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Lawrence Berkeley National Laboratory Recent Work Lawrence Berkeley National Laboratory Recent Work Title KINETICS OF FORMATION OF XENON FLUORIDES Permalink https://escholarship.org/uc/item/1r75j047 Author Weaver, Clayton Fred. Publication Date 1966-09-01 eScholarship.org Powered by the California Digital Library University of California ; •. .. (\"'· .. '!\>:·.. ."-·: 1wo >i; E~·K ·-Loi\~ ··&t~<P\ 7 ~· _. f;. This is a library Circulating Cop~ which ma~ be borrowed for two. wee~s. For a personal retention ·copy, call Tech. Info. Division, Ext. 5545 ~~ ~ ~~-~l~~~(~~~:)(~:50xCr?.~>~,~~~t:;~~Ci~;~)~~=tf0>l~~~~~(~~~1_~l~~n~ DISCLAIMER This document was prepared as an account of work sponsored by the United States Government. While this document is believed to contain correct information, neither the United States Government nor any agency thereof, nor the Regents of the University of California, nor any of their employees, makes any warranty, express or implied, or assumes any legal responsibility for the accuracy, completeness, or usefulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any specific commercial product, process, or service by its trade name, trademark, manufacturer, or otherwise, does not necessarily constitute or imply its endorsement, recommendation, or favoring by the United States Government or any agency thereof, or the Regents of the University of California. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States Government or any agency thereof or the Regents of the University of California. · ·.,!· Special Thesis II \ _____ -- -------- ---- UCRL-17169 :~. UNIVERSITY OF CALIFORNIA LawTence Radiation LaboTatoTy Berkeley, California AEC Contract No. W~7405-eng-48 KINETICS OF FOPMATION OF XENON FLUORIDES Clayton Fred Weaver (Ph.D. Thesis) September 1966 :i (·•. ,,·• ::{·•.' J'J~~>f.:c; 'I KINETICS OF FORMATION OF XENON FLUORIDES Clayton Ji'red Weaver Inorganic Materials Research Division, Lawrence Radiation Laboratory, Department of Chemistry, University of California Berkeley, California September 1966 ABSTRACT 'I.'he temperature dependence of the near ultraviolet :n.·gion of tlle absorption spectra of F and XeF was determined to I+C)0°C in fluorillatecl 2 2 nickel cells wj.th calcium fluoride windows. That of XeF was determiner] 1j. to 250° C. This spectral informatj_on was used to study the ldn.et.ics of the formation of XeF and XeF in the same temperature regions and in 2 4 the same. temperature regions and in the same nickel cells. Experimental conditions were chosen to cause the reactions to ter- minate at XeF or XeF as desired. With a total pressure of reactants 2 4 in the 10 to 4o rmn range and Xe to F ratios of 10 or more the reaction 2 Xe + F ~ XeF .occurred. Under these conditions the reaction was zero 2 2 order in Xe and first order in F over the temperature range 190 to ~·00° C. 2 With total reactant pressures of 10 to 20 rmn and F to Xe ratios of 16 or 2 more the reaction Xe + 2F ~ XeF occurred with XeF as an intermt;cliate. 2 4 2 Under these conditions in the temperature range 190 to 250°C the formation of XeF was zero order in F and first order in Xe, just the opposite of the 2 2 results above. 'l'he formation .of XeF was zero order in F and ,first order 4 2 in XeF~. In all cases studied the reaction :rates were independent of tl1e con- centration of· inert gas which was argon but were reduced by an increased volume to surface ratio. Hence the reactions were heterogeneous, even tl1ollp;r1 they wr;re very re:prodttcible. The actjvation energ:Len were 1miforrn I :v low ranging from 12.8 to 15.7 kcal/mole in this study compared with 10.2 kcal/mole reported by Baker and Fox, who studied the formation of XeF on 2 1 nickel wires with the higher Xe and F pressures of 300 nun each (Nature 2 f. 204, 466 (1964) ). It w·as found that the manometer oil, Cl(CF CJ<'Cl) cl, 2 5 acted as a poison for the fluorinated nickel ca.talyst reducing all ob- served reaction rates' by more than an order of magnitude. A mechanism involving adsorption and dissociation of F on the NiF 2 2 surface is proposed. It yields the zero order reaction rate dependence on both reactants observed by Baker and Fox, each of the three rate ex~ pressions obtained experimentally in this study, and predicts that a rate expression first order in both Xe and F should be observed at very low 2 pressures of both Xe and F • It also indicates that the observed decrease 2 in the activation energy of the rate constants with increased F2 pressures is to be expected. / l 1 Page Ia:bi'04eoti1on 1 ·• ' . ' Apparatus 14 .. k$tr·ia1•:'. 21 St>eot.:ra 22 nurlft;e. 22 XtbtOn D1tluor14e 29 . ' Xend: ..fe.,~uon4• )2 n.r~a•. r Theeret1cal A:r:ial7818 35 K1ne,1cs.Prooectu.re )6 .M~lcal. Operattoa )6 .A'baeno.e ett x.m.on Bexatlttor14e )8 :Gezter&l Bq•tlou• J9 <!. ·D1:abllsa1<m. of JTG'blem:a 41 The .aeaot1on ot x.cm and Plltor1ne 1a.Jxc•sa xenon 4S T!le. :a.aetletl X$·+ P ~ X1JP a Geaeral .<brlt1derat1al 2 2 45 'Vartab1e De]M1'ldenoe 46 · the .aeao•'-On of Xenon and Flu.or1ne in Blteue .Fluorine· 5:3 The B•etlon ·xe + 21' ~ x.t4a General · :Gcma!~tlona 2 Var1a\)l.e Depeu-oe 'to.r Xe + P2 :;:::::!: XeP 2 ''55 The Reaot1on XeP :;;;:::::':: XeF4 ·· 2 + r 2 sa 11 j Contents (Oont§.) 1 I Page ll I Poisoning of the Catalyst 60 ,I Equi~ibrium Constants 61 Discussion 63 Integrated Bate Expressions 63 Mechanism 65 Miscellaneous 69 Acknowledgements 71 I I Appendix 72 I l Bibliography 103 I II I ' i --:. I I .! .1 ·--.. I I I l<:~-: -~1 I I . I '! I ! l I 111 Table JSjY,l!be,r Equilibrium Constants for the Xenon-Fluorine system 2 li.. F.Uthalpy and Entropy of :Formation o:f the Xenon Fluoride Compounds III. Bond Energies of Fluorine and the Xenon FluGrides 7 IV .. 'rhermal Excitation of Fluorine 24 Absorption Ooaff1o1ents of Fluorine 26 VIo Beer's tm.w ' Dat81 for Fluorine at 2918 X 28 VII, Absorption Coefficients ot Xenon Difluoride 31 VIII .. Absorption Coefficients of Xenon Tetrafluoride 34 IX. Detln1 t1(!)n of Symbols 40 IX.e.. Bat~ Constants 46 Bate Constants .50 XI. Aettvaticm Energ-1esan4 Pre-exponential Paotors 52 XII. 'f.h..e Bate Constant k4 59 XIII. EquJ11b:r1um Constant Data at !S0°0. 62 XIV. Def'~n1 t1cm of SYlUbols 66 xv. Deri·ved Bate Express1C)ns 6? I ,I ~ i I Figure I Numbe.r A!tle 1.. ~uil1br1w:n Constants for "I the Xenon Fluorides 3,4 1 2. Vapor Pressures for the Xenon :FlVtorides 8 ). Spectra at 2J0 c. 9 4. Block Diagram of Apparatus 15 5. Response Curves of Apparatus 17 6 .. Typical Response CUrve for the Reaction of Xenon and Fluorine 1n Excess Xenon 19 Petential Energy Diagram for Fluorine 23 Fluortne Spectra 25 9. Beer' s Law Plot for Fluorine 27 10. Xenon D1tluor1de Spectra 30 11. Xenon Tetrafluoride Spectra 33 12 .. Typical h1r of Response Curves for the Reaction of Xenon and Fluorine tn Excess Fluorine lJ, . Typical Set ot Concentration CUrves fer the Reaction of Xenon ·.· and Fluorine in Excess Xenon .,\.i i I 14. Typical :Fluorine Behavtor for the i' Reaction of Xenon and Fluorine _j ~ in Excess Xenon 48 j v F1gqres (COntd.) ll 1 Figure Number l'itle 1,5. Arrhenius Plots for the Rate Constants 51 16. Typical Set of Concentration Curves for the Reaction of Xenon and Fluorine 1n Excess Fluorine 56 Typical XsnGn Behavior for the Reaction of Xenon and Fluorine in Exoese Fluorine 57 1 lHIBQRY9'£ION The problem was to determine the kinetics of the formation or xenon difluoride and xenon tetrafluoride by observing the change 1n absorption of near ultraviolet light. To aoeomplish the kinetics study it ~~s necessary to make a prior investigation ot the temperature depend• enee of the spectra of fluorine, xenon difluoride and xenon tetrafluoride in the near ultraviolet region. Except for very recent work a comprehensive review of fluorine-xenon chemistry may be found in references 1 and 2. The portion of the literature pertinent to this work is outlined here. Further details are discussed in the appropriate sections. The reactions Xe I' XeF 1 • XeF F :;;c-::: + 2 = ~ J, 2 + 2 :~ XeF 1 o3-6 and XeF + F ~XeF 1 • have been reported 4 4 2 6 as well as the equilibrium conetants1•? shown in Table I. These equilibrium constants were also shown tn Figures la. and 1b since several of the temperatures used in the kinetic studies were between those listed in Table I. It should. be noted that the oonstants from references 1 and 7 are more reliable than preliminary ones reported by the same authors., 8 Values of {).lfJ and ().S0 ealeula ted from these equilibrium. constants using the relations 0 0 & • •RTlnKt ln(K2/K1 ) = (6H /R)(1/'l'1-1/T2), and 0 0 0 {:jj m (tiH -& ,)/T agree reasonably well with those deter­ mined b;r other means as shown 1n Table II. Hence, the equilibrium constants a.re considered rel1ablee . However, Table I B!u111br1um Ocmstaata tor the Xenon-Fluorine SJ'stema Reaction Temperature °K -· 298.1.5 52).15 573.15 62).15 ) 67).15 Xe + F = XeF x 1 4 4 2 2 2 1.2:3 1o J 8 .
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