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The Precipitation of Arsenic from Aqueous Solutions

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The Precipitation of Arsenic from Aqueous Solutions THE PRECIPITATION OF ARSENIC FROM AQUEOUS SOLUTIONS. by Mary Glastras Submitted as part of the requirements for the degree of Doctor of Philosophy. School of Mines The University of New South Wales Australia (1988). SR PT01 Form 1 WAIVER THE UNIVERSITY OF NEW SOUTH WALES DECLARATION RELATING TO DISPOSITION OF PROJECT REPORT /THESIS This is to certify that L......... .ti.9.�........ G!.9..�.'.?. ................................ being a candidate for the degree of... ......P.� .. : .. P........................................................... am fully aware of the policy of the University relating to the retention and use of higher degree project reports and theses, namely that the University retains the copies submitted for examination and is free to allow them to be consulted or borrowed. Subject to the provisions of the Copyright Act, 1968, the University may issue a project report or thesis in whole or in part, in photostat or microfilm or other copying medium. In the light of these provisions I grant the University Librarian permission to publish, or to authorize the publication of my project report/thesis, in whole or in part. I also authorize the publication by University Microfilms of a 350 word abstract in Dissertation Abstracts International (applicable to doctorates only). ii "I hereby declare that this submission is my own work and that, to the best of my knowledge and belief, it contains no material which to a substantial extent has been accepted for the award of any other degree or diploma of a university or other institute of higher learning, except where due acknowledgement is made in the text." iii ACKNOWLEDGEMENT I would like to thank my supervisor Associate Professor R. G. Robins for his encouragement and guidance during the course of this project . iv ABSTRACT Arsenic is an impurity in the processing of many minerals, the more important of which are the sulphide ores. Under natural weathering conditions the arsenic component of these minerals is only slightly soluble, but through chemical processing for the recovery of valuable metals arsenic can be transformed into more soluble and less stable arsenic compounds. With the consumption of arsen1c used for commercial purposes not increasing, and the need for removing the arsenic impurity in the processing of these minerals, increased quantities of arsenical wastes may occur. A safe means of disposing the arsenic has become essential. A review of the literature provides little useful or reliable information on the stability and solubility of the various arsenic compounds which are used or could be used for disposal purposes . For that reason the stability and solubility of various relevant arsenic compounds was investigated. A variety of analytical procedures were used to determine the solubility of the arsenic compounds and the stability of the various dissolved and solid species. These results were developed into standard free energies of formation or complexation constants for these species. The free energies were then used to compute stability diagrams for the particular systems in order to predict v the likely equilibrium conditions over a wider field than was covered in the actual experiments. The stability diagrams are presented in the form of log activity versus pH diagrams and these show the stability regions of the various dissolved species, as well as the solubility and stable regions of solid compounds. The systems investigated were the arsenic(iii) sulphur(-ii) water system, the iron{ii) arsenic{v) water system, and the iron(iii} arsenic(v} water system. These systems were chosen due to their current usage or likely application to finding a suitably stable and insoluble arsenic residual. For the arsenic(iii} sulphur(-ii) water system a log activity versus pH diagram was obtain~d showing the regions of stability for the various dissolved .species and the solid arsenic sulphide {Asz S3) . The iron(ii) arsenic(v) water system was studied in perchlorate and sulphate mediums. Log activity versus pH diagrams 1n both these mediums were obtained showing the solubility and stable regions of the two ferrous arsenates {FeHAs04, and Fe3 {As04)z). The iron(iii) arsenic{v) water system was studied in perchlorate, chloride, nitrate, and sulphate mediums . Log activity versus pH diagrams were obtained showing the solubility and stable region of ferric arsenate {FeAs04) for the perchlorate, chloride, and nitrate mediums. Due to the apparent complexity of the vi sulphate medium no satisfactory model for a log activity versus pH diagram was obtained. The iron arsenic sulphur water system and the iron arsenic water system were also studied. Potential pH diagrams were obtained followed by a number of unsuccessful attempts at the hydrothermal syntheses of arsenopyrite and/or loellingite. From these studies it was determined that the particular arsenic compounds investigated are not as insoluble as has been believed from past studies, and some other means of stablising the arsenic for disposal in residues should be investigated. vii TABLE OF CONTENTS Page no. STATEMENT ii ACKNOWLEGDEMENT iii ABSTRACT iv TABLE OF CONTENTS vii LIST OF FIGURES xi LIST OF TABLES xxii CHAPTER 1. INTRODUCTION 1 1.1 Historical 1 1.2 Uses of Arsenic 1 1.3 Occurrence 2 1.4 Chemistry of Arsenic 4 1.5 Economic Aspects 7 1.6 Industrial ·Applications 9 CHAPTER 2. STABILITY DIAGRAMS 17 2.1 Theory 17 2.2 Arsenic Water System 19 2.3 Sulphur Water System 22 2.4 Iron Water System 22 CHAPTER 3. INSOLUBLE ARSENIC COMPOUNDS 30 3.1 Metal Arsenates/Arsenites 30 3.1.1 Magnesium Arsenic Water System 33 3.1 . 2 Calcium Arsenic Water System 35 3.1.3 Barium Arsenic Water System 42 3.1.4 Ferrous Arsenate Water System 46 3.1.5 Ferric Arsenate Water System 48 viii Page No. 3.2 Other Insoluble Arsenic Compounds 53 3 . 2.1 Arsenic Sulphur Water System 53 3.2.2 Iron Arsenic Sulphur Water System 59 CHAPTER 4. EXPERIMENTAL 64 4.1 Introduction 64 4 . 2 Instrumental Techniques 65 4.2.1 PH Titrations 65 4 .2.2 Spectrophotometric Measurements 66 4.2.3 Turbidity Measurements 67 4.2.4 PH Measurements 67 4.3 Preparation of Solutions 68 4.3.1 Arsenic Solutions 68 4.3.2 Sulphide Solutions _ 70 4 .3.3 Iron Solutions 70 4.3.3.1 Ferric Solutions at an Ionic Strength of 1.0. 71 4.3.4 Carbonate Free Hydroxide Solutions 71 CHAPTER 5. RESULTS AND DISCUSSION 72 5.1 Arsenic(iii) Sulphur(-ii) Water System 72 5.1.1 PH Titrations 72 5 . 1 . 2 Spectrophotometric Measurements 72 ix Page No. 5.1.3 Discussion 75 5.2 Iron(ii) Arsenic(v) Water System 84 5.2.1 PH Titrations 84 5.2.1.1 Perchlorate Medium 84 5.2.1.2 Sulphate Medium 86 5.2.2 Discussion 88 5.3 Iron(iii) Arsenic(v) Water System 102 5.3.1 PH Titrations 102 5.3.1.1 Perchlorate Medium 108 5.3.1.2 Sulphate Medium 108 5.3.2 Turbidity Measurements 111 5.3.2.1 Perchlorate Medium 114 5.3.2.2 Chloride Medium 114 5.3.2.3 Nitrate Medium 118 5.3.2.4 Sulphate Medium 118 5.3.3 Influence of Ionic Strength 122 5.3.3.1 Nitrate Medium 127 5.3.4 Spectrophotometric Measurements 127 5.3.4.1 Perchlorate Medium 130 5.3.4.2 Sulphate Medium 130 5.3.5 Discussion 133 5.4 Arsenopyrite (FeAsS) and Loellingite (FeAs2) 154 CHAPTER 6. CONCLUSION 161 CHAPTER 7 . REFERENCES 165 APPENDIX 1 182 X Page No. APPENDIX 2 184 APPENDIX 3 185 APPENDIX 4 186 APPENDIX 5 187 xi LIST OF FIGURES Page No. CHAPTER 2 2.1 Potential pH diagram for the arsenic water system at 25°C. 21 2.2 Log activity pH diagram for the arsenic(iii) hydroxy species. 23 2.3 Log activity pH diagram for the arsenic(v) hydroxy species. 24 2.4 Potential pH diagram for the sulphur water system at 25°C. 25 2.5 Potential pH diagram for the iron water system at 25°C . 28 CHAPTER 3 3.1 Solubilities of some metal arsenic(v) compounds from Chukhlansev. 31 3.2 Solubilities of some metal arsenic(iii) compounds from Chukhlansev. 32 3.3 The variation of arsenic(v) and magnesium concentrations with pH in equilibrium with Mg3 (As04) 2 at 25° C. 34 xii Page No. 3.4 Log activity pH diagram for the magnesium arsenic(v) water system. 36 3 . 5 The solubility of calcium arsenate (Ca3 (As04) 2) at various pH's. 37 3 . 6 The variation of arsenic(v) and calcium concentrations with pH in equilibrium with Ca3 (AS04) 2 at 25° C. 39 3.7 Log activity pH diagram for the calcium(ii) arsenic(v) water system. 43 3 . 8 Log activity pH diagram for the calcium(ii) arsenic(iii) water system. 44 3.9 Log activity pH diagram for the barium(ii) arsenic(v) water system. 47 3 . 10 Log activity pH diagram for the iron(ii) arsenic(v) water system. 49 3.11 The variation of arsenic(v) and iron(iii) concentrations with pH in equilibrium with FeAs04 at 25°C. 52 xiii Page No . 3 . 12 Log activity pH diagram for the iron(iii) arsenic(v) water system. 55 3.13 Potential pH diagram for the arsenic sulphur water system. 58 3.14 Potential pH diagram for the iron arsenic sulphur water system. 60 3.15 Potential pH diagram for the iron arsenic sulphur water system at 25° c at concentrations for iron, arsenic, and sulphur at lQ- 3, 10- 6 , and 10- 4 M respectively. 62 3.16 Potential pH diagram for the 1.ron arsenic sulphur water system at a c oncentration of unity for all species.
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