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Diffusion in Benzoic Acid Single Crybtaj.Ao https://theses.gla.ac.uk/ Theses Digitisation: https://www.gla.ac.uk/myglasgow/research/enlighten/theses/digitisation/ This is a digitised version of the original print thesis. Copyright and moral rights for this work are retained by the author A copy can be downloaded for personal non-commercial research or study, without prior permission or charge This work cannot be reproduced or quoted extensively from without first obtaining permission in writing from the author The content must not be changed in any way or sold commercially in any format or medium without the formal permission of the author When referring to this work, full bibliographic details including the author, title, awarding institution and date of the thesis must be given Enlighten: Theses https://theses.gla.ac.uk/ [email protected] YHACIH SWDim OM WK 80IÆD STATE DwmBiQM m mmoGEM bobbed s o u m à The al 8 «bm itted f o r the degree of D o c t o r ©f philoeophf . .. of. -1 llBlTOrait^r of Glasgow L^OT Roxburgh Me Ghi©o BoB&a AoEoOoBoT* December 1965 ProQuest Number: 10647004 All rights reserved INFORMATION TO ALL USERS The quality of this reproduction is dependent upon the quality of the copy submitted. In the unlikely event that the author did not send a complete manuscript and there are missing pages, these will be noted. Also, if material had to be removed, a note will indicate the deletion. uesL ProQuest 10647004 Published by ProQuest LLO (2017). Copyright of the Dissertation is held by the Author. All rights reserved. This work is protected against unauthorized copying under Title 17, United States Code Microform Edition © ProQuest LLO. ProQuest LLO. 789 East Eisenhower Parkway P.Q. Box 1346 Ann Arbor, Ml 4 8 1 0 6 - 1346 abstract UbbelohdP hps propoeed m protom transfer mechpmism to explgalm oloctrioal conductivity atudio© on p series of crystplllnG organic acids rnd it haa been suggested thrt conductivity increaaes v;ith the degree of co-operrtlve hydro^ion bonding in the crystfilo EKperlmenta have been carried out to teat thi© hypothesis by studying the conductivity and. the rate of proton diffusion^ using tritium bb tracer^ in the same single crystpl© of two organic acids exhibiting different degrees of co­ operative hydrogen bonding? benzoic ecid which exists a cyclic dimer in the solid stete and acetic acid which he© linear chains of co-operative hydrogen bonds extending through the crystalo The acids were purified by distillation^ sublimation and zone refining techniques pnd single crystal© were grown from the melt in a Bridgman ov©n„ Diffusion wrs studied by e sectioning technique using tritium labelled benzoic acetic aeide to obtain the hydrogen diffusion rates \nû carbon-14 labelled - benzoic acid wrs used to mersure the diffusion coefficient of the bulk molecule « The electrical conductivity of benzoic acid vmm ^found to be very low in single crystalSo bein^^ less than 10^^^ ohm*"^ cm%^ 7C^ below the meltim^^ points contrf ry to measurements by IJbbelohde but rgreeing with more recent measurements by Eleyo A proton conductivity was founds however^ in oxrdie acid dihydrate a CO—op errtiv ely hydro^,en bonded pcidg which was comparable th?t found In other hydrogen bonded systems<> A tritium diffusion was observed in benzole aeld whieh was considerably faster then the bulk diffusion mû which could not be explained by a proton diffusion mechMisMo This tritium diffusion was found to vary with the water content in the diffusion cell but a lower limit was obtained which satisfied the Arrhenius equation 4>2o0 ® ® 0»5 _o„4 ' I - HT Diffusion etuiie© in p-terphenyl doped benzoic acid cryatalSp deutero benzoic acid and polycrystallin© benzoic acid have helped to elucidate the meehanism which is believed to be the diffusion of water molecules trapped in the crystals through interstitial dofeetao The carbon-14 bulk diffusion in benzoic acid was found to obey the. following Arrhenius equation « r “ 1 D ® Cl 0 8 ) 3S 1 0 ^^ . ©KP J and can b# explained Im terms of a relaxed vacancy diffusion mechanism o Conductivity and diffusion étudiés in acetic acid were both found to be greatly affected by the presence of moisture and no definite conclusion could be reached regarding proton conductivity in this système AOmOYLUmQMEW£S. The author wiehe© to h is sincere thaKilcs to his supervisor;, Jo Sherwood g for Ma guidance ^ help and oMOuregement throughout this period of research, The axrthor aim wishes to thank MrSc. Ho Fergie for typing the manuscript and his for tracing all diagramso Thanks are also duo to the Scientific Research Council for the award of a maintainano© grant during this course ©f studyo CHAPT'ER I PÜRIP1CATI0W AMD CRÏSTAL GROWTH Xo Introduction <=oc»c=>«=>*=>cae=>ca< 3ato«s.fi^<=5.«»o=>«cjamt=i 3.,^ 2o Purification of Benzoic Acid il a ^ D is tin c tio n CQO<aaot=,C3 CaC3 C3 C=.C=,C=,,^C3 mC=,C3 10 b) %©nO Refining cac=,c 3 C3 a C ;3 c=,c 3 C3 <=,oc=,BaK=,c=,oc=, 2Q 5o Design of Bonzolc Add Cry stale Growing Otom « - - 27 4o Growth of Doped Bonzoia âcid Crystals - -«-«.=>-35 Purity of Bonzosic Add — — — — — « — « — — — — 6q Growth of Acetic Add Crystals — — — — — — — 4 CHAPTER II BÏFFUSSOM ABB COBDÜGTIVITY ŒPKBIMfflTS 1 0 Introduction to JDiffueion — « — — — — « — — — — 49 2 o Préparation of HadioactiTO C=> C=> CT» G> <3 c=a to 3 o Depoeitiom %st©M© W C7 C3 to C3 cs ca to to ito to to ca c=> cr? 4o Bi«4«3Sx^^ion Ann©al Oo^^-itions — — — — « — (64 <^0 Th® ^©c ti osning TocSîUiqu© co — «3c»e=> — c=>c=.c=> — w — — —67 6 0 Determination of Radioactivity In the Crystal Section© 77 7o Preparation of Bi^xusion Samples — — — — — — — — — ©3 Ih© D iffus j>on Xvxporimonts — — — esta — — co — eata, — 0 ^ 4 9o Ih© E3tchang0 Experiments — c^ — iacacsta — cacaacs, ^ 0 5 lOoConductivity Studi© C3 ca cr> cl ;» C:) O CD c cr,> tt> CHAPTER I I I THE RESULTSs AND THEIR INTERPRETATION PAGE 8 Tritium and Carbon 14 Diffusion in Benzoic Acid Single C rystal# 91 b Tritium and Carton 14 Diffusion in PolycrystalliM Benzoic Aeid, vX04 8 Tritium techarjg© between Benzoic Acidy/water Vapour 109 â Tritium Diffusion in Acetic ac M - - - - - - - - - 111 © The Conductivity Studies — « — — — — — — — — — f Tabulated Results — — — — — — — — — — — — — — 117 cmprm IV Discussion op the resoms a Pro tom Transport im Hydrogen Bonded Solid 1 Previous ÇVork — — — — — — — — — — — — — — — — — H© H Gomduo tivity Results — — — coca — — c=,<=,c=,c»(=, 123 h D iffusion im Bomzoio AoM 1 ^uw&&ary of R esults — — — — = — — — — p* — « — — c=. 120 H i-9®l©©ular D^ffu®io m — — — — 130 m Gicaim Boundary DÜ fusion — — — — — — — — 135 IV TritiuFfl D iffusion — — — — — — —— — — — — — 137 ^ Difiusiom 5i,m Aoets.© Ao%d — — — — — — — — — — — — — 144 ^ Oomolusiom — — — — — — — — — 145 ^ i</utur© Work - — — —— — — — — — 1=9 — — — — rimTA LIST OP .ü'IcmRES 1 a Unit cell of benzoic acido b Unit cGl'i of acetic acid* 2 Principle of single crystal growtho 3 Distillation of benzoic acid into growing tabe^ 4 Automa.tio zone refixicr D&Oo 1^ 5 Automatic son© refiner too 2o . 6 Benzoic acid c r i s t a l growing oven.^Oo !« I Temperature g rad ie n ts in c ry s ta l groxving qwu Bo 8 Crystal growing oven 2o 9 Qrysfcal growing v@aeel@o ... 10 'QoVo ©pèctra of p-Tezrphenyl and benzoic aoMo' II Purification and crystal.growth of deuterobenzoio acidp 12 Freezing point apparatus^ 13 Water determination in benzoic acido 14 Tritiation of benzole acMc 15 Vacuum sublimation apparatuso 16 Trltiation of acatie acldo XT Beï.zoic aeid evaparatoTo 18 A cetic acid deposlti on aysternn 19 Diffusion cells„ 20 Thermistor controller,circuito 21 .Fine adjustment chucks 22 Sucli ©ifl apparatuso 23 calibration of benzole acid in cycohaxaneo 24 a Effect of scintillator volxme on tritlxm counting efficiency ’b Effect of benzoic acid on tritium counting efficiencyo 25 Oonciuetivity cells^ 26 Graph of VS for tritium diffusion plane in benzoic acid (large vessels)o 21 Arrhenius plots for tritium anci diffusion in benzoic aod single crystals « ................................................ 28 a^bo urapn Xog^^A’VS ^Ihror tritium aiffuMon Jj (uOl) plan© :ln benzoic acid small' veaselSo 29 Graph VS for tritium diffusion JT( OOl) plan© in benzoic a.crid -under' dry conditioner, 30 Greÿh log^qA VS T^'for tritium diffusion jf (001) plan© in d©xxterobenzoilo acid and p^^TerptonyX doped benzoic acido 31 Graph log^^A VS %^for trltim i diffusion J j (001) plane in benzoic and deuterbbbnzoie. acid simultayxeouely<, . 32 Graph VS g-g^for tritlWa diffusion JT( 001) plane in benzole aeld froBi TH0 vapour^ . 33 a'ptoo Graph logn VS for diffusion (001) plan© in benzoic acMa . ' 34 Graph of’ V8 %^for 0^'^ di.ffusion parallel to {001} plan© i n ’b©ns6ïre acido - *î A 33 Graph of Xogi^â VS for G* ' 'diffusion in benzole' aold. compacte, '36 Graph of logVS % for tritium diffusion in benzoic acid compacts» 31 Arrhenius plots for grain boundary diffusion in benzoic acici compacta 0 ' . ■ - ■ . 36 Graph V8 f€ for ©échange reaction between triti&ted benzoic acid and water vapour« ' ' 39 Arrhenius plot for tritium exchange HgO/benzüic acicVo ' • 40 Graph log^gA VS or tritium diffusion if (100) plan© in acetic acid» 41 AoCo conductit>’ity In benzoic acid compacts^ 42 Time variation of AoO» oonducti’^lty in acetic acid single cry a tale 43 a^^bo AaCo and Bo Co conductivity' In oxalic acid, d'ttj^dr’at©^ 44 Schematic xriew of hydrogen -bonded chains ih cry stals^ INTRODUCTION lo of the physical rncl chemical properties of solids haso imtil recentlyj, been principally confinée to those materials of potential mouatrial importance e^ga aiotelsp semiconducting
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