— __—_— ___ #— -__.__— — ’— __d—’— ”—— __‘_ # ’— _'_'J - ___—_—— — __’_4—- ’ ____‘_ ___’_— ____'__ .— —- ,— , ,_d '———— {—4—— — __’._. — _’_—- ___’_— — ’— ___P—— , ___’—— ’ ____f f ___d—— — ___.’_d __‘_‘ — —_‘_d of - __'_‘ ’ _—_'— ”—— E W THE ACTIVITY. OF THESIS FOP. THE UEGRE U ‘ Yi/iH ia m D‘ Lax S p; r: 1931 Lil-3 " rd '1 L‘ I. l t .4 k Er / ,’ . ..4 I 7 Ilj' [/1]. ’ ." q , . . I I . L -, ‘7?“ It” ‘ ., ,. .~.., 1 £155". a? .3" ' ’V' ‘7! v ”a“. .'- 5.? .' 5. VI. i“. : 0"." $9.“ 5 . ‘ L‘QLI’S?E§$I 2'3)... “ I .fi'i-fih .- " ~01 vii; £34; . ’ o n. .2 ‘ {,5 ~\ " .2. .' . ' ~_ .. .. 2 .. J . . | - I - 3' l. . . . 1 \2 .' ., "2 2 "I -’ .- 3: ._ tiff” - ' :3. g qv-z -. . _. I, ' - .-. 2 ‘ a .‘ I "'- .4 ‘ _v. _ _‘ . . . : '1“. " _ ".“ ':. ’g % _ 2.. rigig' . H a». ;. <._ '- # n"" 13...: I: 1.: L, 2" ' ‘:.‘ 2. ‘f . ’2". -~‘1&~25..‘ ‘\ 5’ . - , .. ' ‘ '. .r‘. - .7 'N . 10‘ _‘ S ‘2.“ .,' £- ' . . 1‘ .' .I '. J) .§__.f‘- - ~v V (urn: ,6 'L', 39!: {31’ Sir . - ‘Qj‘ifj A {fig-5‘54 "A -3?‘! ‘ . 1.25;)”. “ 46‘ " \"1’- . ‘ ' »' “flight." "131‘ ' I." . 0 ,' “‘. 2",, .‘ L “L ‘ ‘2‘.“ , -,.-_ ' ;I‘~ cuff/0"?‘f . 2; . 2.64.3 2- ‘ -. .-x.A-l.--.f. ,. “'f S'T ‘J _ “ v.3“: ' l‘ ' .-. H '. “T. ‘ ‘\-'. f"f.r-"ti:\u ‘igA‘ L“ .."r'.‘..‘i' {LTWW ' '-' '. " 'i"~"-'r"-.-I.M"" a «1' .I “'..1".‘v..1, . ' ‘-. ._ ' .U ’z" -" ‘2" 5'67”» ' . .- :tf»_‘“"-"*’_’-.‘-.'r .-‘ . ' ~ .. ‘f- -- " “'1‘“ ‘ V 1. 5 "if‘ . k... -. ' thaw.“ a ‘g ‘\' I ' . '4 :’. . . " u I ' I l V ' .I I . l'l 0, ' ' .‘. .' ’4 o _ n' .. Q2... 2 .‘ V‘. :l' ‘ {\' ‘ l ‘ ~v’.‘ ‘ "2 4" ‘ . '; I... : ' . . '3.- ‘ . r "‘A fixfi'ia‘) 1 :3“?th #1 \ .. 1- -‘ g" .' ,9; l u .‘-_¢ t’ - N» ' 5 (.‘b V . ‘, - {If-It A .0 . . " ‘4'4‘. 4‘ n C ‘v,,r.‘-\;» ‘> :va'vy-o - - If: '- -'._." ". A D _ I ‘ . . «swapmso2JM—Em ”Au-‘Sy'fiue - _'. : . < ' < .' f 2- , . ' . * , _ I‘ _ ' _ ' .. . .' .'. . - « - ~ . .- ‘ 4 . .. . _. < .- . - . - _...y . - _ , . _ .. . A - — _ ~ ._ 2. “IN-A . . . 4 _ 2, . ‘ . . - - - n . u.‘ V -. - _ . . - ,l - . - a '- _:¢ 4 3‘.“ — . . o _ ‘ ‘ A. ._ . ‘ . I I — n- ‘ ' . . ' 1 4 I , _ .~ ‘ . .-‘ ' ' - ' . ' .m 2 . . - - I, , u . I ,I- ‘ :3!“ \I J , ‘ “{l*:,‘\,!..odfi‘df‘w"' '4 ’35: I ._ ' '\" ~-‘ 2’. t‘v I‘tl\"t"a4 .— ’ ‘ Pt I '. '3 ’ 5 -' c_ I « P 3 "7"“.V.‘ ”fl, .. “ “a: .‘:=‘ 4*. . 3 "hr-{fit‘k-étg‘. - .2 :§?‘.“'.¥’S’~.'J .3. . . .. ~ '_\I,‘"\““::"~L§‘{‘. £23/ I" ‘ ‘ .“'\ in§u.l.‘t‘§m.‘h}2 M 'd 'i '. '. _ ‘r ;,L,- ‘72. . . _ . A’ '4 "x". {53(3): 3; I. L] h “1"?) ~ ' in . ’ 35,35,3‘5111“: ‘Afi‘, .2 ,3. . -‘« ' g-S.‘..‘\‘o\ h ' .w- . ‘35-- ‘23. Q? H.122” é? 1‘» " . N243. ”2...: ch" ‘ j I 2,, '.,'.‘; \vi'."~ ' {A - 'I- '-.'I‘_ '1 :- A f' . ‘- 2.;- ~ t f‘. - . .‘ . _. . ‘_ ._-, - 4 ' "_> ' I ,-,.I\--*. 2': l h ‘ 2, 23:42.2 - 9‘3 . “" ' 9:1 a s 'z \ v is "*‘.- '5 «w ' - i] ‘. . "h .2 1‘.->. ‘ ! pi ’:":’: ‘ ‘ . .. "E; whifitf'f}: q .- " '. I‘ , "l ’. A a: awwfip . . ‘ J. - L33» - . . i; t f- _ ‘l . .- Yfifkfi Nlé‘afi‘rg 2; :V .’ . 3.5 . M. r ' ‘ ’ ‘2??? , ‘ *- v.- - ’. .._. a . \> ‘ Tu ‘2 is“ 2 'b': ' t‘ ‘ ! ££~flfig~§‘" -.v..g ”-73.3". .1 ' ' nas.}‘*’..:*fu,;. 2w ' 'L A ‘1! sca- _ .ll ;2‘ I”; - . U]. . 9:4: (I. '\ r17. -‘ "1 “—‘-.'1-~ - .. l- r A llesib bun luted to the raculty ‘.' 71- mrwr r—w '71?“ " ~— n.ICI-I'J.'L.‘.'; 5mm COLLLQ'E In. Partial Fulfill}: "L of the wlreraenijs for {:13 Degree \ Laster of 3016109 - r 1..-, .,1- Uepdrbmwflu of Chemistry Killian D; Larson June , 1’33 ‘0'. I. ILThODU" TIDE AILD LLTDE:TLAE m . "TD-.1 7’ ~~ . “’3. - - -~ . lge cell H“, LLL, HggL erg + g; ”Le Moaswred 3L con- centrntion from 0.05 molal to 2. e molnl 1L ordew detesaine the activitg, coefficierts of hydrobromic ecie in water, and to obtain more data on the electrode potertinl of th: mercury, mercnrovs bromide electrode. The only Jute available on the activity coefficients of hydrobromic acid are tfie followin“: Lewis and Store)": ('3. 1?. Lewis and l:j..”‘1f“!1 S’Lzorch, J. Am. Chew. 300., 30, 2544 (1917). They evaluated activi‘v coefficiev,s of Lydrobronic acid from measure- meuLs of the cell, H2, 13?, Ager + A3, at conceKLra Lion rs 0.01, 0.05, and 0.10 molel. Bates and Kirecoxenn: (Bates and Lirecqwenn J. A1. Chen. 500.,‘él, 1901 (1019) obtained vapor ocecfinve measuremerts on hydvobromic acid from 5.8 to 11.0 nolel, and calculzitc d the free energv at various concentrations. Livir teton: (R. S. Livingston, J. Am. Chem. 800., 48, 45-55 (1925), evaluated .cLi vitv coefficients by hydrohromic acid from 0.08 to 1.55 molal, usin, the cell, H2, H3 , AgBr + Ag. Earned: (K. S. Horned, J. Am. Chem. 300., El, 416, (1929 gave values of activity coefficiehts of hydro- bromic acid from 0.01 to 5.0 molal. Iatthewg: (Julie L. Eatthews, Ph.D. Thesis, I.S.C., 0&50) discus es actf_v:1tv cochiCJeaas of Fyirobromic acid. (/1 1073 ‘11; 13:] Dr} 0 l-:8t1 H'62-‘IHH'S (T “-cL111.n SteLe Co t:e hvdro" JD, whi and the treat tation. The tunlrogen ordinary Capaci'j, fth ’1 four foot length diameter, a Small cathode. 1'1‘.e cat; on the outside of ”e1 gauze, of the tube exten five pound bottle of of be 03 SUESIALCES es us d were nrenlred as described o. L. .IuUL'Le‘lo, P1lgD. 111113313, liege, QVO), itb the cxceotion of c1izzas rw11e191~31 elxnztroljrticaljyi U of mercurous bu mide after precip- generator usel 001 sisted of on about imo liters wi 'tn 3 rubber stogper carrying a of glass mnbing 1% incles in deliverv tube, qnd tbe W139 to the 1018 was 03 nicgel gauze, and was the large tube. The anode was also and i ,sid the large tube. The end ded to about two the d...‘ bottom of t11e bottle, and was covered wi‘h two thick- nesses of asbestos pager to prevent diffusion. The electrolyte was 15; LaOH. / Fifteen vol J- US was suffi eient pre sure to Operate the 3e aerator satisfactorily. The generator drew about 2.5 anperes on 15 volts. To obtain COLSLah. Operation, three four-volt storage batteries [ere put in parallel with the line in such a manner tint w’en the current in the line was S1111b off, t‘r‘e gge‘rr rowior Operated on current from the storsje batteries, and when the line current was on, the batteries were cbsrged. m» FD. [MW P I {FIR/l. 1— 1_. n+— 1 . f; 2 VI“ ‘ l ’4 ‘t‘rt-‘QNNKQ 7 f 2?; K \V‘Z'\:NL‘ *+ All CATHODE l g: __ __t\ x- M, _ _ _ I fig '—_'*"——"'*MHNOD[ é _ _ _ .4“; a — _ l a I _ __ 2 (.1le BOTTLE i 1 (”Of-7706 ’ DIRWRIH b L ‘“ ‘ * [/0 4c HVDPOGTN CIA/[RH 70R .43 . TO (ILLS MJ . _. I b- ,'v_ .-. _ _ , . - .. .! ,_, - .. ,., , A J- .. ‘0 "141’091114 as it, 0511133 ITO-.11 the generator 118.8 J- .1 . ,..__ (q ,3 3.. .0 ., - passed through water, and then over a JOh platinum spiral .1. to TGWOVG EYE?" L'l-"I'WCB of ox-H» (3.1. d lLe seneratoz we; run continuously for several months with no attention other L.han t} e occasi-orel addition of mall amounts of water, and the ordinary Cure that stornfie batteries would lequire. The mercurous oronide was D“epnced t7 adding 3 liter of . 2L potassium bromide to five hundred 'illi lite;'*s of mercurous nit'ste which was about .OSI, thus lceegirg Kg+ in excess. After precipitatior the wercnrous ar-rwi3e was allowed to se,tle; tue supernatant liquid was d: awa off by suction using a piece of glass tubing on which was a cotton filter. The DLGCioitdte was then washed eight times with one liter portions of evacuated watee; the rinsings were drawn off as completely as possible each .1. '- 1..-- n ‘ 1-: _. - - 1.1.. o g- ine My use 0L suction and cotton filter. EduaxHasned preciuiimfimazwa: transferummi to n 800 cc. -- - " 0 . - , .- o -_ 4-4., .( Erleaumgfiei flzuflc. ‘Ihis VHHflLGJ arulai M’lll'lcfl:pPBClpiJM4w3 was 0 ,3 ’9 6 } .1 K“ then evacuated by usin;_; :2 stepper WM s. L t 1‘ ‘L‘ '\ 1" J- tten dueWCbe; LO zuid.218piiuitor'.fihie Iiitrwijera liars mute the inlet tube, and toe stopcocfi slowly Opened. “we sto;3er was then removed and a SCTBBW o nitrocen was keot go the omen Erlennever, affiaile the 7771 o iacel was rinsed several times with the desired conce ntrstion of hVdrobromic acid. The mercurous bromide was then nllowed to stand unde er the h} Uremic ic acid for at least thirtY‘ _._-_ asix tcnxrs, xvi,?uamt laeest inxo "KN79 c:wr7*es o? ljnlro.13.%)¢ic acid. ‘ ° ‘ ' ' ... . , “q ‘ "a ‘ “7 ' a M"; 2. 1 .1‘-':r‘"a’ _ i”1aiejlljy, tTa; s11s:3e-;siu3a1 ‘3; :LJI CLIL<3MLJ Ji 0 -1 he iii : “*ILL) wro oraic acid was reusfe "red in o a 250 cc. :::r‘31:»'...‘~~:tor:r funns ; sone morons? was else aliel, ”P9 Y”‘ ‘i"iuce shn“e: for at least tw. sni one-Half Hour“ an] I‘e cells filled. III. ATALYSES In an ettenpt to explain some of the di_?f icultfes in getting e.1.f. o‘ecfis on tFe s"°,e1 being studied, it was considered advisable to analyze tte acig from egch individ- The concentration of the stock sci; solution was :1 -. ~- 1--w '1‘ ‘7' . ’ »\ *fi - 1x .- -'. - ,n ‘ J- . .\—'- 1-‘ , ,. SOului nfurolide solut ioi LCLOPQ coin) pit lMUO 9W3 cell, , 4A-, 1-. . v-.. . .- 1 9—1, .« ...- \waen LHVB co: than :‘Iuiorai.as .uuive (3.1 5mflJil, cwi u u: cormysn- iuw+hiou of tlvazicid Dctnwlj. “toPen leuxifwei‘NIV-celfisai es (letepfiircd_LIuUfiLuetricallgcan; silver'idfliiide. livmi the CO} KAI‘pT“HvJOP \nQS O .l_niol:fil or 1333s iflie (NMice'fn_utiLni of the ecpili‘tumt ad acid. ‘ we meter 11- "ed l1" titratingj \.':’t_‘:1 . a. - .0 .,- 1.. s a. -,.- .0 ., L in. stoodsimi werexdmuis n lifiuxa solut i_u1, accoumlci; ncw ume 4. V n v- “.1“ - _. _ r70 -, -, - (c. dethod 0L L. von éoiuory, (L. voo so ho~\ Z. noorb. l‘illgelllo ClirJiLO, -94‘, 25? (192/39 . «in; burettes were used 13.770111: five aii].121111363 1" :3 (a f {1qu no. i :7 $791" '3 371111 17-1170 0. fj milliliter beaker, ten drOps of bromphenol blue indicator prepared according to W. M. Clark (U. K Clark, "The Determination of Hvdrogen Ions”, third edition, p. 91.) Then the bydrobronic acid was run in dropwise until the precipitate turned from violet to cream color. Then small amounts of nercurous n’,rate and hydrohronic acid were added until the end ooint was reached accurately. At this point the precivitate appears partly cream colored and partly violet. Io wash water mo? These analyses showed that, in Teneral the acid , 1 concentrations do change. I ., J (D original corcentrstion of 1 e equiliorium concentration, and the J-1 acid, fie avers change in concentration are given in Table I. All con- centrations are exuressed in mols per thousand grams of .L water througnout the tnesis. TABLE I Iolality of Kolality of Change in Original Acid Equilibrated Kolality Acid (av3.) 0.04757 0.0474 -0.0001 .1044 .104 - .0004 .2868 .200 + .003 .5008 .503 + .002 .8- [.13 03 8 .8358 + .010 ‘J (O Q) A?) o i d) + .012 O O) o d }_J O to in + .052 (3 n3 l4 F4 O (O o no a) m 0 O «1 J 0) + C) hk C) \I (,1 C1 1...] m 0 <1 G) O + O O p. CI: 6. This change in concentration will effect the value of E0 and the activity coefficient. Since the concentration in each cell was somewhat different fro the mean the value of E0 was calculated for each cell, usinf the activity coef'wic m1ts Sivan av refined (1.5. :ar ed J. Am. Chem. Soc., El, 41% (1029). From the average value of E0 for any concentration, the value of the E of the cell at the 1eare23t round concentration was calculate; and ot7z~1er calculations based on this value. IV. TIE CELL: SETEIIG UP AID Isms.njfj TS Tne cell was designed to pe rxit ease of filling, and 3 to make it possible to fell without ad1ittin” I 'J oxvrg. ,11. The hydrogen electrode vessel was made of one inch pyrex tubing, witn the hydrogen inlet tube sealed i11to I“ the bottom. use tube connected to the twe-way stepcock was sealed to the side of the tube. The platinum electrode was a piece of fell about 3 sled into a g1ou1n1 Flags stopper for ’ u the hyd1o snilectr 01e vessel. The nercurous oro1 de electrode was a 25 cc. dis- tilling flask, with the neck leistne1ed. The side arm of the flask was sealed to one arm of the two-wzy stOp- cock. Connection with tre a‘1curv was made pOS"b1e by a tube sealed onto the bottom of the flask. The vessel {'3 o. a convenient l‘l P4 was closed by a ground glass stogper ma. size of tubing and a stepcock. The cell is shown in Fig.2- 3 i 1 E ,L 1L ”rm“ mar—L. .5- “it B!" ML" (6“ - U [flL UEJJEL c Will/M T011: In filling the cell, the nercurous bromide electrode was first flushed with nitroren. ine11 sufficient mercury was introduced to make a small button in the bottom 01 J " " fl " --”. ' ~". "‘ .0 ‘ "." fi , 1"“o I""»' "“' “z _ (‘Ifi A ‘ 1". T“ ' .1 ""‘ tue flash. altrOQen llUudu u10u3d tub Vessel contiMUJlig '0 \ "' ' . -" “ ’- I ~ -1 "‘. JI"' '_ J" .1' ‘ J" .3, '--\, '1 tlusou tine SJAJB tuna, ’1W1_ -1t 1Jwe tog). 'maxt tire 113IWflIBCNJS . - v-1. .0 ,- -1 .. .' :1 -. Jo fill LNG ilash and Side-arm i. idée :1siil VfliS (iranvn 1r; i11to the stepper stopcock. text tn-e s:1turator was flushed out with W11 ro3en, and filled wit in hydrobronic acid of the ease concentra- ion as used in tlie cell. The hydro3en half cell was 11e1 filled with acid while n’tn03en bubbled up through the hvdro 03en inlet 1 .1. 2.11 inc pl stinun electroee (platinized by making it tne a, ’r o o o _ O o catnode in a 1t chlorplatinic aCid sol1dzion con Lnin I" a trac: 01 lead acetate) was put into place, and the cell placed in the thermostit, nni nvaroi n started. leasure1ents cowl' he he3un about one hour after starti1‘13 the 1131-113 3en, but in general no re li :31? 1e measurements could be made before twenty-four hours. The potential :1easure dents were made wi eh Eolff five dial potentiometer ($.012 and 3 Leeds and Iorthrun type K series of ”alvano:1 er The galvanometor and dampi: kev w3 e on a sepaw‘ te shield, insulated " glass from the 331 ield on WM.101 the potentiometer rested. WWW! I CDCDCD wax.” mrtwr/MJTIR n g €321?" .1 : ”D“ 7D j 11 Ego o m an» mvp JCALI A o“o o o RIJISTHNCI JHIE L DING 5 Y5 TEN r. x O T36 vegkisu b1tte2y fol tfie totextiemeter stood on a heavy piece OF insulstgqg hoi’d. “Le “”Jleiifld iron tank 0; tFe oil but? was electrical y connected to tLe pote;tiowetep shield. The d,tai1s of Lao shweldxng system are shexn in uh; @119? 1 (Fig. 3). *‘e Jehefinl s hlJO was aeeoriwi to Jules ('. P. .‘ifie, 5. A1. ”091. 300., 55, 2011, 191é}. “iii? t51-330 ‘;{tIIPC§S m1: ifi=i-ell tile 1 KBRfSUl‘B aeiwtss $131”) 510419 CT] were: 20.000, 25.020, and 5 .5800, as measured on B. of ‘1. S. cwevfiometer To. 493/2. Bhese temperatures were con- stant to au'i-;11i11 .OlOC over: 1011;; periods. [he bath was the oil bath described by C. D. Tuttle (C. D. Tuttle, L.S. Thesis, L.S.C., 1931). '03. 2308” and 2. Me exeerinet n1 daea are preserted in Takle I. All .0 L ‘ ' "- ’ L " (1‘ . V “ “' "‘ I A, “ "“ COflCeruflflulOJS MEG expresses in $013 per lOuO brois o """"' \« u. I. )9.kaqu mmwon. J ).1 DJ. Gated/km... nomon. mo:ou. moo on. wmooo. wwwom. m .. J0 ¢.or .H N “mu i... o ../...u|.... AMHN..J<.V( . MCHOE . aCHC.. HHCOV o Haaom. mmv . mceom. bmw a. .CP\OC O HOCOO. fiCr.CC .\.o\I.U. Q: .o. owwon.o \..\..»\I .J A~CC LL \J..I¢ x.-. HOCOD v on \. mLm _ N... omwom nfiwon mfiwon nmfiom Hafiou mooon moaom wfiwom 02uC: 01.03 nyl.....a «\- ks r r... HHNQG Dam C: DHC 0,;CCrH ud..-.oo wwbwo. W. n. o npbmo 1. .14 O @rb.c ow 1.1. rfl .m..\ n... \J.1... . . n1 O 44 orv or. O Omb.O O G..L - .l’J I \. tuln. \J 1V I.\. .1\.NIJ.O1I...' \. 1-, .1 H... .r_._ .._F,...-\..L 0-? 01m. _- "U CPL..r.4:(\._.\.Hr flunk... 404.2...”900 .ru. 0 03,00 o 0... Use: HH (.C. O m .Mo.-ww .inwHJr: 4'. .I. -..‘un.i.'-. mo. mm m.wn> mo. mm m.bmb oo.om m.amb oo.om m.mwb mm.mm n.mn> so. an ..@n> mo.nm m.Cmb mo.mm m.>wb mo.mm m.mmb mo.nm n.bwb 00.0m m. we 00.0m m.wnb mflhsfimmh nomm.b mo.nm w.mnb 00. DN 0.8.me mo.mm >.mmp mo.nm b.00b Hm mo.m n.bne 00.0w m.cmb co. m m.mn> mm.mn n.mns mm.mm n.mms mo.mm m. pm .> mo.mm m .mmr '1‘..." "v 9 ‘1‘- . m».H.O O m,~ro 0 MW .mfiob floss: "...I‘ ' WONG. \‘ mango. DEMON... OmHOml Hmaom: h... H («CW . da.om. own .. \L H...noo. fiJHuA..OmWO erg QdmwOAJ o nHHo.. omeon. mason. mason. OBOOQ. .A.AJO..).0 LL.. ODOOH. -.\L Hagen. maflca. mofioo. NJ. Fr... -... mamom. booon. o.nCn. tL.L n.HnH ¢.mHH ®.nOH 0.56 . I a ma w.Hb N.®¢ m.mba w.®oa m.mmH O.mwa O. NH m.m@ m.bw m.nm 2) m C\ p» fill—O11. rulr thom H HO p-.. Q) I'—1 L) 10. oesom. - o. 5.6»-qu . filmmms :0 k .1. 444.0 . hi \ (PL 0 All.“ WHNOVM. Q .NQN.0 mOo- .m Nownb @0309. o mHmqumwO Ado “.0 00 4.2.1.0 my... .\0\ CK. 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