inclusion freezing-melting behavior: paleolake chemical compositions

Stable isotopes from fluid inclusion waters
Major element chemistry of fluid inclusions: paleolake water compositions
Summary
Acknowledgements
References

8. Application of mineral magnetic techniques to paleolimnology.

Per Sandgren & Ian Snowball 217

Introduction
A brief history of the application of mineral magnetic measurements
to lake sediments
Magnetic properties
Magnetic hysteresis
Anhysteretic remanent magnetisation (ARM)
Sample collection and preparation
Sequence of measurements
Hysteresis curves
Summary
References

9. Sediment organic matter.

Philip A. Meyers & Jane L. Teranes 239

Introduction
Paleolimnological proxies
Summary
Acknowledgments
References

10. Paleolimnological methods and applications for persistent organic pollutants.

Jules M. Blais & Derek C. G. Muir 271

Introduction
Advances in extraction and quantitative analytical techniques for POPs
in sediment
Transfer processes in lakes
Summary
Acknowledgments
References

11. Near-Infrared spectrometry (NIRS) in paleolimnology.

Tom Korsman, Ingemar Renberg, Eigil Dåbakk & Mats B. Nilsson 299
x

Introduction
Theory
Instrumentation
NIR analysis of sediment samples
Uses of NIRS in palaeolimnology
Future perspectives
Summary
References

12. Fly-ash particles. Neil Rose 319

Introduction
A brief history
Methods of extraction and enumeration
Temporal distribution
Spatial distribution
Source apportionment
The future
Summary
Acknowledgements
References

Part III: Stable Isotope Techniques

13. Application of stable isotope techniques to inorganic and biogenic carbonates.

Emi Ito 351

Introduction
Nomenclature and systematics
of lake-water
Mg/Ca and Sr/Ca ratios of lake-water
of dissolved inorganic carbon (DIC)
Carbonates in lake-sediments
Mollusks
Ostracodes
Charaphytes
Isotope analysis
Preparation of carbonate samples for isotope analysis
Conclusions
Summary
Acknowledgments
References

14. Carbon and oxygen isotope analysis of lake sediment cellulose: methods
and applications. Brent B. Wolfe, Thomas W. D. Edwards, Richard J. Elgood &
Kristina R. M. Beuning 373
 xi

Introduction
Stable isotope tracers in lake
Historical development
Methods
Key criteria for paleohydrologic reconstruction
Applications
Future research directions
Summary
Acknowledgements
References

15. Nitrogen isotopes in palaeolimnology. Michael R. Talbot 401

Introduction
Nitrogen in lakes: forms and distribution
Nitrogen isotopes
Nitrogen isotope studies in palaeolimnology: sampling and measurement
Some examples
Closing remarks
Summary
Acknowledgments
References

Glossary, acronyms and abbreviations 441

Index 493
 xiii

PREFACE

The explosive growth of paleolimnology over the past two decades has provided impetus
for the publication of this series of monographs detailing the numerous advances and new
techniques being applied to the interpretation of lake histories. This is the second volume
in the series and deals mainly with physical and geochemical analytical techniques. Vol-
ume 1 (Last & Smol, 2001) examines the acquisition and archiving of cores, chronological
techniques, and large-scale basin analysis methods. Volumes 3 and 4 (Smol et al., 200l a
& b) provide a comprehensive overview of the many biological techniques that are used in
paleolimnology. A fifth volume that is currently being prepared (Birks et al., in preparation)
examines statistical and data handling methods. It is our hope that these monographs will
provide sufficient detail and breadth to be useful handbooks for both seasoned practitioners
as well as newcomers to the area of paleolimnology. These books should also be useful to
non-paleolimnologists (e.g., limnologists, environmental scientists, archeologists, palynol-
ogists, geographers, geologists, etc.) who continue to hear and read about paleolimnology,
but have little chance to explore the vast and sometimes difficult to access journal-based
reference material for this rapidly expanding field. Although the chapters in these volumes
target mainly lacustrine settings, many of the techniques described can also be readily
applied to fluvial, glacial, marine, estuarine, and peatland environments.
The 15 chapters in this volume are organized into three major parts. The three chapters
in Part I provide an overview of the most common physical lithostratigraphy techniques.
Part II discusses geochemical and mineralogical approaches. The third part of this book
includes three chapters summarizing oxygen, carbon, and nitrogen isotopic techniques.
Following this is a comprehensive glossary and list of acronyms and abbreviations.
Many people have helped with the planning, development, and final production of this
volume. In addition to the hard work provided by the authors of these contributions, this
publication benefitted from the technical reviews furnished by our scientific colleagues,
many of whom remain anonymous. Each chapter was critically examined by two external
referees as well as the editors. In order to assure readability for the major target audience,
we asked many of our graduate students to also examine selected chapters; their insight and
questioning during the reviewing and editorial process are most gratefully acknowledged.
The staff of the Environmental, Earth and Aquatic Sciences Division of Kluwer Academic
Publishers are commended for their diligence in production of the final presentation. In
particular, we would also like to thank Ad Plaizier, Anna Besse-Lototskaya (Publishing
Editor, Aquatic Science Division), and Rene Mijs (former Publishing Editor, Biosciences
Division) for their long-term support of this new series of monographs and their interest
in paleoenvironmental research. Finally, we would like to thank our respective universities
and colleagues for support and encouragement during this project.
xiv

THE EDITORS

William M. Last is a professor in the Department of Geological Sciences at University of

Manitoba (Winnipeg, Manitoba, Canada) and is co-editor of the Journal of Paleolimnology.

John P. Smol is a professor in the Biology Department at Queen’s University (Kingston,

Ontario, Canada), with a cross-appointment at the School of Environmental Studies. He
co-directs the Paleoecological Environmental Assessment and Research Lab (PEARL). Pro-
fessor Smol is co-editor of the Journal of Paleolimnology and holds the Canada Research
Chair in Environmental Change.
 xv

AIMS AND SCOPE OF DEVELOPMENTS

IN PALEOENVIRONMENTAL RESEARCH BOOK SERIES

Paleoenvironmental research continues to enjoy tremendous interest and progress in the

scientific community. The overall aims and scope of the Developments in Paleoenvironmen-
tal Research book series are to capture this excitement and document these developments.
Volumes related to any aspect of paleoenvironmental research, encompassing any time
period, are within the scope of the series. For example, relevant topics include studies
focused on terrestrial, peatland, lacustrine, riverine, estuarine, and marine systems, ice
cores, cave deposits, palynology, isotopes, geochemistry, sedimentology, paleontology,
etc. Methodological and taxonomic volumes relevant to paleoenvironmental research are
also encouraged. The series will include edited volumes on a particular subject, geographic
region, or time period, conference and workshop proceedings, as well as monographs.
Prospective authors and/or editors should consult the series editors for more details. The
series editors also welcome any comments or suggestions for future volumes.
xvi

EDITORS AND BOARD OF ADVISORS OF DEVELOPMENTS IN

PALEOENVIRONMENTAL RESEARCH BOOK SERIES

Series Editors:

John P. Smol
Paleoecological Environmental Assessment and Research Lab (PEARL)
Department of Biology
Queen’s University
Kingston, Ontario, K7L 3N6, Canada
e-mail: [email protected]

William M. Last
Department of Geological Sciences
University of Manitoba
Winnipeg, Manitoba R3T 2N2, Canada
e-mail: [email protected]

Advisory Board:

Professor Raymond S. Bradley

Department of Geosciences
University of Massachusetts
Amherst, MA 01003-5820 USA
e-mail: [email protected]

Professor H. John B. Birks

Botanical Institute
University of Bergen
Allégaten 41
N-5007 Bergen
Norway
e-mail: [email protected]

Dr. Keith Alverson

Science Officer
IGBP-PAGES International Project Office
Barenplatz 2
3011 Bern
Switzerland
e-mail: [email protected]
 xvii

CONTENTS OF VOLUMES 1 TO 4 OF THE SERIES

Contents of Volume 1: Tracking Environmental Change Using Lake Sediments: Basin

Analysis, Coring, and Chronological Techniques.

An introduction to basin analysis, coring, and chronological techniques used in

paleolimnology. William M. Last & John P. Smol
Applications of seismic sequence stratigraphy in lacustrine basins.
Christopher A. Scholz
Ground penetrating radar applications in paleolimnology. Brian J. Moorman
Shoreline and basin configuration techniques in paleolimnology. Dorothy Sack
Sediment core collection and extrusion. John R. Glew, John P. Smol
& William M. Last
Coring and drilling equipment and procedures for recovery of long lacustrine
sequences. Suzanne A. G. Leroy & Steve M. Colman
Sediment logging techniques. Bernd Zolitschka, Jens Mingram, Sjerry van der Gaast,
J. H. Fred Jansen & Rudolf Naumann
Logging of magnetic susceptibility. Norbert R. Nowaczyk
Chronostratigraphic techniques in recent sediments. P. G. Appleby
chronostratigraphic techniques in paleolimnology. Svante Björck
& Barbara Wohlfarth
Varve chronology techniques. Scott Lamoureux
Luminescence dating. Olav B. Lian & D. J. Huntley
Electron spin resonance (ESR) dating in lacustrine environments.
Bonnie A. B. Blackwell
Use of paleomagnetism in studies of lake sediments. John King & John Peck
Amino acid racemization (AAR) dating and analysis in lacustrine environments.
Bonnie A. B. Blackwell
Tephrochronology. C. S. M. Turney & J. J. Lowe
Glossary, Acronyms and Abbreviations
Subject Index

Contents of Volume 2: Tracking Environmental Change Using Lake Sediments: Physical

and Geochemical Methods.

An introduction to physical and geochemical methods used in paleolimnology.

William M. Last & John P. Smol
xviii

Recognition and analysis of bedding and sediment fabric features. Alan E. S. Kemp,
Jean Dean, Richard B. Pearce & Jennifer Pike
Image analysis techniques. Timo Saarinen & Gunilla Petterson
Textural analysis of lake sediments. William M. Last
Inorganic geochemical methods in paleolimnology. J. F. Boyle
Mineralogical analysis of lake sediments. William M. Last
Fluid inclusions in paleolimnological studies of chemical sediments. Tim Lowenstein
& Sean T. Brennan
Application of mineral magnetic techniques to paleolimnology. Per Sandgren
& Ian Snowball
Sediment organic matter. Philip A. Meyers & Jane L. Teranes
Paleolimnological methods and applications for persistent organic pollutants.
Jules M. Blais & Derek C. G. Muir
Near-Infrared spectrometry (NIRS) in paleolimnology. Tom Korsman, Eigil Dåbakk,
Mats B. Nilsson & Ingemar Renberg
Fly-ash particles. Neil Rose
Application of stable isotope techniques to inorganic and biogenic carbonates.
Emi Ito
Carbon and oxygen isotope analysis of lake sediment cellulose: methods and
applications. Brent B. Wolfe, Thomas W. D. Edwards,
Kristina R. M. Beuning & Richard J. Elgood
Nitrogen isotopes in palaeolimnology. Michael R. Talbot
Glossary, Acronyms and Abbreviations
Subject Index

Contents of Volume 3: Tracking Environmental Change Using Lake Sediments:

Terrestrial, Algal, and Siliceous Indicators.

Using biology to study long-term environmental change. John. P. Smol, H. John B.

Birks & William M. Last
Pollen. K. D. Bennett & K. J. Willis
Conifer stomata. Glen M. MacDonald
Plant macrofossils. Hilary H. Birks
Charcoal as a fire proxy. Cathy Whitlock & Chris Larsen
Non-pollen palynomorphs. Bas van Geel
 xix

Protozoa: testate amoebae. Louis Beyens & Ralf Meisterfeld

Diatoms. Richard W. Battarbee, Laurence Carvalho, Vivienne J. Jones,
Roger J. Flower, Nigel G. Cameron, Helen Bennion & Stephen Juggins
Chrysophyte scales and cysts. Barbara A. Zeeb & John P. Smol
Ebridians. Atte Korhola & John P. Smol
Phytoliths. Dolores R. Piperno
Freshwater sponges. Thomas M. Frost
Siliceous protozoan plates and scales. Marianne S. V. Douglas & John P. Smol
Biogenic silica. Daniel J. Conley & Claire L. Schelske
Sedimentary pigments. Peter R. Leavitt & Dominic A. Hodgson
Glossary, Acronyms and Abbreviations
Subject Index

Contents of Volume 4: Tracking Environmental Change Using Lake Sediments:

Zoological Indicators.

Zoological indicators in lake sediments: an introduction. John. P. Smol,

H. John B. Birks & William M. Last
Cladocera and other branchiopod crustaceans. Atte Korhola & Milla Rautio
Midges: Chironomidae and related Diptera. Ian R. Walker
Coleoptera and Trichoptera. Scott A. Elias
Oribatid mites. Torstein Solhøy
Bryozoan statoblasts. Donna R. Francis
Ostracoda. Jonathan A. Holmes
Freshwater molluscs. Barry B. Miller & Michael J. S. Tevesz
Fish. W. P. Patterson & G. R. Smith
Glossary, Acronyms and Abbreviations
Subject Index
xx

SAFETY CONSIDERATIONS AND CAUTION

Paleolimnology has grown into a vast scientific pursuit with many branches and subdi-
visions. It should not be surprising, therefore, that the tools used by paleolimnologists are
equally diverse. Virtually every one of the techniques described in this book requires some
familiarity with standard laboratory or field safety procedures. In some of the chapters,
the authors have made specific reference to appropriate safety precautions; others have
not. The responsibility for safe and careful application of these methods is yours. Never
underestimate the personal risk factor when undertaking either field or laboratory inves-
tigations. Researchers are strongly advised to obtain all safety information available for
the techniques they will be using and to explicitly follow appropriate safety procedures.
This is particularly important when using strong acids, alkalies, or oxidizing reagents
in the laboratory or many of the analytical and sample collection/preparation instruments
described in this volume. Most manufacturers of laboratory equipment and chemical supply
companies provide this safety information, and many Internet and other library resources
contain additional safety protocols. Researchers are also advised to discuss their procedures
with colleagues who are familiar with these approaches, and so obtain further advice on
safety and other considerations.
The editors and publisher do not necessarily endorse or recommend any specific product,
procedure, or commercial service that may be cited in this publication.
 xxi

LIST OF CONTRIBUTORS

Kristina R. M. Beuning
Department of Earth and Environmental Sciences
Wesleyan University
Middletown, CT, 06459, USA
e-mail: [email protected]

Jules M. Blais
Program for Environmental and Chemical Toxicology
Department of Biology
University of Ottawa
30 Marie Curie St.
P.O. Box 450, Stn. A
Ottawa, Ontario, K1N 6N5, Canada
e-mail: [email protected]

J. F. Boyle
Department of Geography
University of Liverpool
PO Box 147
Liverpool L69 3BX, UK
e-mail: [email protected]

Sean T. Brennan
Department of Geological Sciences & Environmental Studies
State University of New York at Binghamton
Binghamton, NY 13902, USA

Eigil Dåbakk
Department of Organic Chemistry
Umeå University
SE-901 87 Umeå, Sweden
e-mail: [email protected]

Jean Dean
School of Ocean and Earth Sciences
University of Southampton
Southampton Oceanography Centre
European Way
Southampton, SO14 3ZH, UK

Thomas W. D. Edwards
Department of Earth Sciences
University of Waterloo
Waterloo ON, N2L 3G1, Canada
e-mail: [email protected]
xxii

Richard J. Elgood
Department of Earth Sciences
University of Waterloo
Waterloo, ON, N2L 3G1, Canada

Emi Ito
Department of Geology and Geophysics
and Limnological Research Center
University of Minnesota
310 Pillsbury Drive, SE
Minneapolis, MN 55455, USA
e-mail: [email protected]

Alan E. S. Kemp
School of Ocean and Earth Sciences
University of Southampton
Southampton Oceanography Centre
European Way
Southampton, SO14 3ZH, UK
e-mail: [email protected]

Tom Korsman
Department for Ecology and Environmental Science
Umeå University
S-901 87 Umeå, Sweden
e-mail: [email protected]

William M. Last
Department of Geological Sciences
University of Manitoba
Winnipeg, Manitoba, R3T 2N2, Canada
e-mail: [email protected]

Tim K. Lowenstein
Department of Geological Sciences & Environmental Studies
State University of New York at Binghamton
Binghamton, NY 13902, USA
e-mail: [email protected]

Phillip A. Meyers
Department of Geological Sciences
The University of Michigan
Ann Arbor, MI 48109-1063 USA
e-mail: [email protected]
 xxiii

Derek Muir
Environment Canada
Canada Centre for Inland Waters
867 Lakeshore Road
Burlington, Ontario, L7R 4A6 Canada
e-mail: [email protected]

Mats B. Nilsson
Department of Forest Ecology
Swedish University of Agricultural Sciences
SE-901 83 Umeå, Sweden
e-mail: [email protected]

Richard B. Pearce
School of Ocean and Earth Sciences
University of Southampton
Southampton Oceanography Centre
European Way
Southampton, SO14 3ZH, UK

Gunilla Petterson
Department of Ecology and Environmental Science
Umeå University
S-901 87 Umeå, Sweden
e-mail: [email protected]

Jennifer Pike
Department of Earth Sciences
Cardiff University
P.O. Box 914
Cardiff, CF1 3YE, UK

Ingemar Renberg
Department for Ecology and Environmental Science
Umeå University
S-901 87 Umeå, Sweden
e-mail: [email protected]

Neil Rose
Environmental Change Research Centre
University College London
26 Bedford Way, London WC1H 0AP, U.K.
e-mail: [email protected]
xxiv

Timo Saarinen
Geological Survey of Finland
Betonimiehenkuja 4
FIN-02150 Espoo, Finland
e-mail: [email protected]

Per Sandgren
Department of Quaternary Geology
Tornavägen 13
SE-223 63 Lund, Sweden
e-mail: [email protected]

John P. Smol
Paleoecological Environmental Assessment and Research Lab (PEARL)
Department of Biology
Queen’s University
Kingston, Ontario, K7L 3N6, Canada
e-mail: [email protected]

Ian Snowball
Department of Quaternary Geology
Tornavägen 13
SE-223 63 Lund, Sweden
e-mail: [email protected]

Michael R. Talbot
Geological Institute
University of Bergen
Allégaten 41
5007 Bergen, Norway
e-mail: [email protected]

Jane L. Teranes
Geosciences Research Division
Scripps Institution of Oceanography
University of California San Diego
La Jolla, CA 92093-0244, USA
e-mail: [email protected]

Brent B. Wolfe
Department of Earth Sciences
University of Waterloo
Waterloo ON, N2L 3G1, Canada
e-mail: [email protected]