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Methods for the Determination of Chlorine, Hydrogen-Sulfide, and Hydrogen-Cyanide Utilizing Permeation Sampling

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Methods for the Determination of Chlorine, Hydrogen-Sulfide, and Hydrogen-Cyanide Utilizing Permeation Sampling Louisiana State University LSU Digital Commons LSU Historical Dissertations and Theses Graduate School 1981 Methods for the Determination of Chlorine, Hydrogen-Sulfide, and Hydrogen-Cyanide Utilizing Permeation Sampling. James Keith Hardy Louisiana State University and Agricultural & Mechanical College Follow this and additional works at: https://digitalcommons.lsu.edu/gradschool_disstheses Recommended Citation Hardy, James Keith, "Methods for the Determination of Chlorine, Hydrogen-Sulfide, and Hydrogen-Cyanide Utilizing Permeation Sampling." (1981). LSU Historical Dissertations and Theses. 3599. https://digitalcommons.lsu.edu/gradschool_disstheses/3599 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]. INFORMATION TO USERS This was produced from a copy of a document sent to us for microfilming. While the most advanced technological means to photograph and reproduce this document have been used, the quality is heavily dependent upon the quality of the material submitted. The following explanation of techniques is provided to help you understand markings or notations which may appear on this reproduction. 1.The sign or “target” for pages apparently lacking from the document photographed is “Missing Page(s)”. If it was possible to obtain the missing page(s) or section, they are spliced into the Him along with adjacent pages. This may have necessitated cutting through an image and. duplicating adjacent pages to assure you of complete continuity. 2. When an image on the Him is obliterated with a round black mark it is an indication that the film inspector noticed either blurred copy because of movement during exposure, or duplicate copy. Unless we meant to delete copyrighted materials that should not have been Rimed, you will And a good image of the page in the adjacent frame. 3. When a map, drawing or chart, etc., is part of the material being photo­ graphed the photographer has followed a definite method in “sectioning” the material. It is customary to begin filming at the upper left hand comer of a large sheet and to continue from left to right in equal sections with small overlaps. If necessary, sectioning is continued again—beginning below the first row and continuing on until complete. 4. For any illustrations that cannot be reproduced satisfactorily by xerography, photographic prints can be purchased at additional cost and tipped into your xerographic copy. Requests can be made to our Dissertations Customer Services Department. 5. Some pages in any document may have indistinct print. In all cases we have filmed the best available copy. University Microrilnris International 300 N. ZEEB ROAD, ANN ARBOR. Ml 48106 18 BEDFORD ROW, LONDON WC1R 4EJ, ENGLAND 8117629 H a r d y , J a m e s K e it h METHODS FOR THE DETERMINATION OF CHLORINE, HYDROGEN- SULFIDE, AND HYDROGEN-CYANIDE UTILIZING PERMEATION SAMPLING The Louisiana Stale University and Agricultural and Mechanical Ph.D. 1981 Col University Microfilms International300 N. Zeeb Road, Ann Arbor, MI 48106 N^ETHODS f o r t h e determination o f CHLORINE, HYDROGEN SULFIDE, AND HYDROGEN CYANIDE UTILIZING PERMEATION SAMPLING\ 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 xn The Department of Chemistry by James Keith Hardy B.S., Cumberland College, 1973 May, 1981 For M a m a , She worked for this as hard as I did. ii ACKNOWLED G^NTS The author acknowledges with deep appreciation the contribution to this research of Dr, Philip W. West, whose patience, understanding, and guidance enabled him to see his way through the challenges of this work. He is also greatly indebted to the members of the research group for their helpfulness and common sense. The author would like to acknowledge the support given by the National Institute for Occupational Safety and Health, U.S. Public Health Service Grant No. 2 R01 OH 00666-03. t a b l e o f c o n t e n t s PAGE DEDICATION ................................................. ii ACKNOWLEDGMENTS............................................ iii LIST OF TABLES ...................... ..................yiii LIST OF FIGURES. .................................... ix ABSTRACT ................................................. X CHAPTER I INTRODUCTION................................. 1 PART ONE A PERSONAL CHLORINE MONITOR UTILIZING PERMEATION SAMPLING............................. 3 CHAPTER II INTRODUCTION ........................ 4 A. Sources of Chlorine....................... 4 B. Importance and Health Effects............ 5 C. Present Methods........................... 7 D. Development of the Present Method. 8 CHAPTER III EXPERIMENTAL ............. 11 A. Apparatus for Exposure Studies ......... 11 1. Basic Design of Equipment for Chlorine Exposures.................... 11 2. Design and Preparation of Permeation T u b e ....................... 11 3. Calibration and Use of Permeation T u b e ....................... 13 4. Preparation of Standard Chlorine Atmospheres ........................... 15 5. Permeation Device for Preliminary S t u d i e s ................................ 15 6. Humidity Studies....................... 17 7. Temperature Studies ................ 17 8. Interference Studies................... 20 9. Design of the Personal Monitoring Device.................................. 20 B. Reagents and Materials ..................... 22 1. Fluorescein ............................22 2. E o s i n .................................. 22 3. Chlorine................................ 22 4. Fluorescein-Bromide Reagent .... 22 iv PAGE C. Analytic Procedure, 23 CHAPTER IV RESULTS AND DISCUSSION .................. 24 A. Theory of Permeation in Polymers............. 24 B. Determination of the Permeation Constant. 27 C. Experimental Conditions for the Determination of Chlorine .......... 28 D. Effects of Temperature........................ 28 E. Effects of Humidity .......................... 28 F. Response Time . ............................... 31 G. Effects of Absoifcer C o n c e n t r a t i o n.......... 31 H. Effects of Light...............................33 I. Effects of p H ................................. 35 J. Evaporation Study ........................... 37 K. Interferences..................................37 L. Field Tests ....................................40 PART TWO A METHOD FOR THE DETERMINATION OF PERSONAL EXPOSURE TO HYDROGEN SULFIDE......................43 CHAPTER V INTRODUCTION............ 44 A. Sources of Hydrogen Sulfide ................ 44 B. Importance and Health Effects ............. 44 C. Present Methods for the Determination of Hydrogen Sulfide ......................... 46 D. Development of the Present Method ........... 46 CHAPTER VI EXPERIMENTAL . .'........................... 48 A. Apparatus for Exposure Studies............... 48 1. Similarities to Chlorine Studies . 48 2. Preparation and Standardization of Hydrogen Sulfide Tank................ 48 3. Preparation of Standard Hydrogen Sulfide Atmospheres...................48 B. Reagents and Materials.........................49 1. Hydrogen Sulfide ....................... 49 2. Hydrogen Sulfide Prepared Tank .... 49 3. N,N-Dimethyl-p-phenylenediamine. 49 4. Amine-Sulfuric Acid Stock Solution . 49 5. Amine-Sulfuric Acid Test Solution. 49 6. Ferric Chloride Solution . ........... 51 7. Absorbing Solution ................... 51 v PAGE 8, Sulfide standards. 51 C, Analytical Procedure. ...... ......... 51 CHAPTER VII RESULTS AND DISCUSSION................... 53 A. Determination of the Permeation Constant. 53 B. Environmental Effects ................ 55 C. Response Time ................................. 55 D. Sample Stability............................... 55 E. Interferences................................. 62 PART THREE A PERSONAL MONITOR FOR HYDROGEN CYANIDE EMPLOYING PERMEATION SAMPLING ........ 64 CHAPTER VIII INTRODUCTION ........................... 65 A. Sources of Hydrogen Cyanide ................ 65 B. Importance and Health Effects .............. 66 C. Methods for the Determination of Hydrogen Cyanide...............................67 D. Development of the Present Method ........... 68 CHAPTER IX EXPERIMENTAL ............................. 70 A. Apparatus for Exposure Studies............... 70 1. Similarities to Chlorine Studies . 70 2. Design and Calibration of Permeation Tube.......................... 70 B. Reagents and Materials.........................72 1. Hydrogen Cyanide ....................... 73 2. Barbituric Acid...........................73 3. Chloramine T ............................. 73 4. Pyridine-Bai±> ituric Acid Reagent . 73 5. Chloramine T Solution.................... 73 6. Buffer Solution...........................73 7. Cyanide Standard Solutions ............ 73 8. J4> sorbing Solution ...................... 74 C. Analytical Procedure...........................74 CHAPTER X RESULTS AND DISCUSSION...................... 77 A. Determination of the Permeation Constant. 77 B. Effects of Temperature.........................78 C. Effects of Humidity ........................... 79 D. Response Time .................... 79 vi PAGE E. Sample Stability , , , , , , . 83 F. Alternate Analytical Finish, 83 G. Interferences. 86 CHAPTER XI CONCLUSIONS..................................... 89 REFERENCES
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