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Studies of Analytical Separations. Darrell James Donaldson Louisiana State University and Agricultural & Mechanical College

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Studies of Analytical Separations. Darrell James Donaldson Louisiana State University and Agricultural & Mechanical College Louisiana State University LSU Digital Commons LSU Historical Dissertations and Theses Graduate School 1962 Studies of Analytical Separations. Darrell James Donaldson Louisiana State University and Agricultural & Mechanical College Follow this and additional works at: https://digitalcommons.lsu.edu/gradschool_disstheses Recommended Citation Donaldson, Darrell James, "Studies of Analytical Separations." (1962). LSU Historical Dissertations and Theses. 774. https://digitalcommons.lsu.edu/gradschool_disstheses/774 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 63-2768 microfilmed exactly as received DONALDSON, Darrell James, 1935- STUDIES OF ANALYTICAL SEPARATIONS. Louisiana State University, Ph.D., 1962 Chemistry, analytical University Microfilms, Inc., Ann Arbor, Michigan STUDIES OF ANALYTICAL SEPARATIONS 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 D arrell James Donaldson B.S., Loyola University, 1957 August, 1962 ACKNOWLEDGMENT The writer wishes to express his sincere appreciation to Dr. P h ilip W. West under whose d irectio n th is work was performed, for h is h elp fu l guidance during the experimental work and in the preparation of this manuscript. The author would like also to express his thanks to Dr. Maurice M. Vick for his many valuable suggestions and to the National Science Foundation under whose sponsorship part of this work was performed. i i TABLE OF CONTENTS PAGE ACKNOWLEDGEMENT............................................................................................. i i ABSTRACT.................................................................................................................. v i i I. INTRODUCTION .......................................................................................................... 1 I I . EXPERIMENTAL..................................................................................................................14 A. Solvent Extraction of Thiocyanate .............................................. 14 1. Reagents..................................................................................................... 14 2. Procedures........................................................................ 16 3. Factors Involved in the Extraction of Thiocyanate...................................................................................... 19 4. Selectivity.............................................................................................. 24 5. Determination of Thiocyauate in the Organic Phase . 29 6. Recovery..................................................................................................... 29 7. Development of a Procedure for the Separation and Determination of Thiocyanate ........................................... 31 B. Separation and Detection of Antimony ............................................. 32 1. General Considerations ......................................................................... 32 2. Reagents..................................................................................................................33 3. Procedures........................................... .........................................................33 4. Development of a Test for Antimony......................................................39 C. Separation and Detection of Calcium, Strontium and B ariu m...................................................................................................................40 1. General Considerations ......................................................................... 40 2. Reagents..................................................................................................................41 3. Procedures ........................................................................................41 4. Reaction of Calcium with Ferrocyanide ...... 43 5. Analysis Scheme.............................................................................. 47 i i i PAGE I I I . DISCUSSION.................................................................................................. 50 IV. SEUECTED BIBLIOGRAPHY........................................................................... 53 V. APPENDIX ............................................................................ 57 VI. VITA ............................................................................................. 76 O iv LIST OF TABLES PAGE I. Solvent Study..................................................................................................... 19 II. Equilibration Study ...................................................................................... 20 III. Effect of Acidity on Thiocyanate Extraction............................. 21 IV. Effect of Initial Concentration of Thiocyanate on its Extraction .....................................................................................................22 V. Effect of Different Mole Ratios ofZ%CS on the Extraction . 23 VI. Effect of TBP on Extraction of Thiocyanate.......................................... 23 VII. Temperature Effect .............................................................................................. 24 VIII. Effect of KOH Concentraion on the Recovery ;df Thiocyanate...................................................................................................................30 IX. Resin S t u d y....................................................................................................................34 X. Effect of Ammonium Chloride on Precipitation of Calcium . 44 XI. Effect of Ammonium Chloride on Precipitation of Calcium . 44 XII. Effect of Ferrocyanide Concentration on the PteidlpTtatlon of Calcium....................................................................................45 XIII. Acidity............................................................................................................................. 46 XIV. Titrimetric Standardization of Thiocyanate ..................................... 57 XV, Solvent Study................................................................................................................58 XVI. Effect of Acidity on Thiocyanate Extraction A. 0.1M N itric A c i d ................................................................................................59 XVII. Effect of Acidity on Thiocyanate Extraction B. 0.5M N itric A c i d ................................................................................................60 XVIII. Effect of Acidity on Thiocyanate Extraction C. 1M Nitric A cid .....................................................................................................61 XIX. Effect of Acidity on Thiocyanate Extraction D. 1.5M N itric A c i d ................................................................................................62 XX. Effect of Initial Concentration of Thiocyanate on its Extraction A. 0,05 M/1 63 PAGE XXI. Effect of Initial Concentration of Thiocyanate on Its Extraction B. 0.01 M /1 ....................................................................... 64 XXII. Effect of Initial Concentration of Thiocyanate on Its Extraction C. 0.0002 M /1 ...............................................................................65 XXIII. Effect of Initial Concentration of Thiocyanate on Its Extraction D. 0.0001 M /1 ...............................................................................66 XXIV. Temperature Effect A. 20°C ....................................................................... 67 XXV. Temperature Effect B. 40°C ....................................................................... 68 XXVI. Effect of KOH Concentration on Recovery of Thiocyanate A. 0 .5 M ...................................................................... 6 9 XXVII. Effect of KOH Concentration on Recovery of Thiocyanate B. 1M.........................................................................................................70 XXVIII. Effect of KOH Concentration on Recovery of Thiocyanate C. 4M . ................................................................................................71 XXIX. Standardization of Calcium ................................................................................ 72 Graph No. 1: Spectrophotometric Calibration Curve for Thiocyanate....................................................................................73 Graph No. 2: Spectrophotometric Calibration Curve for Z i n c .....................................................................................................74 Graph No. 3: Plot of Log TBP Concentration vs Log Distribution Ratio ....................................................................... 75 v i ABSTRACT Solvent extraction has been extensively applied to the separation of cations but its application to anion separation has been for the most part ignored. The present study was undertaken to determine the conditions under which the extraction of thiocyanate was favorable. Different solutions of thiocyanate were shaken with 1:1 tri-n-butyl phosphate (TBP) - methyl isobutyl ketone (MIBK), and after separation
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