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INFORMATION to USERS the Most Advanced Technology Has Been INFORMATION TO USERS The most advanced technology has been used to photo­ graph and reproduce this manuscript from the microfilm master. UMI films the text directly from the original or copy submitted. Thus, some thesis and dissertation copies are in typewriter face, while others may be from any type of computer printer. The quality of this reproduction is dependent upon the quality of the copy submitted. Broken or indistinct print, colored or poor quality illustrations and photographs, print bleedthrough, substandard margins, and improper alignment can adversely affect reproduction. In the unlikely event that the author did not send UMI a complete manuscript and there are missing pages, these will be noted. Also, if unauthorized copyright material had to be removed, a note will indicate the deletion. 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University Microfilms International A Bell & Howell Information Company 300 North Zeeb Road, Ann Arbor, Ml 48106-1346 USA 313/761-4700 800/521-0600 Order Number 891S686 Characterization of humic and fulvic acids extracted from surface horizons of contiguous Alfisols and Mollisols of southwestern Ohio and their influence on mineral weathering Novak, Jeffrey Michael, Ph.D. The Ohio State University, 1989 Copyright ©1989 by Novak, Jeffrey Michael. All rights reserved. UMI 300 N. Zeeb Rd. Ann Arbor, MI 48106 CHARACTERIZATION OF HUMIC AND FULVIC ACIDS EXTRACTED FROM SURFACE HORIZONS OF CONTIGUOUS ALFISOLS AND MOLLISOLS OF SOUTHWESTERN, OHIO AND THEIR INFLUENCE ON MINERAL WEATHERING DISSERTATION Presented in Partial Fulfillment of the Requirements for the Degree Doctor of Philosophy in the Graduate School of The Ohio State University By Jeffrey M. Novak B.S., M.S. ***** The Ohio State University 1989 Reading Committee: Approved By Dr. Neil E. Smeck Dr. Frank L. Himes Dr. Sam Traina Advisor Department of Agronomy Dr. Gunter Faure Copyright by Jeffrey M, Novak 1989 DEDICATION Laura and Andrew ACKNOWLEDGEMENTS I wish to express my appreciation to my advisor, Dr. Neil E. Smeck, for his advice, ideas, and short-term financial support through this investigation. Apprecia­ tion is also given to Dr. Jerry M. Bigham for his invaluable guidance in soil mineralogical investigations as well as other aspects of my research. I would also like to thank Dr. Frank Himes for his valuable assistance and guidance during the organic matter extraction and purification phase of this project. I am also grateful to Dr. Sam Traina and Dr. Gunter Faure for their suggestions and service on committees. I would like to thank Mrs. Sue Shipatilo for the NMR analysis. I would like to especially thank Mr. Lee Burras, Mr. Sandy Jones, and Dr. Billy Jaynes for their excellent advice and participation in soil sample analyses. I would also like to thank the Department of Agronomy, The Ohio State University for long term financial support. To my wife, Laura, for valuable assistance in preparation of the manuscript. VITA August 26, 1958 Born - Elizabeth, New Jersey 1980 B.S., Delaware Valley College Doylestown, Pennsylvania 1980 - 1983 Graduate Assistant Department of Agronomy, Iowa State University, Ames, Iowa 1983 M.S., Iowa State University, Ames, Iowa 1983 - 1989 Graduate Student Department of Agronomy, Ohio State University, Columbus, Ohio PUBLICATIONS Novak, J. M., and A. M. Blackmer. 1983. 15-N Tracer studies of reactions of nitric oxide during denitrification in soils. Agron. Abstracts p. 159. Novak, J. M., and N. E. Smeck. 1987. Characterization of humic and fulvic acids extracted from surface horizons of contiguous Alfisols and Mollisols from south­ western, Ohio. Agron. Abstracts p. 189. FIELDS OF STUDY Major Field: Soil Morphology, Mineralogy, and Genesis Studies in Soil Science. Professors N. E. Smeck, J. M. Bigham, G. F. Hall Studies in Humic Chemistry. Professors F. L. Himes, S. J. Traina. Studies in Geology and Mineralogy. Professors R. T. Tettenhorst, G. Faure, G. D. McKenzie iv TABLE OF CONTENTS Page DEDICATION .............................................. ii ACKNOWLEDGEMENTS ....................................... iii VITA .................................................... iv LIST OF TABLES ..................................... x LIST OF FIGURES..................................... xiv INTRODUCTION ........................................... 1 CHAPTER I. METHODS AND MATERIALS ........................... 3 1.1 Site and Pedon Selection................. 3 1.2 Morphological Description and Sample. 5 Collection 1.3 Soil Characterization ....................... 5 1.3.1 Sample Preparation.................... 5 1.3.2 Coarse Fragment Content .............. 6 1.3.3 Particle Size Analysis................ 6 1.3.4 p H ....................................... 7 1.3.5 Organic Carbon......................... 7 1.3.6 Carbonate Content ..................... 8 1.3.7 Extractable Acidity .................. 8 1.3.8 Extractable Cations .................. 9 1.3.9 Duplicate and Data Expression .... 9 1.4 Clay Mineralogy .......................... 11 1.4.1 Fractionation of Sand, Silt and . 11 Clay 1.4.2 Fine and Coarse Clay Fractionation. 12 1.4.3 X-Ray Diffraction Analysis........ 13 v TABLE OF CONTENTS (Continued) Page II. DESCRIPTION OF THE STUDY AREA AND SOIL......... 16 CHARACTERISTICS 2.1 Location and Physiography ................ 16 2 . 2 Bedrock G e o l o g y ........................... 19 2.3 Glacial Geology ........................... 20 2.4 Climate and Vegetation.................... 21 2.5 Soil Characteristics....................... 22 2.5.1 Morphological Description ........... 22 2.5.2 Particle Size Analysis............. 24 2.5.3 Chemical Properties .................. 3 0 2.5.4 Mineralogy........................... 31 A. Clay Mineralogy of the Fine .... 31 Clay Fraction B. Clay Mineralogy of the Coarse . 45 Clay Fraction C. Clay Mineralogy of the Total. 59 Clay Fraction III. SOIL ORGANIC MATTER CHARACTERIZATION........... 67 3.1 Introduction................................ 67 3.2 Literature Review ........................... 68 3.2.1 Biochemistry of Humus Formation . 68 3.2.2 Extraction, Fractionation,......... 72 Purification, and Distribution of Soil Humic and Fulvic Acids 3.2.3 Chemical Characterization of Humic. 80 and Fulvic Acids 3.3 Methods of Soil Organic Matter Extraction . 101 3.3.1 Soil P r e t r e a t m e n t ..................... 103 3.3.2 Alkaline Extraction .................. 103 3.3.3 Separation of Humic and Fulvic Acids. 104 3.3.4 Purification of Humic Acids ......... 105 3.3.5 Purification of Fulvic Acids......... 106 3.3.6 Purification of H u m i n ................ 108 3.4 Methods of Humic and Fulvic Acid .......... 109 Characterization 3.4.1 Functional Group and E4/E6 Ratio. 109 Analyses 3.4.2 Elemental Analyses.................. 110 3.4.3 Infrared Spectrometry ................ 110 3.4.4 13C CPMAS NMR Spectroscopy......... Ill 3.5 Results and Discussion............. 112 3.5.1 Extraction of Humic and Fulvic Acids. 112 3.5.2 Humic and Fulvic A c i d ............. 119 Characterization A. Elemental and Atomic Ratio .... 119 Analyses vi TABLE OF CONTENTS (Continued) Page B. E4/E6 Absorption Ratio ........... 124 C. Functional Group Analyses......... 12 6 D. Infrared Absorption Spectra. 129 1. Humic Acids ..................... 129 2. Fulvic Acids..................... 134 E. 13C CPMAS Spectra.................. 138 1. Humic Acids ..................... 140 a. Aliphatic Region ........... 140 b. Oxygen Alkyl Region......... 148 c. Aromatic.Region............. 150 d. Carboxyl Region............. 152 e. Carbonyl.Region............. 154 2. Fulvic Acids..................... 155 a. Aliphatic Region ........... 155 b. Oxygen Alkyl Region......... 159 c. Aromatic Region............. 160 d. Carboxyl Region............. 162 e. Carbonyl Region............. 162 3.6 Summary ...................................... 163 IV. HUMIC SUBSTANCES IN WHOLE SOILS ................. 165 4.1 Introduction........................... 165 4.2 Literature Review ........................... 165 4.2.1 13C NMR Analysis of Unfractionated. 165 Soils 4.2.2 13C NMR Analysis of Fractionated. 166 Soils 4 . 3 Materials and Methods ............... 168 4.3.1 Sonification of Whole Soils ......... 168 4.3.2 Collection of Organic Carbon... 169 Enriched Soil 4.3.3 13C CPMAS NMR Analysis o f ..... 170 Organic Carbon Enriched Soil 4.4 Results and Discussion............... 171 4.4.1 Particle Size Analysis of Fractions . 171 Collected by Sonification and Sedimentation 4.4.2 Percent Organic Carbon in Collected . 172 Fractions 4.4.3 13C NMR Spectra of Fine Material. 173 from Whole Soils 4.5 Summary ....................................... 176 vii TABLE OF CONTENTS (Continued) Page V. INFLUENCE OF SORBED HUMIC SUBSTANCES ON THE . 178 DECOMPOSITION OF TOTAL CLAY FRACTION BY SULFURIC ACIDS 5.1 Introduction.................................. 178 5.2 Literature Review ..........................
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