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THE DETERMINATION of SELENIUM. the Louisiana State University and Agricultural and Mechanical College, Phjd., 1969

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THE DETERMINATION of SELENIUM. the Louisiana State University and Agricultural and Mechanical College, Phjd., 1969 Louisiana State University LSU Digital Commons LSU Historical Dissertations and Theses Graduate School 1969 The etD ermination of Selenium. Robert Lewis Osburn Louisiana State University and Agricultural & Mechanical College Follow this and additional works at: https://digitalcommons.lsu.edu/gradschool_disstheses Recommended Citation Osburn, Robert Lewis, "The eD termination of Selenium." (1969). LSU Historical Dissertations and Theses. 1681. https://digitalcommons.lsu.edu/gradschool_disstheses/1681 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]. This dissertation has been microfilmed exactly as received 70-9081 OSBURN, Robert Lewis, 1936- THE DETERMINATION OF SELENIUM. The Louisiana State University and Agricultural and Mechanical College, PhJD., 1969 Chemistry, analytical University Microfilms, Inc., Ann Arbor, M ichigan THE DETERMINATION OF SELENIUM 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 Robert Lewis Osburn B.S., George Peabody College, 1962 August, I969 TO LINDA who understands. ACKNOWLEDGMENTS The author wishes to express his gratitude to Professor Philip W. West, who, through his penetrating insight, calm for­ bearance, and timely encouragement, contributed so much to the attainment of this goal. He also wishes to thank the United States Public Health Service for providing the funds during the entirety of this work through U. S. Public Health Research Grant No. AP 0072^, National Center for Air Pollution Control, Bureau of Disease Prevention and Environmental Control. The author gratefully acknowledges the financial assistance received from the "Dr. Charles E. Coates Memorial Fund of the L. S. U. Foundation donated by George H. Coates" for the preparation of this dissertation. iii Patience is bitter, but its fruit is sweet. Jean Jacques Rousseau iv TABLE OF CONTENTS PAGE DEDICATION.................. ii ACKNOWLEDGMENTS....................................... iii QUOTATION............................................. iv LIST OF TABLES ....................................... viii ABSTRACT ............................................. x CHAPTER I. INTRODUCTION .................................. 1 II. CONVENTIONAL METHODS FOR THE DETERMINATION OF SELENIUM...................... 12 A. Titrimetric Methods....................... 12 B. Gravimetric Methods....................... 13 C. Neutron-Activation Analysis............... 15 D. Polarographic Methods..................... 16 E. Photometric Methods....................... 17 1. Spectrophotometry.................... 17 a. Particles in Suspension........... 17 b. Equivalent in Liberated Iodine.......................... 17 c. Pyrrole Color Complex............. 18 d. Diaminobenzidine Complex ......... 18 e. Miscellaneous.................... 19 PAGE CHAPTER 2. Fluor imetry........... 20 5. Emission Spectroscopy............... 21 X-Ray Fluorescence Spectroscopy ...................... 21 F. Ring Oven Method ................ 21 G. Catalytic Methods...................... 22 III. THE DETERMINATION OF SELENIUM BY THE HYDROXYLAMINE OXIDATION METHOD ........... 2k A. Introduction.......................... 2k B. Preparation of Reagents and Solutions.............................. 27 1. Standard Selenium Solution ...... 27 2. Hydrochloric Acid................... 27 3. Hydroxylamine Hydrochloride Solution.......................... 27 I4-. Sulfanilamide Solution............. 27 5. N-(1-Naphthyl)ethylenediamine Dihydrochloride Solution ........... 28 6. Interference Solutions ............. 28 C. Apparatus.......... 28 IV. RESULTS AND DISCUSSION...................... 30 A. Preliminary Experiments................. 30 B. The Oxidation-Diazotization Reaction.............................. 37 vi PAGE CHAPTER C. The Coupling Reaction..................... k6 D. Concentration Studies..................... 1. Sulfanilamide (p-aminobenzene- sulfonamide) ........................ 52 2. N-(1-Naphthyl)ethylenediamine Dihydrochloride...................... 55 5. Hydroxylamine Hydrochloride........... 58 E. The Standard Recommended Procedure................................ 58 F. Interference Studies ..................... 61 G. Statistical Evaluation ................... 71 H. Conclusion.............................. 71 SELECTED BIBLIOGRAPHY................................. ik VITA ................ 92 vii LIST OF TABLES TABLE PAGE I. Effect of Acid Concentration During the Oxidation-Diazotization Reaction ........... 35 II. Time Study for the Oxidation-Diazotization Reaction at Room Temperature............... 38 III. Temperature Study for the Oxidation- Diazotization Reaction.............. 4l IV. Time Study for the Oxidation-Diazotization Reaction at 60 Degrees Centigrade........... 44 V. Time Study for the Coupling Reaction at 60 Degrees Centigrade...................... 47 VI. Volume Study for the Coupling Reaction .......... $0 VII. Concentration Study; Sulfanilamide, (p-amino- benzenesulfonamide)........................ 53 VIII. Concentration Study; N-(1-Naphthyl)ethyl- enediamine Dihydrochloride ................. 56 IX. Concentration Study; Hydroxylamine Hydrochloride.......................... 59 X. Variation of Absorbance with Concentration of Selenium(lV) for the Adopted Method .... 62 XI. Interference Studies of Diverse Ions ............ 64 XII. Statistical Analysis of Absorbance at Various Levels of Selenium(lV) .................... 72 viii LIST OF FIGURES FIGURE PAGE 1. Absorption Spectra of Various Concentrations of the Coupled Product....... 33 2. Variation of Absorbance with Concentration of Hydrochloric Acid During the Oxidation- Diazotization Reaction.................... 3 6 3. Variation of Absorbance with Time During the Oxidation-Diazotization Reaction ....... 39 4. Variation of Absorbance with Temperature During the Oxidation-Diazotization Reaction................................. 42 5. The Effect of Temperature During the Oxidation-Diazotization Reaction on Standard Curves for the System...................... 43 6. Variation of Absorbance with Time During the Oxidation-Diazotization Reaction at 60 Degrees Centigrade...................... 45 7. Variation of Absorbance with Time During the Coupling Reaction at 60 Degrees Centigrade.......................... 48 8. Variation of Absorbance with Time During the Coupling Reaction at 60 Degrees Centigrade................................ $1 9 . Variation of Absorbance with Concentration of Sulfanilamide (p-aminobenzenesulfonamide) . 5^ 10. Variation of Absorbance with Concentration of N-(1-Naphthyl)ethylenediamine Dihydrochloride............................ 57 11. Variation of Absorbance with Concentration of Hydroxylamine Hydrochloride ............. 60 12. The Standard Curve for the Adopted Method................................... 63 ix ABSTRACT Selenium dioxide has been used extensively as an oxidizing agent in organic chemistry, particularly for the oxidation of alde­ hydes, ketones and unsaturated hydrocarbons. It is well known that selenium dioxide can be used to oxidize hydroxylamine hydrochloride to nitrous acid under acidic conditions. A new spectrophotometric method for the determination of submicrogram quantities of selenium dioxide has been developed based upon this reaction. In a strongly acidic medium, (6.8N hydrochloric acid), even trace amounts of selenium dioxide (as selenious acid) oxidize hydro­ xylamine hydrochloride to nitrous acid when heated at 60 degrees centigrade for a period of 90 minutes. When sulfanilamide is present in the system, diazotization of the amine takes place as the oxida­ tion reaction proceeds. The diazonium salt thus formed is stable under the reaction conditions employed. Subsequent to the oxida- tion-diazotization step N-(l-naphthyl)ethylenediamine dihydrochlo­ ride is added and heating at 60 degrees centigrade is continued for 30 minutes, resulting in the formation of a highly-colored coupling product which has a maximum absorbance at 5^ millimicrons. This approach to the determination of selenium takes advan­ tage of the extreme sensitivity which is inherently present in anal­ ogous procedures for the determination of nitrites. The method therefore provides a means for the spectrophotometric determination of selenium in the 0.01 to 0 .2 parts per million range. The method is sensitive, reproducible and accurate and should be especially useful in air pollution surveys where a knowledge of the absolute concentration of selenium oxides in the atmosphere is most important. CHAPTER I INTRODUCTION Selenium was identified as an element in 1817 by the Swedish chemist, Berzelius, in a residue from the production of sulfuric acid. It was named from the Greek word, selene, meaning the moon, because of its resemblance to tellurium, which had been discovered earlier and was named from the Latin word, tellus, meaning the earth. The chemistry of sulfur, selenium, and tellurium are similar, but their abundance in the earth's crust varies. Sulfur occurs freely in abundant quantities, while selenium and tellurium are rare with an estimated percentage of 10”4 and 10"9, respective­ ly. Intensive explorations in the United States have not been suc­ cessful in finding large deposits of selenium.
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