Portland State University PDXScholar Dissertations and Theses Dissertations and Theses 8-1-1967 The ion-exchange chromatographic separation of the components of the product mixture resulting from reaction of trans-dichlorobis (ethylenediamine) cobalt (III) chloride with thiocyanate ion William Trew Jordan Portland State University Let us know how access to this document benefits you. Follow this and additional works at: http:pdxscholar.library.pdx.eduopen_access_etds Recommended Citation Jordan, William Trew, "The ion-exchange chromatographic separation of the components of the product mixture resulting from reaction of trans-dichlorobis (ethylenediamine) cobalt (III) chloride with thiocyanate ion" (1967). Dissertations and Theses. Paper 377. 10.15760etd.377 This Thesis is brought to you for free and open access. It has been accepted for inclusion in Dissertations and Theses by an authorized administrator of PDXScholar. For more information, please contact pdxscholar@pdx.edu.
AN ABSTRACT OF THETHESIS OF Wil I iam Trew Jordan for the Master of Arts Degree in Ch mlstj:y Date thesis is presented: August 9, 1967 Title: The Ion-Exchang~ ~hromatographic Separation of the Components of the Product Mixture Resulting From Reaction of Trans-DichloroQis(Ethylenediamine)Cobalt(III) Chloride with Thiocy~nate Ion. Abstract approved: Theod re Major Professor A MI CA& fe d
THE ION.EXCHANGE CHROMATOGRAPHIC S 밍 PARATION OF THE COMPON 밍 NTS Ob" TH밍 PRODUCT ivjixttjr밍 RESULTING FROM REACTION OF 밸핀효 -DI CHLOROBIS ( 퍼 THYLENEDIAMINE)COBALT(III) CHLORIDE 시 I πi THIOCYANAT 꾀 ION by William Trew Jordan ABSTRACT The object of the resea~ch was to study, by means ofion-exchange chromatography, the product miχture resulting from reaction of 호펀옆 ~o(en)2 따꾀 Cl a 뼈 SCN-. Q 효흔 - and 뿔편 - [Co(en)2(NCS) C 괴 01 had previously been obtained as products of this reaction. Ho 뼈 ver, the poss 土 bility of the presence of other products consistent with the nature of the reactants could not be dismissed. These include the dichlora, d 土 thiocyanato, and aqua compleχes. 맘 le constituents of the solution resulting from the reaction were separated on a column of Dowex JOW-X8 resin by elution with hydrochloric acid. 안 le eluted fractions were evaporated at room temperature in order to obtain cr,ysta1s to be usedfor infrared spectral analysis and identification. Three pr 土 matγ fractions were e,;. the'column. The first, eluted with O.s 잎 HOl, was identifi 원 ::'5 할흔편 믿 (en)2(ncs)c꽤 Ql by analysis of the infrared spectrum. Two types of crystals were obtained from the secondfractiort which was eluted with 1!1 HC1. 맘le first CIγstals to form in this solution were orange 土 n color and were identified by examinationof the infrared spectrum
as.2 웰,- [Co(en)2(NCS) 0 꾀 01. The second c 웹협 Is ob 훨 ined from 빼 sa 빼 fraction were shown to be 띨 -[C 애 n)2(ncs)cl]c1o The c 뀐없 Is isolated from the third fract 土 on, eluted with 3 뭔 Hel, were also identified as 짧 -[Co(en) 2(NCS) C 꾀 Cl. On the basis of obserγations of the column elution and an analysis of the ultraviolet spectra of the eluted fractions, it 찌 as concluded that band #2 때 S 뽑 -[Co(en) 2(NOS) C 괴 C1 and band 해때 B 웰 (Co(en) 2(NCS) (H20)] C12. Aqua 펴 n of 띔 다애 n)2(ncs)c 피 + 때 S bserved to occur on the column as well as in the eluted solution. In addition, rechlorination of the aquated compound was found to occur in the eluted fraction so that after elution the second and third tractions were mixtures of the unaquated and aquated comple뼈홉 No c~stals of dithiocyanato or dich10ro compounds were obtained in the separation so that the reaction was demonstrated to be essentia1~ 1:1 between the complex and thioc,yanate.! 펀묘를 - [Oo(en)2(NCS) c, 괴 C1 was found to comprise forty-nine percent of t 때 typical product miχture. Since other products were present only in very low concentrations, the comb 훌 ned. 월 애 n)2(ncs)c 꽤 01 and c 혈 - [Oo(en) 2(NCS) (H20U 01 2 contents was estimated at roughly fifty mole parcent. 一 -. ~
APPROVED: Major professor v Hea~ of Department Dean of Graduate Schoo { 1 Date ~ 강 af fl 당 fo7 thesis is presented
r 체 E :f0 뼈 * 팩露 씌 At 양뽑앓 CliR 짧 AAT: 웹협월 A 함 H 훌.c Sf! 함흙협 AT' 효앙빠휩톰 rl 휩 E c 행뿔함앉혐훌쐐 T 훨웹휴치 F 돼휠쯤합웹꾀삐 CT 願셜썼 j 원휠함 E 훌構.T 효빼훨 FR 홉빼협훨짧 T 훌협뼈웰함 뿔짧鐵 * 휩 3:CHL 훨협협홉후훨 { 휩 THYL 월 N 월양뿔폐歸빼홉 ) 휠짧鎬 LTC:!! 호 i 휩헤 L 훨함짧흩 호 T 웹 T 웹 $ 압 A 힘 AT 혼 :,1 랩뼈 월 Y WltJt 빼 1 Tr, 훌뼈 4 웰 렐빼합 빼 T 댐홉 a1 웹 함f 협훌빼 "f 훌않 t 월 f 협홉합r 훨웰월홉 f훌 F 홉휠힐, ty 짧함짧 tj 훌협웰뭘f 홉 f 휩캅얹 J I 톨훌훨호빡햄짧 tj 휩흙 μjtl' hn홉nt 홉 f 홉홉혐ul 흙빼없8합훌쯤합r 샘홉휩훨훨T 옳휩훔훌뻐훨훨 t 훨F 학 f Art 훌 웰빼웰훌 rtr 轉 I 양 t«> 훌 Ch 홉빼 I 훌 tr Un 헬홉 r ft 훌월납양훌뽑 I 활 I 훨회 of 혈 f 팎 1 훨협짧짧 홉 A.MI 양 h 양 If 홉 Id 쁨짧 tt 홉빠법 ; Or 훌짧웹뼈, A 엽휩 U 훨 it 웰, 11 홉 67 PORTLAND STA-rξ 딛 OLLEG e. LIBRAR~
AC 훌빼압해 t 훌훨짧웰햄 T 쌓 l'u 훌웰 u 휠 ho 휠톨훌 훌 h 홉홉 to 훌 x 함 r 훌훌훌 h 훌홉훌 r 훌 tt 훌 t 월 d 톨훌 to Dr. 밝 I 훌뼈힐 re A 월훌힐 h 웰훌훌 l 셀 휩 rd 훌훨홈힐 t 훌웰 n 양쩔 th 홉휠홈홈홉뭘 r 월 h 훌 nd 한훌 1p 훌훌훌 pt' 훌훌 * 훌합 in 훌양훌 I 홈 th. 훌흩 훌. H 훌 i 홉훌훌훌 t 홉 fult 훨훨휠. 끓 at 훌훌홉 J.'. 빼합 it4 홉 훌 n.d 뭘 Ir. 훌훌 nn.l 훌합. 훌빼합 Dum f 협합 t 훌 ch$ 훌훨훨 l 훌 ivtc 훌 g 훌 nd to 웹합훨 앓蘭 n 홉훨월 J 훨짤 d 빼화 I 앙 'h 훌훌앓 y1 휴 4 잊었 tn 훌훌홉 1( t. '.t'h: 훌홉 th 훌훌훌훌훌홉끓 i 훌웰 1~ 훌훌훌웰햄훌 thl 휠향홈 to lll1 W 훌훌훌 I V 홍월 ld.
TA 합 LE OF CONTE 빼 TS...! $ 애 TRφDUCγION.... II I. φ 홉 4 훨 CTIVE 했까 ilt F 짧 $ 힐 ARCH.. Jt.... It..... II. I휠해 EX짧AN원릎 l...,:.. If............... <I.... 111.1뼈 FRAR흩 ) s함 'Eer찍 A,;................ " III If.. III III I! 훌v. 힘 { 훨 R ACTI협빼. t.. l!ii III It.. ".... l.. " if... If.... II... I I!.. I. I빼TR휩휩YCrI때빠 Tβ THE EXPE 빼 $ 써환빠 r흙lw 때홈휩 t. 1Ii.... II. 뿜R훌함MATI칭써잉F 암 { 홉훨,TARtI빼월풍짧M아OUND " III. 1M휠總 At1 좋빼 eel 搬붉N 짧월활활훨 f 훌빼 } 짧 꾀 ct 훨싼렉홉짧 * III iii 흉 XP 휠 R 후 M 훨 NTAL '"........... P 훨웹훌 l I I1 훌---?ι1 흘,. 에? 영! -- 14 호월 * 좋힘빼필 XCHA 빼췄 E 홉훨뿜 tarat 훌협빼 훌 '".. it 예 홈 4 v. 훌훨짧 ~ATION φf CRY 훨 TAL 월.'!II 흥 톨 t 월 VI. I 빼 FRAI 합 ED 홉 F 홉 CTRA ~,,- it t!.. ιzjj f i * l i 톨 II, 21 fil. 爛행앓훨훨함, 權합 LTAAVI0 않좋훨뿜홉搬 A 까 \ ~ ill if 까약 훌훨 VI 후후.. IE 합훌뼈 4 뿜 ~ι 밟챔 E 鍵훨. 짧 I 빼헤 l 와뼈 08)CI] 양 I CO 싸뽑뺨필 α 홈뱀 * 탈함 R 협 D u.cr-a 빼 X 짧홈홉 i 풍 'ii - - - -! I II 째, $ 웠 A 해 ALY 월효훨 F 합 RC 웹훨 Al.T 휩 γ ELECT 햄댐뼈 EP 합월훌 T 효월생 ".. D1. 홉 ζ 삽월월 X 합햄엽,p fh 활훌헬뺨활 R 짧빼않빼 T 밟. 댐훌훨삐 Ll 홀..... iii 홉빼滿빼야찍 γ...... *.. il.................. II.. if...... 뭘했 합훌훨 L 후협웹함 APHγ i.................... ~.. «"!II '".... " " 흉쩔 47 4 홉
IN 멀 RODUCTION I. Obj 흩 ctiv 흩 f th 휠 R 훌홉 eareh In r 훨 C 률 nt y 휩훌 r8 th 훨 techn1qu 훌 of ion- 홉 ;goh 훌 n 훌훌 ch:romatogr 훌 phy h 홉 s found u 훌훌 ful applic 훌 tion in th 용훌 r 훌 a αf φordin 훌 tion ch 홈빠훌 try. 1..7 Previou 훌훌 xp 훌휠 111'1 훌 nt.rs""~' have 훌홉 P 훌 rat 훌 d 8 훌 om 훌 trical (e 훌훌 Itrans) i80. mers and p 훌 rforu1 빼 di 홉 plac 했 14 월,tlt r 훨 acti.on 륭 on ion... 훌 xchange column,. It h 훌 s be 훌 n the primary ob~ 훨 ottv' 훌 αf th 훌 pr 훌훌앓 it 할훌훌훌훌 :reh to 홉표 t 홉 nd the applicability of 1on- 훌 xehang 훌 chromato 꿇 raphy to an, 합 1.a1y 훌 뼈 of prod 다 ct mixtures re 훌 ult1ng from r 원 actions which produc 훌 coordination cqmpound 휠 밀 I 흩 inittal plan called for the 홉 tudy of a 훌훌 ria 홉 of r 훌 actions originally carried out in th 훌 beginnin 훌 of the twenti 훌 th century by the 8 not 훌 d Swiss ch 훌 lo1 홉 t Alfred Wern~ 룹 r.- The work h 훨 rein disoussed ha 홉 b 홉 en canfin 훌 d to one of th 홉훌훌 re 훌 ettons, n 훨 mely th 훌 t between 훌훌웰헐 dichlorobie(ethylen 훌 diamin 훌 )cob 훌 It (X 훌훌 ) chlorid 홉 and thiocyanat 훌 10n. Specifically, th훌 probl 훌m 118 훌 be 훌n to d훌 t훌 rrn1nc훌 what :I. 훌 obt훌ined wh훌n the mix; tur훌 resulting from the above reaction is pour훌d onto an ion... 홉xchange column and then elut훌d totith a su 훌 table 801v 훌nt It wa훌 hoped that 뭘 orne knowl훌dge of th흩 composition of th원 product ttl후xtur휩 might thereby be gained. That 훌uoh an effort has, in 훌행ne m윌홉sur홉 J been successful i 흡 th훌 thesis of thi훌 paper. I 훌. Ion Exchang 훌 맑 loe term 효으딛 ex;c_ban2 e. i 홉 basically 홉훌 1f- 훌표 planatory, ref 당 rr1 n 훌 simply to the r 훌 placement of on 훌 ion by another in association with a
2 count 융 r :lone 빨 tis r 홉 l 훌 tively simple concept, howe ver. form 훌 th 훌 ba 훌 is for' an 1mpr 뭘훌 ai" 훌 numb 휠 r of chemic 훌 i 훌 epa 합 ations," d1 훌 plao 훌빼 ent reaction 훌, and an 훌 lytical 훌 o.11em 훌훌, 훌 nd i 홉 re 홉 pon 훌 1bl 훌 for th 훌훌 xist... ence of alar 훌훌 body of hi 훌 hly d 훌 :valop 훌 d th 훌 ory. 10 While Mo 훌훌훌 and Aristotl. 홉 hav$ b 흩 en clt 훌 d by th 훌 mo 훌 t 홉 orupul0u8 Q 훌 h i. 홉 torian훌훌 s the.1r 륨 t to r훨eo훌n1훌훌훌nd takeadvanta훌훌 of th훨 prine! 힘 l 훌s :Ln\Tolv빼d in ion eχchan용훌. :i. t 합합pe용rs th훌 t the origin of modern 1nqu~ry into lon-exeh훌 ng훌 ph훌nom훌n훌 can b홉 trac훌dto mid...nine... teenth century In훌 Ian빠짜훌 th th훌 dt홉eov훌r Y of b훌홉e or cation 홉 :Kohang. in 훌 i1. In 1 홉 45 an :Bngl 효훌 h chern 훌훌 t n 없 n 훌 d Spence wa 훌 htr 원 d by land~ otmer H. S. 말 lamp.on to f iltd out why 빼 nm 엉 nla was dl 홉 app 홉 arin 훌 from hi 홉 11 m훌,nura h훌훌ps... Wh훌n Sp 휠no 훌함 our 훌d an auunon훌 tim 홉ulfate s()l ut:l.on throu 잃 h a colw 따 1 P 훌 ok 월 d with 훌 i1.. c 훌 lcium$ul at 훌 W, 훌훌 pre 홉 ent in th 훌 $olution 훌m휠 rgin훌훌 t the 10' 빠훌r 홉nd.. A thorough 훌 tudy of th훌훌 ph휠nom"" 12 anon was undertalζ훌n in 1850 by J. T. Way-- who attributed th훌훌e cat.. ion~exchangtng prop 훌 rtl 훌훌 to th 훌 clay or 홉 1um 훌 no-rd.l 훌 C 훌훌 te portion of the 훌 all. 맘 1 훌 f :lnd :tn 홉홉 f Way and 엽 pena 훌 'Sov 흥 d th 훌 w.y for further 13 work 뭘 nd, in 1907 톨 Gan 훌, 훌 I 강훌 rm 훌 n eh 했 11 훌합. tnt 할 duoed a 홉 ynth 훌 tic alumino... si1i cat 훌용 61 to b 흩 u 홉웹 d for wet 융 r-soft 훌 nin 용 A momentous tit 훨 J> in th 홉훌 volution ofion exch 홉 ngers W' 훌홉 t 훌 k 홉 n ln 14 1935 whentw 월 n 홉 li$h cb 훌 m 훌 at 훌훌훨. A. Ad 훌 rna and 훨. L. Ho lm 훌훌...~ di 훌삐 covered that c훌합tain bakelit홉 r훌sins (in th:i s c훌훌훌 ctru 훌h훌d phono월raph r ecords) could 홉혈압han휩 e cation홉. Th훌yshow휠렉 that the lon빼월xchanging prop흩rti훨 s of thelle mater훌 a1 훌 were du훌 to th훨 pr흩 sence of phenolio -OR 훌roups which, under condition홉 f sufficiently high ph. could 훌xchange hydr잉genion for anoth훨r cation. Ad훌msand Holmes proceeded to
3 훌ynth 훌훌 i 낄 e a more efficl휠nt resin containing the more acidic sulfonic 훌c1d 앓roupe, which prov훌d to be th홉 forerunn훌 r of one of th훌 most frequ휠ntly, 않윌d modern ion... 홉 ](chang 륨 resins. A typic 월 1 mod 훨 rn lon... 훨 xchan 훌훌 r 훌 sin i 훌 Dow 훌x50W-X4, which was employ훌d in th훨 work present랩 d in this pap훌r.. Dow$:X SOW X4 i 홉 one of a numb홉r of cro훌훌 link훌 d poly홉 tyren훌 r 홉훌훌n훨 which OW훌훌 their ion빼홉xch웰nging 15 properties to th용 pre홉 ence of 훌ulfonic acid groups. - 대 - CI-I- 머 -- 대 -- - 대 - enε- cf- chεr 끼 rll M+ v S 짝 케 + γ sqh -cfl- 다 jr Re 훌 in 홉 of thi 훌 typ 훌 are pr 홉 P 훌 r 홉 d by 훤 φlym 월 r1 zing $',~yr 훨 n 홉 u$1ng divinylben 혈훌 n 월 a 훌 a at: Q 홉 slinkin 홉 -8 훌 nt. ljl =CH~ ι7 l 끼 + ~ H--CHr 끼 CRr- CII = 연 and th 훌 n 훌 ulfonat 훌 n 훌 with 훌 ulfuri 앙 or chloro8ulfonic aeid. - 대 -CHr- 여 -(1-ε 셀후요 t ~ (1 _.,(J r
4 The dear 융휩 of erqs 훌 linking can be controlled by adjusting the amount of divinylb 흩 nzen. 훌 US 훨 d. Cros 훌 linkin 훌훌 san 월 g 홉 saity sine 훌훌 tr.ight chain pφ1y흩 l 훌ct:trolyt훌월 are soluble wh훌rea. s oro훌 $1훌uk훌d polyrn흘 rs are insoluble.and 'fot' rna훌 tpurposes anion 훌xchang훌 r mu훌 t bein th홉 solid state. TQO much ero 홉 slinking i 홉 nqtd 훌훌 irabl 훌.hOW' 홉V홉r, since the re 홉 :Lnmu 홉 the 훌 bl 흡 to$w 훨 11 in o:rd 훌 rto 훌 ceo 따 nodat 훌 diff 용 r 훌 nt 원 1z 홉 d 16 ions andf 훌 c11itat 홉 th 훌 mobility of e~ch 빼양 ing ions.-... G 훌 n 훌알 ally. 월 wid 홉 selection of to 훨훌훌 us i 훌 a ". 훌 11a.bl 홉혐훌 th vaj;"yin 홉 degr 훌훌휠 of oro, 톨훌 - link 훌 ng and acid 훌 tr 훌 ngth. 짧 i 훌 appropriate r 홈 sin 1 훌 aho 월훌 n for spe~ c1ftc task. That 홉 uch 17 훌플 ins m 훌 y b 홉 u. 훌 d. to 훌훌훤훌 rat 훌훌 on 훌 in a mi :x tur 훌 t 훌강 ue to t11. 홉 fact that d1ff 훌짧 nt ions are 훌 ttraeted to a part1 cular r 홉홉 in to a d :l ff 휠 r 훌 n t. d 훌훌 re 홉. 'B or 훌헬홉,mpl 홉 i 훌 dip 때 sitiv$ 훌 on will b 훌 mar 훌 훌 t1ton 훌 1y h 홉 ld by 홉 cation- 縣훨 11. 훌 n 훌훌 r 훌훌 1:n than 홉 'monopo 홉꿇 ive 1. 엉 n. Iv 훌 n ;ton 훌 φf the $ 훌 to 월 eh 흩 n:g 휠 will <tiff 흥 rin t:h 훨 d 훨뭘할휠훌 to whi 양 h th 휠 y 훌 re held bya part.ieul 월 r r 윌훌 in d 휠 pending on t' 훌 l 뤘 t1v 훌원훌훌훌 ~ internal 끓 pol 홉 m 없 lent, eff 훨 et1v 홉 cha 휠醒 * 흉 nd ability of th 훌 solvent from which the 훌 on 훌홉 axtr 훌 ct 흩 d to attract the ion. G 훌 n 훌 rally, th 훌훌 r 훌 ater th 흩 diff 훌 r 훌 nc 훌 g 훌 n i. e 훌 n prop,rti 흉 s, the b 훌 tt 훌휠 the separation wh 효 ch can be obt 훌 in 윌 d. Chrom 훌 to 훌 raph 훌 C 홉 epal'at 훌 ons by In' 훨훌 n 홉 of ion 훌 xehang 훌훌 re u 훌 ual1y C 훌 r 셉훌훌 i out in g1 훌 S 훌 CO 훌 umns p 홉 leiζ 훨 dw 훌 th r 훌 sin. S 홉 V 흩 ral column t 월 ch... n1qu 훌 s ax' 륨 available. but th 홉 most common one for thi 훌 typ 융 of work. 17 and that whieh ha. 홉 b 홉훌 n us 훌 d h 훌 r 훌. is elution d 홉 V 훌 lopment In this m 홉 thad. a 홉 olut i. on conta 훌 ning the ions to b@ 홉 eparated is poured onto the top of th 훌 column of resin. and 휩훌 the solution begins to run
5 throu훌 h th흩 r 룹 sin. ions from the 훌 lution di훌place like~charged ions in the resin at the top of th홉 column. wh윈n all of the solution has been adsorbed onto the r쩔홉 in. a suita.ble solv용nt 훌흩 allow훨d to flow t:hrou앓 h th훌 gφlum.nbed at 훌훨 te용ady rate. 월olv잊nt ion흩 di훌place thos웰 φf the mi똥 tur훌 d따nwar4 on the column packin훌 ) but a.t differ 흩nt rat 홉 s d$p 훌 ndin용 on th흩 r 훌 lative e훌홉 e of displacement of differ홉nt i ons. If the iop. 홉 ~n "11.1훌홉tian.b 훌 orb 11앓ht in th훌 \71 홉 ibl훌 r 홈월ion, th훌n a form훌 tion of eolor싫 b훌nd월 will b홉 obs훌rv짧 n th훨 colu 麻 \. ElutIon with the solvent 훌훌 eontinli훌펴 until e훌oh b훌nd hasp훌훌s휩d thrφu홉 h the column and h~ 훌 be 훨 n colleat 훨 din ~ 훌훌훌 P 훌 rat 훌 cont 훌 in 훌 r. Und 훌 r th 훌 prφp 홉 r conditionsaa 따 npl 협 te s 훌 P 뭘효 at10n ofth 훌얼힘 mponent 훌 of the mixture m 흉 y thu 흩 b 웰 obtain 홉빠. Sel 홉 ct10n Ocf 11 prqp 훌 r r 훌휩 in 훌 nd 훌 Iu 휠 in 잃 solvent is impqrtant. It i 훌 d 훌 sirable 효 h 훌 t th 훌 bi 훌 t 펴홉 b 훌 camp 휩 ct and have 밟 lax p.boundar1 훌훌. If th 홉 solvent 훌 tr 홉 n 훌 th 효 $ too gr 훨훌 t 01" 훌 f the 훌 xchanging ion of a P 훌,rtieul 훌 r 홉 olv 용 nt is ad 릅 orb 훌 d t: 엉 o 훌 tron 훌 ly by ther 훌훌 in :lnr 홉 latioo to th 휠 ion 홉 to b 윈훌훌 parat 훌 d. th 홉 batu 훌훌 will 홉 pr 훌 ad 훌,nd run to 훌훌 th 훌합 and 훌 poor 훌훌 P 웰 r 윌 tion will be obt 훌 in 휩 all 않 1 t Jt, 훌 oth 홉 r h~nc1, the 홉 luting 훌 olvent mu 홉 the 훌 of 홉 u fic 훌훌 nt 훌 tr 훨 ngth to.a llαw the band 홉 to mo 항흩 and 휩훨 par 훌 t 훌 cont 훌 nuou 홉 ly. Optimum condltion 훨훨 r 휩 Q.l' riv 훌 d 빼 t by 홉 proc 훌 8S of t17 싫 l 훌 nd errol;".. 훌 nd it isrtot unc 빼 mon to ch 홉 n 훌훌 the 훌 tr 홉 ngth of th 홈 eluent during the 훌 lution. TR 훌 :1.1: $1: report 월 d 훌행훌 ration of coordination compound 휩 by ion"" 휠 xoh a.u 훌 e chrom 훌 to 홉 raphy was carr! 훌 d out by Kin 훌 anddl 원 tnu~e 홉 l &n I952 Using Dow 홉 lt-50 re 훌훌훌 n th 훨 y 를 e.' 명훌 rat 훌 d 훌 mixture of the h 홉 xaquachromium... (II 랬 i on t [et' (H2탤]+++, and its monφ.. and disubstituted derivitives.
홉 탈 r( 찌 C 휩 (H 랬 I 끓 4+ 훨 n 협다 rc 애휠홉 I 월 n~.2 웹 ) 싫 +, by 홉 Jutln 웰빠 tth P 훌 reht 함... 1 웰 웹월 I 획 II A 훌훨월 p. 합훌법훌 * 빼빼짧 n 훨빼뿔 r 훌훌 I 입 f 훨해 tn Of" 빠협 r 3 홈 Incr 훌빼훨 In 앓 탤 h 훌 r 협 t, 훌 h 훌 m 훌 R 휠 P 협훌 I tty 홉 I 關멸훨빼 I 협황 φf 훌 ftr 훌 t" 騙합 th 훌 trtl 함훨훌 Itlv 휩 10 빠 l 빼 S 를 t. 댐 훌 vi 빼짧빼 U 활훌훌홉빠웰명 I 빼훨훌함훌 rattn 훨 l 활 n 훌훌 f 빽 I 훌 f 홉 r 훌 Rt 힘 h 훌 r 협활훌 In thl 훌 훌 f 맑홉 A...erj 홈 in 혈훌힘빠 w 빼 # 훌함훌함 f 훨렐 I 합훨웰홉훌 P 훌 r 훌합 Itl 책훨훌홉훌헬빠빼 trj 훌뭘 t. 훌협빠 f 빼훌 r 훌월 yl 빼헤홉훌홉뼈홈 n 훨활원 tit 합훨훨훌훌 I 훌웰 헬 I 함훌뽑뭔훌훌훌 In 뼈 I 함활 i 협 R 웹빼톨 nt 월 nd 懶빠 * 훌 h 훌빼합 to 훌훌함훌 r 훌 # 훨빼빼 i 훌 tuf" 훌활훌앓鍵 * 톨 R 웰짧뿔훌 * 달웰빼 i 홉 ) 4' 關훌 j 꾀 + I 껴 f 한 I 훌 w 훌빵. Th 훌 tr 월爛 I 훌輔 i 훌 rh 훌빼 t J1 g n 월 n 합합 I 함홉 l 훌 m 짧쩌훌 nt w 훌훌훌 }μf 홉빠 Ifr 훌 t with 1 멜빼훌휠 t tn 훼 th 빼빼훨 훌암확 I 훌 I 훌협빼훌함빼뭘훌훌 I 뀔 f 훌월 with 헬쩔 애톨 CI.. $ 빠힐훌훌웰합빠셉흩 { 훌휩합 m 윌홉,. of lnv 훌훌 t1 휩훌랩 r 훌 h 훌함훌훨.,.,. 1 홉빼협 \I t, 월휘 * 홉빼윌혐홉 n 훨훌훌훌體 훌 tj 휩 I 훌뿔훌협훌협 l 훌 trl,1 합., t 홉짧 n 훌 f 훌훌 f 훨합훌 r 옐 In 월 tl 앨 n 훨앓뼈혐힐 un 혜훌 An 빠 mb 홉 r 했훌 빠렇 h 홉騙훨 F 홉홈 { 활함홉 h 훌 * 홉협훌훌헤협훌 rf 옐업 n 홉웰힐 y 뼈협 " 합 I 혜휠윌 W 엉 rk 훌 r. 홉 빼 f 빼홉암훌훌훌빼훌때 tov, 홉 F 훌 tty. 해 J 빼할홉와 l 효빠홈 훌휩쩔훌 h 훌 y r 훌함웰 rt 홉웰훌훌짧를 r 훌 tf 협 n of 훌i훌φ 훌빠빼앓홉聽 * 활협 { 빼뼈홉 >4 빼짧싫훌 # 활힘騙 { 蘭훌릎앓h 홉월짧훌암웰, th훌觸 H뭘 4 f 웰t"m,. 홉해웰뼈 1 황월혔 t혐靜납훌훌빠훌뼈힐훌,. Ilt훌훌월...1 훌합 f협훌빼함ar톨률훌활 I 훌훌no r... _'*,....,+ r...,...'~,... + ~ r... ", I,.... tr 빼홉챔騙훌 f 훌 i 훌훌 La 합훌 III 홉 l..j', L' 隨 { 훌껴 >.,J 빼 훨 )'., 1 흩훌빠셜않훨 (tn)..,.! 빼합 'I t L 싫찮 L 훌훌 J I _nw L: 훌훌 홉훌 P 11 훌짧 7, 빼활압짧훌셉훌앓협 111, 0 웰톨훨휩빼 1<1 빠첼훌훌합훌 f 합훌빼 th 훌함 r 협 vi 웰 u 훌 tv u 뼈 r 훌빠 훌훨 I 훌뭘휠 t 훌훌빼웰 tr 빼빠홉 i' 훌없헬홉 f 훌.f 펙 I 빠 1 휩홉體 n 홉 f 웰 f 훌 t-r 훌빼혜월훌훨 hr 훨빠짧 m(l 훌 X) I 혈힘훌 I t' 햄봐홉 mlxtur 혜톨 r 홉.ulfln 앓 fr 빼 tt l" 훌훌 ct. 활협 tu 합빼훌훌힌 * 훌뻐 * 훌빼 I 함함빼 r 훨 htor...... 훌 # 훌빼뼈빠함4뼈훌훌훌 1 셉In thle홉cy훌n 훌 * 훌! 훌P옐훌엉훌 I 뼈훌 f 훌웹 * 빠훔 r훌 l 훌 tlv훌빼빼ount. 양 f thet 뺑훨 i 훌蘭 l훌 "'1홉 I 빼훌빠훌웰ttll' 휩 rl 닫mm' 뼈 tur 홉, 홍협 1 웰훌 1, 월 1 뼈양 I 협kt 훌훌n 법 Myr 훌 * 휩휩 f ttl홉용f 뼈빼I 훨월랴훌 훨 Y CI햄햄협I 홉훌 } 평빼 fn At 혐햄훌 l 훌r휩훌홉훌홉훌함홉r 훌t훌셉훌 '1 鋼 tr 홉n훌 I 훌總 er훌합, [0뀔빼} 훌Cf 훌 ] CI 훨n 월홉양 } 찌빼뼈 f 蘭懶훌협φ fe훨 In φnty f 함 U r' 짧훌 ntl 뼈훌 f 훌體 tn I 훌휩 gth t 훌혐 l'ι 뼈 1m' 톨홉홉옐 U 훌 tto 뼈
7 7 뼈빼 r 웰 훌휠훌빼 fty, M 끓 h 훌 'f 훨 l 빼 I 훨 t th 훌빼냐 V 홉 r 훌 tty 협훌빠훨 by 훌홉 k 훌, h 률훌 훌 rrl 훌헬 <) 빼 t th 훌훌훌혐훌 r 훌 tl 훨嘴합홉함않 n 합홉 f 협 f 9 훌훨 m 훌 f 합홉훌 I t 홉椰훌 F 후 of 웰빼 f 웰 I 밝훌 tl 휩 n 훌훨뼈합합혀흙빼홉훌 R 웰훌훌 "m 빼 tt 빠 th 훌볍홉월 f 훌훌 * 헝빼 i 홉 h 홉훌홉 F 훌 r 훌 flo... q 훌훌훌 en p 훌 f 뼈縣훨홉훌훨훨빼홈 tl 훌 h 훌첼. 혹 nth 훌훌훌웰 R 엽훌 If 협 the,. 훌빼 P 빼 F 훌 tl 함 R 홉 th~ 훌 tran 훌 h 흩합빼홉 rh 함흩빼 lw, 협 Y~ 훌휠훌 4 홉 n -..J 빠 t 빼 d ftr, 홉흥 XX 효., Infr 훌 f 홉옐 $ 함훨훨 lt 홉 빠 홉함 tou 훌훌양함홉 rl 빼훌빼빼 r 훌빼 he 앙 h 톨방훌웰훌 rtf. 빼훨빼 t h 톨 n.-, 활 )( 홈 :h 훌 n 짧훌훌홉함훌 웰 t,." 홉 G 훌웰훌훨빼훌 frot 활훌 l I 훌헝빼홉암홉협휩 IV 홉없훌 # 훌앙훌훌 of th 빼빠 t 훔 f 훨 r 훨 R 힐밥훌 In ttl 홉 훌함홉협훌f협홉, t h. 훌훌F활훨 I 훌훌 1-" 함 'I t빼뼈 l 훌훌암웰합 ttr훌viφ 홉 t r훌활 1 훨n홉 f했f 함펙f빠혐웹홈훌훌 * 앨셉훌뼈홉tf 훌합훌함빼홈홉 tl휩훌tl 렐n φf h홈웰훌웰f훌훌 # 훨빼 ~t 휠h 훌훌훌P 훌F훌 flon h 빼렐합용훌빼홉훌훌훨빼함 'f훌1 1\ 홉삽 t, 1h빼f 함f협뼈 } 훌빼힘홉f훌한훌훌훨홈훌n 활홉했I빼빼1훌 # 헤 Ilf훌f훌암f 웰빼훌륭 I 빠혐 r 훌 vi 활 U 훌홈를함뿔,11:. 홉 nt 훌홈뼈홉힐斷 1 훨훨 u' 웹웰 et 빼월홉빼휩 F 홉 r 협훌웰빼훌암훌 명암빼훨훨 r 홉 d J; 함헤 rl'l 훌렐 t 빼 I 홉훌훨 tv, 훌훨, tn) 훌훌빠홉함헤 F 훨 μ 빨홉폐웰 nt 훨훌협 I 헬빼... 빼훌 h 훌 n9 홉 휩휠 I 압聊 1 훌훌 ttl 훌 t 홉합빼 } 훌훌훌빼훌 I 웰훌 f 홉빼앓합훌 n 빼 훌납,.r 빼 d ( 힘홉 rh 훌함훌행와 # 힘훌 양 1 빠剛 l)~ It 빼빼훌 k봐했빼n 훌훌훨훨tf 빼훌홈 V 빼훌 pr훌훨빼혐f 홉n 웰 빼훌f, 훌h훌f룹總 * 훌I 웰협씹 I 훼關훌f앓훌 u함훌펌빼 tutt빼th Th홉 φbj훌합thl훌훨 f ttl훌빼헬牌 r1 빼홈빼f빼繼함월 r. 함협rt훌월 h훌r훌 h빼훌빠룹뿔 " t뼈협tf흡j".',tt방 f힘훌활짧빼훌웰훌l 챔훨암훨fth훌함r훨웰월훌tl암 I 혔뼈r훌 r훌훌μ,., 암헬 fr 聯홉帥 rtf흩찌! 훌r t' 홉훌훌률 1 협껴빼n빼훌1th훌어협뼈 Itt 훌햄훌! 훌홉 t 훌빼 (, 훌 h홉빠 ttl합 앓훌훌 { 훌빼삐뿔훨鐵 { 훌훨 { 홉함짧 t 빼합훨 )C 낀 cl 휠ry홉 # 훌II 월햄 fr빼 f빠빼함r형법μ훨 f 빼 I 빼 * tut" 훌, t협홉함짧훌훨i 했 flt 함흥해 t.b훌훌월1 짧훌협훨톨훨 f 훨 l 웰홉 pr훌행핵양f 훌월양입 tdn협 t b홉 r 짜 I 홉월웹할 t. It 뼈훌훌빠훌활훌훌훌훌 r 월 tn 훌 f 합훌협 f 훌, t 합훨훨 f 훌 1 ", 함훨훌 itl f 홉 ld 홉 ntt 훌 i 빠 * 훌훌 tl 함 It of tft 훌, fr 훌활 tt 빼혐훌훌 l 다훌 td f 암뀔略 험훌렐훌뼈했암 "F: 웰 r ttll 홉합 ur 합휠훌훌 It h훌훌훨홉홉함양뼈합함홉빠i 홉빼t t혈 f훌 tv 뼈훌훌 'I I ty 협협뻐fr홉f홉협훌함홉훨tr훌훌웰빼빵y. Fr협활 tic훌법훌홉 } 없훌빼 If" 훨In ttl홉 i 합원 * 훌X휠 h훌헤협훌 쩔훨 l 혜f뺨l 빠흠r훌웰 f.owe빼 # 협훌헬홉P훌r 빼 * 훌훌tro홉월해 f훌if뿌홉f 훌훌웰r 홉납빼titery훌輔 I 훨빼훌F홉훨훨짧In흉멸. c함y훌 f 훌 { 훌
훨 I 홉웰 I 합홉혜 In tnl 훌 ",,,l,.n 훌 r' VI 鷹뼈햄빼 n, 爛 U 협 # 훌넬 In 챔훌 * 홉훌훌 I 웰빼 br 홉빼 I 법훌 # 훌 II 합웰 f 웹 r Infr 빼 r 훌혜합싸폐 I 훨휩 i 뺨훨 rt 셉뼈톨體 ty, 훌뼈 f 웰홉체다홉 ntlty 합懶 rk 혐훌법 b 홉훌함 짧짧 t 훌뤘 nth 빼 I 헤훌 웹 r 영합훨흙훌협 fr 혜훨훌홈훨훌 r-dh'l 훌합활 R 훨웰 m 뺨휠 und 훌훌훌 n 렐훌뼈힘흩 f 함웰 rtl 훌 3 협했 f ttl 웹 # 關훌關빠휩납 R 셈훌 1 예훌 nt} 훨훌 I 휩협헬릎 10: 훌활 fyr 훌 l 합훌 dt 훨 fh 훨훌훌 훨월 * 휩 In 훌빼 h 훌 r 훌 1 훨 $ 협 1 훨훌빼훌흙훌 U 훌훌훌합웰댐압홉혔 It 룹빠합 f 홉함웬 rt 훌셉 h 홉 f 홈홉 tilt 훌웰 f ttl 훌 Jt 훌 t 월혜 웰 f th 훌 In 뺨훌 F 훨혜빼협빠썩 Itr 빼,vI 휠 ftt 짧 P' 옳 tr 훌웰 f 짧옳 l 훨빼훨훌轉훨활 } [ 훨훨 l 빼 l 뀔... ( 빼협월 } 끓 (:J -Jn t 뻐홉훌행 t t 웰훨 # 홉홈홉 澈풀 Y 홉빼 pt 홈렐 * 훨월훨 φr 혀 fn 훌 tt 양염 웰헬略함합 U 협웰홉 ttl 훌훌 h 촬 n n 훌뻐훌 n 협휠웰함뭘했뼈 rtt, 합홉 $ 훌 tum 합함빼 I 폐훌빼 I 훌 빼홉 tho 빼 훨훌함 f 횡혈훌 r t.n 훨훌합 11 웰훨합앓훨뼈렐훨홉 n 합 } 훌훌홉훨 r t 휩훌 r 훌 f 훌폐훌함홉활홉 r 홉 l 혔앙협활법협 홉 I 웹함훌셀 1 합.1.1... ~~~. ~ I 빠 I 훨훨홉 by 훌., 빼훌협 I 밍훌한압앓 월훨 nn 훌 It An 훌 'V 훌 t 홉 φf th 홉훌훌훌압훌합 t:r 빼훌 h 휠 W 훌웹 훌빼빼 t 활빠홉훨 F 합 tl 홉홉혐 $ 홉繼 i 빠훌함훌훌함홉협 tr 뭘關훨, t 빠훌 tr 빼빼훌홉했쩨빠힘삐혐뭘랩훌 ntn f 빠홉 f 활 f th 홉활 l 훌짧짧빼혐웰 μ 빠 J 빠., 힘훌 f 훌휩빠 It 빼빼훌빼훌 tr 輔월 f 훌셉輔훌빠훌혈함횡 r 훌 tj 합원 훌훌훌학월 * 웰 훨 1 훌훌 l 홉활,f) 훨월 f 합 훨훌훌훌繼 r 월 :In 황 f 협뭘뼈짧협 Itt 훌 { 빼훌홉훌환蘭용 ttl 훨훨 i 휩훨 f 훌훌힐 l 홈뭘 Itt" 훌훌빠 { 월 It 繼 f 홉 I 함훌 f 홉뺨훌 J 헬 * 훌훌 II 월훌햄 'b 흰훌훌 f 훌휩홉 l 뼈헬빼훌훌 ttl 훌헤 * 함홉 빼쨌 f 황홉뺑빼훌,trt. 흥웰휩 1O 1 홉홉월 { 홉 l 빼혔훌빼훌 r 훌 tty 훌혐, '1 협훌혈 I 홉빼빼 # 혐빼때혐 $ 빠, 홉 tthj 훌 tim 훌 i 함함 # 협췄빼 R 넬훌밥훌 t... 합뽑훌빼輪 r 했홉 tt 협협빼 I 홉빽 In 월짧빼懶빼훌 Jr' 렐훌. '. 훌훨빼斷훌휠 f 없훨휩 r 월 In 빼 fl. 힐빼훌鍵헤뭘향웰앉법훌 j 훌웹웰 It 빼轉 I 빽웹 t. 훨합웰健 협 r 홉 U 훌뼈홉함홉훌훌 lbtll t 웰 fut., t 훌 I 빼협웰 I 홈훌훌 F 홈협홉홉훌 in ttl 홉 i 함훌 f 훌 f 훌빼홉함훌훨훨 F 훌훌홉홉월 rlt 웹,. 1 합 lw 훌훌훨훨협 l 뿜훌웰 * 빼빼 rtltf 훌압빠 빼I 짧훌rly, 짧짝 tn 1 웰훨훨I J 훌훌빠훨I 輔 f합훌 홉함훌활tr훌 합훌 R혜 I 繼훌f 활f bl 훌 I 홉 th'v' 훌빼훌 * 빼 I 훨.d 혐훌 l 훨행힐훌!ttt 훌 Xl 홉關혐 I 훌웰훌훌훌 H 했훨훨합훨 I 압책훌빠 ttl 뭘 tt 빠훌함훌훌 k 1 빽 * 웠훌훌 I 쌓 야 1I 했 f 홉뼈體협훌협빠빼뿔훌훌 { 빼빼體웰 I 훌활 I 홉훌웠렐 f 빼뼈함댐홉 l 활빼빼 f 함훌웰셀훌 n 합 y lnth 훌 홉함 $ 힐 tr 않빼훨훌훌뻐홈 tt 騙홉 Is 빼웹빼 tr. I 빼훌함훌 " 황 rt " 훨홈 tu 합 } 헬훌 f 홉 ttl 훌 t 얄홉훌합 r 뽑혔 t 뼈훌 bo 빠없혐웰 ttl 월 1 tr. t 함양 Y 훌합휩훌 It 짧홉 n 빼홉 t 합빼蘭뿔훌 r. 빼 In 훨빼 1 옐훨훌., 훌 r t:_ 1f t 빠 1 웰쩔훨 # t 웹 Y 훨홉 tj 첼훨 f 훌볍
웰 f협웹 빠 ft훌f훌 d 훌함홉훌훌 f빼합 f 없헤삽빼월훌f 훨 f 훨f뼈yl 훌합훌압 I 훌웹 tn훌협n헬蘭밝11 해훌 ; 휠헬b빼 tt"'"' {IX뿔l 훌짧협PI 홉 )(1훨홉휠합원 * 훌 tn. 헤형훨훌휠r웰 ln합혔웰 thlo휠網함빼 f 훨 Th했훨홉F홉훨웹훌 to m휩힘훌훌훌v훔함홉 t, f합홉헬뼈흩혐활할빼훌훌t 휩樹編월 * 훌 t렐빼h I 할r훨합합빼훨월y, 렐훌뼈f뼈f홉 tl협웰 th훌 縮홉i 홉빼훌훌빠웰훌 thy, 훌빠홉빡I 빼밤 i 함빼헤 J, t함합짧훨맑훌, 밥 % 훌 Y 훌 t$. 홉 1힐합빠훨 빠빠뭘업 ttl협 t t폐웰 r빼툴짧 t 활협빠훌 f뼈빼훌빠헥짧빠빼없낼홈홈혔앙훨빼 빼1 월홉월 I 핵월훌빠훌훌명 t훨행 Iff 훌r휩빼 tt 빼f홉 훨흉훌빼훌훌빼활 t 협훌압빠률암훌빼훌 t 훌빼훨 f 훌 In 월짧 n 흙훨꽤 R 첼훌 t 빠 It 밝짧 ty 혐훌빼 1 협 f 훌 th 훌 훌활훌훨 tt 홉짧 th 훌홉 I 훌짧繼쩨빠활웰뼈녕 4 훌 tt 훨 훌훼 f 힘뽑혐훨홉함훌훌함빼 f 웹훌 f 훨, th 훌 tr 훌 h 홉 爾쩨륨 o 써 J'td enl 훨 rt 홉 홉흉 1웹 1 홈廳빼빼r'rl 훌 훌n활 1 됐웰훌훨협 - 훌 f웰웰 I 빼헬 tit훌 rn1r 빼r훨책 훌빵홉활f함훌 훌f 빼홉웰 f홉 f 훌 f 빼웰훌껴 1 화찌웹繼 ut, 훌 F 휩흩웰할 I 훌훌헤 : 홉훌함홉힘훌 I 훌협혐훌흰훌합 f I~ 합웰 l 輔 )... '( 빼뼈 ).1+ L 쫓첼홉 r~ ~. ~'.,+ 훌짧 L 짧 I 훌협 i 훨렐 I 싫 ~ T 혐홉 훌훌홉 1 願훌학 f 빠홉훨홍앓쁨웰빼 *! 혈훌훌혈 # 협 f 騎빼빼홉 1 l 야톨 (... 훌 1 훌 t:r 훌짧뼈 " t 협훌, 1 훨훨합혈빼 * * 협離출합 ttl 훌훌뿔홉 關빼홉 tr'. 훌확훌 f 璥 "m 훌 tl 웰삐, :t 협홉 1: 홉휩휩 爾 } * 방 협홉훨kt 합 훌밝훌 훌웹剛 $ 훌륨뻗 I 웰 쩔훌훌했補훨 tj 합함 f 훌 n 헬 t뼈훌 훌휩짧 ~ 훨빼 * 폐 함훨훨kt활 to훌 쐐빠짧함훨훨 k 훌 n 홉행웹 t.l 훨빠훌 til 훌홈훨뼈훌홉 t 함훌뭘 ttl 빼훨함협훨훌함빼 n 훨훌양, tw 젤 f 흙 $ 훨앓훨 1n ttl 홉훨함훌활 tf'" 헤빼훌 f t 붉 $ 홉짧 I 훌網헤훌 F 훌휩법잉 Aly 웰 n 홈 1 함 # 한훌홈영 f t 하훌 tr 훌 R 홉 l 혐 흥합홉 * 짧협휩짧 n i 찌훌빨훌첼 l, 합혐 t 훌빠혈 1 훌 I 빼 :'t[f1 홉훌 tt 웰빼 tf 關합홉빼.1 f 훌웰體 n 훌훌훌 1'n t 합훌훌흙홉앓 tr 훌휠 f 흉 l 훌훌협생 tr 훌헤훌홉 r 합빼협훌輔암 f 훌 (7;. 행뿔 * 한 뼈합홉합 I 顆 dn 훌훨합훌! 합훌함뼈협홉 * 빠 " EAt- 휩빼생빼 l 싹 } 힐윷 { 빠 繼뭘, r 훌 I 훌훌헬협혈 J 훌합 tj 합웠홉 # 활 f 함법첼 rlt 홉 fl 훌흙 f 밸함합활훌합훨 Y 휩 h 훌빼협훌 rl 훌 In 훌화훨휩훌 If 홉 r 훌 n 빡훌셉짧행훌훌 훌헬,,, 훌 # 협협협훌 h.t t 하훌한훌웰 I 합 n 랩짧 * 홉협협觀 ll 1 훌 훨홉훌 } 웰월훌빠홈할 f 빼훌 혔 f뺑웰k 를빠훌總빵 I 활V홉셀 f훌법 i 홉 t1 합훨ul 훌b bit 홈繼훌협 I 훌輔훌함훌 호합 f빼 i 홉 r, 훌웰 1 뿔암협홉혈합훨훌 훌셉훌훌형휩훨짧轉 Jl t 훌함 'Jlltt 션황합 f 뻐훌훌합훌r뤘함함 tj웹함활훨훌 t 협률훨 * 뺑했함훌훌빠빼 I 폈 f월홉훌협훌 ctf 뽑홉 f" t-b홉훨 I 훌짧웰빼뿔활빠월웰훌 i 뼈훨훨씹짧 1 홉합 ftlt l 월훨휠활훌납함 r훌웰 I 휩륭뼈빼훌함훌훨 fr홉웰 f t 암훌휩훌훨懶 pi 훌홉훌훌 * 휩헤앨훌 f빼앓 & 훌찌 I 활 f삐 l 협빠훌혜 '. 휩짧 I 혐훌 } 홉훌월훌 '.lt( 훌 Ill; I 행합1 훌 1 훨훨훌월 hi 뼈 It 훌빠 ttl 홉훌활 OJ Ittl 엄혔 a 혐훌훌훌훨織훌뭘했 협월훌웰월훌 * 훨 힘훨함함톨 * 뿔 } 빼 I tγ 훌홉 t v! 협빼 til 합훔센훌셀 I 敵염 In홉웰h 훌 l 훌 te rt 빼혔윌.. H 웹빠뼈 V 훌함를뽑협혔훌훌빠웰짧훌 f 빼빼훌훌훌뼈홈뿔훨헝 * 협협훌홈 cry 훌헤훨 H 뻐 II 훌 r
10 훌뿜 tlttln 짧훌훨합합활합 r in 폐 t 廳휩 d 뼈훨 훌훌 hγi 훌협확 eu 협얹 in 홉합蘭 l 함 I 훌뿔훔홉 1 훌훨혜 I ttl 훌암빼빼 f 휩峰 I 합활 R 휠 I 월웰훨합 th 훨 t t 힘홉 J 훌 f 황훌휩 f 훨 It 힘 t 훌 활혈 tl 훨 n 협 f 웰짧 l 빼해훌홉 r 활빠빨훌합빠 # 함휩합 i 훌 tbr 훨흥 '. 형 R 빼빼 $;' r: 웹훌함휩힘홉 I 빠 i 혔 f 빠 r t 혐홉 j 홉함 ltttl 웠짧 햄훌함 1 훌 } 훌휩 4J 홉웹빠 협따훨 trr 합훨빠 th 훌 t 웰 Iff 훌 f 빼빼휠홉훌 f 웠훌 YJr 廠훌 fr 빼휠 fen 합 'f" 훌홉함혈總 f 합홉 f 합 l",,tn 훌 월 iff 톨 ~r" 훨 It t: 염 U~ 댈훌 r' 훨훌합홉짧繼 # 훌혐룰 rb 훌 R 훨훌훌훌 I 휩해 껴맡홉 r 轉합 I 없함빼험 f 훌 h n 훌훌 h 홉훌합홉 tu 빼짧헬 I 훨훌훌 hi: 뼈휩 If 웰훨빼셉흉 X 헐협빼 n 형훌 r 홉훌활 tlo 헤 IJn 홉홉 r 홉 th 짧훌 tro 홉 I 합훌 r thl 합휠 Y 훌 i 암훌홉훨 It 협훌 n 옐 h 월훨 r 훨함 I 훌훌훨셉융 chiφf 엽 1. 1 헬윌 n 셈 til 훌웰혈 f 없웹훌 tj 협해뼈.,.1 함훌훌 Jtlv 홉훨휠훨월 It.. 팎 i 홉앓양융훌훌 l 훌웰 f 훌 l 헬훌 n 훌 { 법 I 없 ht 휠 r 함 bl 훌 4 훌 th l 轉홉옐 l 빼혐 In 흉 ) e 췄훨훌 Itt 훌효훌 1 합 II 훨 rl 셀훌훌혐볍 F 훨 f 훌훌훌 I 빼헤업 f 훌휠짧뼈 m tttl 항練훌 R 훌 t 훌훌함홈 f 힌 h< 훌활 t 합활혐빠 I 關 I 빼 t p 웰한훌 1 웰 R 홉 l 합훌훌 I 맙 tt 행화 훨 ntil 합 h 훌협 # 훌행. Wern 훌 r 흩빼 1 훨 fff 훌 # 훨훌합 rte 훨 Qtl 훌 # 합홉 r 훌홉앓훌 t 훨 n til 톨홉짧훌 I 1 훌뼈 I 협頻썩 앓훌 * 헬헤웰햄韓 l 뼈 E 훨휩행합 i 쩔 4 챔 훨 } 할 IJe, 훌 f 聯 th 훨훌繼 i 輔뼈 { 활 t 함 f 훌 " The 합짧 양觀째합청 Uft 웰협 f 훌률흩 Ilt 훌홉법 'r 훌합 at ) 흩體,f" t 훌 ttl 훨 f 뼈엽협 h 懶암훌훌월 } 빼 t.r1 훌 tr 빼협훨 활협陣 f 함 f 훌짧 I 합훌합혔성휠 It 빠 f 뼈 rftl 훌 F 홈함휠햄햄홉캡협빼 i + + 十 +C- CI CI
11 The cis i 훌 Qll1er has b 양훌 n r 훌홉 olved into its optically 홉 ct i.v 훌 eompon 훨 nte and has b 양훌 n 훨 hown to a 째 uate 률 rapidly with h 훌 atin~h in aqueou 훌 25 solution.
12 훨 XPE 흙 $ 빼 E 협 TAL I. IntrQ 않 μ 훌 tl 훨합짧 tb 합 ; 짧앓협홈 r<1 없흉한 f 홉 I g 훌 r 끓, J 밟홉 f 훨 * 훌훨 pt 훌 V 훌협빠홉 tvttl 훌 'b 훌훌 1 짧함 I 홉휩했 th 훨 r 훌훌뿔홉 f 합 i 쩨홉훌 짧 run # 월훨 f 훌훌휠 fl 행함월 n 렐 til 했빼홉轉 F 훌홈훌 * 힘훌훨 f 셀웰빼홉훌 t 홉 b Ion: 빼홉 X 획 Jh 짧 $ 휩훌훌험 r 훨짧훌.. f 혈웠 r 홉함 hy. 뼈협합 ro 빼뻐활짧 * 함합훌홉홉함웹암월 f 훌빼빼줬앙 I 렐 f 뼈훌흙훨홉 I 월훌빼 tt 훌 t 훌웰활 y 훨顯훌짧훌훌싼홉 I 합빼轉협蘭훨훨 f 훌웰縮홉흩짧훨반빠빠훨뿔鐵뿔 활양 { 췄빼훌짧 i 함휠훌 I 해휩 1 뿔양 ut: 얄휩협 I 짧흉 { 훨 f 훌웰 f 빠 ttit 헬뼈빼합웠홉한 * 빠빠홈 ttl 홉훌휩훌짧뼈압활셉함 d 훨훌 r 훌 n 함 4 했홈합빠. 훨 I 혈 $ 함훨훌훌 i 힐 II' 웹훌웹 i 훌 tl 훌 n 훨 t u 廠 홉 ; 빼훌훨 n 홉 bf 빼 f 앙함 F 짧훌뻐함홉 * 혐혹 # 훨밟빠 짧 l 훨함잉월 r 휠입황빼 rtj 협협 * 합훌 f 홉함 I 홉활훌셉압 tor 합협혐첼 n 훌 f 홉훨함휠홉 19 염 Ifl 빠 n 홈 fr 휠홉 f 홉 1 빼 n 협 fttl 빼훌했뼈협 I 합뭘 ton 훌 l 훌훌함 In 햄훨聯훨했훌 rh 훨 r 훨쉴홉 * 협셉홉압 nt 짧 dh 홉책 t tn 빠 11 짧활월홉훌 h 뿔홈암 th 훌웰 f 훨함 l 뭘 f 훨휠헬혐함함월해혜훌훌뼈펙 f 험뽑폐합 hi 힌웰뼈에합양합빼협 * 합협 un 했홈 $ 뼈단 t 행훌 { 훌훌 융훨혐 f 홉훌훌 n 훌 1 합 ttl 훌함훨훌훨훌 I 흉뼈 m.f 훌 fur 홉 * γh 홉합합훌때 휩, 빼 셉뿔 t 훨홉함훨훌빼 t 휩훌 ft t 흉훌뱀홉때랩 In 휠뼈 # 빼 th 훌훌훌 i. 합뼈 i 함홉 1 蠻션활앨 4 웹혐 ) 짧 t 싫 + tl 훌 1 훌廳홉한 I 휠빼 tf 했휩함 f' tb 홉짧짧 * 빼 n tt 훨 k 협홉함 l 廳 i 鋼繼냉 fo 웹했 i 활 l 싫 + 훨 1 홉 } 편훨 l 總홉 l 빼 웠 l 휩비 + 훨훨鍵 to [ 짧 輔 i 훌 t 購형 )cil+ _. --, 짧활 Lc합훨찌 } 짧t 협합휩 3 앓jl 짧짧 to [ 짧 { 짧 i 쩔 t 熾월 1 싫 + 호 n ~ 빼웰 ftl 훨월 i 짧훨합앉.' 훌혐웰확 I 헬옐빠빼 # 훨합함 r 합법 U 했훌 of 홉,"y of th 훌월휩잉 IV 홉 훌 tla' 했 옳뽑홉월힐 { 월웰훌않. Tn 홉 I 염없홉 t 11 훨훌 I 햄 tt 훨짧합웰 $ 짧월홉 r 홉함 I 훌웰휩책 by 빼월輝 r 흩 h 웰빠홉넋협 r, 뭘 f' 훨 th 훌렐 hl 협 f 짧웰함합 U 함훌 i 훌 t 빼 γi 훨 n 훨웰 1 빼 nd 빼휩 l 훌훌 V 훌 F 훌 t r' 휠찍웹혹 h 휩 l 빼 tin 합 훨찮홉,..t, 훌협웰 f 합홉훌 I'l l 훨짧 V 뼈했홉훌 φ II 활.n 웰웹뭘훨합훌활협함훌함헝 rt 랬웰 to b 훌 hi 월 h 해 ] 월휠 - f 훨훌 I 훌훌훌함 t, 짧웰렐빠홉웹빼용월 en J 쩌훨 Q~.I t 협웰빼훌 f 斷 ι 홉웰 th 웰뚫 l 월 R 빡앞훌월홉 * 양힌 I 훨 nl 짧Cl 앓J+ 뭘f홉 k암훌懶 f앵펙옐섭웰홈홉함휩훌웰 I'γ # 합總뼈환월 ( 홉뼈 } 홉 (H 20) 꽤 +J합훌?
13 뾰 d 휠훌훌.. [Co( en) 2(NC 휩 )c 꾀 + ha 훌 be 훨 n 홉 ho 빼 to 훌얄 uat 홉 t P 훌휠 ti 압 ul 훌 r1y.t 화합홉t훌d t 훌mper훌 tux" 홉훌훌 to.2. 훌훌 * 달o( 짧훌 (NO휩 )(H 20) 싫빠. The tran 홉 iaom 홉 r 훌 l 훨 o a 예 u 훌 t 훌훌 but 훌 lt a much low 홉 r 휠훌 t 훌 th 훌,n th 훌뭘훌협훌 arm 28 훌 nd 월 ppr 훌 :-1 훌 hiy αnlyat t 훌 mp 훌 r~ 훌 tur 훌훌훌 h 앙 iv 홉 SO d 훌훌 r 월훌훌 s. 빨 I 훌 latt 홉 r r... ~.., JI.-... iilir....., 냉 + 훨뼈 pound 훌 t 훌 spee 훌휠 11y 훨훨.. \9o(en) 훌 (NO 훨 )(H 용 0) 씹 j 빼 19ht b 홉 Cφ 훌훌뭘 at' 홉 d pr 협 b 훌 b 훌훌 αrnpq 빠훌 nt 훌 Qf th 홉 pro 없 at m 훌행 tur 훌훌훌 n 훌훌훌훌웰 * 훌 ad 혹휠짧홉 * + 탠행 n)2(nc 훌 )c 겐짧훌 known to b 훌 pr 훌훌훌 nt.. 뼈 th 훨 t 훌.ot10n 훌홉 carr! 훌냉 out 훌 n 휠헬 U 홈 0 월훌홉 olution 훌떼 d r 훌 qu1r 훌훌 h 훌훌 t. Fo1:'tunat 맡 11 infrared 웰 P 홉 etr 빵 홉 n dl 훌 tin 뿜.ti. 훌 h a1 훌 of th 훌홉 bov 훌 "'0 聊홉 dcom 햄 αund 홉 효 1. Pr 훌 P 훌 ration of ξh 홉홉 t 훌 Irt 훌 n 홈 Compound 짧뿔.. f9o< 짧 )2 C1 싫 C1 w 빠홉 pr 훌 P 훌 r 홉 d by th 홉 m 홉 th 훨 d 양 f B 훌 i 훌 at:. 훌 9 압 lx hundr 훌 d 홉 r 願훌 of a 1 힘함훌훌 훌 :nt 홉휠 lu 휠 ion of 홉 thyl 훨 ned 훌훌 m 훌 n 훌훌홉 add 훌 d. 햄 i. th 훌 tir 뿔훌 n 앓.to 4 훌 Qlut 훌 on of 1 60 g. of 힐 00 훌 l 휠양 hlorid 홉 6~hyd 합훌짧훌 n.500 till. 휩 fw 훌 t 훌휠 111. 홉 2 1. b 훌훌 k 훌합 or bqtel 웹. A v 짧훌»);OU 훌훌 tort 훌 rmo 훌훌훌활훌훌 <;IX' 훌聊 n ( 톨 '1' 훌 i 훌훌훌훌 dthrou 융 h th. 훌훌 olu 훌훌 G 봐 fa 활 10 빼 t 1 용뇨활 ur 훌. (Lon 훌훌양훌훌활빠 t1 헐 n c 빼 US 훨홉 un~ 웰훌홉 i t;" 훌 bl 훌훌輪 @ 폈 d 훌 1: 1 강훌훌 ct 훌 on 홉 to t:: 훌 & 훌함 lac 훌.) 및빼훌훌 hundte 뭘훌,ll! 뼈 flftyxn 훌 11 훌 I 훌 ter 훌 0 끓 cone 훌 nt:r 홉 t 홉 d byd 합 chlor 훌훨훌 c1d 훌뭘웰 dd 훌 d, 훌훌 net th. 홉홉팅훌 ut 훌 on i 훌홉 c'\t4 훌 pφ 휠 at 훌 d on 훌훌훨훌훌 JXl b~ 톨 th un.til a ecru 홉 t fo 할빼홉 φv 훌합짧홉훌 uri 홉멸뭘 (7 흘 Om 훌.). 쫓 h 훌훌웰훌 utiqtl. 훌훌빼 110'1 훌,d to coo1 and 홉휠훌 nd 탤 V, 훌뿔찌훌훌 ht b 훌훌 0 휠홉 th 훌 b 할훌훌 :ht.. 훌훌훌빼웠훌옐 U 훌짧 pl 훌 t 훌훌 Qf th 훌 hyd 1:' Q 짧 I 함홉 td 홉 P 좋 th 훌옳훨輸훌.~ fq 훨 m 훌합훌 f11t 훌함훌 d. 맑 i 훌홉훌 a 뿔훌 wa. 홉 h 빼 w 훌 tb alcoh 홉 $ 훌따 d e t:h 홉 r 빼,nd. d 짧훌 d 훌 t 110""'. At thi 훌 t 홉 m, 훌 t 훌 tu 휠훌 J th 훌 h 힐 'cbto 훌홉 :n cblorld 훌훌훌 l 훨홉 t. 훨 n 웰 th 홉강할 "1 톨 t 훌 $ 훌 crumbl 홈 to 용 dull 뿔훌훌 n 훨 S 햄願 r. Y 훌훌 ld 83 훌 (52 함훌 r c 훌 mt b 빠톨훌 d 훨 n th 훌 $ 획 hy! 홉 n 훌 d 훌훌 min 화. 멸 i 훌홉홉願합윌 @ 합 on 훌 w 較훌짧훌 low 빼휠 10 훌훌 1y. How 압 V 훌얄 J aft 홉 r flit 훌 r- in 훌 th 훌 crystals, th 홉 f11tr.-at 훌 w. 훌훌홉 iv, 훌 lpar 홉휩훌 dfurth 훌 r unt 훌 1 훌 t eru 홉 t 휠 d 당 ver a 훌훌 tn, wh 휩 1" eupon 훌홉홉 cqnd b 훌 tah 책 c.ry 빼 t 훌끓 wa 훌 obt 훌훌 n 훨 d. 발 1t 훌 p ::r: oe 훨톨 g 혐훌훌 r 훨 pe 훌 t 홉 d 훨 ucc 훌훌훌 fully a th 훌 rd tim 홉 but th 훌 G 합 y 훌 tal 훌 obta:lned on 훌 foι1rth 훌 tt 鄭 lpt w 홉 f 홉 contamlnat 훌 d with light... y 훨 llow-
14 훌 r 홉 en 1.1 훨 edl 훌...shapedcrystals. U 홉 :tng half 훌 mount 홉 of tho 훌 egiv 홉 n in the abov 용 :Ln 훌 truct10ns 흩 a total yi"ld of 58 홉 ram 훌 or 7.2.6 p 훌 r 엉원 nt WEI 흩 obtain 훌 d. Th 흡 c()mpoun~ W 훌훌훌 na1y 훌 ed for cαb 훌 it by an 홉 lect:rod 흡 po 훌 ltion m홉 thod-3o Tfl훌 P 節 C홉nt cobalt c훌 leul월 t휠d 01" 활o(C 2 N훌H 8 )C1 2 ] 01 1, 훌 20.6, 홉 nd th 휠혐 er c 훌 nt found wa 훌 20. 정 ( 훌훌훌 pas 월 47). 훌뿔 때훌 R 홉 actto 따 b 훌홉 W 활홉 n 靈짧 * 흩 o( 훌 n)2c1 찌 Cl and S 짧 휩 훌n 훌 tγp :l al 1:' 훌act홍on훌 20g. (.072 mo끓 ) Qf 후표짧훌 얄o( 훌n 2012]01 'II월홉뭘훌홉훌 01V' 휩d 후월 3뭘빼 J 양홉 훌 t 홈r. Nod 흩r훌 t홉 h훌훌 ~ing 'II훌훌 n홉 홉홉 Bary to 홉 ch:l휠va com뱉했훌훌olut훌on. l' 빠n홉d :L훌t훌 1y u훈q합 addition of 홉 $olut훌on φ 6 If 8 g. (.α70 mol핵 of lcscnln 1 5 mi. ofwat홉 r. fln훌 gr 휠en cry훌 tal훌 of 뿔짧홉톨탈o( 훌n)2C1찍 ] 홉 쐐 form홉 d 훤 't o훨훌훌광. Th훌 result훌 ng b:r훌훌ht... 훌r 훨en slurry wa홉 h홉훌t훌dwi. th 얄on훌휠훌nt 훌 tirrln훌 un합 lcomp~ 훌t e. 홈훨 l'ljtiφn of th훌훌re 節훌olidw훌흡힘bt. 훌ned at about 85 d 훨gr$e 훌 맑I훌휩휠 lut효양nw빠 " 1:11월n 훌 11φtV훌d to eo합 1. A J 률r훌홈 qu훌nt 1. ty of p 懶 l 홉짧 Y 홉 t 훌 1s φf 훌훌훌 * 월 t 훌 n)2(ncs)c 괴 Clpr 융 cip 훌 빼 t 홉 dw 훌 thin 훌압 hour. 맘U~ ery훌 t훌 l 훌 W훌輝훨 i훌훌red on a 훨갚chn훌t 훌una훌1., "', 훌훌h훌dw1th 짧 P 훌 :r C 훌nt 흩 th"nol, and dr1훌d in 훌훌t'. Th홉 d훌훌p을 v훌olet f훌 ltrat홉 y훌홉ld홉폐 Illor 홉 of th 훌 pu~pl. en:)' 홉짧 l 훌 U 함 n furth 윌훌를훌획뼈훌 m 훌 훌 n on 홉 P 훌 rt 없 u1 훨훌 훌 n 홉 t 뭘,ne 용 Wh 흡 r 훌훌 h 훌활 olut 훌 on w 훌훌훌 110 햄훌 d to 빼 훌,nd 0\1 훌 l:'tl 훌훌 ht b 했 @ 얄훌훌,ny cry 훌 tals W' 홉 r 훌훌훌앨훌짧 edt 흡함 P 휠 @ 옳훌,m 홉 t 훌 1y 18 g. φf th 훌 eot 빼 φund 爛룹 obta 훌 11. 훌 d. 빨 i 홉황 l.ud. ty we 훌 n 협 t,ho 함훌향훌 r,d 휠 te~11lin 훌 d. IV. :ton- 훨훨양 hange Sep 훌합 ation. A number 0 훌훌 φn..,. 훌 ~cb 願흙휩훌 $ 힘훌 r 훌 t 훌 on 훌월훌 th 훌용 produqt m:txtur 홉
l 흥 resultin. 훌 from th홉.bove r 훌act훌on were Q훌rri홉d out. The 훌월rli 홉훌 t on홉 $ W훌합훌 of 훌n 훌징 {plot' 훌훌t훨1:yn훌 tur훌훌 th훌 O핵홉ctiv휠 b짧ng to 훌훌훌 how In홉 ny band 홉 form 훌cl. wh훌 t th웰y1α 양lζ훌멍 t 훌k. e. tq wh훌 t 흩x: t 홉ntth 훌Y could b훌훌훌p"" ar했훌d j and 빼h 빼t klndand 룹 했다홉th of 빼utln훌홉olv훌nt 훌hould b휩 U훌윷d to p홉rio: 빼웰n Qpt훌rou빼훌훌함훌할훌휠훌on. 훌ot뻐흩훌 I홉輪 :1." column Ii홉F훌뿔훌t 훌on훌 w훌훌훌 훌1:1' 1 훌et out to 훌홉잉I훌 t훌 mat홉할11훌훌 f엉합 identifie훌 tionpu: 할뺨08훌훌 F훌n훌 11y. thl' 훌훌훌홉 F 훌짧훌 tl 잉 n 훌 w 윌휠홉훌 i 훨휠 form 훌 d f 훨 r th 홉훌당 1 훌 purpo 훌훌 of 훌훌 tltn 훌 t 훌 n 홉 th 훌 r 월 l 홉 t1v 훌함 ropottl 합 11n wh 훌밝 1 th 홉함 roduct 홉 훨함훌 form 홉 d. :It 훌훌 USt홉ful to d홉홉cr뼈훌 onlyone typ훌.eal 홉훌뱉r 훌 t10n h훌짤훌. Any vall' 훌훌 훌 on 훌 ob 원 er" 훌d will then b홉 d ;t훌 cue홉홉d. 뼈Olt ofth홉 coll빠 un 월홉par~ 훌 eialt훌 w훨r룹 ca양ried out in 휠o mi. gla$ 훌 bur훌 t 홉. A 훌 I훌훌홉홉 WQot plug wa홉 1n활홉rt홉d 훌bmve th훌훌 topoock to r 홉t훌in th 훌 r 훌 a 1.'ll. 빨 l 홉 r 훨.tn (Dα 훌 x50w"'x4 훌 nd 뭘 OW..XB 14' 훌 lt' e u 훌 ed)w 훌톨 W 월 sh 훨 d with the 월φIv훌nt 1: 원 h훨삐월홉려훌nit훌훌11y for 훌 lut1n훌 I 훌nd then pour훌d in 홉훌 1u. 휠할y 훌ntQ t:h홉 c:ol\ 熾... 뼈Or훌훌al" 훌 'fit 'W~ 훌.introduced through th홉 top of the colu빠 l 훌혈냉혹all앙w홉d to run throu훌h the훌 r홉홈io, th홉 solv' 빼nt 1홉vel n홉v훨r b훌1n훌 al10햄훌d to.11 b흩 low the t월p 힘f th훌 column of 양훌홉tn" wh 훌따 th 홉 r 훌훌 in h 빠 d 훌훌 ttl 훌 dw 훌 11, 훌훌훌앓 ond gl 훌훌훌 We)< 훌 1 plu 훌 'w 훌훌훌 n 빼 ert 홉 d 훌 t th용 topo th훌했훨in e합l다ron to pr휠 'v훌llt 훌 ts d1 훌t"upt훌on wh홉n intra... duein 훌 th홉용 olut 훌 on to b훌훌naly껄웰d, 훌nd tq tilt 훌r out in훌olubl훌 matt훌r 홉U잉h 훌훌 d때at 를빨i훌훌α1v훌nt wa훌 th흩n al1q뱀훨d t훨 flo빼 to th훌 l 훌 V훨 1 of th홉 upp훌얄훌훌훌훌훌빼cql plug and 훌훌 pol" 할 ton of th훌훌 olution to be analy훌훌d w 첼홉 po 빠 t 훌 dintφ th 훌훌 col 뱉 tn. Wh 홉 xl th 훌 solut 훌 on h 뼈 빼 11 휩 n tφ th 훌 l 톨 V 훨 l of til훌 uppe합홉 l훌uj' WQQl pio훌 l 홉 lut 훌n훌훌 olv 훌nt Was a말웰 in introdu 휠훌d and th훌r 홉aft 융r 빼훌 :Lnt훌훌n훨d at ~ 훌 con훌 tant 1홉V훨 1 approx1m훌 lt훌 ly 앓 5 ml.. 훌훌bφv 홉 th 홉양훌홉 in col 따앙n 웰 1 1,1훌nt w: 훌 8 훌ntrodue 훌d th합 0 1,1월 h rubb 훌r tubing from 훌
16 1훌훌k place렉홉bov홉 th훌 level of th홉 top of the bur훌 t. Th훌 flow rat홉 was a협압훌 t 홉d 'by means 양 asel:" 훌야 elar뺑 to incre훌홈훌 very 훌r홉dually and a constant 11훌훌ld was nud.ntaln훌d at th훌 & 훌sir훌d lev훨 1 by drawingth홉훌훨c훌훌뽑 off with 훌n 훌홉.p~rat() 할 A. A Continu 협 u 훌훌 lut 훌 on In 4 parttoular run 1 ml.. of pr윌duct mixture, from 훨 '1h 훌 eh no cryst~ 앓훌 had y휠 t form홉 d. w훌훌함 받훌 tt훌do onto 훌 col빼n pack홉d with 1)ow훌표월OW... X8 r 홉훌 :tn to t!l h훌 i 밟lt of 29 em. 월 lutiqu wa 월 b 휠g납ow 훌 th 0.5 엎 HCL, Q con홉 t훌nt h훌ad b 훌ing mainta훌n홉.d at 23 ml. 홉bov훌 th훌 r훌훌훌in. 맑I훌 flow rate wa홉훌pp1" O쳤mate1y 0.7 ml. p훌합 minut흩. E훌rly in th훨 elution three color훌d b홉n웰빼 b 훌홉훌,n to 훌X tn; 웰 bro훌d d훌x-k viql훌 t low훌 17 b훌,nd (11). 훌 som. 훨 wh 웰 t em 헬 11 훨 r r 홉꿇었 ah b 홉 nd a 훌 hart d 훌홉 t 훌 no. 홉 b 훌 h 훌 nd ( 밟 2). 훌 nd 훌 V 훌휠 y nar합ow l" 홉 cl band 훨 t th웰빼p of 휠he 양oll빼ln ( 總 ).. A훌훌lution progt' 홉훌흩훌d. S훌맡at' 훌휠ion 훌,mproV' 훌d. 확nd b옳nds fftl and t~2 mov훌d 앓r훌du훨 11y dα없 1 th훌 휠 l빼in. 헤 ~l mov'in월 m합홉 t r훌! 흙 idly. 홉v홉,ntu훌 11y. 縣훌훌뺨.rat핵 1ntφ 홉 slowmφv훌 ng 1훌훌ht-r짧 링olar홉d b빼,ud ( 빼2b). and a.. mqbil 훌 re d.d 훌 eh boll와d ( 빼 2a) Wh 훌 n b 훌 lnd 11 h 훌 d 룹 lu 휠 ed.th 훌훌활 r 헬 \8 휠 h of the 훌 lu 홉 nt wa 휩 incr 훌훌훌빼훌 d to i 편. 멀 h 훌홉 olv 훌봐 It eα11te 轉 d betw 홉홉 n b 홉 nde 웹훌 n<1 빼 2. wa 홉 합 10r1 훌용 s. 1ndie 월 tin 흙 th 흩 It 훌털 ompl 훌 t 훌훌훌힘훌 trat10n 잉 f th~ 훌 seft 훌 ction 훌 had b 홉훌 n.ccom' 뺑 11 홉h훨d. 월nd th훌 t no 훌qu훌 t10n h훌d (} 휠cUX't"ed in band 밟 1. 뼈훌nd 뼈b b 훌cam훌 xno효앙 d 훌꿇 fu 훌월 a 훌nd the ar홉훌밟 ~ 휩훌n b훌n웰빼훌 and b훌.nd #3 (which had b않un to 1.'Q()V훌훌훌CJWly a.ft휠r th훌 eh훌n훌훨 1.n 훌 luent 뭘 ξr 훌n훌 th) was lightly pink~cαlor훌빡 tath훨r than th흡 off특whit훌 color of eh월 re훌훌 in. Aft 홉 r b 훨 nd (;2a wa 홉 eoll 홉 ct 훌 dth 훌 aoid 훌 trength '(fa 휠 :Lncrea 훌훌 d to 3 M. and b 훌 n.ds 12b at 뼈에 ~3 Wf!X-E! elut 홉 d. B 훌 nd IF3, a 홉 di.4 훌 11 b 훌 nd 홉 J spr 훌 ad
17 out 훌 om훌 :what as it!nov짧 do따 l thecolumn. A light pink band remain훌d at th훌 top αf the cφlumn wh훌ell could not b 휠 collec. t훌d sine훌 훌 t sp:r훌ad 빼nd bee훌m홉 V웅ry di :Efu홉휠 "With f다rth훌r elution. A r 훌흡 ora of the.abov홉 를훌P훌tr훌 t10n w훌훌 k훌pt i훌nd :Ls 11' 훌produe 홉d h훨r 훌. It W~ 훌훌 run without ce훌훌ation, x 輪 u훌ring a tot뻐 of 31.5 hou엎 s to eom" plete. 홉 ICORD OF 1 훌 LUTtON 뚫멜월휩 1an 홉홉 d o 2hr$. 35 min. 5 hra. 50 t힘훌n. Con 빼힐 lt 홉 훨 lut!on is b 뤘 gun with 0.5 앓 HC1J. Band 홈램 1. 뺀 2. and 짜 3 h 홉 V 홉 cl 훌 ar1y 홉웰훌짧 t 홉 d. *3 look 훌 quite 홉 mall at this po1nt. 1;1 :L훌 well s 홉parat흩dfrom 뺑2 which h훌훌 all' 훌훌t lnto 훌훌휠합ong low뭘t' and a. weak upp~ 휠 band. 12b 뾰훨. 20m:Ln. 없 l 훌휠 e 앓 ion b 훌합 F 월훌 n ffi2and 빡 :3 is 11 앓 htpink tn 용 t 훌훌 d of th 홉잉 ff wh 훌 t 홉 of th 활 r 훌훌훌 rt t tndtc4tin 훌 itl om 휩훌홉 tel 훌훌 p. 훌 r~ 훌 t1on. 14 hr 홉 40 III 흥 n. l 월 hr 훌. 19 hr 훨 II 2 월 min. 25 hra. 31 hr&. 30min. B 훌 nd 쌓 1 is com 밤 l 휠 홉 1y 훌 lut 훨 d.»:11.1 훌 nt :Ls 휩 ha 웰 gad to 1 웰 He 깎 # 훌 a h훌빼 훌 lut 훌d. 12b 1. 훌 v훌ry f홉훌at. dif훌u훌훌 Elu 융 nt i 훌 chan 용 ad tα 3 월 HCT1. #3 has 훌 luted. Shut off. B. 훌 nt 융 t't' upt 훌 d Elut 훌 ons. The above 훌훌 par 훌 tion 톨 ~a 훌 run w 훌 thout 휩 topping the flow of elu 훌 nt through th 흩힐 01 빠 ron 훌 t any tim 용 _ but most of thos 훨 ea:rri 홉 d out w 융 re
18 (du 휠 to the 1훌n용 th of time nee융g 양ary to com함 let휩 a 밀홉pa :r ation) shut off a numb웹r of times when they couldn t b 훌 checked within an hour. Xn columna which were elut훌d over a greater len앓 th of time, with fr흡 qu홉nt interrupt훌 n. it was obs 휠rvedthat 효wo or t:hr훌훌 more bands ()rm~d bt\! tw솥 en th훌 '2b and 밟3 bands ooth훌 φlutnu a.t th 훌 훌Xl' 융ns 훌 of band i쐐훌 Sine홈 th훌g훌 뼈nd훌 훌F훨훨훌짧d to 훌흰파t φf꿇 from b훌원d 빼훌훌I th했 w홉1:' 0 l훌b흩 l홉d #2b t #2c. and #2d. thre훌 b홉tng th휩 most ob 훌훌 ~rv핵 J and u률 ually just two. In 엉,ne of th훌 last 훨홉p a.ratiqns mad흠. the #2d band wa 훌 much stron 훌 er th훌n band ff2 a. by th훌 time 밟2$ 홉 luted. It 훌깨rentually b휠 C훌me clear that the n때 뼈nds t'1er홉 홉ppearing wh협n elution was r 훌홉umed following an int월rr u.ption~ indicating that 홉om훌 thing had happened to th훌 m빼tar! 홉 1 in b훌nd ff2 durin, 훌 빼 흩 tationary period. 빨1훌 bands formed in thi. 홉 manner 홉pp 훌ared to elute 훌 t about the 홉arne rat훌 and w훌 th 않l홉 g 廳훨훌랩훌ngth 훌cid 훌 s band ;3. 훌짜 all of the s 훨parattan원 it was noted 함lat the r훌훌ion b홉 two홉en b용nd훌 *2a and #3 waa a 11 훌ht pink color c. Oth 홉 r Comment 홉 on ] 휠 lut10ua In some Qf th훌 c.olumn 빠utions which w훌re ] 책t' form홉 die w-a 훨 ob홉훌rv훌d thata\lt밟 l.t- viol홉 t band s 홉pa합휠 웹d from th훌 rest of th훌 훌0" lution 홉nd elut훌d 빼ithin Qne balf hour of commene용m훌nt of 훌 lution. A 홉uff 훌eient amount of th훌 s fraetion to obtain crystals wa훌 nevt1r coll훌at홉d, but it 1훌 hi앓,bly probabl훨 that 훌 tw훌 sa n홉utt-al but pola;r compound. III addition to th홉 light pink band which remain흩 d at th웹 tφp of th훌 column aft원r elution of band 뺑3, SPm홉 v홈ry d훌rk brown material wa홉
19 ab 훨orbed on the top of the column, and could b휠 mov훌d a 1 훌 ttle 없, 1y with 6 엎 or 훌 trong휩합 He::!.. Other 훨olutions were tried 흩Ul 홉 lu훌nte but none was found tc b홉 & 훌 sat! 홉 f훌e t:qrya홉 HCL. Sodium chlorid 홉 was found to be too 를 trφngly f훌 :~ored by tl1. 훌 11"$ 훨 in a훌 op함 g홉d te t:h훌앙ompound댐 to be 뭘훌P월rat홉d, a훌훌양 \Tid훌:ne. 훌d by th홉 fact the톨 b훌nd훌홉p:r 4훌훌d and ran tc)g~ 훌th훌.): when it wa훌 us휠d. 룹od 훌urn th뼈cyan훌 t홉 pi'φv훌d to b훌훌0$' 훌 :wh홉 t b훌tt홉r than 멜odi합m chl 휠 ide. 훌nd w, 훌 s u훌홉d t휠훌.dv.ntag~ in 혐1"1훌P 훌 'r:tn훌 th훌 thiocy훨 n훌 t훌 salts of th훌 campl훌x흩 e for 1 nfx' 훌r 훌d 흩함홉et1;i4 A pt' obl훌m with u홉ing s홉 It 홉 a 룹훨 luting a 휩훌 nt 훌 W 훌훌 th 훌 tl wh 훌 n th 훌훌 l 피 t 홉 d fr~ 훌 et10n 홉 w 훨할윌 evsporat 홉 & to αbt~ 훌 in cry뼈a1홉 crystal훌 ft' otnth훌훌 lu훌nt 'Would p1;" 훌cipita. te betα휩훌 or copt" 흩cipita. t훌 with th용웰홉 sir훌d 훌휠 it. It 14'< 훌훌 thought tb훌 t p훌rhaps U홉훌 :> 훌 neu t: r 훌훌 1 eluent mi훌ht be pr훌fer뭘hl홉 to ~ 훌훌 trongly 월c1die on훌 but as홉홉ntiallythe 홉am훌합훌suIt훌빼윌r 홉잉bt훌in훨d 훌lndth홉훨ompo따 u.t훌 1n 옐U훌훌 tlon 훌pp훌at to b홉 quit훌훌 tabl훌훌n strongly ac훌d훌em훌d 훌뭘. v. 훌 sqlation of C 합 y 홉 $ 훨 18. 효 n otd 홉 to to :obe 훌훌 n pu;t 홉 crystal 훌 휠훌 nfr 훌,1" 홉 d 훌 p 훌 etr 훌 1 an~ 훌 11 홉훌훌 it wa훌 n훌 훌a 훌ary 휠 o I흩iV POt" 월 te the 훌r: 훌 t훌on' elut훌d from th훌 ion- 홉xch훨n! 훌eeolwnn. 훌tl th협꿇t홉 t 훌 tt훨mpt훌 to αbt훌훌n cry홉휠훌l 훌 in tht빼 m짧tn훌,r.. th훌 solution훌 W홉합훌훌V훌pOX'4훌짧뼈훌 t 1양wh훌훌Lton a hot p1훌 t홉 until th 훌 y b 옳 cam 훌홉 uffic 훌훌 ne1y cone 홉 ntt.' 훌 t 홉 :d fa 합 cry 홉 t~ 훌 11 훌할훌휩 it 때 In to 강 ceur. Cl 훌웰 t. c010111 훨당빼 cry 홉 t 훌 I 룹 W 훌 r 훌 ob 훌훌훌 in 홉 d f 합 011\ th 훌훌 f 훌 rst fraction. 훌 t W 었훨 au 월 P 휠월 ted, and 홉 ub$ 훌 qu 홉 ntly eonfix'ul 훨 d by 훌 positiv 훌 flam 훌 t 훌훌 t for pote 훌 S 빠빼 1, th 뭘 t th 월휩용 W 윌,t' 윌 c.ry 훌 t 웰 1 홉 φf 얻 at 훌훌훌 & 따 n chlorld 홉. Wh 훌 n th 훌 solution w 훌 s evaporated further.,,1.01 흉 t cry 홉 tals copr 훌 e :1p1tat 홉 d w1th
20 the calorle 룹 s on 홉 s. Evapor 홉 t1φn of th 흩홉월 eond fr 흩 l Q. tton over a hot plat 훨 re 홉 ult 훌 d in the fφrmati on of 훌 >mall 융휠원훌 n ory 홉 t 훌 l 훌 about the same color as the 월 t월rttng compound t 훌鐵활편o(en)2 C1 흉 ]01. Th:f.s wa 휩홉 surpri 훌 g 홉 inc 훨 the $olution from which th 훨 cry 홉 tal 훨 prec;d,p 훌 tated. was r 훌 ddt 월 h 훌 n color wh 홉 rea 훌웰웰활 Fα(en 꿇 01 꾀 Cl i 훌훌 re 훌 n 1 월 gφlution. 죄훌홉.[Co( 홉 n)2012] 01 률 hφwever. i 훌 d 웹 rk viol at and. it $$ 훌 m 홉 d r 휠.asφu 빠 ble to hypath 융합. 홉휠 that the t 풍 an 협 form h 훌 ld :i. sorn 훌 rt 홉융 d to th 훨 cia which h 훨흡 b 훨 en repol"ted to b~ 월 31 the mqt'e stabl 흉 form in 월 old 월 olutionφ 월 inc 홉 it app 홉 a1" 휠 d th 훌 t h 용빼 ting 101 훌 htb 훌 caus:tn 훌 r 홉 arrangements to oocur; 17φam t 훌 m 함앓훌 ture 훌 vapotat1on 훌훌 n 홉 따 R 훌 hood w 홉 r 홉 att 훌 m 함 t 원 d. Und 훌 r th 훌홉훌 (iondtt :Lon 훌훌 uneontam1n 훌 t 훌렐 viol 훌 t c r:y 홉 tal 홉 were obtatned 죠 rom th 홉 first r 빼 cti.on. It 훌틀 11k 홉 ly.how 훌 v 훨 tt, tn_i: col 월 't less C 얄 ystal 홉 oipφt 훌훌 si 따 xl chlo X' 훌 d 훨함훌 It:. 홉 not 1so1at 훨 d. notbeoause of th 홉 m 훌.thodofE 훌 vaporation u 훌훌 d, but b 훌 cau 훌협 so d1ffer 홉 nt strength 훌 lu 훌 nt wa 월 U 훌홉 d to 훌 lut 훌 it' 훌 otion 에 ~l. ach:l 홉 vt 다훌훌훌훌 paration fr 빼 nt pota 훌훌 tum iqn. Addition 훌 11y, 훌 l 양 훌할훌 훌 d at 휠홉 n 훌 th would hav 훌훌 10 빼홉 r ehlor 훌 de 1Q 찌 cone 활 ntr 월 tion,. r 홉 qllir1n 훌 nto~ 홉 evaporat1orito r 휠홉 chs 훌휩 ur 훌훌 tion, 훌 lthough. th :t 훌 훌 ctox' wouldt 훌 nd to ufi 훌뀔 tbαth I(Cl andthe v 훌 01 릅 t c 짜 npound in th 훌홉 ame way. '1'h홉 cry 훌 tal휠 i 홉 olat 훌d rom band #2a by 홉 low 훌vapo합 ationat t'oql1l t윌 iillp.~atur. w훌r 용 s1용ntile 훌ntly uti 騙 r훌nt fromth 홉훌 bta!ne 훌d by e.vap" oration OV훌11 a hotplat휩 Aft 윌11' r~lativ훌 1y little. ev훌 poratian had t웰ken place. 1훌ky ot'an홉 e Cty훌 t훌 1s formed on the top of th월홉oluti. on. 앞lee훌 w훌re 0011훌eeed on a. filt 훨r. Upon furth웰1:' e'vaporat 훌따1. ho' 패했훌 r. fine r 휠dd1sh cry훌 tals wel' 홉 obt훌 1ned and 1. t app 홉 ar 훌d that 훌 ither two
21 different compounds w융 re pre 홉훌nt in frac휠 ion p2a or one compound w훌홉 crystallizing in two diff 당rent fo홉n s. Nα gre훌,n crystal훌 wer윌 QbtainE펴 in th홉 room t em받 e:a;ature 훌 :va.poratiφus. Slow 훌vaporat!on of fraction 웹 yielded cry원 tals similar to theredd1sh cry훌 tals isolat윌 d from ff2.a. G훌nerally, 훌홉uffici웰It amount of 홉 olutiφn wa훨 not obtained to 1801훌 te cryst훌 1s r야n r훌etton흩 #2b f #2e, and #2d. V 효. Infr 훨휠홉 d 앓 p 원 ctra Th훌 potas뭘 iurn bromide p훌 11훌 t method w훌 s u훌홉d to prepar융 cry윌 ta11in홉 sarnpl휩 s for infrared ap원ctra. Sp훌ctra w훨r 융 recorded on P 월rkln... Elmer 137 ln racord and a 융엉kman 짧 l양 record:tng spectrophotomet 융rs. The IR-12 w훌홉 th훨압1φr홉 us 흩 :fulo the. two aince :l. t re$olv 홉d a. gr 휠 at 용 r numb 흩r of absot' 함tion pe.k$ and gav훌 mor훌 preoise w, 훌 1a numb흩t' readin, 훌 $, Prec1휩 e re뼈 :Lng홉 w훌r 홉 n훌eessary sin강훌 the, spect 뼈 of th훌 앙mpound홉 to be separat훌 dw휠ore simil훌 ;r in many reap 홉 ets. N휩 :V훌rth훌 less, th뭘 spectra obtain홈 d from th홉효nfr홉cφrd w훌t훌 φ u 홉훌 f 합 campa웰훌on purpo lij웹휩 and a. numb 휩1" of th훌홉훌훌peet얄훌t.ax' 훌 1명prαdu 훌d her훌. 홉i훌nif! 양홉ttt points c.one홉왈n:i. 다훌 the 훨nalys1훌 ;0 th 휠 때 fr 훌r 훌d spectra ar홉 not훌d below. A. The 훌 nfr.r 짧훌합훌 ct 할훌없 f th 훌 viol 짧 crye r: 훌 i 홉 fr 짧 l fr. 훌 etlon ('1 obtain 훌 d. by 훌 lution w1 th He1J 훌 nd th 훌 t 훌 for 훌훌훌훌 un1 훌웰할 b 휩 tn 훌 chloride salt ( 홉홉훨 figur 훌찌 } 훌 howed 홉 ingl 훌 a.b 훌양뼈 t 훌 on p 원 4k 홉 aro 삐 t1d l6oo m--l ~l ~_~ o~n.. nftn -1 훌 nd in th 훌 1100",, 1150 em. - f and 870...900 om. -~ t 홉 gian 홈 j thu 훌훌 nd 훌 G 훌 tin 홉 that it is 0 1.7 the 훨 ran 홉 Qonf1 훌 ur 훌 t10n by the cr 훌 t 훌 r 훌 aof Mort! 홉 and 32...1"1... ~... _... 33.. _ ~... 34 Bu 훌 ch» 熟웰 :nb 훌합 l 훌 :ln 웰 nd 월 ail 훌휠 J~- and B 훌 ldw 훌 n r 훌훌 F 훌 ct :lvely. 훌 th 홉 oompound w 홉 r 홉 f tn 홉 l 훌홉훌훌뀐 nmetr :1ea1 c1 훌 form, 합 tα 훌 b 훌 orption peak 훨 would app 홉 ax' in 휩 a 힘 h of the8~ region 훌
22 표 Since a. single strong thiocyanate C...N stretching peak was... 1 abs 훌 rved 1n the 2100 em. - r 원훌 ion; th 훌후 E 훌표훌.dichloro complex wa.s ruled out j 1 월 4ving as th 홉 Qnly t 빠 o possibilities 훌훌훌표뭘 - [Co(en)2(NCS)Cl] Cl. and 앓훌탤.. ICo(en)2(NCS 월 ]01. Thξ fαrm 훌 r wa. 훌 eu 훌 l pected. and subsequently cαnfi:nned by comp 홉 rison of th 홉 frequ 훌 neie 홉 of absol ption peaks in the 윌 P 훌 etruiu (se 용 figure 2) of crystals 1 홉 α1at 홉 d by 홉 vaporat1on of b 훌 nd #1 (obtained by elut 웰 n with NaSCN. and ther 홉 fore) as 훌 umed to be th 월 thi 앙 cy 훌 nat 훌 $ 홉 it) with 힐흩 ak 훨 reported by ι 3 월 r"'..,~., :Chamberla1n and Bai.lar-- for 훨웰월 :-LCo( 훌 n)2(ncs)c 핀 SCN. TAn L 홈 1: 0 때뼈 ~AR 훌 SON OF l? 활 A1{ FR 휠 QUE 뼈 훌훨홉훌 N THE SP 훨 C 짧 A OF 뚫많월 i 펀 훌 n)2(nc 월 )c 펜 sen A 때 D 빨 IE VIOl 휩및 CRYSTALS FRIαM 월 AND (;l 繼짧.~ WO( 때 I 앓 t 뼈 (8)0 괴홉때 732 em.;-"l 7 월 7 112 훌 2α5 훨 1141 "v 훌 01 휩 t Cry 홉 tal 월 732 em.- l 787 1127 2060 2140 c. As will b 윌 recalled. two type 훨 f pr 훨 cipitate w 훌 :r e obtain 홉 d from fraction #2 훌 싫 laly 밟훌 of ttl 훌 in 풀 rar 훌 d spectrum of th 홉 or 훌 n 홉 e cry 훌 tal 홉 ( 훌훌훌 figut' 홉 3) which formed. itt 훌 t au 훌홉홉훌 t 훌 d that th 홉 compound W 홉홉 a cis i 훌 orner 훌훌 nc 훌 two p' 훌 aks app 휠 ar 훌 d iu each o.fthe crit1eal... 1...........1 re 훌 ions. 월 round 1600 om....l. 1100-1150 휠 m. -, and i 훌 70 goil cm. I φf th 훌 홉 pactx' 때.n r 훨 corded on th 훌 I 꿇 i'm12. There wa 훌 on 훌 strong thiocy 훌 n 훌 to p4 훌 ak.. 1 in th 휠 net 훌 hborllood of 2100 em. '~""J rulin 훌 out the iichloro compound. 옆 1e 훌훌훌 Mdithiocyanato eompoun 강 wa 웰 rul 훌 d out 훌 swell 81 no 홉 this would C 훌 US 훌 the 홉 pp 훌훌 ranc 홉 Qf t 찌 o atro 찌훌 peak 뭘없 the 2000.. 2200 om... 1 r 홈 gion. Comp 월 rison of th 훌 spectrum φf this com) 뼈 und with that φf
23.{ μ.mμ내섭hl껴띠日.[띠 디뉘여μ밍α떠섭 멍φ엉μ U밍μ.[디법되μ뉘블멍띠μ디 [이서뿜섭 뉘니U띠μ써日 μ써m.[여μm Rμuφ.되μ씨 日의μμumQm엉띠μ떠μ내섭뉘ω.되μ써 섭 뉘μμ Q 껴. [떠여 }매 H-매 -(띠?f.n &υ-흘)*4f뼈닙객k띠4띠xx책뚫 F@ K l() ("If) r 에..-....-. 1 J ) 시- J k l j l 1-1 tl 1 셔.!, i tl 1 ț l f! }i 7 U 1 n
24.영μ u애μ배디뉘μ띠日h띠 섭뉘.여μ띠W떠디 엉띠영μ u띠μ릅다m띠쯤되μ뉘 P엉ωμP [ω터후다 뉘μumμ써日 μ써띠 [mμ띠 Rμuφ되μ써 日섭μμuφQm성ωμ때μ내디뉘ω되μ써 디 뉘μμ QJ1.N 띠며 }잉HW(ωZO&U-효)F Fm 갚띠넓나벼xgx작상솜 Fg K, c l..-....- l{") 한. ~ M..- @,... Ll I I I Ll l I I.L I.I J 1.t~1 ; LJ! 11 U L J LLl il Ll ttl LJ.i I LLlL.L.l. L Ll.LI..!.l L l.i l.lllu.ll.l-.ll L1.I -l.j.i_i -J...I. I I_l_~+.j, I... ~ I-...H-+J I- - - --- - - --- -_ I.' r " I 1 j _.1 I 1 '" I 1 J',. I." '-'-'-L' '--'_I :L L-'---'-'--' --L.'_L'.'...I.-.'---'--'_..L...._._L...--<I--'...._._._..._._>-+-._._._..._._.--'-+-.._..._...._._ -- FJUR a1m4 il lhf 11+ jjtf d1f!hjii EW 찌 jttirtr II L i 1 1 (아 F 앙fξu a l(')..- a N "
25 m 셔여,갱μ utμ내디 nμ이日 [띠l디뉘껴μωP떠섭뉘성ω영μ uφμ며n뜸다 뉘μU띠μ써日 -μ내면띠 다뉘띠μ피 -mkμuμmμ뉘써ω되μ써 日디μμU띠@띠먼φμ띠μ써디뉘ω.되μ써 디 뉘μμ Q 객.m 띠 PM HKW& νw 렷쇼) p!( 그 c
26 1 i N F 예
vmmz녁녁치kr있q?&μ샤때cjσ 짜싸 27 명nZω효 m- 디十 - 뚜 { 프파 : 靈 ff 繼첼 t 뿔릎렸 1: 품흡 F 짧懶폐따 tl5 鍵짧뿔빨짧텐뿔f 긴F띈 } 짧聽繼 Kin 짧EE ~ I-I- 벼 - 괜 f 瓚 ] 뚜략, I- - 녁 낙 # 띔購센녁잭짧 ifeii 택똘담날뀔 i 韓 f 편繼 :R-+ 카 - 파 r 밟 tj 후캅 =tj 工 ttt 니 --1---l-----\..-- I- -f- -j- -- 뉴 - ---t-t- 니 첼않 f l L T i Au k G a e 뻐써빼셔싸 N뼈,m 때-,따려F내g O C Pec r ke n 2 m a l1li r 때쐐야-μ.mec와돼- m 7Fnc1= 體 f 麗드 ;,,"-.-,-, ""'I~I '->n 에파 -I~ 햄 ~: 잖 900 800 700 WAVE~ 애업 tv\ber CM-l C-c rl i-h s-2do 2 l l 떼@ o,,{ i n 2 2 0n a &fc K mn염 l d ---i 때I c n R -- ) li. p - n L J i n @
1-1 해)m녁녁껑gζ싸 때 매괴뼈n 라싸싸. 다l28 十네 -t--t 上 - ZQ 난 따 1= 1--1--1 뉴 - πn호mk효ym 닝갖 @ mvwi---!- -1-1- 1-1-- -J--I--I--1-I-l-~I- 밤써애n 사U 니[ H- I- -I-W-I-U~ 3설또 -1---1-1-- ; 口 ± 휩 =t I-+--i- 풍2낌뚜 η - - 밟걱 =11= 밟밟그 : 趙뺨니 =tttt 빠1-1- I d n JA 鍵빼따'-- 서μ때따d. 싸따-@ dr e gp 야t s-0%-f no 태,o-lAur-- oc m ν r 2 a l N C, 야L 핸--H r CM~l 파 C샌난m, 1Ln니eN i μ 때뉴내 - 찌따없 끼따) 돼μ %a,t 빽 : r짧i많 1700 1600. 1500 1400 W 흙 VENUMBER 얘- cfoc 뼈g-2 니ll
i -fgκx성m섭뉘m먼μ u띠μ써nμω디뉘여μωp며m디 엉ω엉μ u띠μmn** 디 뉘μU떠μ내日 μ써hkm. -. ~ 니 미까샤 μ 니 IIμu u 샤 니샤샤 니 ιυ 이 냐 1: 샤 rr jj ~ 1ηJIffL1 펴며며川띠빼씨끼삐빼빼써 川 } 川川川내내씨川 m미밤바싸 m바배따 j1# 씨바싸까따 nrr @ [) [) @ -.-~-r_r_~_r_r.... r 0-" "1-""...-,. -.- - - i ~ : f 1:i 따버씨 7 밤 υ~, - :f 十 l j _._a 4~._'.._._.._ _._._ 11iij~ 끼川 r 1νU 꺼니l μ 깨니 -t--11 tmt 6 it! 비따비써씨.--(따겼n 야않상 A생N.-...- { F :n:m 서 Jj 니 때m 낭넓썩써 흘U R }띠때R 밤 # 논텀 j - { J L;j 파 1 K 원 팩서)써서악합합 얘 {} [}*닝I.e) 샤녀. 끼끼μA m셔떠μmknμ성u디 uωmω되μ써 日섭μμuωQm엉ωμ매μ써디뉘φ되μ써 다 뉘μμ (버핵.h 띠며P얀29.디 g 꺼띠l
30 8.갱μ u매μ써섭u μω日꺼띠l디뉘 펴μ띠%떠티 엉띠엉μ uωμ매디밤u(여당z)n(검) 디]8떼세띠써 염업uω캄엉밍μ띠업디뉘ω쉽써 섭 뉘μμ @해 펌α겁M,..- C 애.- r--(따?ι n 않녔#않앓싸 깨닝핸때패때kg,헥학파it F(아@k씨-}- 1------------------콰꾀ly{-i내tLμU*개헤파Ut [}(냥[}[){] P--힐μ{ %μ떠뻐에 3 앤낼협에씨.η J 1. 끼
31.성μ u매μ써디hμφ日서띠l디뉘4μφq떠디 엉ω엉μ uφμ띠n뿜섭 뉘μ디띠μ써日 μ써{)φ디뉘mμa m.[mμm RμU섭띠ωμ뼈ω되μ써 엽PμμUωQm엉ωμ띠μ써디뉘φ되μ써 디 뉘μμ (뻐혀.m 따여 }다H-매. M []α 엉[} NN
32.엉μ 디띠μ써디Hμ띠日H띠l다뉘여μ띠A얘섭 멍띠엉μ u띠μ셔디{내{디n(섭ω) P,m디띠μμ써 日디겁이이@m엉밍업μ써섭뉘밍되μ써 섭 뉘μμ @쩍 일컵{]잉법
33 멍페영μ u띠μ서p안hpn(섭밍) &,웨띠내 日디섭Uφ@m.멍μ u띠μ써디hμ띠日 [띠l디뉘껴μωw떠섭 멍ωμmμ싸섭뉘ω-되μ내 디 뉘μμ (버해--셔서띠여섭다HW* 빼 F 얘 풍 법비 학환irL(') ~', \
34.영μ umμ내섭hμω一日h띠 다뉘U냉μ띠@떠섭 엉밍멍μ uωμm후디 뉘μU얘μ써日 μ밖언이섭뉘띠μa m-[띠μm Aμum되μ뛰 日섭μμU띠Qm멍밍μ때μ써디뉘φ되μ내 김 뉘μμ @혀.NH 며여섭댄H힘\
35 후훨... [Co(en)2(NCS)Cl]Cl (s 홉 e 1 훌 ure 8) indicated that th 훌 yw 휩 r 훌 not the s 훌 m 윌. 맡 1 훌 only remaining po 훌 1!11bility 훨 pp 훌훌 r 훌 d to be 표훌훌 담 (en)2(ncs)( 헬했괴 01 2 sine 홉 th 훌 only oth 없훌 V 홉 :l Iable 1 훌훌훌 nd 훌 n th$ 홉oidia a탤ueou월훨olut1on w훌훨 H 20. In ord홉r to test this po 홉 sib훌 11ty, 뚫 - 활 o(en)2(ncs)a 펴 C1 was di 훌홉 φiv 홉 d in wat 윌 r and the solut 효 n h 홉 ate.d over a hot plat 홉. Aft 훌 t 훌 bout one third ofthe 홉 olut 훌 on had 훌 :vap... or 훌 ted. it was 훌훌 t aside to cool. Dark 합훌 dory 홉 t 훌 1$ (only 훌 lightly 36 solubl 원 in wat 훌 r) form 홉 daft 뤘 r 훌 bout tlf'o hour 훌 i 묘홉 ldw1n 훌 nd Tobe h 훌 V 용 d 월 Imon 홉 tr 훌 t 뼈 th 월 t.s 훌훌," ~o(en)2( 빼 CS)c 펴 + aquates with r 훌 tention of 홉홉 metrical 00 찌첼홉 urat. 훌 @ 화 to 훌훌홉 i 닫야훌떼 2(NC 월 )(H2 0 편. 훌 t w 훌훌 th 훌 refor 훌 * 훌 $sum 훌 dthat the c 없 n 햄 ound which had b 훨훨 n pr 훌 F 훌 r 홉 d a 훌 d 훌훌 cribed abov 훌 W 훌 $ 훌훌톨 } 달 훌 ~n)2(nc 윌 )(H 앓 0)] C1 2 Additlona1 홉 upport for thi 훨 as 훌 umpt10n ws. 홉 Qb 힘훌 in 홉 d fr 뼈 l 훌 n 훌 X 훌 m 훌 nation of the infrared 홉 P 훌 ctr 따 i 덩 f th 훌 comp 앙 und. 짧 I 원홉 P 훌 ctx'\ 빠 1 r 훌 cord 훌 d on the 18... 12 indicated th홉 pre홉융no훌 of coord훌n훌 tec:l th10cy훌 nat휩 ~. Gonf:1rrn원d th홉 ei홉 conf:lgurat훌on and d1 훌t 훌d 홉훌홉n훌표10훌ntly from the $P 홉ctrum. of th흩 un훌quat훌d compl훌훌 A c함mp~ 홉rison of th훌훌p훨ct합밟 \ of this compqund ( 홉훨융 figur 융 4) with that of th$ flak훌y orang훌 cry홉t훌l훌 t 흩olaeed from fraction rfl:2a (Be훨 1. 훌u:r훌 3) 훌nd훌 훌t흩d th홉 t the two compoun d. 훌懶 X 훌 1d 훌 nt1cal. D. 맑 I 훌훌합훌 et :r U1ll of tn 휩훌 quat 홉 d cα11lpqund differ 윌 d from that of the unaq,u 훌 ted compound in 휩 q 짜 at 훌 worthy way 훌. Firs 힐, an add1tional, mφderately 훌 trong absorption p 훌훌 k 홉 pp 훌훌 r 훌 d at about 715 em. - (9 훌 g 1 훌 ure 5). Second. th 흡 h:lghe 감 ft:' 훌 quencyp 훌훌 k of the two in th 휠... 1 ne 훌 ghborhαad of 1600 am.- L wa 홉 edt 훌 pla e. 훌 d to 홉 1 양 war fr 핵 u 훌 n 양 y by about 35 em. -1 (8 홉훨 figur 훌 6) 발 I 훌훌훌함훌웰 k$ have be 홉 ;n a 홉훌뿔 n 홉 d by Mot't" 1 홉 and
36 37 Busch - to the assymnetric deformation of th 홉 NH 2 group. E. The sp 윌 ctr urn of. the reddi 밝 1 cry 훨 tal 훌 obtain 훌 d from fraction "2a ($e 훌 1 훌 urg 7) lnd 훌 eated th 훌 t it w, 훨훌훌 cis compound.. It app 훨 ared th 훌 t it might have b 훌 en contam1nat 훌 d by 훨 am 휠 of th 훨 first compound to crystallize rαiii th 훌훌훌 m 훌훌 olution. How 훌 V 훌휠, a campa 첼훌 on with t:h 훌.pectr 뼈닮표훌훌.[Co( 훌 n)2(nc 월 )0 펴 Cl ( 훌훌홉 figu 휠 e 8) in, 녕 ieat 훌 d that th 빼 y were th 훌 same compound. F. A comparison of th 홉홉 peetrum of th 훌홉 r 훌훌 n cryst 훌 ls, obt 훌 :lned ft' 따 l fract :1on {;2 1i1 by e'\t 훌 POt attngovet 훌 hot pi 훌 t 훌 t 훌훌홉 :lgur 용 9) 힘 f 훌야 i th 훌 t of 웰뿔 률 σ(e 매 2C1 꽤 C1 ( 훌융 e f :L 훌 ur 홉 lo)lndic 홉 t 훌 d that th 홉 y were id 홉 ntical compound. 훌훌훌 rlu 훌 P 훌링 t 훌 d. Q. A 홉 tudy of th 훌훌 P 훌 ctrumof th 훌합훨 d ~om,ound obta 훌 n 훌 d from fraction :JrJ ( 훌훌훌 figu J!' 훨 12) lndicated th 훌 tit w 훌훌훌훌철 툴 홉 n)2(ncs)c 괴 C1.. 1....._,'"... AA 1... t"!'a -1 Twop 훌 aks app 훌 ax' 휠 d 훨 round 1600 양 m... and in the 1100-11.50 em. -,. 월 nd 87Q 900 cm. R I t 훌훌 ions. Only on 룰 thiocy 홉 nat 훌훌 b 홉 orption p 훌훌 Iξ 훌 pp 훌 ax' 홉 d... 1 in th 훌 1'1 훌 i 훌 hboth 잉 pd of 2100 em. ~) 할 uling out the S 훌훌."*dithiocy 훌 nato and 훌훌월 d1ehloro compound 훌 * 월 nd the p 훌 ak fr 훨옐 U 월 Uc;l! 훌훌 c10i 훌훌 ly m 홉 tohed those of th 훌 lnfrar 훌 d 훌 P 훌힐 truro φf c :L 훌 * 향 t 훌 n)2(no 월 )C 꾀 C1 ( 홉흩홈 1 홈 ur 훌 8) v. 효 I. Analy 훨 is of th 훌 Ultraviol 홉 t 앓 F 훌 ctra. S:i.nce cry훌 tals of th훌훌arne compound were 1801홉 tedfrom 훌 eparate fraction홉앓 lutedwithj r훌영pectiv훌 1y. 1 훌nd.3 mol훌r HCI j 훌 lutions, i.t was obviou홉 that 훌om홉 chan훌훌 wa훌 occur휠 in훌 in at 1흠a훨 ton훌 of th훌 fract훌 on빼 aft월r 홉 lution from th훌 column.. It W~ 훌훌 thought that an