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A System for the Qualitative Analysis for the Rare Elements by a Non-Sulfide Ches Me

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Louisiana State University LSU Digital Commons LSU Historical Dissertations and Theses Graduate School 1957 A System for the Qualitative Analysis for the Rare Elements by a Non-Sulfide cheS me. Archie Oliver Parks Jr Louisiana State University and Agricultural & Mechanical College Follow this and additional works at: https://digitalcommons.lsu.edu/gradschool_disstheses Recommended Citation Parks, Archie Oliver Jr, "A System for the Qualitative Analysis for the Rare Elements by a Non-Sulfide cheS me." (1957). LSU Historical Dissertations and Theses. 220. https://digitalcommons.lsu.edu/gradschool_disstheses/220 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]. A SYSTEM FOR THE QUALITATIVE ANALYSIS FOR THE RARE ELEMENTS BY A NON-STTIFIDE SCHEME A Dissertation Submi tied to the Graduate Faculty of the V' isd me State Un;versity and Agricultural and Mechanical College in partial fulfillment of the recmirements for the degree of Doctor of Philosophy in The Department of Chorrj - '^ry by Archie Oliver Parks, Jr. B.S., Sul Ross State College, 19U2 .A., Southwest Texas State Teachers College, 1 August, 1957 ACKNOWLEDGMENT The author ie indebted to Dr. Philip W. West, under whose direction this work was carried out, for his patience, encouragement and assistance during the course of this investigation. He is also indebted to Dr. 3uddhadev Sen, Father W. J. Rimes, and to Mr. George Lyles for their encouragement and stimulating interest in the details of the work. Furthermore, he wishes to express his extreme gratitude to Mrs. Virgia C. Parks whose patience, tolerance, and moral support were indis­ pensable. ii TABLE OF CONTENTS Chapter Page I INTRODUCTION............................................ 1 II EXPERIMENTAL PART...................................... 8 III THE SEPARATION OF TOE ELEMENTS INTO GROUPS.............. 21 The Separation of the Selenium Group................. 22 The Separation of the Osmium Group................... 23 The Separation of the Formic Acid Group.............. 2h The Separation of the Thiocyanate Group.............. 25 The Separation of the Basic Benzoate Group........... 28 The Separation of the Fluoride Group................ 29 The Separation of the Hydroxide Group..................29 The Residual Group................................... 29 IV THE SELENIUM GROUP...................................... 32 V THE OSMIUM GROUP........................................ 37 The Separation and Identification of Osmium........... 37 The Separation and Identification of Ruthenium....... 39 TL THE FORMIC ACID GROUP................................... U2 The Tantalum Sub-Group................................ U3 The Tungsten Sub-Group................................ 52 The Gold Sub-Group................................... 55 VII THE THIOCTANATE GROUP................................... 60 VIII THE BASIC BENZOATE GROUP................................. 66 The Separation and Analysis of the Rare Earth Sub-Group.......................................... 71 The Separation and Analysis of the Iron Sub-Group.... 77 The Separation and Analysis of the Aluminum Sub- Group.............................................. 81 iii The Analysis of the Chranlun Sub-Group................... 86 IX THE FLUORIDE GROUP...................................... 93 X THE HYDROXIDE GROUP....................................... 100 XI THE RESIDUAL GROUP........................................ 106 H I THE AUCALT GROUP.......................................... Ill LIST OF REAGENTS AND TEST SOLUTIONS REQUIRED FOR EACH GROUP.............................................. 118 GENERAL LIST OF REAGENTS AND TEST SOLUTIONS................ 122 LIST OF SPECIAL REAGENTS................................... 125 BIBLIOGRAPHY............................................... 127 VITA........................................................ 132 !▼ LIST OF TABULAR OUTLINES I The Separation of the Eleaenta Into Groups............ 20 II The Selenium Group..................................... 31 III The Formic Acid Group (Tantalum Sub-Group)............. Ul IV The Tungsten Sub-Group................................. 51 V The Gold Sub-Group..................... ................. 5U VT The Thiocyanate Group........ 59 VII The Basic Bensoate Group................................ 65 VIII The Rare Earth Sub-Group................................ 70 II The Iron Sub-Group...................................... 76 X The Aluminum Sub-Group............... 80 XI The Chroaium Sub-Group.................................. 85 H I The Fluoride Group..................................... 92 H I T The Hydroxide Group.................................... 99 H V The Residual Group..................................... 105 XV The Alkali Group....................................... 110 ABSTRACT The non-sulfide qualitative analysis scheme of West, Vick, and LeRosen has been expanded into a system of cation analysis which includes twenty-nine additional elements. The methods devised have been combined with the applicable procedures of Noyes and Bray to introduce provisions for the detection of selenium, germanium, osmium, ruthenium, molybdenum, vanadium, tungsten, tellurium, tantalum, niobium, gold, zirconium, titanium, platinum, palladium, rhodium, iridium, thallium, scandium, yttrium, lanthanum, cerium, thorium, all the other rare earth elements, beryllium, indium, gallium, uranium, rubidium, and cesium. The elements are separated into the following groups: 1. The Selenium Group - Selenium, arsenic, and germanium. 2. The Osmium Group - Osmium and ruthenium. 3. The Formic Acid Group - Antimony, bismuth, molybdenum, tin, vanadium, tungsten, tellurium, tantalum, niobium, zirconium, titanium, gold, mercury, platinum, palladium, rhodium, and iridium. U. The Thiocyanate Group - Silver, lead, thallium, and copper. 5, The Basic Benzoate Group - Scandium, yttrium, lanthanum, cerium, thorium, all other rare earth elements, aluminum, beryllium, Indium, gallium, iron, bismuth, zirconium, titanium, chroaium, uranium, rhodium, and iridium. 6. The Fluoride Group - Magnesium, barium, strontium, and calcium. 7* The Hydroxide Group - Cadmium, manganese, cobalt, and nickel. vi 8. The Residual Oroup - Zinc, tellurium, molybdenum, beryllium, tungsten, and vanadium. 9* The Alkali Group - Lithium, sodium, potassium, rubidiun, cesium, and the ammonium ion. The Formic Acid and Basic Benzoate Groups are divided into sub­ groups in order to facilitate the identification of the elements. The sub-groups of each of these two groups along with the elements present in each are given below. 1. The Formic Acid Oroup. a. The Tantalum Sub-Group - Tantalum, titanium, niobium, zirconium, bismuth, and vanadium. b. The Tungsten Sub-Group - Tin, antimony, tungsten, molyb­ denum, tellurium, and vanadium. c. The Gold Sub-Group - Gold, mercury, platinum, palladium, rhodium, and iridium. 2. The Basic Benzoate Group. a. The Rare Earth Sub-Group - Scandium, indium, thorium, cerium, lanthanum, yttrium, and the other rare earths. b. The Iron Sub-Group - Iron, bismuth, titanium, and zirconium. c. The Aluminum Sub-Group - Aluminum, beryllium, and gallium. d. The Chromium Sub-Group - Chromium, uranium, rhodium, and iridium. The existence of a non-sulfide scheme of analysis which retains all the pedagogical advantages of the traditional system, but lacks many of its inherent disadvantages, should result in added emphasis being placed on the presentation of qualitative analysis to first year students. The availability of an expanded system based on the same approach which vii Is suitable for presentation to advanced students should Increase the rate of adoption of this scheme. viii A SYSTEM FOR THE QUALITATIVE ANALYSIS FOR THE RARE ELEMENTS BY A NON-SULFIDE SCHEME CHAPTER ONE INTRODUCTION The problem of teaching the chemistry of the metal ions would be a difficult one indeed if the material were presented to the student in a direct fashion. The primary difficulty would lie in the great manber of isolated facts, with no immediate application of this information, which would be presented to the student. More­ over, the formulation of sufficiently detailed laboratory exercises to demonstrate the properties of all the elements would be a formi­ dable if not impossible task. The effect on the student would be the stifling of his interest at the precise moment when he is in need of his greatest amount of motivation. A solution to the problem of teaching this phase of inorganic chemistry to which instructors have resorted for decades is to present it under the guise of qualitative analysis. By the study of a systematic scheme of analysis, the student becomes familiar with the chemical properties of the various elements, and is stim­ ulated by the experience of seeing the immediate application of his knowledge to the solution of chemical problems. The fundamentals of chemical equilibria are illustrated in the laboratory in such a manner that the degree of retention is high. Therefore, the student learns the material in an organized and connected fashion, witnesses 1 2 the Immediate application of his knowledge of the chemical properties of the elements and of chemical equilibria, acquires the laboratory techniques required in subsequent courses, and, above all, is moti­ vated instead of being repelled at a time which is most
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  • Formation of Niobium Oxides by Electrolysis from Acidic Aqueous Solutions on Glassy Carbon

    Formation of Niobium Oxides by Electrolysis from Acidic Aqueous Solutions on Glassy Carbon

    Macedonian Journal of Chemistry and Chemical Engineering, Vol. 38, No. 1, pp. 39–48 (2019) MJCCA9 – 767 ISSN 1857-5552 e-ISSN 1857-5625 Received: November 13, 2018 DOI: 10.20450/mjcce.2019.1623 Accepted: February 1, 2019 Original scientific paper FORMATION OF NIOBIUM OXIDES BY ELECTROLYSIS FROM ACIDIC AQUEOUS SOLUTIONS ON GLASSY CARBON Nataša M. Vukićević1*, Vesna S. Cvetković1, Ljiljana S. Jovanović2, Miroslav M. Pavlović1, Jovan N. Jovićević1 1Institute of Chemistry, Technology and Metallurgy, National Institute, Department of Electrochemistry, University of Belgrade, Njegoševa 12, Serbia 2Faculty of Science, Department of Chemistry, Biochemistry and Environmental Protection, University of Novi Sad, Trg Dositeja Obradovića 3, Serbia [email protected] In this study niobium oxide films were formed without peroxo-precursors from three different mixed acidic aqueous solutions on glassy carbon. Linear sweep voltammetry and potential step were techniques used for electrochemical experiments. The simultaneous and consecutive electrochemical re- duction of water, nitrate and sulphate ions provided an alkaline environment with oxygen in the near vi- cinity of the working cathode, which in combination with the present niobium ions, produced niobium oxides and/or oxyhydroxides on the glassy carbon substrate. The formed deposits were analyzed using scanning electron microscopy and energy dispersive spectroscopy and appear to consist of NbO, NbO2 and Nb2O5. Both the niobium and acid concentration of the electrolytes used influenced the morphology and particle size of the deposits. The formation of niobium-fluoride and hydrogen-niobiumoxide com- plexes is addressed. Key words: electrochemical deposition; niobium oxides; acidic solution; glassy carbon ФОРМИРАЊЕ НА ФИЛМОВИ ОД ОКСИДИ НА НИОБИУМ СО ЕЛЕКТРОЛИЗА ОД КИСЕЛИ РАСТВОРИ НА СТАКЛЕСТА ГРАФИТНА ЕЛЕКТРОДА Во овој труд е изучувано формирањето на филмови на оксиди од ниобиум што се одвива без пероксидни медијатори од три различни водни раствори со различни рН вредности на стаклеста графитна електрода.