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The Quantitative Determination of Sugars by Gas Chromatography and Aconitic Acid by Colorimetry in Sugar Cane Juice and Molasses

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The Quantitative Determination of Sugars by Gas Chromatography and Aconitic Acid by Colorimetry in Sugar Cane Juice and Molasses Louisiana State University LSU Digital Commons LSU Historical Dissertations and Theses Graduate School 1971 The Quantitative Determination of Sugars by Gas Chromatography and Aconitic Acid by Colorimetry in Sugar Cane Juice and Molasses. Louis Byron Fournier Louisiana State University and Agricultural & Mechanical College Follow this and additional works at: https://digitalcommons.lsu.edu/gradschool_disstheses Recommended Citation Fournier, Louis Byron, "The Quantitative Determination of Sugars by Gas Chromatography and Aconitic Acid by Colorimetry in Sugar Cane Juice and Molasses." (1971). LSU Historical Dissertations and Theses. 1920. https://digitalcommons.lsu.edu/gradschool_disstheses/1920 This Dissertation is brought to you for free and open access by the Graduate School at LSU Digital Commons. It has been accepted for inclusion in LSU Historical Dissertations and Theses by an authorized administrator of LSU Digital Commons. For more information, please contact [email protected]. 71-20,592 FOURNIER, Louis Byron, 1943- THE QUANTITATIVE DETERMINATION OF SUGARS BY GAS CHROMATOGRAPHY AND ACONITIC ACID BY COLORIMETRY IN SUGAR CANE JUICE AND MOLASSES. The Louisiana State University and Agricultural and Mechanical College, Ph.D., 1971 Chemistry, analytical University Microfilms, A XEROX Company , Ann Arbor, Michigan © 1971 LOUIS BYRON FOURNIER ALL RIGHTS RESERVED THIS DISSERTATION HAS BEEN MICROFILMED EXACTLY AS RECEIVED THE QUANTITATIVE DETERMINATION OF SUGARS BY GAS CHROMATOGRAPHY AND ACONITIC ACID BY COLORIMETRY IN SUGAR CANE JUICE AND MOLASSES A Dissertation Submitted to the Graduate Faculty of the Louisiana State University and Agricultural and Mechanical College in partial fulfillment of the requirements for the degree of Doctor of Philosophy in The Department of Chemistry by Louis Byron Fournier B.S., Southeastern Louisiana College, 1965 January 1971 ACKNOWLEDGEMENT This writer is deeply indebted to a number of people who have done much more than their positions demanded in assisting to accomplish the goals of this research program. It is a pleasure to enumerate here these accumulated debts, both intellectual and personal. Dr. Luis E. Vidaurreta, who conceived this project, and Dr. James W. Robinson, who graciously consented to serve as the chairman of my graduate committee are thanked for the roles they have played. Among the staff of the Chemistry Department of the Louisiana State University, the following people deserve recognition for their genuine interest and helpful assistance: Walter L. Patasig, Ralph L. Seab and George A. Sexton. The staff at the Cotton Insects Research Laboratory, Entomology Division, United States Department of Agriculture, located on the LSD Campus at 4115 Gourrier Avenue provided laboratory space, equipment, materials and consultation. Heed 1 stress how Important they were? The following members of that staff are thanked "for everything" since they were under no obligation to do so other than wishing to see that a graduate student get his work done: Marcus L. Burks, Dr. William C. Nettles, Jr., Dr. Howard R. Bullock and Dr. Norman W. Earle. In particular, the first two are thanked for submitting both toy facts and my interpretations to conscientious scrutiny. The use of a gas chromatograph for a short period of time and and electronic Integrator 'Sfhen the chips were d<*m" was provided by 11 I our area Hewlett Packard sales representative, Donald L. Sharp. Apparently he was right when he said, 'Veil, I'll never sell you one, but maybe I can help get you finished." Thanks, friend! I Mr. Milton Yates, President of LabTek, and Mr. fiano Harris, Jr., President of Precision Sampling Corporation, both of which are located in the Baton Rouge area, are thanked for being available "anytime" for materials, equipment, or just plain "talking over" problems which arose periodically in their specialities. Dr. John Seip and Mr. Fred L. Gayle of the Audubon Sugar ! Mill, LSU Campus, are thanked for providing samples of sugar cane juice and molasses for analysis as well as for several useful discussions and analytical determinations. Finally, this writer would like to thank his family for the care and consideration they showed throughout his educational efforts. His parents, Louis Joseph and Irene Meyers (now deceased) Fournier, are openly thanked for establishing the desire for and appreciation of an education early in his life and then making every possible sacrifice to aid in the achievement of that goal. Similarly, his wife, Judith Bates Fournier, furnished understanding and motivation, as well as actual physical assistance, in finishing this work. Thanks! ill I "Half of the Scientists who have ever lived are alive and working today." FOREWORD The above quotation is an idea popularly used today to indicate the rapid progress which is being made in every field of science. Our fields of endeavor are so numerous and progress made in I each so rapid that a major problem in the scientific community is the dissemination of information to the layman. It seems paradoxical to spend countless hours in research in order to solve a problem only to have that solution remain buried in professional journals out of sight of those very people to whom the solutions mean so much. Indeed, the attitude of many scientists today is such that they are more interested in their work in a "research for the sake of research1' manner (and perhaps for some personal glory which increases in direct proportion to their number of publications) than in really solving any problems. It was this attitude which indirectly stimulated the research program described herein. The sugar industry is in one sense the mother I of modern chemistry since so many branches of chemistry stemmed from attempts at understanding what was happening in sugar related processes. Unfortunately, the child has not acknowledged the mother and the chemistry profession has gone on to "bigger and better things'1 leaving its creator to wallow in the antiquity of its own processes. iv I Of course this attitude was not premeditated, but it is sanctioned by most modern educational institutions who believe that sugar chemistry and sugar chemists died with the advent of the Atomic Age and that certainly there are no real problems worthwhile investi­ gating in so old an industry. Unfortunately, nothing could be further from the truth. The real crime of the matter is that the field of chemistry does now have at its disposal the means with which to study more thoroughly the problems which beset the sugar industry. The same analyses which took years previously could be run today with modern instrumentation in a matter of minutes. It was the intention of this research program to make an effort at applying the techniques of quantitative gas chromatography to the analysis of various juices of importance to the sugar industry for the major constituents therein. As was soon apparent, only the determination of the main sugar constitutents is practical without extensive separation procedures. For the main acid component of sugar Juices, aconltlc acid, gas chromatography was found unsuitable. However, a rapid colorimetric method of analysis was developed which could cut down the time of analysis for aconitic acid in the sugar industry from several hours or even days to just a few minutes. ■ To illustrate the extent of the problem of communications mentioned earlier, it seems noteworthy to stress the fact that the i methods, reactions, and, of course, techniques used in this research work are not new. They are, for the most part, only extentions of work (somewhat modified) which has already appeared in scientific journals. Only the application to the problems of the sugar industry is new. vi TABLE OF CONTENTS Page ACKNOWLEDGEMENT............................ .................. ii FOREWORD.................................... .................... iv LIST OF TABLES.................................. ................ xi LIST OF FIGURES ................................ ......... xiv LIST OF ILLUSTRATIONS............................................ xvii ABSTRACT............................................ xviii INTRODUCTION...................................................... xix LITERATURE SURVEY CHAPTER I. SUGAR AND SUGAR CANE A. HISTORY............................ 1 B. MANUFACTURE........................ 5 C. REFINING........................ 9 D. PRODUCTION.......................... 10 E. THE SUGAR CHEMIST...................... 10 F. WEIGHTS............................................... 12 G. METHODS FOR MONITORING SUCROSE....................... 13 H. DETERMINING REDUCING SUGARS...................... 16 I. OTHER ANALYTICAL METHODS............................. 17 CHAPTER II. APPLICATION OF CHROMATOGRAPHIC PROCEDURES TO SUGAR SOLUTIONS A. INTRODUCTION......................................... 19 B. PAPER CHROMATOGRAPHY................................. 19 C. PAPER ELECTROPHORESIS................................. 20 D. COLUMN CHROMATOGRAPHY.................... 21 E. THIN-LAYER CHROMATOGRAPHY............................. 22 F. GAS CHROMATOGRAPHY.................... 23 CHAPTER III. TRIMETHYLSILYLATION A. DEFINITION........................................... 25 B. REACTION............................................. 26 C. THE MECHANISM OF SILYLATION........................... 28 D. THE TRANSITION OR INTERMEDIATE S T A T E ................ 37 vii Page EXPERIMENTAL CHAPTER IV. EXPERIMENTAL FORMAT AND GAS CHROMATOGRAPHS ; A. INTRODUCTION . 40 B. GAS CHROMATOGRAPHS USED IN THIS PROJECT..........
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