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Ultraviolet Emission and Absorption Spectra Produced by Organic Compoundsin Oxyhydrogen Flames

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Ultraviolet Emission and Absorption Spectra Produced by Organic Compoundsin Oxyhydrogen Flames Louisiana State University LSU Digital Commons LSU Historical Dissertations and Theses Graduate School 1969 Ultraviolet Emission and Absorption Spectra Produced by Organic Compoundsin Oxyhydrogen Flames. Vega Jean ott mithS Louisiana State University and Agricultural & Mechanical College Follow this and additional works at: https://digitalcommons.lsu.edu/gradschool_disstheses Recommended Citation Smith, Vega Jean ott, "Ultraviolet Emission and Absorption Spectra Produced by Organic Compoundsin Oxyhydrogen Flames." (1969). LSU Historical Dissertations and Theses. 1692. https://digitalcommons.lsu.edu/gradschool_disstheses/1692 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 70-9092 SMITH, Vega Jean Ott, 1937- ULTRAVIOLET EMISSION AND ABSORPTION SPECTRA PRODUCED BY ORGANIC COMPOUNDS IN OXYHYDROGEN FLAMES, The Louisiana State University and Agricultural and Mechanical College, Ph.D., 1969 Chemistry, analytical University Microfilms, Inc., Ann Arbor, Michigan ULTRAVIOLET EMISSION AND ABSORPTION SPECTRA PRODUCED BY ORGANIC COMPOUNDS IN OXYHYDROGEN FLAMES 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 Vega Jean Smith B.S.j University of Alabama, 1959 August, I9 6 9 ACKNOWLEDGEMENTS The writer would like to take this opportunity to express thanks to Professor James W. Robinson for the direction of this research. In addition she would like to express sincere appreciation to the faculty and staff of the Chemistry Department at Louisiana State University for their teaching, encouragement, and assistance. Of the technical staff in particular she would like to thank Mr. J. R. Hoffman, Mr. G. H. Sexton, and Mr. E. T. Keel. The loan of an Atomic Absorption Instrument by Beckman Instru­ ments, Inc. is gratefully acknowledged. "Thus it will be found that, in general, Salts of soda give a copious and purely homo­ geneous yellow. Salts of potash give a beautiful pale violet... Salts of strontia give a magnificent crimson. If analyzed by the prism two definite yellows are seen, one of which verges strongly to orange... Salts of copper give a superb green, or blue green. Salts of iron (protoxide) give white, where the sulphate was used... The colours thus communicated by the different bases to flames, afford in many cases a ready and neat way of detecting extremely minute quantities of them;..." Herschel, J.F.W., Encyclopedia Metropolitana. p. kjQ, J.J. Griffen, London, 18^8. iii TABLE OF CONTENTS Page INTRODUCTION........................................................... 1 A. GENERAL REVIEW OF FLAMES AND FLAME PROCESSES.......... 1 1. General Background................................... 1 2. Flame Spectroscopy................................... 1 3. Some Energy Aspects of Flames...................... 3 k. Chemical Reactions in Flames....................... 6 B. GENERAL REVIEW OF THE USE OF FLAMES IN CHEMICAL ANALYS IS.................................................... 8 1. Flame Photometry...................................... 8 2. Atomic Absorption.................................... 11 3. Atomic Fluorescence.................................. 17 k. The Determination of Nonmetals by Flame Photometry and Atomic Absorption.................. I9 5. The Use of Organic Solvents in Flame Photome­ try, Atomic Absorption, and Atomic Fluores­ cence.................................................. 21 6. Reducing Flames and Chemiluminescence............ 23 C. PURPOSE OF THE INVESTIGATION REPORTED IN THIS THESIS. 2k DESCRIPTION OF EXPERIMENTAL CONDITIONS............................ 26 A. DESCRIPTION OF THE EQUIPMENT............................. 26 B. ORGANIC COMPOUNDS STUDIED................................. 28 C. PROCEDURE................................................... 29 iv TABLE OF CONTENTS (Cont'd) Page RESULTS AND DISCUSSION................................................. 31 A. EMISSION SPECTRA.................... 31 1. Wavelengths of Band Maxima and Identification of the Species Emitting............................. 2. Comparisons of Emission Spectra Produced by Different Solvents............. 46 3. Emission Profiles for Fragments..................... J2 4. Sensitivity Estimates for Emission Bands Pro­ duced by Excited NH and CH Fragments.............. 79 5 . Effects of Varying the Hydrogen to Oxygen Ratio in the Flame on the Emission Spectra.............. 79 6. Effects of Aspirating with Hydrogen instead of Oxygen on the Emission Spectra...................... 8 7 B. ABSORPTION SPECTRA.......................................... 8 8 1. Wavelengths of Band Maxima and Identification of the Species Absorbing............................ 8 8 2. Comparisons of Absorption Spectra Produced by Different Solvents................................ 102 3. Absorption Profiles for Fragments.................. 140 4. Absorption of Atomic Lines by Flames and by Organic Solvents...................................... 146 SUMMARY.................................................................. 169 REFERENCES............................................................... I7I v LIST OF TABLES TABLE PAGE I. Emission Bands Produced by the Oxyhydrogen Flame........ 31 II. Emission Bands Produced when Hydrocarbon Compounds or Organic Compounds Containing Oxygen were Sprayed into the Flame...................................... 33 III, Emission Bands Produced when Compounds Containing Nitrogen were Sprayed into the Flame..................... 36 IV. Emission Bands Produced when Compounds Containing Phosphorus were Sprayed into the Flame................... 37 V. Emission Bands Produced when Organic Compounds Con­ taining Sulfur were Sprayed into the Flame.............. 38 VI. Emission Bands Produced by Oxyhydrogen Flames into which Organic Compounds were Sprayed............... 4U VII. Solvent Aspiration Rates........ ............................ A 7 VIII. Absorption Bands Produced by the Oxyhydrogen Flame jk IX. Absorption Bands Produced when Hydrocarbon Compounds or Organic Compounds Containing Oxygen were Sprayed into the Flame................................................ 9 8 X. Absorption Bands Produced when Compounds Containing Nitrogen were Sprayed into the Flame..................... 97 XI. Absorption Bands Produced when Compounds Containing Phosphorus were Sprayed into the Flame.................... 100 XII. Absorption Ba.nds Produced when Organic Compounds Containing Sulfur were Sprayed into the Flame............ 102 XIII. Absorption Bands Produced by Oxyhydrogen Flames into which Organic Compounds were Sprayed................. 103 XIV. Absorption of Atomic Resonance Lines by Oxyhydrogen Flames into which Organic Solvents were Sprayed..........I55 XV. Emission Signals from Unmodulated Flames......,..,..... 160 XVI. Absorption of Atomic Resonance Lines by Solvent Sprays....................... 161 LIST OF FIGURES FIGURES PAGE 1. Flame Emission Spectrum Produced by Manganese Superimposed on the Background Emission from the Oxyacetylene Flame........................................ 12 2. Diagram of the Equipment Used................................. 27 3. Emission Produced by Excited Water Molecules in the Oxyhydrogen F lame ..... 3^- U. Emission Bands Produced by Excited CH and C2 Fragments... 35 5. Emission Bands Produced by Excited CN and NO Fragments... k-0 6 . Emission Bands Produced by Excited PO Fragments........... ^1 7. Emission Bands Produced by Excited PO Fragments............ k-2 8. Emission Bands Produced by Excited CS Fragments........... k-J 9- Emission Produced by Excited CC1 Fragments................. 4 3 10-a. Emission Spectrum of the Oxyhydrogen Flame at a Height of 0.75 cm............................................. 50 10-b. Flame Emission Spectrum of Benzene at a Height of O .7 5 cm.......................................................... 51 10-c. Flame Emission Spectrum of Butyl Alcohol at a Height of 0.75 cm.............................................. 52 10-d. Flame Emission Spectrum of Pyridine at a Height of 0 .7 5 cm.......................................................... 53 10-e. Flame Emission Spectrum of Tributyl Phosphate at a Height of 0.75 cm............................ ............... 10-f. Flame Emission Spectrum of Thiophene at a Height of 0 .7 5 cm....................................................... 55 11-a.. Emission Spectrum of the Oxyhydrogen Flame at a. Height of 2 cm.................................................. 56 11-b. Flame Emission Spectrum of Benzene at a Height of 2 cm.............................................................. 57 11-c. Flame Emission Spectrum of Butyl Alcohol at a Height of 2 cm.......................................................... 58 vii FIGURES PAGE 11-d. Flame Emission Spectrum of Pyridine at a Height of 2 cm ,................................................... 59 U-e. Flame Emission Spectrum of Tributyl Phosphate a t a. Height of 2 cm........................................... 60 11-f. Flame Emission Spectrum of Thiophene at a Height of 2 cm.............................................................. 61 12-a. Emission Spectrum of the Oxyhydrogen Flame at a Height of 3 cm............ 62
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