EVALUATION OF REDOX SYSTEMS AND INDICATORS IN ACETIC ACID The”: Ior I‘IIe Degree of M. S. MICHIGAN STATE UNIVERSITY Nahida AI-Qaraghuli 1958 all” 27) EVALUATION 0? RED! mm ”ID NDICATORS m LCETIG ACID ATEBSIS mum: to the School of Gum-to Studies of Human auto College of Agriculture end Applied Sci-mo in W (11111111116316 of the remix-wt. for the degree a: MSTER OF SCIENCE Wtdmm 1958 ACWWT memflm-Mutowhcnncm momma-Mum: WM. VITA nun MAL-«um I“! ”N’DWUW911‘Q w W m 31¢ School BM, Iraq (19104-1916) Eon). College of Ola-1m and PM Baghdad. Iraq (ISM-1952) up... mandala. Bold! mmuwwm (195!) TABLE. OF COHTEET‘I‘S nIlim‘mcmneeeeoooeoeeeeeocoooeooeaeeoeoooeeeeoeeeeeeeeeoeoeeoeoo ":3 EH. mmhImLI¢OOOOOOOCOCOOCQCO...00.0.6000...GOOOOOGOCO'OOO0.0.0it mmueuoeoeeeeoeeoeeecuoee0.000.000.0000oooeooeeooeeoecee- PPBMtim O: Solutimauuuuuunu.u.............u... 1. 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It ammememmmummmommmmmw mmcmpummmmmmmmawu Wmmtmmwmnuobmdmmm,mn~ mm.mmmm. mthenmhnmthmamtmmmmmgtmmo: mmmnmmmmmmwmdwum Whmudhufi). mmumdumum) munmmummmttmmnmm. mmmmte(fl)hubeanmummmg wmutummtymwmum.mmvwmmnm wow-mama. ' mobJMdthumx-kmtodmlopemmeumu mumtwmmormmwmm. Applies“. of Whammutnfimmumdiod. mm 1' we. maummam 'm' "°"‘ "'" 3. mm acid - Depent man. 3. Pueblos-13 mid . W 'AR' nude. Can. 701, up. u. 1.6. h. adamant-annex 'mgnt- mmmw. S. rmmmu-Wo Manned". 64mm mmmuua.mmsnmmco. mi. 7. ferric chloride a Purified ”PL-her Mental-:3 B. W Hmnitnteomte IV 0 G. W 381th W Go. 9. lea-run mfiu.a. Wannabe-4mm. 10. mm-mw-Wco. 11. M mum-no - leak “ream. 12. o-W-G. munch-mace. n.3nmx-udowmmcuum). WWW-thmmum. hem-awn 15.Wawxmcm(mumm. 16. nmm-mmcm. ILMWOOM'W. 18.nm-mu-W'w m. 39. cmmmuuu. Wadfih'w Oe. ”.muma-wmmm. naum-wmmgmmutymuma). Preps-Mann! sebum 1.mmu.tu.c.o. 10.011um1morscammunmmmumm1lum mammal-inns preparedbydiuelfingo.61woteod1nn mumemdw.zon1.parchloriowmmtodtolooon. ummmmma. z. W 2113:3112!th), (mumdma). «a mmmm.sm5°rormhmms.hemm Whmnmmmumumo.o1nmm. mmuemmuumwum1nmmun. monom- Mummmmmuwwmwm. Lat-mam» gwmgumnmmmwuamumn. mmmmson.ammmmwmmu mammumm.mwmwmgmmfi. mmm-mumnummmmm. mwnmmnuummdbmummmormmm— lug-dinning. unnummmmwnmmmmm maniac-tam. strummmummmm umummmummmuwmm «them. mumunummwumpmm wmmnmmmmmuummwum «u. m “mm-am done mummy. Limo-Woman» mmuwmmmmwunmumtm “etc-Wmmodvflhmmhoftm. InueWi-omtmapemhlmte,eo.01lee1nuenu me3.msmotMm.)r6a.ommn.m1-1 mmmawmummumumm swam-mammtmummmamaw Manama. mmmmmmummm, htttpedpihtd.ummlntimmtflwmaheaooch MILO. Mmhtimmewndvithmmflm new”. muofilso‘auumdotmplmthmumul Whnmdtmmmblflofl.do.ml mmuufl.» mumwmmmmm mxmmmmu,utmmmmo¢ummu an. Mm.wm-ltumum. huefimhmtmmmmu0J93mm “find.“mmmmflfMByOSth cum. mrmmmumwm mummm,hnmmmo-pnmmmum, wemrdmhretmmmpdm-uuthflm «wrmemummrmmmuu coin. App-mm Ammm-Wmm,mn,z,mmror Weaken”. AWMMMWW mummmnwmumummmmm- format-endpoint. mumfimmmum mm. WMNMMhWth-W Munda- tho-mmnuummmmum mnuam. Wmmumumwm mummmumm. WWWW rwnmmmwummummhm wwmrmmmmmmm umwmwmummotmmm WWatm-nmdmtmmm mmmwmnmm. nmmmun ummummmmmmmmmm mmmwmmmm. Somme-elude mmwummm. ammummwmmmm wwmm. mmmmmmmmmm umgwm. mmnmmummmu WW. m,mryuuhmuwmmmumdu-m mummmmumwnmu m.(1). mmdmmhmumtunmm eta-inmate“. w,ummmwmwmuuu mnem. WMm’MWd-mm mmmmmmmuummwm moth-W. math-mmwmmaoJxmm-a «mmuumum. hummus-Mom Wumdmm. mmmwmmn ummmmemmmnmemww hmumanmmmmmmm mm-mmmtumuwmnnmn. mm rummwwwmosxmmm- enumuumhumwmwm. mum mummtmumdnmmmunmm Mama-Ann. mmAu-Wm‘ mumm'upmm‘u‘umu. hummu- mcmnmtmum05nmmpmhmnmw ummmnm.(1)wmtmnummmma mmmmn‘ummmmmmudm amen. mmmu'mwummmm: mm. mmmmumemumm mummummmmmamm. c K é ¢PT IN Hg ax Hg + Hg;(0Ac)£ $AS BE STO 5 FIBER! A B FIGIJRE-l- MERGUROUS ACETATE ELECTRODE Meteor 8W Withmmmulmlmhrflmem, it” moummmummmmmmm unmwmquMmmdm-wm. motmmmw.mmmnmmmtmmmum timbmhmm. nmnmmmumuumwm amumnmmmmmummwu mmmmwummmmmw. LWWoaupl-uu mammaotmmmmmumupm mummmpflw-thmmumwmm Mire-mum... mwdem‘wmuw Manna-am. mummmomlmmuu mwmmumnmo,mmn.aomlm(n)u mwumhutm.muummmmmm mllufimumumewipimtmd. mum mummmwwmmmmmamu. «www.mmmmmwbmnmmm magnesium» mmmrormmu 9.6mm. mmwcimmmmw. m'WuWwammmmn-md mm. ‘ Wmmnmmnpmmmam e-WWWumWhufleflm—W «mum. mammmmummaomnoammum mmuummumnumomxmm} mm «ammo-thmmmmm ummmmmm. armament» 0.9mm» mtmmmmmmumuo.w nu. mmmmnoAfioma-«mmum We. mmnmammmmmumw~ WMuethmwMI-m. upma- www.mmmmmumn m1. m1 mm at «mm mm: hm ammulrv) ~ o-mmn'mm corms: AS mmmx numumumamnwmavmm mmummnmummaomum mnmwnummumumuuoml. cmwuwmwmmmmmmm mama-1. ' ' Wuwmnmmmmumumoromn mmummunmummw nhmmumwonmpoxmmmur. m.- MmMWMMemueolm-wwm mum-nun. homunlwoolntimofo-phmthmhno-tm emu! WMunmethomWflmumot mwduemfl. Edmthaindicatarmtflad,amtio- mun-mm cloudinesMDuth camn(xv)m uda. mun-n thmmmanmuo.éoownmmwm Wm.to.930m1t. nmmmwtmmo: «mmmmmuummmmummu ummwmmaéuthm-Iv. 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MW' at qu-uw mama“): c.01uemm Mthummuhmmpthebediphmw hairline. mumMmMmew-eimuhtm mummummmumwnmaenmm Wanton-W. ummwuumumu omxmmmacdimummmmgzummmwmumOMH mmnmuarmmmtmmmmm mmmuummmmmwmmwotu Maddaehupmhlodnmidmmuauy. bmumthe aha-need perchlorio wide precipitate tamed. Emir-five ll. of omummouommmdahmwsoanhucmwm lxummumum. Itmtomdthetthewutor mefiWeWB-mpadmvflhdthullar OJIpmhlefleacidlolntm. nllmmmmmmnmmrmlmmmtum Wmo.hoovo1tanammmmtmmmuo.mo wit. no.5:mmmummumwotommm1mm mwmoaéownmmbmmmmmnwéo an. mmummmmmummmm wmamnmrumumum. mountain-mm MWWWMMWmmmWWWW mum. mmwrmmwamu mmmmnmuawmrumdmclanIpu-cm ablation. Anettmptmudeumgdifixwflemmummnuwhthe ”Wflmflmottmmhlmumummllh ammummamu. mummmw hmutbmmmWeolmemwmm Ma.wmmmummuummwm mmmumozrmmumummumln ammumuthomncmm). mmmnmdtom mummmmrmwwmmm. AWe§Wmmmlmdummmm nummmmmmmmumumammamu umemllmmmumnmummnuma Muhammdumga. omdropdtmepuvhlmteeohm hmuumeummmor-uuummuushm upwumpmommammw. momma-m memuihmmmedm-mmmewm M. mwmwmummwaum nmummummmmummmm uwummmu. mommmenmmm mamuummuumtmmummwmmwu also. Lama-bin... mmmmmmmmmunyum ummummmmuammunmom no mfinmmmumfimflemmnwmbme mmmummmwMammuum-ma. mum-1. «omnmmmmumMmmwu-ston. nummwmnmmwmu'mmmuw. mun-mama: mm. m fmlpotmtmmo.165 van wmmhmmeto.020volt. mznmmuum mmotmmmmeuomsvon,mmwum meme-sumozswn. mmmmmmmeu mumumm. Mmmdiatmeteolarewge wmwupomm. Mwmuuotthendeem, num(m)ulnumoonmdpumnneleottheindmflor. wetmpummunmmplmmamnymbmu animator. maxetmmanmmmumumo: mmuumumm(m). mum-mum mmmmmmummmmnm. Wetmmmmmummatmmmuu umm(m)mnu.butmmpmoboam. mum-Lemma. mWohwflhuflummdemmmh tmmmmutmmum‘mmmmum. no mummmummnotmumum(m)m uhmgmmammmmuaunm. ummmmmmmmnmmmh mum. ho nMWmoMMc-I mucuwutmwmmtyornmuomn wmuummmmunm .wnmwumdmmuomlum mmxunmumwvflomnmm. umtuuummhmmmmm mmumno.mnn. ”Whptvtantmwlt 0.950 volt.- flu tern]. potential for the malaise oxidation was 0.685 volt». The WW “trauma agreed with the Mentor titu- tians u than 111 m1. III. mm mm or 301mm own m min) nmmnnmam AS nmmma --. - mm -'-w~--‘-.—..--o---Ah—fi—-o——.—n ‘nh“~"www—swflw--—*.OIMIM1-.§Ii-“ ”WA—Mn. 31' Mane n. Go {IVI Indie-tor mama-1o 35 25085 ~‘ 25 25.80 ....... 25 25.80 25 25.85 mutt-Immanuel. “matted-Wm: complex uuwnmnummwmumumm\m Itmtamd mtmmotuquobWbywn-uwmwumm (mn)didmtoeimideufl1themotneq./m1.obtunadby WM moan" (Table II). S.W1nd1eetoreon Wmmumwmmmummgrm chloride with um Illa". The indicatordidnotvorkbmu the manmmmmm-mmmpomtmdnrm mutation. mrmmmmummobm by upswing tmmmmummmmnmpmoruummw portion! to help dieeolve the ferric chloride which was incomplete]: callable 1n ecetle eeid elme. m0£llm1nt1anetneutrelred1neoetie ecumdelfimdi!!! 1n mpect to perchlorle acid was titreted with titanoua mlfate. It we! found that in either eolntlm the break in potential we too eerly end thet m efter the eddltienot one :1. of titanoue Innate. Be an. 1ndieetor m neglected because we could not get are 1211'th 4 me the foul potential or the petmtlel et the break which eneblee themdlctlmotuunsthemtnlreduenlndloetormnrlme m. m” 17 WWWOFMXWMDM Fowl 1’0;th , Potential et Syetu Iv. Cole: Cheese affirm” 1295 iltro-o-plmnthroline tea-rem complex 965 or"-cr“ (1 n 3.30.) 930 r-"a." (1 H mm.) 690 ' 6,05» 200. 620 o-Phemnthrollne tame complex 660 860 2r," ~03 I. 610 to” «- r." (1 I 3.50.) the WW (1 l $10.) M30 WW (1 ' 3:334.) 335 new?” blue (1 I mm.) 175 21” «- 11“ 4-150 ‘__. A“ .m— _-—_._ A A__ w m w..— _— w 1 *VI. nercuroua acetate electrode. 16 Thin work was done to study m reaction-mum eyetene, indicate", end eppncetlone to mm studied. he: the titretim methetoml potentmmrbothmteneendlndioetore,thepotutm et the eminlence point, and the potentiel etvhieh the indicetor ehenaed colorwerereed. Lmiun hmltntomnu end pom-mu aloha-ante we need ee mddninaegmteheeeueeottheireelnbmwmmeefl. fitenme ulteteveeueedeeeredueinzmtendituemred bydieeolvingtitenmneteltnemmreoteeetleeemplnenlmm acid. Ituepouihleteobtelnenrletyotmeutntmbyvemnc thetimotrefluinz. Titration: were done potentimetrieelly using e epeeielly panned mum“ retmelectrodeendepletdmneemgeleetrede. Ineomceeeeitveedeeirebletocheoktheneultebyordmwlndmtor titntione. The following cheerntlnee were lease 1. Rue paedhleteeerkuthtitenme eolntianunderen emmmotnltrogeninordertoredneethente of mun-um o: um by the etmoepherzle mm- 2. meow-”dumpleemefleetedbythepreeenceot etronzeeldeeucheepemhlorioecidendeulfimnoecid. AefluemmntoteeidimreeeedthebmkinpotmtieIOI (J 17 the eyetm increased. In case or the dichromata-cbmmic system unmade acid had the some effect. The titanium system as also affected by the presence of strong acid such as mptmrie ecid. 3. um: eultate m etandardized potentiometrically with potassium dichromte. L. All the indicatore used were soluble in acetic acid and the solutions were stable for a long time. S. The iniicetore which show poeeible application ere o-ghmnthroline I'm. complex in the titration of eodinnmletevithoermlvinllpachloricecidmd in the titration of eodinn aide with cue-inn IV. Kitro-o-phmthroline-i‘ermue complex applied in titre. timofeodmmmrithcermmfl. Bothindicatore show a. distinct en! sharp color change at the and point. me CITED 18 LITERAW CITED 1. Kolthoft end Monger, "Volumetric Anelyeie 1:,'I pp. lOSolhl, Intel-science pmliehere, Inc. Belt lurk, I. 1. (19M). 2. wan/an we end Chem, .1. An. cm. 800., 5;, 3908 (1931); 55,. 265.9 (1933). 3. mm, J., J. Am. Chem. Soc... 92, 2133 (1927). 1.. mm, 0., m. n. mm, mm Stete Unirmity, (1951.). Se Mil, We Ce. Phe De M. W 3““ Unimi'ty, (1958). ham-imam Reculte Arranged in the Order Hmtioned inthe M Titration of o-thenthmline—Fme Complex 1 R in Respect to Perchloric Acid with Cerium IV 22 .8 990 o 370 20 .l 689 S 61.0 20.2 690 g 2 1,333 12 660 21 702 21.. 1.110 13 661 21.2 110 2h ! 11112 u 6& 2101. m an . w 15 661 21.6 m 25 _ 1:50 16 670 21.8 721; 26 1155 13 676 22.2 820 28 use 19 631 22 J4 390 29 1163 A.‘ ___._ w A __ -__.._ __.. A“ w“. a w— ___...__ m ._._. “w, w 4 __..__ i.— wet—.7 __ W TitretionotficdinnOnhtevithCeninRee-aceot o-ththroline-fcrrme complex en en Indicetor n ummummuhmlaeil umumumcmn m Eocene 34:6." Jone“ nunDDDD DDDnDu t. m www.mmmmmmmm . 4344...“... act... e mu n ’99,,” nnnn immwmmmmmmmmm and» Jen n 01235788 e. mmcmmhamlmiewm w “m wnuuummu _ halt I1. m 55m i3...» inuufiflnw mmmmmmw $33,. nuance” Mmmmmmm ozamnmu TitretionotSodmnideinLcctinicidan inPa'chloricAcidUithCec'imIV K1. Wt m. Wt Hi. ”01‘ o 603 12.2 610 13.6 1150'. 2 608 12.11 620 13,3 11;; . I; 610 12.6 630 111 1260 6 610 12.8 630 15 ~ 1275 8 61.0 13 I 635 20 ‘ 1300 10 610 1.3.2 1000 25 1310 12 610 1.3.1; 1230 \ M A...— 4 ____ .g... A“..— .k“ A..._ . _s_.~ _. Titration of Dimmhxnine in Acetic Acid 1 I in I Pcrchloric Acid with Cerium I? A 111. ms 121. Knit :1. unit 0 380 20.1 500 23 825 2 381 20.9 570 21: 81.0 S 382 , 21 63.0 25 850 10 392 21.2 705 26 855 12 too 21.1. 71.9 28 860 13 1.00 21.6 170 30 865 11. 1.02 21.8 780 32 81c 15 1.10 22 790 35 875 16 1.10 22. 805 So 890 13 1.22 22. 310 20 use 22. 812 30.2 1.60 22. 820 20.1. 1.68 I I I I I {I II I I I II I I I ,3 Titretion of Potassium Dichromte in Acetic Acid 1 B in Wt to Sulpmric Acid with Iitencuc Sulfate O E I Kl. Wt 10.. molt X1 0 930 1.3.2 858 1.14.55 1.1.0 10 950 1.3. 860 1.1..6 3-20 20 939 1.3.8 8&9 1.1.10 so 25 932 hi. 81:0 Id.- ~58 3'3 910 1.1;.2 835 1.5.5 ~75 to 900 ““5? 650 1.7 «coo Titretionoffietlviuefilne inlceticicidll in Perchloric Acid with Titenone Sulfate 121. ”volt Kl. Wt 141. Mt 0 250 35.1 130 37.2 60 S 200 ~ 35 .9 129 37.3 4.0 10 185 36 125 31.5 4.8 15 175 36.2 121 37.7 «SD 20 170 36$ 119 33.8 «55 25 162 36.8 105 3 35 138 37 90 ~85 75 1.2 .100 I I I I I I I I I I I I I I I 23 Titretim of Ferric Chloride Iith 21m Suliete 0 31.0 g 275 33 210 2 315 260 ll. 18 3 292 9 260 15 170 I. 285 10 259 16 150 S 280 11 21.5 13 120 6 280 12 230 22 80 Titration of We in Acetic Acid 1 II in Respect to Snlglmric Acid with Titenoue Suli‘ete m. molt El. limit El. molt 0 375 26 318 21.6 2R) l 370 26.2 312 27.8 80 2 355 26.1. 310 20 5 350 26.6 308 28.2 ~55 10 31.5 26.8 305 28.1. .62 15 31.0 21 300 29 ~75 20 335 21.2 290 30 ~90 TitntionotswmmahtetithCeIVinPremeot mtrc-o-ththroline-Forrme Complex ee en Indicetor ‘kh -—— A A -___-. . , r A wuaflm V'—v—a-‘Q'v-nn-“um-—\M~mm”-..aum-- 10.. Mt m. belt no. wait 0 61.0 23 720 25.85 885 S 660 21. 730 26 111.0 10 680 25 71.0 26.1. 1185 15 690 25 .3 71.5 21 1210 20 710 25 .5 750 30 1250 21 112 25 g 760 35 1270 22 715 25- 790 I Titration at {trams Mata with Potassium Wt. Ml . “701% El. Walt H1. 3701‘! 0 .150 23 235 213.5 600 10 450 23 .1 270 a .8 620 15 'I- f 23 .3 31,35 25 65:5 20 ~120 23 5 3 £11 25 .5 730 22 .. 89 23.7 1.50 26 750 22 oh .- 65 23 «9 500 27 790 22 06 " 1«$5 23801 533.0 29 810 22 .8 DO 2!; .3 590 31 {330 Titration of Cerium IV with Sodium Doubts in Acetic Acid 1 E in thloric Acid — “re—W... M “awn-a.— ....-.....—.----. ‘1... . .-..' 141. m1: 141. Hmlt m. molt o 810 15.8 1300 17 780 3 1270 16 1160 11.5 770 5 1280 16.2 950 1.9 760 m 1280 16.}; 660 25 750 15 125 16.6 810 so 720 15.5 1230 16.8 8-30 38 20 "5 ”8 w ”0 N m3 U I