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I. Gravimetric Determination of Palladium with Di-2-Thienylketoxime

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I. Gravimetric Determination of Palladium with Di-2-Thienylketoxime University of Windsor Scholarship at UWindsor Electronic Theses and Dissertations Theses, Dissertations, and Major Papers 1-1-1968 I. Gravimetric determination of palladium with di-2-thienylketoxime. II. Gravimetric determination of gold with di-2-thienylketoxime. III. Nephelometric determination of gold with di-2-thienylketoxime. Jesse T. Gerard University of Windsor Follow this and additional works at: https://scholar.uwindsor.ca/etd Recommended Citation Gerard, Jesse T., "I. Gravimetric determination of palladium with di-2-thienylketoxime. II. Gravimetric determination of gold with di-2-thienylketoxime. III. Nephelometric determination of gold with di-2-thienylketoxime." (1968). Electronic Theses and Dissertations. 6056. https://scholar.uwindsor.ca/etd/6056 This online database contains the full-text of PhD dissertations and Masters’ theses of University of Windsor students from 1954 forward. These documents are made available for personal study and research purposes only, in accordance with the Canadian Copyright Act and the Creative Commons license—CC BY-NC-ND (Attribution, Non-Commercial, No Derivative Works). Under this license, works must always be attributed to the copyright holder (original author), cannot be used for any commercial purposes, and may not be altered. Any other use would require the permission of the copyright holder. Students may inquire about withdrawing their dissertation and/or thesis from this database. For additional inquiries, please contact the repository administrator via email ([email protected]) or by telephone at 519-253-3000ext. 3208. I GRAVIMETRIC DETERMINATION OF PALLADIUM ' WITH DI-2-THiENŸLKETOXIME . II GRAVIMETRIC DETERMINATION OF GOLD WITH DI-2-THIENYLKÉTOXIME . Ill NEPHELOMETRIC DETERMINATION OF GOLD WITH Di-2-THIENYLKETOXIME. BY JESSE T, GERARD A Dissertation Submitted to the Faculty of Graduate Studies through the Department of Chemistry in Partial Fulfillment of the Requirements for the Degree of Doctor of Philosophy at the University of Windsor Windsor, Ontario 1968 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. UMI Number: DC52621 INFORMATION TO USERS 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 bleed-through, substandard margins, and improper alignment can adversely affect reproduction. In the unlikely event that the author did not send 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. UMI UMI Microform DC52621 Copyright 2008 by ProQuest LLC. All rights reserved. This microform edition is protected against unauthorized copying under Title 17, United States Code. ProQuest LLC 789 E. Eisenhower Parkway PC Box 1346 Ann Arbor, Ml 48106-1346 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Approved / Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. ABSTRACT PART I GRAVIMETRIC DETERMINATION OF PALLADIUM WITH DI-2-THIENYLKETOXIME In this work the reaction between palladium(II) and di-2- thienylketoxime in strong hydrochloric acid solution to form dichlorobis (di-2-thienylketoxime-N, N') palladium(ll) in quantitative yield has been applied to the gravimetric deter­ mination of palladium in the presence of a large number of diverse cations and anions. A statistical comparison has also been made between the developed procedure and the standard dimethylglyoxime procedure for bivalent palladium. The procedure was studied to determine such factors as oxime solubility and complex solubility in acidic alcohol solutions, effect of pH, effect of alcohol concentration, effect of reagent concentration, range of palladium concentration applicable and effect of stirring time. 11 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. PART II , GRAVIMETRIC DETERMINATION OF GOLD WITH DI-2-THIENYLKETOXIME The reaction between di-2-thienylketoxime and gold(ill) ion has been studied in order to set up a gravimetric method for the determination of gold. The precipitate formed was analyzed for carbon hydrogen and gold. The reagent and gold reacted quantitatively to precipitate gold. This fact was used to set up a gravimetric procedure for determining gold in the presence of a large number of diverse cations and anions. A statistical study has also been made on the developed procedure. The procedure was studied to determine such factors as variation of reagent concentration, range of gold concent­ ration applicable, best oven temperature for drying, temper­ ature limits for developing the complex and development time. PART III NEPHELOMETRIC DETERMINATION OF GOLD WITH DI-2-THIENYLKETOXIME In this work the reaction between gold(lll) and di-2- thienylketoxime has been applied to the nephelometric determination of gold. A large number of cations and anions iii Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. were tested. The procedure was studied to determine such factors as effect of gelatin as a stabilizing reagent, effect of pH, time of developing, optimum concentration of reagent, temperature effects, optimum dioxane content and reproducibil­ ity. IV Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. ACKNOWLEDGEMENTS I would like to thank my advisor, Dr. W. J. Holland, for his direction and assistance throughout this research work. I would like to thank my committee for their valuable criticisms in preparing this manuscript. I would also like to thank my wife and children for their inspiration and understanding without which this work could not have been done. Grateful acknowledgement is also due to the National Research Council of Canada for its financial assistance in the form of a scholarship and research grants. Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. TABLE OF CONTENTS Page TITLE PAGE................................... i ABSTRACT.................................. ii ACKNOWLEDGEMENTS....... V TABLE OF CONTENTS. ....... vi LIST OF FIGURES............................... X LIST OF TABLES............................. xi PART I GRAVIMETRIC DETERMINATION OF PALLADIUM WITH DI-2-THIENYLKETOXIME Chapter I INTRODUCTION.................................... 2 II EXPERIMENTAL. .................... 4 1) Materials and Methods................... 4 2) Procedures. ...................... 5 III RESULTS 1) Solubility of Di-2-Thienylketoxime and Dichloro bis(di-2-thienyl- ketoxime-N, N') palladium(II) complex................... • • . ......... 9 2) Study of Variation of Acidity........ 9 3) Study of Variation of Alcohol Concentration.......................... 12 vi Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Chapter Page 4) Study of Variation of Reagent Concentration added.................... 12 5) Study of Variation of Palladium Concentration............... 12 6) Study of Variation of Time of Stirring. ............................... 17 7) Results of the Statistical Study....... 17 8) Effect of Diverse Ions on the Determination of Palladium(ll)......... 21 9) Results of the Elimination of Interferences........................... 21 IV DISCUSSION.................... 25 V SUMMARY AND CONCLUSIONS.................. 29 PART II GRAVIMETRIC DETERMINATION OF GOLD WITH DI-2-THIENYLKETOXIME Chapter Page I INTRODUCTION. ........ 31 II EXPERIMENTAL.................................... 34 1) Materials and Methods................... 34 2) Procedures............................. 35 III RESULTS............................ 38 1) Composition of Gold Complex............ 38 Vll Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Chapter Page 2) Formation of Gold Complex............. 38 3) Study of Variation of Acidity......... 40 4) Study of Variation of Dioxane Concentration.......... 40 5) Effect of Reagent Concentration....... 40 6) Effect of Oven Temperature............ 4$ 7) Variation of Temperature for Complex Formation..................... 45 8) Effect of Gold Concentration on the Procedure............................. 45 9) Results of Foreign Ion Study.......... 45 10) Results of Elimination of Interferences......................... 55 11) Time of Standing...................... 55 IV DISCUSSION.................................... 57 V SUMMARY AND CONCLUSIONS......... 63 PART III NEPHELOMETRIC DETERMINATION OF GOLD WITH DI-2-THIENYLKETOXIME Chapter Page I INTRODUCTION.................................. 65 II THEORY............. 68 III EXPERIMENTAL.................................. 72 vxii Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Chapter Page 1) Apparatus........................... 72 2) Materials and Methods........... 73 3) Procedures.......... 'Jk IV RESULTS.......... ............................... 78 1) Composition of Gold Complexes........... 78 2) Effect of Protective Colloids. ......... 78 3) Study of Variation of Acidity........... 78 4) Effect of Time of Standing........ 80 5 ) Reagent Concentration Study............. 84 6) Effect of Variation of Total Amount of Dioxane.............................. 84 7) Effect of Variation of Temperature.....
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