SOIIIIIILAIIOII COUNTING OF 32p WITHOUT AOOEO SOINIIILIIIOR III AQUEOUS SOLUTIONS AND ORGANIC SOLVENTS‘,AND ON DRY CHROMATOGRAPHIC MEDIA Thesis for the. Degree Of M. S. MICHIGAN STATE UNIVERSITY RANDOLPH THOMPSON HAVILAND ' 1970 ‘ [HESUS gag. LIBRARY II? . (I'Mrchigan State ‘ University P y... “JJ'Eh ‘. Cr“ t > : ; . .. O- 6’3." 57:”? ? p.5q‘: :- _v .«n‘vv‘wnw ‘3." 0-9 35 uv .vL...r.i. 1,024 ‘1..\-I':h)."; 'J’ I" : may w. 9 19~In1 II ' 1.“ .‘11' f 1 q n" ?) Bl..'r|'.£“~a‘flrl ”as 3‘4) EICEA-IJL‘ ion #1 a; it. .v-‘d If? ""T7""I'“=UES.SQ'TET’TOT33 NT.“ G?"3‘*C SQ!.~‘.I'¥Z?3?S—, Frndolph thompson inviland serenkov radiation produced by 3:9 m Ros possible a convenient and efficient method for determination of 33? in virtually say asmple utilizing conventionol scintilloo tion counters. Orgxnic solvents provide high absolute O efiioiencies -- the highest efficiency measured, pyproxi- ""3 m tolv 80f, wss obtsined with toluane. fporoximstoly SOC rbsoluto efficiency in obtain-d in aqueous solutions with very littlo vrriation when strong acids, bases, or salts are yrosont. Vapor 9nd silica gel give similar ’_‘ O fish eff encioa with no liquid present because Karaoke? rod- intion occurs in polyethyleno and in 31933. 53mp183 pro complotoly unaltered by the counting. Counting conditions are constont for :11 ammolos. The efficiency varies with volume. solution connosition, and vial material. ?ffi- ciencies relative to voter for 0 wide Variety of aqueous solution: Jul orgnnic solvents have been fietorminod using a rapid, highly accurate m thoa. ‘- *7 ’T‘.‘ 1‘ ‘ ’7 71". gs " .‘I D "r\ l" N ‘31 ‘ Ii ,3 3 3,! i‘: -..) .3", n i I I (’ t; . J ”)1: u .U v ‘ 33' Y “ 7‘ I V I": 'l 3’ I - i “‘ 1 1, W- ; 4 ' L) .5 1 1 (J.- I 2‘ J I ‘;‘o ‘ J _‘ O ‘ . - l: 4‘- . 31-; n I"l . o . r. , i'huOlqh .nowuson «:vil:no e -*"I ”r? I: 3‘ aux}: I,’ f‘zut'smi t t ed to :iCMiflvn étrte University in nfirtirl fulfillment of the requirements for the éefiroo of O 5, Z, //s"-/ .rw/f~7a . O f} T ‘. " I"? 7717‘. ’ 33' s I, L . - ‘ bk} flhia resorrch UTE nuugortzfi in wort t“ Oran: To. 3? 73:1 f .y _. -,. ‘. 71.! J . ‘ 6": .1. e . w 3,, . . you .ho Iivision of wooobolio LiGiUE? of the F' .t. n, ' - ,- 'v‘. - p o- 'A 45.. 1' .u‘ T ? LxLCT‘t‘gll. 5‘s 3 e'ica . (3‘1 :dtl.\.-.E.ollow~ ing the obserVItion in this lIborItcry thwt 3"»-3Ibeled 4“. Iibh fion"JfLOh.l lusfi rumewis suggests thIt such con- photholl 32.53 in clMloro arm 53 well Is “‘3 in WIter can be ccunted utilizin3 Eerenwr ov "IcIItIon, I t? orcuflt czar nstion of th mathod has been undertaken. in ..i-,-~.I‘;\*9 f“ I f, . f -§ ' 1‘! ' 'Iw’ "I I." ,. 1.1 absolute atIndIrd, IVS-017, II 0.01 I H3FOM’ were obtsined ~31] 3 3» CIrrierofree Is ”3 'Ifih in 0.0? 3 P91 III a I I T Iron V w Pnglnnd inclenr Corporrtzon. SIIgOI-s‘eI- If ( h :h 33013morizedfi frnm Swans) Ina Iur111cd yeast ET' acre 311ts fram 1r. J. 1. Irirl-y. batman 10. 1 mayor and K. Ferck glI ea-bncked 511101 351 G IIItes ('Iin. In 1‘ ' nstvumor ts. .nc.) mere IIIIO3Id for the éry counting Cb exwerimonts. “11 other chemicals ware reagent arréo, and distilled wzter III used throughout. 7.“ n uiflhteer Il cv~I1t3 Iolweu%"1flne Virla (recIurn f' instruments, Inc.) here severally used, ml 11 oufln xSiml golyeth3lene V1518 Ind ZO-ml glass viIls (”Icknrd instru» nt Co.) were also em3103ad Is indicIted. Unless other. wis -e I ecifiied, co mating Ira performed un1ng I Frcksrd 1:1—CIrb Firgui a 1c1.»1‘1rtion “‘Cct“0%e er, 10131 3310. 11 sznrlea rare mrintI* ined It’ I1 Oi in the refrigerated couzzt n3 chamber. -.'. ‘ tv -- -' - I 1" .1 -’ y . . 3 ‘~.. “1.. " - an ’ - O 111%.nlaenb coau1t1onat Q t12ufi 1033 a; 2%eointe e?‘ 1‘ 3. D 1913: h 1fl~t s ectrr1o1 in wager at V1rious grin 801323 :8 ( H. 1} rovo.: l :1 m~t L’"fiificfint port: as cf the afiect- m 119 below 50 and above 1033 (11b1trsry discrimia nator Civieiona) the 1’inite limits 1101-1111“1 3 em11oyefi. The b”Cka0u“& 12% 13 "i.‘;”-to Eiscr’w‘11uo settin3 (O ouo) 18 39 3‘2 at maximum (lQDfi) 313m (“2&19 1). Tot only £0 thesa c01dfi 30:"13 provide mrxinum efficiencv, but 11.110311 radar the count; $111.9 931.61111.-2.11111 11.1.11 1321;160:121. 01' grin (313. 21). t infinite u18cr’1 after sad n13 .un.r1i o*t:..k,..., f; :e o 13.1; v 111'. 1.1119 with (1319111305 in 1:110 (301121 1.1.11.3 “systan” (V111 nd COEtGfiuQ) in the efficiency. inite discrimin .tor Batti.113a re”. quire determinzzt;1on of gain Outing which va.; with vial materifil, soiution composi- 1£on ( 13. FT), and volume, 11-11111 b: 0:: you die reduced to 1? GTE (Txble I). 1rficiency Varies n th a male volure bot 11 has use of tie countln3 chamber kfld vial seawatry :1d bec~wu a th "system" 1115011119 {1 11211211011 of 11'1139-111-1111212‘3011. 11;;1t'3.121um volumes are 13ml in 15-31 10-131hv7016 vials, 15 ml in EShul; ol'ethvleno vinla. nné 10 ml in P$¢ml 31955 vials. its 69 iendence of oiL ciencv 0:1 volure ( £3. 3) restricta "he volume r: ngas within L effici. or cg of he citinum volume to 8-13 ml in li~m1 “"ethvlene vials, 13-19 ml in 25-ml poly thylene vials. nna 7-11 ml in Joni 31155 vials. '1hcso vrlues racy V133 b3w3€ :11 C01“Lh“fi on the couz1t1n1 chm nber geometry o1 wny1garrt: culw instrument. 31:11:16 1 8110113 the {ébaolute ei’i‘iciez'zcy i111 1.1.6.5611 11!: £335 2:9 1nd 11.”Aite Bott.ln3s trad nflicvtes the r1339 observed with 9:3 fixsurune ta ot“av thrn the one uaaé. x 3?. Lerenhov Peak Eeight Encctrum: 91 in *rter in Volyethylehe Vinla. , 13 ’11 of stow-é. 3E3): in 10-0 H Pakflygh' 131} 7.5. in 10 m1 writer at: counted in 211 152.1311 polyethylene vial. Spectral aectiona of SO erbitrpry diacrimjwator divisions were counted at the gain settings indicated. ihe third channel wns held fixed at infinite discriminator- (O can) and maximum grain (100,-?) settings. and scum in; events were terminated when this channel registered 105 counts. counts in the spectral sections are exgresaed as per- centsyea of the sum of counts over all aeotiona at tha indicated gain. °/o of Total Counts mo _ _ _ _ _ _ _ _ . .m I .‘ .09» ”.5 b0 o\o _OOo\ _0 .. . 1 be. /,h\ o x 60,. . .. 3 m .. Jon». \ I. \o.\c.luleuv.oou.oarotl [ 49 \ , 3“ 1919.61 . 00» . \IOI $909.09 0. )9 0 F? . . . p _. . .6 83902.00.‘ N00 R000 000 000 .000 8 03013339 Figure ‘ 3' I.‘ Trhle l “baolute ?1riciencyr feranhov Counting : in ater in nolyethylene Eigla {3-3 t J.-£ p1 aliquots of the absolute staminrd were L-m yelgethyleno virls. a. 0'- -illing with wrtcr rt (h 4, 6139 mains, and waighing the aliquot. the iocumentia Ldéed to 9.9 ml or ther in l ripettes were calibrateé by f Geigy Isotone Teeny stles (7) here used for deony cer- rection. Ermplaa were equilibrsteé to tamycrature for one hour before coauting in refrigerated instruments. Thirty anmnlea Vere used for 911 Eaterminationa. fn aver- 330 0: 3.5 1.10% '3 was obaervod. ?en-minuta counts on riity vials containing 10 ml water wars used for the back- ground dctcrwinnticn. The gbsolute errors include thow$hfi uncertainty in the absoluta standard, the uncertainty in tha pipetta calibrfition, and the anmyle éevintion of tn counts from 33 armples (9 meraura of both pipetting :nd counting errors) 9POUngatod accoruing to the theorem of error prepafiation (S). The uncertrfinty in the decry correction is negligible with resnect to the ther errors. .1 ”gnawfiwa w.anuofiomu v nadaarcq nocmomwm an rawau vb ”cwwmeanua «pawn mswaafifiawa fiodmhwWOHm .... u. . .. .. 5. H. .... 3. ,. vlfi...“ . L”.man.....?.,z.fl._v no mc:wooc 9...: mamam acnmwnmm uwv: o Mumwwnfiwmwm an finMwafifi mama mam MUMHSwwa aumnwmamnnaad mmwnwfimm. E .m. 2 fl awn mHofl ‘w WW.» waflwoma $30 ‘ nwmm “Ozzy HM?» vim Saw a u m \m :" - \ new *1 H 6M H 1,. w r v k . h .3 vhf-".5. n “otimo for Various Eubstrnceo in *olyothy- lone Virlo. ?: infinite Tiooriminntor Settinfi {O 00.). P: finite Ii86?imifixtor gettifig (53-1000). 10 ,1 of stock 3 in 10"“ Z'Fr- flip-431‘, o 7.5 (HfifiBPJp or isobuttnol swturatod'witfi finftfou (solvents) or: mixed nit: 19 ml of the solutions 'indicetod Ind counted in 13-m1 polyethylene vials. one cunnnol or the instrument use main- tnirxod Ft 0 .0 discriminotor and 10;in grin set- tings, and the grim of the other two chrnnela u!8 varied 2t the indicated discriminstor sot- bings. Counting events here toqninntad when the fixed chrrnel registeroé 135 counts. Counts as 9 function of grin rre exaressod 93 percent- ages of he maximum count obtrined 5t Optimum gain for the particular éiscrimintbor setting. Every tniré point is plotted. % of Maximum Counts I I I I I I I I 1 Discriminator: 0-00 I a . oro orm 95 Toluene " 90- .. A I E I i I I 4 l I Discriminomn 50-IOOO T ,- Water '00 — ofififizfia J " .. O Oékéb $§O ; If? x \é°\ 3 o 95.. 1°» Ao‘ _ .. /° / \ \Ao Chloroform 3 «9:3 /° \‘/ - 90- // Toluene ; "‘ 9 II B l 2?] l l l l‘ I l l 20 4O 60 80 IOO 0/0 Gain Figure 2 1a: :m ojtlm.m Counting volume . I I 3‘ u -3 . n 19 :11 o: ehocu 3 “i in JO :4 - u 0 p C 33 7.5, Hrs m1} rod «ith 1 ml of EEItBP 13 Virla of the tyoos inéicntoo. Volumo you incrorsefi in 1.3 Uzl irwo omenta to the moxiuum capsoity of:‘ the Viol. One minute counts were tnkon it 0 . disor;minItor and 1305 gain sottinga {thew 3?.9 rcsr3t3 obtnir at finite d35crim1nztor :nI’i 0 t1 Gian gain aottifigs). S x 104 com were .‘1, Y“! (1“ ob aimed at minimum efficiency. 11 miterinla are m\1L*:'wofi rt - notr rlt t orxturo 1n the refrigerrted counting ob m-rber. Counts as n Innotion of volume are eayrosued :5 garcooo.ga3 of 2% a moxirun cou;t ottnirsfi to oItqum voiure for tho oortioulnr vial. finoortuinty one to counting error is 30.53. 11 0/0. of Maximum Counts .00 mm . 00. mm m0. ___~_fi____——___d________ \ O b o\ > e I) \ b. / / 0\o bx 0/ o b o >\ o / / \O b.\ 0 D .. e / .. o >\ o /. \D wsv/Nm 3. hoEQsEmaw . , / __________-___—___-F___ N b m.m .0 _N 3 .m .mNONN Nb /. — @0203 838a <35 A mm - wzmmmi .... n 0.0. 0.0m 0.00 0.. _ 9m 9m 6 No ll’ ’ {i [ 1 M . ‘l 1 1:11 1‘4 savanna. ammpawcaow “my 1? 3:933. Sanafipnmnafi a i .- HOOK. 02.5» munvraow “Odom fi.o.aw Margo“. 3W3 Hum.» M 0.9 Manama. Hwo.r‘w_u.m Mangwag $3». 3...? rosnw‘ofl 5“. M. w Po moflwSO www.m.w cow waning £32.". H H10 fiauuana wom.m_n m.s 933mg “Swim a 0.4 QMSwMomuem 5p .3: “are n H.” amfluamuom: M . .4}; 30.3 5 9m amouuug mg me mcuwuw A¢\4v waom_w 0.4 omnuuaamuom: mMH ~¢\d~ 0.0.Mw m: H. naewuawwuoa «Haw mac: Humvv.s o.w amnwuumo a u“: Aexdv wwwew » o.¢ finHuMQ‘Mwwm #3. A4}; + 3 53 gram ~33 & oh 0.m.m xm¢o ,a ”a ammw fivam u .oonwwacomv mandoaw manuapuso»oa mawnane «a wuaou yawnawdo mwnwauonaw “my Managua, Mxnuagauaéow G i... Haw mafia unnmuemummo wouwmw .«xqv M. 59o w o.» v.0 3 mmpo a »fi omowunnwucmnmmc monouw A4\«v wHo.o.fl H.w «0 Hbmfififls 1 . Manamwaenua fieno vawwonamg an »nmuomnam RU 950 Hamasa «a waywo m. .v axoauw «van «we HQJ¥H auuano«a nebmnunoa.om mix 95 awedanmnow umnauanan anw mgmnka. 19 222 Coufitgnmi Since Herenkov radiaticn occurs in the vial walla. 35? on paper or silica gel can be countad with no liquid present. Eelfaabsorption reduces efficiency with increysing area or mass, as shown in Figure 5. Cut. tifig the paper rectangles into pieces-v3 x 5 mm reduces thi error fin. to position variation for on. counting event from g 1.33% to g g 535 Table a). rdditiou of liquid to tho vial: generally increasea efficiency, but d¢es not L reduce th poalticn arror exaept wren the liquid alutaa a significant frsction or the radioactivity (st19 h). é Glass vials gavo sgproximgtgly 60% afficiency relativ¢ ; to polyethylene vials for chogped 9390? (st19 h). Sprpy- 1mg tbs pagers with color—farming reagents redncaa afriu cianey, probably because of incrsesod salfabaorption. ggéggectbffficigficy Feterminsglqgg5 fiuenching of fiercnkov radiation by colorad solutions can be wasessod by tha usual channels rfitio (u) find external abandardld nation (3) techniques. Our reunite (¥Igure 6) confirm those of Knit: and F111: on the utility of the external stendnrd for color quench correction, proviéed mavauraa 9r. taken to avoic'i the observed «9 2:53.! variaticn in extemal standard counts due to variation in polyethylene vial characteristics. Glass vials exhibit variation of less than or aqua, to * 1:5. Sample voilmne mxst be mm con- stant. If counts arc ton low for @ccurate channels ratio - . .Cnm I lfinila this work we: in progress, Efilzen end $ren¢el (6) reported counting of 3”? on membrene filters without liquie. Our infiepandant experiments confirm and extend their results. £0 (Y 1 l' alv ?‘ . Merennov Mfsiciexcy volative to water Ior Try Prue? 5nd Silica Gel re 9 inaction of «ray and {75785. a“) z Tr ETQL. pH 7.5, wars fiinetted into 10 m1 of A I .- lO‘pl aliquots of stock in 10' h M M water (15 Samples ehch for prper 9nd silica gel) or on to npnronrinte rectangles or Ihstmen Ho. 1 paner or silica gel G plrtea (E. fierck, glass- backed). Iha rectanglea were then flooded with methanol. drieé, 2nd counted in li-ml nolyahty- lane vials r: 0 co diacrimimtor Md 1230.." min metbiags. “his yrcccfiure ggva a non-unifonn alstrlbution of rrdiatctivity bimilrr to that obtainad after fizrtition cbramntogrcphy. "Pho;- pad“ paper wra cut into pieces «'2 x 5 mm. Un- chosyed rectangles Of ybpar were positiDned oithar fltt on the bottom of tha vials (1 9nd 9 cm?) or around the circumference, but nnt comfiletely covering the entire inaiée well (5-55 cm‘), and were not crumpled. inch point representa the avarwge sf 3 aamplea divided by the swarsge of the 15 standards for the material. Vertical bars renresent uncortrinty fins to armrle flsymmotry sud pipetting array, fietarmined by QPOJPQ‘tiGn Of the BMm lo deviations for the samples and the atandarda correggonding to each noint. ' min- imum of 3 x 134 Ct? were detected. 9: Fflper and silica £01 I: Silica 391 only 21 EfficienCy Relative to IO ml Water 5 I 1 _ _ _ _ \\\\WIIII \CDOSOUUmQ UOUQH I I \\ I _00 1. .W \ [WI] L :// W/W” . /I/ J. I 2.80 WQQN Mug 1 F LO 0 Figure 5 m0 .. ., w/W/ /M/ . M .NO _ b _ _ _ h. . Nb mb N_O.O 5.0 No.0 No.0 . >80 83 v P _ _ — p — _ _ 0.0m 0.0V O._m 0.: CNN 005 9:8 09 2.0%. 6v 5;mplea argqrrad vs in Vifiure S More counted 9 min- 3;;-un of ten times {or 1 minute with sri. nti on of t?e sample tstvezn chJ M'.; -73wIL igd snugly it” iItiu I3 co ranted. Fifiufds were then vdfiefl: or sharing we? l‘ceI in glvsa vivls uni tdo .:rocc flzure re ested nf'ter a 35-minute equili- r:. P\ br*tion gerioé. f m4n;uun o; I x lJ' Cum Ens detected 2. n. '. '. «.z -."- ..- 0"v| . . .- . ‘ II, _' ‘ f _ l' ‘7‘ ' ‘ ."' . ‘ ‘ Lt .:uL-JJ-s-‘Jadl 6+;1Ciflhcj 9'51 L21 0 “a (-LJ 301';an 3» (101' 1- i¢a lJ’V'A'J 1 mrturizls Hare ”"Etui’fih Mt -natru- ..3 . ngn 59ttihffl. 7‘ ‘- __‘;* . I-_+ THCIZU t8 .:f36313;,1.13~3. an;1e «Hs'iztioun are tha marsh as sea obsarvad :Tmn lflul mi.r:ute counts mIth intcnwefliats vgitntion on 3 ‘1; [en‘ent sww'198. If one count on one Bangle it garb {'3-0 :.Ied, ti‘lfl 8mm (average) value lies within 3 3001‘ the V°1ue OhthiQQd. nv‘ vernga of f5,d'£ 1 3.?0p::~t3¢ p aitian array ior 311 relative efficiencies: i" 0 min * ET;.mrx fréf. b . a... . ,c .I. .. . . «...I4I».AU~>~\ “PQC . a-.. J .... JM fl .... HI MU ..u 0 “.1...” \u C ..I ..I )3: u N w u ...c w o x, u (MA; Hat.» w... h. H.“ .rvcw HOAI an.) $0 4 MIm MI, rob wow . .fl . M I M J A I VIVID?!»- . .3255 :9». M.“ Him... nac;wmrfi 1wfic4 A innia‘..[ » Mu 3w 1 Ll- I'II ‘11 I.” “J a... wuuw&wnm ...Q 5;, m A.“ 1. :1 tiiIius-Ileiznliilli3 .?.l.llillti8¥tti12§.ti£ 3.9.... u w . A I.“ H o L..... “..I... .. m ..uw c.p o.v 3.u I? 9T a. I u m. P.” wm u.~q m.L Q.m II; no ¢.mw J.4 0.. .c Stunt I I what .M by! I t i i Maw r I if firm: I. M . mmawnmm39wmm How Ivzaw wan wwwwow map an3 anfiwmu M...)- l. Ian-J1 on. H”. b .M. L. . ..I I \ L.. .4. .. «.10.. I. u .. a . I , t I; I efiuawm49 wwwmawwmaq no fiVOLJam mawInpqc no Maw amwwawwuaw Au madmawwmwhvm.w.v .fiam Anfiav 4“ nuwma {Iqu coufiawwwwadm r I mwmu II Ha 3w wowswga we FM 2.3 HIMANLQM. HMToO wwwor Haw.m va-r - I so 1 I. \u . I OI. . H Min-LU. mw.o¢ Hm#.m www.w ww#.w Hw:.m HHnIO 1111111 .:.I! .. mumwn mnw an; A03 v w.uu nva IMMIWMMQ n smnwmmnm no vowmuwWIHwfia.h v If. .!f a. w¢ MW.¢QU:J:Q aw Eu x 3 m A.o~. HrHIoA Ham.r. m coaq Hmu.m w0@.u wv ¢.Hw m0$¢® Hw~.u Hm m.ww ww@.w Hue.@ no L.ma IIA.0 HAHIQ 41 um “I. w. a.ublnr -umw.n wwm. {Olav Tuenchifig of ysrankav ;:d£ tlan ’ e?lee a? 13 n} gc1;e‘h3iewe Vlrla conu t.*~3.;1r‘:. In 1:) n1 'ctm- was cmxr‘izesd :‘ive tit-ms. for ‘5 .2. 2313‘.th with" «.338 3:31:43?"th SiTlFé'T‘i'gf’P-‘Ii‘. 33:; 0 I. III 1 1.~\'-( ’3' v x ~I m n "-1 q. cf: av?;m;W‘t¢ na 13 . gran watt kgs. :ha co;- areé aoluiions hora tman Cm-G( and t.i¢ a vials racountgd, and fine rrtjo: m.‘ ‘1 A... a “ .. -l_’ . mu I: :3 ' 3.3:“: I} 1"} unfit. my a . 7 k W' I ' x. T‘— (30“.: 34.1.; “A, 1.4.}. in“ {I i 5 «a? wr-a cwmuterj with 5*. £35??? unagrtweinty (”qu to the Obaervefi counting error, which may have be 9,0. cIL“*3 by vvristiowa in v3:1?911 trIickIeza. .al'tIvo 9;“ificie mac tbs Emma samplaa us: arfi t3 tEE‘motEod given in firbl F with un’ 88 ta watar were detorniaeé ed wM th the a? to n31 sta320~ o“ c sénty- ting to cahw“.n rr- ' -At9u51.- {ascen- trntiam *Cflfefi warm :5 icllers: cth¢1nna blue. 1 3“,“. a £7 3~1 '- - -' ‘- ~.-. r". :3- ft; Janna D l} 3 11: '1 S"; .' 3. 1" 07’ fl 4 i .3 1hr .. ".- ' Q 4* "I "i‘; ‘ A ..p 1,} :5. - 51.31.5933! OJ. L: (73331 “93 01:56... go‘” p; Efficiency Relative l0 Water °/o 26 '.. I F |00 " Methylene blue 5 o .. 80 — / " A 60 - A '- aA/ . . ./ 4O — KMnO4 - 20 - ° " ‘o k l<20ré07 0’0 . 0’0 0 _ ._ . I ‘l I 0.2 0.4 0.6 0.8 External Standard Ratio Cpm quencher Cpm waler Figure 6 LC éetermihntien and re exteenel ctrnfitré fie net EVEilfizlag e plot can be canetructee relating cgtical éeeeitg t0 0 . I J awaiting efficieecy 1. e e geek height afiectre with vi:1 reiees ' 1 C l“ :1; (3 ‘39 g *5 9.:- {J 5:? ‘2). ea If? a H I mimetion cf qnefiehing by e thaefieea rrtio enplied to the exbeezml Estm'zfierd ccmiate tr: 5! 5653. Determinatien or ralativ. efficiencies in colorleas solutions using the external atzneard has net been possible. slthough change: in oxternel standard counts occur with changes in system composition, the Versation is partially dependant on renters inéependont of the Cerenkov effi- ciency, erobebly variation in collision creas-acetion for Compton ueattoring and pair yroeuetion. Even when tho variation in aolution cameosition is defined (0.3.. 1 gradient of Reno 0 in water), the Variation in alternnl ltsnderd counts due to Variation in glee: V1513 Makes it impossible to eatermina raletiva efficiency ennnges smaller then hfie Peek height aeeetre of either the exter- nal sbnnfierd. 3;? in aolution. or dry. show too little variation with efficiency changes for a chrnnela ratio t9 b. useful. an!” 2‘). '.T_ ..m £1“ a.“ . {unwa- —‘v ~' #5:". ngg-f’r 5". .5- I lel'.‘ Ox); 0 5 lfiglicetEOfia rho Fimltetionsfigfi.gaowgoegltfih lho relatively broae gain oetima observed in aqueous solutions (Fix. a) one direct deto not presented indioato that color- less aqueous solutions eon be counted ot the gain ootimum for enter and finite window with relative efficiencies essentially ieontioel to thooo obtained at infinite window, The smell changes in relotive efficiency observed with wioo Verietion in aqueous solution composition (93-1oeg, Tabla P) indicate that for routine work not requiring grantor thantfiié' scourecy, the obs-.1130 in efficiency with changes in solute concentrstlon can be neglected. Chengos in rolebivo efficiency in different mixture: of chloroform and methanol era eloo smell enough to be noglootod (lrble 3). Fho oxoonontiel relation between count rate and volume from 0.01 to 0.5 m1 shown in Figure 3 is consistent with obsorotion of a fraction or the “cremation by the water, while geometrical rector. (centering one height of the column of voter roletlvo to the photomultiplier tubes) flppetr to be the major actorminents above 0.5 ml. The roletivo efficiency of 1 K 6551 (100.6%, Table 2) inéia onto: thee self-absorption can have oonaldoreblo effect on the obeerved efficiency, since tho high rcfrnotivo index of this solution (:1 Q 1.35) should hevo rooultod in increased fierenkov efficiency. The Viol materiel elao effects the efficiency, es in apparent from the date in ?nblo 8. The observed firfi con thus be roorooontod by: coma. fill‘nlns «5 use") (33.7122 where :1 is the detection efficiency or the instrument, as and 3v are the Cerenkov efficiencies of the solution 1—: .. 99 3nd V191. and n1 mné n; are geamatricfll fpctcra Which Vary “3th volume 9nd vicl conct-zct1 n. “ha resulting relative efficiency oxrrccaian is: n 5" ‘ n?” '2' w “too a 1 “F “g“v Therefare, the ralctiva efficinnclcs in Tables 2 93% 3 vary with volume and 7131 mmtarinl but cra indeccndent of the casclutc cfficiency proviécd by ray infiiviéusl instrument. They upply to a rcnfia of lnlO ml in 18-ml polyathylene V1515 and era ha more thrn 1? below thc re- lativc efficiency rt 15 m1. In Efldml glcss vigla, relative efficienciea in 10 m1 volumes arc from 3-5? higher thwn those raconted, and incrancing valuma in the range 1.15 ml caucas increasas in relative efficiency cf 3.13%. Vficc~ufigofi5 Since a significant frcction or the WW total counts wicn 13«ml ammwla volumes is due tn the V191, vicl chxrzcteriatica must ta held constant re? thg metficd to be rsyrcfiucitlc. Polyethylene vials which hkve haen used for scintillation counting muct not bu used for Cerenkov cauuting unlana they have been extensively aockcd in solvent: (c.g.. chloroform) cc rcmcvc scintillator containac in the vial walls. Variable increases in mana- rent Eerenkov efficicncy of my be 15% have been obscrvad with nolyathylana vials scahac in toluane or cicxanc ??0~”0”3P scintillator, and crclcngcd caching 1n hat watcr cud dctarncnt does act csusa c nignificqnt dccrcasc in the lava] of ccntcminntiou. ?hough thcrc wna no detectc fbcc change in arricfiancv or peck height awestrum ior *uc counted in tolusna or cicxcnc scintillator in 71813 containing nbaorbed scintillator, the externsl strnficrd counts increased by as much as hé?, 9nd the peak height chctrum with the external standard was sufficiently 618- carted to proéuco c 30: changa in a gresct channels ratio. 3-9 31339 most autcmstic external etanfiwrfiizfition systems defiand on 3 Channels ratio with the exterr r1 fltdnd rd, absarhed saint tillvtcr‘must o refia*ed Irom the V3? 313 of yolyet 3.31039 vials usefl for 3ormel scintillation counting. Tb. permeability of nolyefh; Lane to or-“rnic solvents paaes a mare gamerrl Pob3am a nee solutaa may be fiesoait- ed in the V351 'rllfi if solu‘5 ions rewrin in he virla for more than t few heurs. 30 aigniffiannh shah _aa in garenkov Lfi3ciency have taen oban rvad Hhan salventa are present in the via-V1 mils Macrame é 33.31.34? with toluene). but toluefia and benzene, which avarorfta 0&1? slowly {ran the #321 walls, kého csusa 1: are: 803 in axt erngl standard can? t: oi as ta 13 . This is grobably fine to chemgaa in firzv iraternct ion cNfirrcter35t3cs, rath ‘.er than incregsea Sn Eereni :av 61 ficieacy. Tue ass of glass vials circnmo vanta tiese ?rahlema at a 25; decrsrse in efficiency. fio abss'3333n problems hrve Lean encountefied with aqueoua solutions cauntefi in polyethylene vinis. Cz- emicrl 0r yhysical ghensmana which result in & nonohamoseneeua d3stribution of rafiiogctlvi'y in the vial 3311 attack tha offécian»y. If an rqunoua 54* 30 in poly- ethy194* a cunt: zins 3‘33 and all ions in the ammmle are below 10% “, e-ficie;cy increaeas with than because 0f aésorgtian 03' the phosphnta to the vial (:igura 7). The incrofisa exn ba u? to 3% in {h knurs 533 up to 103 in #5 hfiurs. In @1353 vials, efficiency decreases by an morn than 23 in hfi hours, but fiecreacee of 1933 thxn 1? occur even in 0.1 F tfigfi‘na’ nfi 7.5. in ma ease is there defiant: 533 eff iciancv ch{.ge in lfi'houra. This effect hwa been notefi afily when the lsbeled cOfigound is ortho- 7u03“u.t6, and t;% prcsa"ee of most ions except Tris sné """" .'~.'S at :13) “3’ prevanta the effect. :33: should {also be not.ed that tr 9 nolwte.ta comrlez of inorgznic OIthDflhOSphfitfi bindfi Very EtPOfl IEjIF to $0133 Lu31913 Vizlfi- ‘Isr,_-fi1—w-r.. __. . T. -3m~—— «Li-i: - aigura 7 % I'lQO 3 a 3.1 m1 3112*ot3 of gtack fl Here mixed 8 c¢ucentrat1033, asuntefi immediately aster mixing find fit ithPVfilfl fifterW&rdg ’he vials were storad in the refrigeratefi counting chamber. aha éita ago a the i chtnfie in meant rate re- lativa to tfigt gredic;ed by normal decay and was comp tad for each inéiviéual vial according to: (sugarvcd c m.nt tfima t)- {Gtflfirved O“f ct G time x 6 Ebaervéé éfimwhv 0 Line 37690; fee 5-. y ‘2 Palyethylefia virls 61333 visls .‘1‘1 l8 if; cogrgati chi correction fl~.w-_——_~—_———_——-_——‘_J—#_——— _AIH~ARA~__ ‘_~ . Change in Counts (Corrected for Decay) "/0 +5 +m I N O o 6-35 _ _o-_ -6-» z «5 am om jaw :43 .NO 3» Figure 70 + + + Change in Counts + ' (Corrected for Decoy) °/o . l j — J. a _ _ 1 55mm <55 A u... N I _..r _ ./W .. Zulu—Qua?— o I 6.33 .1111?! I N l Iéoawq. x 11am 5-4x: \ a .. a .. .052 1 P _ _ _ _ . ’ Figure 7b 0 me am. ‘ mm .8 _ am .50 . .330 2:3 Our wit” essefl‘ Eel fixtures. conditi iLsu7e rnewozhc 'bu - 1 15%? *he follouiafi rnvrnt gee a: ore1=ov counting *ve been u3§ n? zed out by otherez one. ,1ouuh Hire} .9. 14 ? x1num coun.iug volur1e is lifiited on; 7 t7 v ’o efiéefl soffitfilfinfor is refiuireé. ..O! a '1 _. 1. Theirs s mules mfg he countefl 3x6 recovered :or v ‘ " “P 5- I" "- A' N)“ r a ‘,: ' ‘ .. ..‘fi *. .~' .3? ‘ M" s J.‘ Q resulte gnLKCxLL LMML *Leee ,anutfges msy he P6511285 1 every 3”x-con*ninirg system of Liologicel ' '1’ 7‘ ‘0' - . ' \ 5" . ,. ., . ’ ~-. ,' -, ._ w 111:: toe run-.exr ca.::- o: 63.11 :;t 43‘31‘13‘1113 an: e 4‘ g 1'7. ' 9 ('2 I.» 5 e13 rust be taeon to 5" ~ " r s . ~| 1 . - I . an. ~ ' y 01 jo;;o*;31ene v1:1e, the ensures: and co: ovenlefice of Lfi?(..03 CouuoLne meLe it the me thou f1 0:. choice 36‘, in - fi 1 A." _r‘ ‘ --. -or cer~ 7 o: ;. .Jtan V‘p' 'J’Ar. 7. fl. 7. E I U. 36f§2.%=fi":r"fi'f 13' :13?:::?. $11 5.1. . 331E?C.:{1m 2730333571 6113. {”1111 6:11”: TO. 313, J nuary 3936. r. 4 , pus—‘11 - .‘- 1"- :,l ~ . i' l _ ._ _ 1" 3 {.I,'E.';;.,:1' :11" “*1. 1?. :0031'fl'“9. 1 «1' 70 {Flick}. «1:3 1-1“:- '5 ...2 «7 1 'r- ‘ :1 1? '1 - ~31 1, L. .., rum 51310. E. u., 1n€1 ;¢1. war. firoe., 3?: 7&0 (1903). 7111'"; '- a 1.;- ‘h , ' 1.313.317;- ~ ' 1’ 1 .. "' 31:11.11. 51.1.1, 5:. 3. g. 8st J'.w:...:1; . 1.. ffflf. (1. "331. F‘f'. m - m m 1 .13»- 1r“.- -- 1 .r. .. .-"- flingiyz, irtrpfuptzpfl ta fheAjfienr7 offlfrrer, l fédisan *ealey. 1957. H§:$f¥, 3., and #323?35, 3., 1311. ficrkafi., f6, ;' 1113', it". (E’Gitor). #1131 m1: 33133135, 61:11 witzon, oigr rhsrmgceutlcsls, rréglgy, flou’York, 196:. Lyfifizfifl, v. ?., =nal. i¥0fifiam,, :9, 313 (}959), regg.'fi. 3.. ‘ntlo Phsfi., hi, l?53 ‘19fi?)¢