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Council for Tobacco Research

30th Tobacco Chemists Research Conference [Scheduled 761000 Nashville Tn]

Date: Oct 1976
Length: 13 pages
HK1345019-HK1345031
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Type
AGENDA
OUTLINE
Depository Date
29 Feb 1996
Named Person
Leffingwell, J.C.
Aromatic Intl
Mallard
Strecker
Enzell, C.R.
Swedish Tobacco
Kallianos, A.G.
Lm
Davis, D.L.
Univ, K.Y.
Rogers, J.D.
List, O.F. Conference Participants
Univ, M.N.
List, O.F. Conference Participants Affilations
Vickery
Gaines
Bacon
Mcnair
Speight
Smith
Patterson
Tob Sci
Alexander, M.
Allen, R.E.
Anderson, R.A.
Arrendale, R.F.
Baggett, M.S.
List, O.F. Author Index
Request
131
Site
Hockett
Box
119
Brand
1r1
2r1
Z00000, Reference Brands
UCSF Legacy ID
ajg2aa00

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~bf1~ Te6acce ;hEfsttfrfS ReSearc6 Coh f erPtrce , NasFrrrla, Tcnrl, 1976 ffoMOAY roRRfRO i R:fg Opsigg Remvks ged Rdcem. • g:1g SYYPOSIUU Lgif CtepOsUtgg Yg Pkystgal prgp.etlas 1g ReI:XM te Sweklgg Qealfy Yg +1rNa • 0r.figrriy geakes, PrulUleg 9:05 NITMlM:F.N CIWI•OnFNIS OF LrAF ANO TntIR RRt: f10R$RtP 1'(1 SHIRK/M. ffL'AL/TY AVR ANOMA. I._C. Leftln$ve1l, /lroutics Ioteraatlonal. 549 Webb ind. Drive. 1t.P.., Harletta. C/1 16007 of a< .or- annn reoo kne.,n aebeceo nnd emvkn conetitc?ntg, gpproctmately 222 or thls number are n1trORen~~6 fn nature. Xenr ef ehe yuettt:-e of' Ni+ottnna tebocvm are attrtbur.d dtrectly to at least a portion of these ch.nltal entftcec. to eddttton- the de..eiopmunc uf !levor and aeow nuatfcS In tobacco fe lofluenced ro a large tlegteg by nttrogen cnmponentg of the leaf vhleh give rfae to the for.auon of boch nlteogen-g eontetnfog and non-nttrogenoaa flavor and atos chemiialg vla tLtllard and Strecknr Lype reeetione dur[ng curtng, egtng, peoeeweteg end eeaNtog .regee. Fapbesle ..tll be ot.eea In chfe fevicv on the fgtlugnee thet gueh eheaful crao.fer.actooe pley fo che dev.lopoent of tobaeen flovne. - 1- TiRPENOtO C.atPeNETiTS OF LP.Ar ANn TXk1R RELl7lOy5XtP TO StqD1.ING Q;•Al.tTY litD 9:]U ARnXA. G. R. Ense11. 5vedfel, Tob.cco C..., 5-10ae2 Stackhola. gveden Rccent w~.df~n ot the volatllr constltuentn nf tobacco Iwve revealed that a large rowber di thege .my be vteveJ ae d<ge.docton eroJw .s derc..a rre., ebree e.pee of precureore% chvnberganetae, labdanoldq end carutenold5/pulyfeopren:ldg. Hany of thex nerf:npre- netae pe..e.. n.vor prope~ttee, and tbeY tm.atttute e, fmportant part of the tobacco and tobacco smok,. arnea. Present structural and eter..cheetcel knovledge of che prg- curgors gnd tha products prnvldea a eieane to .ch/eve sn loMlgl.c into tbe undarlyfog reacttuns. Th1s sub]ect vlll be dfecuesed In the llgnr of tw Rav Investfgatt..ns lnvnlving on the one hand a qbnto--ozygooabtor.-ctudy-cf the-mogt-probable 19bdanofd preoursor: abfenol, and oo the othar, e decallad axoef attm of th. chauges that vola ile conetltuents of Vfrgfnlg tobacco dlaplay vhan the fcee•~ green leaf tg taken throogh the atages of curfng and aglog. 9
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YDNGAY YORNIN6 - SpagshlN 9: 55 rR,:.aLa.S AND ACIDS tN LEAF AND TItEtR REI.tTluN5NIP TO SNOtING QUALIT'l Aya A3dNA.-- A.-G. 1(allfst.es, Rrsearch Departuent, Llggett and Myers lcba[ca Cr+apa'ty, Durham, HC 77707 :`te tobar<D plant elabnrates a vtde varlecy of pfienolf<o and aclds. the nature and relattve amounca uf vh;ch depend to seme estent on genetic And env.ronmeotal tactore vett a avItvra: practlces. Phenoltcs and aelds play tmportant roles In the b,ochtmiscryvAnd Phystotogy ot the plane dureng tcs grovlh, mwei~y. and aanoscenc.. Ct s;gnllgc-e to sccentlets engaged In the agr{[ultural and manufactuf/ng aspects o[ tobacco to the fect that ptcenullcg and acids are tnvoived in poet-hsrveac change. vhtch occur duting the curtng and aging procesees. Tnasmuch as theae processes are cogntred .m setvl lo deceolntng the "qwltty" of tobacco, msny studtea have attea1 ced cotelate phenallc and acid composttlon ot tha leat to smokieg quality an- sroea. A revicev ot the itcerau,re on thim subject will torm the main thruat of thta Prepeo:a- [toa. 1831 INTEl1YISSION 10::.5 sA.FS A:.D LIPI7S tv LEAq AN'J TgEIP RELATIONSNtP TO SNJaIRG l1UAt.lTY AND AR.9tA. D_L_ Da ts, Uneverslty of gentucky. Lesingcou. KT 40506 A r mbei et v+ and t[ptds a e praseet tn eobae<o leat, 4ome of vhieh eontrl'ovte dtrei[ly to smoke aru9J and qualf[y, uherea9, othera elthPr enhance [ne product ot have no[ been descrlbed as tlavor or quallty related. Also, the quallty and qaanttty ,f tcaac.r Itptds vary emns the dt[terent tobacco types. A part of the unique Tu:k sh tobac<o tia.or M1as bern attributed to lou molecular weight fatty aclds. A number ot te.ece fatey actda ha..e bren J59ntlated vtth tebaeco flovot Includtng isobutyrte, eo- .ale.ic, ..e nrt..ataet<, <sv•{r. Detmtete, end stearte a"ids. Othar maJor tatty a lda in tobae.o Ieat are Ifnolrle. ltnuienle, olele, lau[tc- myrtselc, and the methyl , m o! othef faety a~tds. ~oiM1<s gr.+vD ot L1pld•, • sme of ,.hlcl, a e preaent in gTea eter awunts In flue-cvred than in burley tubacco are the glycoiipids and phosphollpidt. e Inosltol Dryosphogly<osDhingeliptda tuve beta charaCtertied. A nvmber of fatty al<onol• ha+e blrn tdmt;/ted In tobacce lemt. Another group of llptds, the phyta- •trrols, nave been Investigated In tobacco lest and smoke. The srecole occus me tree steroi. aterql rseers, ecery1 glycoslde, and aeqlated .teryl glycosldes. The gentctc control of these conmtituents mlll be dlsewsed. Aroma relaaed hydrocarbone ranting frem tt_ to Ct„ v;th C,. aad C77 compoundm being predominant, bave been tdentlf.ed. lieaphytsdleoe, a major COastituant of euted tobacco, has bmen reported to .nhane, tobaceo caace anC arome. Tbe nnttcular ws of tobacco conaists of aeveral hydra atbaaa t«l.adteg haatetaenatmne. gec.ntly, dtaateraotgoaers of ~,8,13-duvatrians-l,l-d o1 vare ftm,aa to be rjor cgNpooentg le the ttu ftom burl.y tobacco leavt:, 10 MONDAY MORNING - Stmgat lam - S - lt! lU I'HYSIfA TIFS. Durham. I. PRnPLR J. P_ 0..8 NC 777 T1YS OF LEAF AS ,_r_e and A. R. 0] TNDiCAT Mt[chem, ORC t'e t-n.MI L1g[ctt-4-M CA1. A`.D yera-Tob 5`:.ttlNr r-r,R- aa[o Lonpany-, Thc relattonshlps betu[t-n pl-ystcal, chemical and smukt.g penpertt<s .,f leaf tobaccos can bc• very useful in that an individual can develop t+e art of uatnn any ona of the three-to-sake-ceita ln-estt matee.relattve to the other auo. The primary use oi theaa r elat/onsnipe fe to use the r}yatcal snd/or cheulcal prcperllr> to auate estlmates o f the s mok;ng propertl ee. the d.vrloprnt and u<e of these rolat;on- ships and certain lfattatipna relative to them ara diccuased. 11:16 SYYP0SIUN SUMMARY - Ot. Narrar Seggas lt Sg 6oMCN 11
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NONOAY AFTERNOON 2 Ep TECHNICAL SESSION - SECTION A Or. Rsger A. Aegertae, arssUlug 1 Ou I'•,iSII-TIn'. UI Bl•'S)`•rN1S15 A'•C NtTAgr•llS>I up TIIC T'rBACCn AtKA1t1IDS US NG Pdilt•t5'+RS t...:1(1IYtAG uNTi' 1'•rnG (W :.n 1:•-Il A7nN5. t. trcte. n c _ DaD•+rtmet.f r[.entstry• Cntvrrslty of 'tlnncsol.r. Ntnnrapolis. NN 55455 A- lnr •Iaadv.,ntage In -tng IIC-`tNR In the stndy n[ the bfocvnthests of natural rr••d.,-t, fn hfgl_rr pt.•nrs f> the natural ahunJanre of I'C fL.l'). Thfs problem can be naturol <1rc•c+•.ented by Ir•JI'•tt c•"rounda -ich contaln cvnllgv"••s I'C utoma. The oc+urre.'re of Sucn J-hiy t..belt•d ;pecies 1s 1.1: • 1•IZ • O.ul2IZ. Due to s9[n•sp n d••..niy lab•IrJ "u•leculrs o( this tvie are d.tected in the f It:-tl4g as vel.,[e 9e..Ya sycse[ricrllv lOf.,ted a ot tha slnelet reats arl. 7nn frr,m [svla[ed faC e .(5,6-' C Irat.+Itnlc acid. cunt9tning 8l: of ihe d••ubly IabelCo mOle[ule , , prri..rrd by t`e I..11m+ing routr: It[EIaethyl lod/de • nltronetitane • 7-nltTo- aIJ•h..rt• 0111. • 3-n,trn9ulnaline - f-omino9ufnollne •.;,fnollr+n • nicotlnic a fd. -o~eaa-m:nta[raaofr::s-compt».nd-tcnt<nt-lana-labarwm- tabclea-nteartne, n rnleet-tte, an n.hastne. and ana[abine .ere obtained. Evan though ehe speciflc fncnrporatlrm of he C lnlcotin!< acid Inro nlcotine ws only 0.07;, sstellltc peaks vere readfly dr[ectrd at carbons 5 and 6 ot nlcotlne tn Its 11C-tiMg spectrum. The resulte nf' te-d- t+s n.z ]abeled nl<otlnt< acld to N. gla,.ca vill alse be reported. E'x'•tt'•e-IIF- A,.T:.-trY nF SO•tt - ACr.EfTUn W:JY/ullDs. !_C_51_r- Blnrne*'siry 'Ieparteent. `lotth Carollna Stalv Cnlvarslty. Raleigh. NC 27•07 A n,,a.. nr + a<<r~rnr <..•rn.nJ+ ve e tested rnr an cew.•la•..r-libe reapnnne nn eobnco Ira.r> r T.•tra[iuOf'+ethylrne, m.[hylrf6nCyanideI lrfinethyl phagphttE, DhnsDhorug ;rt(1•.•rido• and carbnn n.nn„xide gavo an ethylene-llke response in tobacco leaf srltation. Ethvlcne v s[1•e mnat acttoe compound tseted. Those conpounds vere s1to ar[tvr en the standard bran absrlRSlon tesc. Trc.e :oepvunds are ^ acceptor acids. They dongte electrons to a metal and then „ hdr.w electrons lntu • orDimle. Tn<y also give a s[rong [:ans effect. A1[houpy it yan_+ot be eaid that ethyl<ne atts os ;laota ehrough a trans mechanism, 1t can be satl that tooa<vnd. en(<n ;tve a etrong trans etfert also gtve .n echylene-1She response in ptanee. e.,its indle.ce chst e greac number of ..nmpounde are cawble of givs+g an ethyLeneeltLeeresponse lo plants. Thfs aspect vfll be dfscussedo 12 I I NONOAY AFTENNOON - SECTION : 7[60 tVAIrA7ION Oi Tnt l,fYtt.T OF NDnli1tA11nh5 IN .nl CURI!a: Ji ril_7R 6RII•t'•R IrA4', tNl.fl'UIVr: iFnxl.l. TxUtNt.Nr• g9 WINiTOgI•.b 9pOTItN LtvF,$. A. t.•.•.<11• U._I.[rlvr{l,l,t• l. N<rllnuson, M. Alesanelr. C~SUlJdated CIA,r Corpu[atlun. Llaetonhnry. t.T nA011 i'revt••vx v•rk 1•aa Jrm•m.aratc•d rhe lwpurtsnce of tobacco proteln lev[•ls ac vell as the rnrfu of suluelc/inaolunla• nttrogcnnu cnnatltuents (pr+tetn/non-protvtnl to Ircf and 'nnkinA 9t'allty. A ranvrnicnt• raDidamethod vas there(c'e desired (ut Protein deter- minatlon wh)ch 'onlJ beuillt)ed hnth to mnnetor and to IsaOgs the eflect of alteratlons In the curing rrocrss of <fr.ar tubac<os. For l,ttal ntlr.M1a•r. the Cnlvman Nltroqrn .lnalytrr (CSd) + s satlsfactorv. For pr•'teln nltr.rRrn, f•+ur mvcnnds tr , I~•nted: the CM1A. Vl<wc•y. r'-einea. and ga<on pro<.d.,.as On tF. basls of almnlt<It•. .•., twe Nacon 9roced- va• adorred. Analys/R of proteln levels uas uttllaed to follov lobac•a under eevrral eepcrime•+tal < rfns ragieen- t+l , nvontdonal Wed• (b) alr-<are..t<> a« eler.t<a rnre• end td[ rontrulled envlronmentornnm. Tho cif.,l vf thr• Aruvti. r,RulaunA a ent 7-<hloroethyt:•...n9hanic actd 1'IeAI v-, ..i-n evaluated undt•r tltn (nur cnr7ng reglmenn. CEPA promote, read[ly v•asutable st•nestrn.e and probably docrv-.,eed rurlnA tlme. 1•00 COi161NIn F.hFL1T~ oF ETNR(JAND vA1.C1'Ai:•l. NIC•is (RI..Nta u~ >• , ,.•.1'Ixl;lc ni YLI'I•ft'Ain rrlg.tCCr1-.C; Y_Su~•.., Pi.•Tng, .+1 A-Ayrlra.ll.rai-t~•:,nr..rtn,[ Ir,r..rtnr„t. '1. C. State Univ.•rsily. •16rlrull ral rx+rrim.nt Slati'n. Yalrt~n, Nl 7/wn7 I•r.•,rfo•~u .Yra•rf,,.re [. I~J[...t,•1 [~+t mtdrlb r 1•1••R r 1.•r .+ .. .J..<o• n arvtn. <urtnQ nnr tn tvn d.lya and lurl tnna.mptl'•n by •r?rrRta[tc,5f?5> vlt1.•nl •I•rrr<[.wir <•~•n•'> t•. r n14w1ald <enl••~t. Fir1d a~pl..atr .+f el• bernuse II ,Ilmin.tttc nlgnlfi,nntlyrredures the need f•+r b[tn yellnvinx,lhs pntrnll.l h '•r a sla,tar rreaa.et,•n tn <urfng etmo. l.u~r,l. I50 m)p pcr plu+t• v,. applIod as a 11•ray in thr ov half ot Ih,,rr:p after the _ m I~.,If h.+d 1•rr • v,•rt.~a i~,rwully. Tv0-to.tl+ree . n-Inrcr th .-i•L,nta v- - m••.h.[ni•.Ilty ;.lrsod, ttnJm/Jribs •+ere rrnwheJ hy rnller>,l•hatvd'•al~'. harva,trr. Thrc. ~1-'vc ~trc rr•InlreJ ta 6'•IR cure thr tebarco nerause [(r • di tho vt•lin„tnR and m{dr/b drylnA rba,es v n'+t-. ';ulard.-- RtJur-ing-vug-rrs .tnd ta-alalha4n7ds-tnr- tht•-rambfned-.thrcl pl'•r: mldr•b .ruahloA tr.atment '..re 1).0 aoJ ).ltl, respert[vely. Tnba,co <nl•Irctod ~+nly t•' tnc laidrlb t ushinp trt•atment containe: 1:.5: and 1.70k total alkal•.IJa. Yal•,a•s fnr lhe aunlrul matellal vrre s11Aht1 highpr, 19.h1 snd 1.w91. t:vred ,+rigl.t v rld. u.r rer<a•ntasY raelo of thc <red vetght t• the [rrsb vrtght, ws IY.B. Iv.t. .rnJ 18.92 (nr the c.•mhinsllon treatm.•n[• che <•.she' e:drtb trnatment and the rontrul, renpoltively. Frum this work It appears that t•hrcl treatment combined utth 1•<ecuring mldrab crushing o(fers the potentlal for halvi+g total curing tlme vlthout aJvve.olv offectina leaf ov[car• alkalolde er cvred velgn: yteld. 5:30 INTERMISSION 13
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i MONOgY aFTERN00N -SECTION A VAgIATIJt: ,K Tul'AL PutYPR;N(ILS IN FCUh-tnRED TOBACCO CULTIVAHS wTTH UtCATInN Ahn StA•h PutiiTItIN. R_. E._w(111sn.vn and G. R. Lwynn, OYforl T.bacru resrat.l+ Iaboratvcy. USDA. ARS, Ott/ord, NC 27565 and N. C. St,te Un/va•rslty. Rsletgh, NC 17601 ioba•.a samDlwe feoe if relea..d v-+rlett- or five-c••raJ toba•co frnm the 19)S Or'1•ral tar/•tY frsta at ceven 1•+catinne tn Vlrgl<rl•r. Nvrth f rnllnn, So•rth Carnlln.t,.and.GcarRi. hen•,I e• by lk pnsltinn, The rlet(ee d al,ZCd c. na/~ard /o total pelyp rta , 1)3. 944; NC 12. 95. 98, 2716~; S•elght v<rr:a C•rtrr 254' 25g, 119, 347, 411~~MCwt r IL 72; -tnd vlrlcl•,la 1N:5. tllghly slgnfflcant dtlferenrPs In th• poly- ph,n••f cnntents fr•n rnr n.,ltom l1.6U;). mtddle-O.h5;l, and-top-(4-)92)-ebalk-poHtlons vefC ubtarnrd. Htghiy s(gnillcant differenres In 4olyphenol contc•nt for the varl•tles wcre also oblalned. Thc ranR< ws only 3•05S (5pelgllt G-18) to 6.057 (Copnr 258) The d,lfrrentra tn poiypl+m••1 levels due to locatlons vere greater than the dlffvrenc s atgrtbvtable co varittlts. Palyphenol centencs by locwcton varlyd [rom a lov of -.s6Z In $puth Catollna t0 4•4b= a[ g/nston, North CArollna. Data presented In fnd cete thac there are rattaatons 1. the levels of polyphetnls gtudled. Greater differen es pernaps could be oLcained floe other vartetle. and tobocco lntroductlone, - 11 [[rt:c.s of APP6ICATION RAT&S ON 1W,P.IC NTURAZIDE RESIDUES IN BIIRLfR i(BACCO. 41n A. F. Nac6rrer. R. C. Nichola, and 0. 7. Chortyk, Tobacro Labn.wtnry, -Agrtc•riturat Research Servtce, UV~, P. O. gn• 5677, Atbena• GA 30606 T1e late and stae:llrY of eaielc hydrat(de (MN) applied to 8urley tobacco and sot) vere xan.n•d by determfntng MH restdues• darlrv cohacro :,Iote vere treeted with /Rf raneing trnn o e-tenth 912 mg/plant) to lvice 11~0 ngfDla+[) th.,• nnrpul apnlftat/on rater ..t vartoua stagce af auturity• snll -plae M: w<re then deter,ined ,.e seraYrJ dirrctly .Itl+ 1.835 MM/m2. ResLd<,-tl q•,antltfes of nnrgreen and c red leave< from varlous Stalk posltfons, Rr<en and c red atalk+, ani foote as vr11 as golt. The analy9es were carried Out by eethy) alcnhol estrarrfun, atum na <vlunn chrmatog'apttY clean-up, derfvattration with N,O-bls-(trinethylsllyl)acetas=dc fgSA) and gaa rhrosutogrephy. CC analyses vere perforecd vith a 2 a a 2 s S.d. g.ass coltr.. panrd wtth 202 Ov-I1 on 90/100-aesh_Lnit)aoaarh 1t-HP: The effects of dlfferenr appilca[lon ratea on Ohe rea/due levele or both green and cured Iravee, etslks- and roots, as vell ns the perafeteeee of ,01 In aotl, vlll be discv•sed. 14 40NOlY 1FTERNOON - SECTION A -:Z - gF.rA NAhIATIfIN if[erTS ON 7OBACCO. L/_ r-anrx and 1. V. Fanrr, lhe AISF 4:30 Tr+hniral f<•nter, AMP Incorpnrpted, e89 Nnpc St.. Stanf+`rd, CT 069,17 whtle It Ir k,.•,vn t•,at /••nirlnR radl.tlon eaue<r chemlrat and Pl.sacal channwe /n • ..•+l< tfs•+.+a•, rr1.+tlv.ly Ilttlt fe knovn eonCtlning radlatlarn nffe<1.. on tht phYa:<al ner.1 -nad • tl••n p,nprrtice •.f tobwcco. effnrt t +t~dv rnJ,atirn r~an8es In tnhJ•r.., n~n•pllr., v rtlp.•.eJ to beta rBYa (nlgh rnttAY-tlectx~=ns)a:tlfl.faY)r- p-d-J by hlKhdlscharge. Vfrglnla Rr14ht tobacco w s Irr-id1 tted at dn4et up t" 50 BraJ+. At tl•i9 m.rlmun espnsorc nbvfoua cl +nqes obeen.eJ lncl•.Jed. a Jarkrn+ng In rotur, nn Incrr.tse In britllenr•os, .1 l•ufling cf the steme, and a a.Inqc In arnaa cj•ararerrl•ti•s. Analysta nf the trradlated-to6artc shoved-a -bstanifal-Inrrrace tn v.tter and organic solvent eolublPn. These Increa,ee were rnstulared tn tnvolve rup- t-,rinq of natur.tl p•,lymertc cubstances and were fnvestlgated by <:ant.~inq ahanga•r In deatrln anJ pestin content. In general the cell+liose conta-nt v reJuced ,,nJ tbr drrtrln tonta•nt fncrcaaei. The pecttns ..- e quantitatively unth•rn,;ed hut qualllati,n•Iy movlficJ• ['or eomn:rlaun purposes. sanpies w alee err,dtat.•d ae 1. ,,n-1 ]5 HrnJS ond resu{ta fnr selected analysls ,v^ Included~rr Because of nodlfied 1`hvtllral prnpertlrn, tho (rradlated tobacco tr +nverted Inta rcconstltu[s•d sheel before cigarette aample man++far:tvre. These eigat-rttes-and-approprtate-ronttol•~-v •cked -/nr tar and nrlected gse-phase couponeo[s, vtth no .Igniflcant di[feranrtsr< rnund- MONOAY AFTERMOON 2 00 TECHNICAI. SE:S10N - SECTION 8 Or_ Ribhars A. Manaiag, Presidlag - 1 METNnU rnx TNt uertrl+INATItlN OF pART111 , 517L DtSTR1gIrTIuN tli' CERTAfN SrOlcr 2:GH 1'(ell`<,Ni,hrS. .:. _Y. „urta• an,l Y. 5. g-+pr,tt, e<•aearct. labnratnrrer, Tennrssea• Yaetn,.n Cnml+any, 0ivletnn of Ea,:tnan KeJ.tk r:ompany, KlnKSp••rt. T'e 11662 Aac,ada- Imra•tor, v. ar d t•, determine the partl Ir wttr dtclrtr•„tl••n •,f 1(v+ ., r8a„lr -•nP••vn•Ir-tnJ thr na trtnt~i+,arti••~lal< tr -(tPN) r a . moYe. T... c e,,Je ts .ht<h iha• pY1nrlPle Il+..l Part1<la•r In a v•,tattatrean 1^r•t,t n sllde Jlaced tn tnc• Palh tf tbri: n+omcnlun fs sufflctent too-r e the dr.,q s r rrt.•d ty thr a/r- +tr . cparalcJ uxr pat[/la`s Inln four fractl•.. nf 0.25, u.5n,r1.14, and I no In JI'..rter r ,)S-nl/1-sec puffe v e dr.vn fr••s a<Igarettr Iht~<•L;h thc a tc• c-idr lnparl••r.lntha nvke drpostts were ImmcJiatel. dis.nlvld in 1d I d1-~th.IL•rraoldr an•I dravn lntn -1 cap/lI•try I„be-lortterd-evepbrat- n-of-r,.n r unds ann vr ..•lnt. 7Pa1 ~•< mt•as•,rs•J sPsctrophulometr/ralty; Indolc, nlrot.na•, dfctnyl•phthalat.•, n•+rphvtene, nnJ ntvphytJdfcne v s• Jotermtned by tapfll.try eol,nn qa+ chron,tloArt;hy PI~t nl [hr distr/bvllon nfrtdnc campour.d and the TPY o a Ivncclon of r partlrle slte .. n- str•<cted. Th- five unpnunde tnvastlgated verc d:+ttfbuted t^ a patta•n slmilirto that of the IPM. Thus, It te unlikely that the se ectfve (tlttatlon of a speclfer caspound can be achieved by selettlve flltratlon o a glven staoke particle sta<. _ 15
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1 YONDgY IiTERNOgN - SECTION g 14 A Mttn•`D /-,R :nF Si,-Dr OF AiR DltVtlO tIGAgl-fTFS• .1. N. Rpynnidg aoC '• P. 7:IU lT+eelrr• Rest•arrh Deparcnent, R. 1. Reyn<•Ids Tobacco Company, Vtnaton- aiem. Ht. 771n! .d <. dhd c nsteta A usetut method Fnl the study of atr dllured rigarettsa uAs devrsed. The mrth< ot tn<[rcing the venn laled pnrtlon of a cigurectr ri[hlna vecapl that aoparnlts IC tr.,o tne a endcng atmoephere in vnlch the burning coal Is located. The vegsel ts +start/yvsuepl ulth argon. Trapptng of the eutnatresm Rae-phasr smoke and anal s1s for nry;en, nltrogen snd argon yfeid data uhlch are uaed to cai«•let< the vercent nlr dtlotton and thc amounc of o%ygen consumed. Ti,e traDped amoke can alaa be analyg d lnr ether gae-phaet cumpnnenla. imports^t adva^tegev of the merhod are as fol/ors: The eamP ctgorette ylllds Int•rna- t/<m reg.rdtng Ir dlivtlon and aartten c umption ae veit as gas-Dhaae snoke <on.anents Congtant attention to the clRarerte durtngsanoklnR ts not raqulred. At verr higA feveia ot etr dtluatoe n ea7stances to Ilar are added to the veet/latlon etream• The lethod rso ba wed to study dilutlon Introduced by perforated or porous cigarette vrappets sa vel< es that tntrodu<ed by eeuthpieces or filters. - t5 TME CFFFC7 OF DIFFUSIDh ON TItE Dlr.tyERy OF EARgON MONO.tfDE FROM CII•ngE• TgS- R. p. Kaker and gA. Crei.i_- /:re•<r p<a.wrcl• end Devetopment ten[re, Brt[tah-Amerltan Tobarco f.ompany L/mited. SaulhaepCon. 509 IPg, /btnpeh re. t7.K. puhltsl`ed llterature dev rlbi.g tl+e ditfuston ofHb<arbon mo ostde threvgh <fnwr<et< peper t! r• Pv<-d wrlelly. the affect < n be < n91de[ll; ln Rone CrgarPCtt dPelgnu, Jlffu•.ia•• is swre tmuortanc [han air dtlutten r.- rnntrolitng carbon enonoxlde mafns•ream dcl.very. D.f/uslon nf carbon tronoelle can be described by a one-dimenglonal Ficks Lau. A m.r¢ .etallyd eapression of the lev Is presenceJ w+tch inrludes t<res governing dltfuslrn throvah thr tobacco bed and avay from the outer surface of the paper. aa ue11 as a term xoverning dlffusion through tSe ptper• A dtftuslon cell va`+ designed end construtted uhich perdts d+termination of diffuaion coefficlents through the paper. kesv{es are presented tar model systems tn vhich carbon mono.ide/alr (or nitrogen) mistnres are drawn through un//t :fgerettee- These experteents ualidete the equat on and lllustrta a number of cfgaree[e design taaturea which cn atf<ct the e:[ent t< ..nich ditfuaioo occure- Thus the need to coorider diffusion In relation to carboR Imoaoaide deliverfea Is dmne:raed. _ 18 NDNDIY /FTENNW - SECTION R - th - r. nu Ut:TtgMINATIUN nF GRRnIYA% t7N FILTLR NuD MATVXIAL 8v eyi uF I IOIrID (Jlw,yATJ r.eAl•Ilv. K. L_ g-i.h, and T. r•. M.rtll. gc.rarci. D.<•nr[m.nt, g. J. keYnalds T.•bavo r:,mcany. Vcnelon-Satem, t<e 710? A m• h••d Is -srrlbrd th•.t permitn tl+e quantlta• Ive d.-terntna I- ~.1 t<rbn.•ar nn tellnlnnt• ac••t1le filter rnd materlal. rhe pro-du[e rPqultPn d S.•%t./.I C%If.+rtlun.•E 1Jtd Cathuuax /rom r,•11`dosP acetate tuu rlth etlanel, .rwp~rtlnn •.r r e snivent• and ••nlutrnn nf Ol,e t-rdur In 9:1 rhloroform:TIIF• A 11y u!d chroau••gr.pr.tc end d<•reral- +.+tton ts r..rrl<d <n.e vlth e.•e LS-tn „Sryragel, 100-A eolwnns• q:l rhlnfofOrm:IMf colvant elutlun syatcn, and n dllferentlal refractive /ndes detector. At.<• desrribed Is a quaittettve H.feening pracec•tre for rapld tvalo.tton ot onknmm ,mplea for [nc prcarnrr o[ iarbovax. This is < ae by adding barium chlnrfde and .Itltatunbe[Ir aclJ to en aqueoug extract of thtfilter. A cloudy prec/pitate tndi.ates the prese,n'e of C•+rb<+v:r,l- nata u111 be prcwenlyd to ahou the prectsion, rc,•rndu<Ib U 1tr• .na r <rr vato<. rn< thna. srar,a t<.t tr<.e.<nt ot [he isu .+ous the relaef<e stanaard devlaton for [tte methnd to be 22. 3 20I(ITERNISSIDN - /7 w- t: 1•` trtw, anli-rDl FIItRATtON. +_ n t,rh and n. <-• utckrnv, <.ei.nP,f FIbf19 t.•mpanY, nnA 1,.14. t.hatl•.etr. sC Tl.r r/lt<.rll•n 1•rul••'rtl•s nf rhe h••<e and t••La rnl••nr+ nt I,Itee <IR+relt•'c . •~`In..i tu I•r v,dn h-irkRr~•en.l Intn•m.,lr. ,ICCn f .. r ... ,Irr. n ,flle`.~...trw ..na llltrr e r.a tur Dareleul<. r n.•tlrr. ~alrr~,•ntr[~tlnt•Fand a don-r,rnr.l r~.r <. r<t1ae with n nat .,•I ' rrvrapp.,l but ta. The .d 1-<1 ur to•r 1+•.~.r bnlt lrnxtl• rm t.- 1 f,fitia~ncv nfra .+tt. Ird «11••L,.r <rrtate Ilitrr u•.c at•o Ine•••,tlRatcJ. Tlra •Ilf;uclon and (fltratl<•n nl Caa•plt,.<• satertals n .ludlny-cer-bon-_ _-xede-car-m•n-dr--Id.•; ond w vPtai-urganic apnr•phd+e CoMp^ne,tcrerv nt-asr•t<d and .<•n.pnrrd with lltrr:rtnre data. It u o fou-•1 11,11 ••pcn - t•nlllnted ann nv. rappr•t .• rlnecJ t-harcn hnttc arc hlphlv ef(•rtive Ilitern lor v..ter .•nd a nbiy rlt<•etlve fur owrerculate nntter, nr<nttn-• .ind t r The ••1•rn butttPff+/- ctrnrtc•t fut partlcul!te matter and uater are rl,ther ti•~nthus•va• •for riosed bults, r.•Ilerting IhC diffusion nr v..p^rs uul of ll.r ,`P•r •r,PPa•r. \.rottne and tar vhlch w• VrrmarllY tn Il.e .onJ<•nsCd ph.aau have sfmli. r<nnvai efllf.rntlew In oPPn and aluaed h•.tt.. Tl.e dlt/uwtonal loas of gas and vapor-phase caw`p~m<ts la apprect.',ble t^ upv^ b,tt»• ond is relatld to the moltcalar +otght of eho ma ertal. tn cloacd bucrs tnCrC la aIIY =tetle ar no flitrattonal re••oai of vapoe p..aae <ampooents• A notable 111. ..e11••n ta m<thanol, vhich la adsorb-dan the motst tobacte. 17
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1t0N0AT AFTERN00f1 - SECTIOM N TUESDAY NORNIB; /:00 TECNNICRL SESSION - SECTION g Or. Nflllam R. Jabmsaa, pratitUeg • Ig - o':'„MATEO GcTrlc.•tINAiION OF CiTRATE IN CIGARETTE PAPbR. w. A. harvey, < In Philip Morris Research Center, R1<.ueond• VA t]715 Cttrates as ritrle a<ld fn cigarette paper o sfmultoneovely eatracced and esterl ted vitt, sultur/< acid-orthanol solution. For pa+er ta}•en from clgarectee, a vaeh vftt vsctc-vrehannl ls neteseary to seaove eateta or escerfftable aterlal prior to tie estra<tlon-<a[erf(I<attoe. T4r ~strrtfted estra<t to eubmftted to an AutoAn,lycer vhere the trtmothyl cltrate t.a converted to the hydroramlc acld bi hydrosylamine. The hydrosamic atid, ln turn, lolmy a red color vfth ferrlc lon. pe<n.ery n rltratc addrd to "blani'• cigarette paper avetages 1042. The ralat/ve s:endara devLatioe at tt.e 3-atgma 1eve1 r J2 for pwper before lt ta used er <It+reerea. For paper .emoved lrom scanderd cigarettes, the relative deviation ls r131. Comparlsons vlth the kobot Chemist and gas chromatographlc procedu[e 9te given. Tee advantagcs aDd dlsadvantagas of the AutoAnalyaer proeedure are lieted snd dt.cva.a<. A:N.aNOr,r(SttaL MATNEMATICAL MODEL OF STF.t07 DRAY $%:INING A710 PRFOICI•I •N$ OF OILPAU CIrARETTi BENAVIOR. L J. Ohlrmlller• H. w. Sandveky and H. S•-roerfteld, t,uxgrnbetm Lab. James Forrestal Campus, Princeton Dniverst y, Prtn<etcn, NJ 6g5f•0 DI:vtIAl'Itl•/f OF A RI.PRIIDUCI01l METnOD f•< DETiRMrg.tTtnV irr r.,TAt. tnIATIIE nnSt.c (TVU) fN CIt.AR TOgACCDS. w_Cart~rlghl, A. Corr+rll .,nd v. S. nlender• t'onnollJ:,trd ra Wrr rorpnratton, Gtaa on'•ury• CT 01,031 anJ R. Prire• Lutllff Tnl.;rr. n CO. • R/<1•mnnd, VA j]jj4 Eap.•rimentatl..n r tc•1 to <•vtabllah a a1mpl- reprodurlble T`:O .lnalyal9. Ihe /n<ludrd tndl•ator tyne. nnno- us. diprotonatod •cid• codlun IyJr..eldc pnllatt .,dJlri-• varlatt•me In the basic distfillna selullona f-,Iaurvs of trls••J1um p1,vaN•,te cixP) and oodlum hydroride). T•P source• Tatc af dletillatlnn• am•.unt of ,:Iwt1li.,lc, -ple slac• and rotlo ot sa-ple ssce to fSP sulurfon. Thc rewults dem-rer..[cd thnt [h•. bcs, ,•,rd p,tnt I• obcalncd vltt. thc achroya:lc Im1reJ, fndicatpt. No Jlf/cra,,:e rrsultcJ frnm u nf enn, or dll•rotlt ac/d+• prr•r r or ab+rnce of zndlum hyJr,•aidepellrte• TSP eu . from mletures ei Tar nJ.nnd Wm- I.yJrn..tdcd p.alr-nf-J1-a litaflon, annunt ntdl~tll.,tP, bample slrc, and tatlo uf s.tmplr blte to TSP •.nlulfon v,,rr {nllucntial tn Jettrminfe the Tvb yfeld. aas,•d on Ihe~c o„parlw<nts. u I.o-n n.,mple +Ire and r•rte o( dl=tiliatlon to yfnld 500 cc distlliatc sn )0-a0 minuaea repre.,vnt upetnum condlttons for r.st reorodvcfbtll(y. The_ratlo-of- - I•5-cc T5P per :n6 mg S.,mpie-fdry ,aetsht) .a. adnr+td. In[erlabnratory <,m1r.+r/K.•ns nf TVR daea mrat be n<r.tinlted carefully slnta a chanme In operating parumet.rs .a resuit tn signl/icant diffrrences. - 21 - 9,1/) wanlp'tatten of the t•fflucnt smoke cnmposftfon (rom a[Sgarette v'Il be fa<Ilitateby a ~11nd mndei of the eembuatfon and eaoke fnrma[lon peesese. A tirat a[ep to*'ard suth aueodel 1a presented. • n; nefey• rhe s/1wtlon <onstdered first is steady drav ssok:ng (rnm ICnltlo•. .t nne,dl:•na:onal eodel of the attual tvo-di4anslonal burning proctas te dertved (too the usu.J conservattn, laws fmass• vomt•nrum energy, speclea). The <hemlcal proce..es arv slaPilffed by Ihe concep[ 01 grpuping o( rtacttons. The modei thus tn•Ivdes only a one-step char estdatfon e aceton and s o-step pyrnlyois reo<t[on the atnettc parametets of these sre obt.lned by chermal analyots of tobacco. Othe: [nput psreeetsra, notabty convecttve heat transfer coefflclent, are meamured valuer. Model predletions of the effects of flw rate and oxygen concentrution on burning cate aod Dree•ure dcop a a<ompared vith experlosocal [esults. ReaaonabLa sgrefaelt ta fouM for these ovarall behavior parameters. 1111.I,SpACE ANAIYSiS itF 7UBACrO wlTll Tltb\ TIUPS. r,. t. RIe• R. A. , loyd .. nd C:1. Mlllrr, R,•searah Ueparrment. r. J. Reynolds Tobaccn.:,•mpany, wlnoton-Satvn,, NC 27102 A mrthnd n an.rev:a• [nr vplalllr compnnents In ehr t,r+•Lraco v.,r•.r uf ror..;r.s vna dr..rl.yeJC irll•.m •,a•: v s]Iay..r; thrnvgh a<ola-n ~f xruund t.•b.,.<o anJ 1~•r rlutCd vr.l.tlllr < .tit„en•s ~ rr a...•rhed by a micrnporra p.,lymrT tt..~, of T.nar GC•~. fl.•- l - G5 nm lon.ls r:C ir.,p vaa p;ac.•J 1n the heated •nlec[t,.n l•rt .•f a x.,a ,Lr•it[..drapn and thr vnlatllr ml,t~•rr tranvfa•rrrd antu an ov•1t1; eolvvn le+pe.- st.•r.• pr~¢r.,m•nln•t tu :nn• t; acp.,ratrd the 7n11vtdurl .omponrnte. h•a.fsl•+- e var-+r cntl••rtn rarumrtut. were Inrreutigatvd• anJ 11 vw. fuund t hnt a•^11•-••• ( lov .' 11 0l/ min f.,t 7.0 I,r at L 1" Cthr••uP,h 37.A it a•f t•,baCCn i ery ret•r••dua Ihla lattr vol.,t(tc rr.•f,lo •• tl.v gas <hrr•matuxrnma r.ut-c y urrJ and bnrleY tohar.usr,h.veJ rlualita[tvr dtff,-ran.r. In [helr ht•adapace vapor pr,fflts. Flue•<•,red xradrs d11(t•reJ pr/mortiv , a q•~.,t•[I[ative fashfnn. The amovnt» rt the f wr mu<t plentltul ru netitv- ent. tisuual<~r..l.l.-i.yJ,-• •m 7athylbatyralJ.•hyde, n- .eraldehdr, n•LraanJl. a.,d6•nctl•yl• 5•htpten-;-one) rete ,••mp:,red betveen gradrs and s',nlflcant Jlt/arenu s fonnd. Royclt frnm ttvc burlry gr-,Jrs also Indleate a correlatlan betvaen analytfcal resvlts and gradu. Thus, Ic apI•+.rrs posslble to distinguish be'veen tobacco gtadee on the beals of thelr headspaco vapors. In addition. 73 dtfferenc componente In the flue-:..red headspace vere tdenttlied-vtthCC/MS. Of t]rase• IT had not been prevtouaty raport•d in toba<co. ~ 18 19 tr, a INQ
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1 TUESDAY NGRNING - SECTION A trat •.utarlLE C,L~[ratiEb75 UF rtUAR ANO BURLCif TnBACCCS. II• Kaneko. 9:40~ T• Fvil++vr1. R. gazoRS and M. Nogucht, Central Research Instttute, 'hr Ja;xn f•,hacto and Salt Public Corporatlon, 6-2. UmegaokJ, Midorl ku, yok~nrna.; 227. Japan- N.•.trai stram-dcet/ilates of an ether extract nf !t.rnila c/g+r tobacco and a dlc,lero- mrtrane rriratt ol Amettenn buriry tobacco vere srparated by JIgtlllitlon under reduced p-_re foll.ved b, sll,ric acfd eul..mn •nn~ma ography. tsolatton of the cnmP•nenta uf <r.m:lra tractfem. abtalnad by Cu1umn ahrom4togrephy vas a omplis6rd hy pret••rettve GL. n.e tdenttrication of indtvtdaal GC peaks vas made by 19. NMR and MS. Tha follov- in5 c ..nnda hava been Lsolated fer the first time a natvrel Droeucts: F n eigar tnbaoco: norambreinollde; R-(a)-1-ISOpropyl-3-hydrozyDentanoic acid iarto 2,3•dtmetnyi•4•nydroey-2-naa<nolr acld lactone; 2,3-d/mvthyl-6,4-dlhydroxy-2-no.enate ac/d laeten., 3-hydrory-B-dam•>scone3 3-hydruaydlhydro-g-dam»r:eene;-From-bor-I^y- ebxco~- R-(-1-1-byArn.>none; 3-hydroxy-8-1ono1; J-hydrosy-7,8-dehydro-0-lonol; deh dro- Inllntlde; ph/toruran. Iso•srr: o( 8.1:-e.+oxViand-L4-en-1)-eIa vhLch had been Isolated froa Groek [obac o elsa t•.~nd n nun11+ t <tther n ambrelnnlide n 8,12-epoaylnbd•14•en 1Jvmle v.s fm,nd to borley tobaeco• gurley tobacco ls rlch in degradrd carocenotdo 0 dertrfent ln labdenned <o¢povMS. aemlcal vola[tle Components of Manl18 tobgtG are stoll+r to thoae nf oriental tobneco. - 21 - 10:+0 A MiTU00 FCN :HE RAPID, QUANTITATIVE DETEMIINATInN OF PGtE ANn TC•TwL S.aJ•,tESOL IN TOBaCCO. g. F. geveraon. J. J. Ellington, P. F. Schlvta aocr, Arrendgla. Tob•tcCO Laborstery, Agrfcultural Researcb Serv1 e, and e F. tSDA, P. 0. Bnx 5611, Athens, GA 30604 S.,lanecol, e crtregq.:[cryanotd slcdrnl, has bem shovn to be an important leaf p acursor ot palyn.aele+r e~oatlc Aydrocarbone a( smoae• A rapla•-repr.adoc-[ble-GC moEhod-f•e-tot-al end frer solanesol vag developed• Tlre analysis of the 6rleethyletlyl dcrtvative SMS) v s perforxd on short De+sll 300 GC-cclcung. 1,3-Otmyrtsrln-uas-ad-ag-Interna stac-dard. •• setanesM v s a.termtnea by gllylatten of the ground tt•barco or tts heaaue e tract. Fnrrto<al solanrsol, the grnund tobacco or 11. heune e racc t+aa aaponlfted rlth ethannlic tOH. Acidlftcetlon and heam,e e.trs<tlon yielded a saspla sultable lor s1tY[atlon and CC anatrete. Tl+e tollovtnt solanesot concents vare determined: he:ane estract of a coowerclsl flue- vr w towr.o.2.603; hydrolyats of sbove heaane sscract. 2.981; direct analyeis o vhola tobs-co, 2.702; base hydsolyafs products of whole tobacco. 3.112. The procedure sa ap;.tcd to other tobacco types, and the algnlficante of the free, bound, and totg wlaneaoi vatues vill be dlseussed. lt2g INTERMISSION 20 I ! TUESDAY MORNING - iECTION A -2L- 10:50 -C1IANLLr-..1H-TOTAL LARBOl6y;•-AWD 7n3At, A! :AlA;1D-CO`.CFATRATIONS-Iy 8L'81-LY - M. J. Kasperbauer gnd 1. H. Solley, A~S, USDA and Dcpt. of Agronoay. Unlverslty of gentucky. Ceaington, gY 40)06 TUBACLn IFAVSS DIIRINr• BULK OR rONVENT•OhAL AIR-CtRtNt:, N. A. AnJvr-_, The rffc•cts rt a b.,lk-curing rrg/me on yuallty-:alated chemical c•,nstltuents in gurley -bnsco .. e In.,ratlqwred bec•'tvee of tl.e Lnoe-a:vtng potential of bv1Y-<vring opera- tlnna. Total rarb.rnyl and total alkalofd coneaatratforra v e deterel,.ed 1n NY 14 tesf sampled ac date of tnpping, dste of harvest and :fter either an B-dav balk-cure of primed leavea or c qntlonal a1r-cnring. The trbstco v a grovn onder c entlona: production procedmree at the Ky• Agr. Eep. Sta. Tarm at Leztngton, ty. Gre n-harvvated leaves-frron-enp; m(ddle and b6ttom posltluns on the stalk vere s-parated lnto lamina gnd nidveln cunponentn. frceze-drfed, ground and stored to darkness priur to assay. Cured Icavea uere separated Into tamina and etdv,ln cuoponents after c.Lring. Carbonvla e dctcrmined as thclr c esDOnding 2.4-dtnltrephenylhydraronrs ahieh veee -era-+tad- .r1th ..14a11 to Iorm e q,.fnotdel Son. Th1e ton a, ongly cbaorba • t•90 nm,ncen ateblllzed vlth methanol/pyrtdtne. Alkalolds ve*o deLarminad by tha Gr1f(Lth proce- dure. Preitminary r a.,lce [ne/c.ee n aignt[t<ent diftteneee /n .llulo/d levels betuzen bulk-curad and atr-<urad lamina and m/dvrin esepies. Rowver. b..lk-cnred mldveLn eanples t.ed htgher levola of total carbo~yls than alr-cmred mldvetn aamples. Both cut•InR procedvrew louersd c.arbanyl <oncentrealona. 11:10 0 pUAdTITATtvE METHDDS FOR TOBACCO LIPTrS. J. J. Elltneton, P. F. aaamrcn-SOrvteei uSnAr P.o-. tier 5677. - Atbena. P,A- lDb[14 .Matl,o•.IS-for the-quantLracf-re-determtnnt/anaof-nw,.bytadFSnr~ hydrocarbon-wxa•s, sterols aNJ mnJor fatty oclds ,.ore developed• Ovanefteth n of Lndlvtduat caanento, as vell as quantitatfon of gtoopa of tomDOnenta, v ethtt+ed. g.mple. of ground tobacco va hydrelyzed vitn nlNatl, ac7dlrled, ond eatracaed sfth heaane. From an allqnot of thls ratract, the msJor fatty acids vete de[ermined by :C ef enesr ttimrehyletiyl ilMS) derivnt(ves on a colutan packed with Deas11 300 6C• A astoud allqvot v stparated en /llcl, acid. Paraffinlc nydrxarbone and neophyt.dtene veie eluted with heasne and deterofncd by CC on the Desgil eolumn] glutton vtth 102 eethannt In ether yielded the eterol-oontafning fractlong. The gterola vere coz.erted to their TMS derfvatlves and deearmtnad by GC on an SP-2250 colom,. A typical analyats of a flue-cured tobacco 8ave th+ follov(ng grortp valuesi fatty actds. 0.68I; sterola, 0.222; hydrocarbon treaes, 0.141. n•ephytadiene, 0.092. Results obtsioed by thEs method vglc compgrablg or superior to proc-duese ttlvolvlnz tht[1-layer chroma- tography or other Isolation methods. 21 5<hlotrhonrr, and A. I. Schepartr, Trbecco iJboratory. Agriculeural
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TUESDAY AFTERgDON - SECTION A - ut - A i./-.nTSCJtltit•lhc SFhst7A (OR DLTECTtUY OF :OSAU'n SMngE PARTII:ULITE$ N ' LO txP_ i~At 5y5rtliq. r_Fyt11y,R1ns, T. M. r..yle. and ). A. Stokety, Tobe•co r• ,e 6escur.n Progran, 6ak Rldge Nattonal l+tboratory, Oak Ridge, TN 78J0 A<• . r~tallv av+ftab:r c••mbfnartun ltsht-emitctng di„de (i.En)•phorotranststor divlce u.et useJ !•r Jctect/un of tnbarcn smoke partttulnt<s In tnhalation eeposure syscees. Ierred 1tMec f900 nmt emllteJ by rh.• Itp element of che devlce /s acattereJ by ehe mc•ke a sol, and the scattered light ia deteeted by the plroteta•anwt.tr eiement of the s~ . The wtpvt or the pDato[(anat6roT is dlsptayed on e rerolder to provtde n tnsca•.unewa .nd conetnueus reodnvt vhlch fe *eletcd to th.• concentratfen of 1!.e s•.t tn the 1®ediate vicinity of the devire. Reapunoe of the eneor ts directly pr..p.•-tlonsl ee . eel c entrafon and ta affect<d vary lletle by changes tn tlt partic(e s/xe dlstrlbvtlavnof [he w ael Inftlal teate ahwed that the epecifi: trspunse of the device is independentnof clgarette type. She . s useJ to deta(atne the ten<ent[a[inn and dlatribution of ameke aerotile 1n i+,hdlaClonerDUSUre systems• Studles on the VaIton Hwrisontal Smoking Machlne .atre shuvn that sunke ptrttc•tlatee ete uniformly dletributed 1n Che eaDeaure [heober .+d that ehere t. de..rase in varcltuiate e entrscion ever an esposure peTtod vhftl ls linearly releted to the stlrrtng raCe. ADpllcatlon of the sensor for routine mosttor- Sng of febelatton esposuree rlil be dlacussed. rvEL METnnU rOR T/1E DC•TE1rHINA:ION OP iORACCC7 PILLIeG VA:.UEg. A, g. anon, - il _ • i;n~ 8ra.m 6 Ltlitamaon Tobacco Co.. Loulaville, rT 40Z01 hha.cu ftlltng value analvses commonly requlte that the nample moigturc cnntent fa I • rclatt•.rir rurrou range. Thla ta to sllov , rrectl~na for varta[tons in the nis[-rr•re:atcJ DlaeticltY of che sample partfcles. A method haa been daveloped w Ich atr.rt:y r, res the ttlling value of cut tobacco samDlus at any moietvre level. At• tsaespectaliy s,./ted for measuring filitng traluas during praceesing at et...+ted motsevre levels or during drying. The method say be appl/ed to samples of eut tael,•a, erems or seconeucuted tobacco and blends of these materials. ~Thc molsture <nntent and plastjclty of the toba«o eample are adluated durtng the +ly./a by eqotltDtaclon al[h an apprapriace etathanol/veter aeture• Thla 6olvcnt -1stvre condl[toning pro<adnra does eot sigelticanely change the cobarco particle stre. Tne opecific volvme f che sample 1e decermtned by compressien fe s graduate, ritnaer vnate a braee vetght- sesuita are nor.aliy reporced ae spaelfie volumt: on a Idry velght basis. r:g INTERNISSION i'gg RUSINESiYEETING 24 l:00 TECHNICAL SESSION - SECTION ! Dr. Nlebasl R. Ggeris, Prasldisg 9:06 TUESDAY NORNING TnE ESTIMATInN nr cteME uETALS IN TOeA,:CO AND CI.;ARETTE SM"bE. U. Splntrr, lmp••rlal Tobncc•• Ltd, Rcxraoch Dept. Ealefgh R:.ad, grietol R53 I4r, Enx:aod The trclmtuue /•f vntartlC nydrldC R••ncratlnn 6nd atomlc ab+orptton spnrtrophot~mr:ric drtrc[.nn haa hrrn apf•ILW tn IhC Cntinxitlorv of 1TBlnit, arLlmnny, Dj6mVih, ar!enlum and te11or1nm 1n tobarco and tl,;.rvtce anv+te. interleran<es Ir. ehe dptccttou of ehese m eat. by comp.~nnda prr•.••nl ln ctmPl~e havc bren examined. Addltt.,n of EUrA t..a bo.•n round,•to ellminate lntrtferences due tn the prC9cnce of utheT Netaip, particularly nickel. Thr ecthnd of dotr<tt n 1.ne bcen tnvnd to be alnPie• (apid, nnttlve and preclee. The Drntedure is capabte ut' detetetng It•ea than 19 ng/g of mct>Is in tohacco. arsulte nill be preaented for tho d>rrrmioatton ef ,+ a1. •* robac<o sa.-Ptv+, .. tnttlc trop grades from a vorloty uf geographleal loeationsrand P'aot posu tons, and aloo fnr sama eonmerefai blenduJ tobaccos. iLe Irvels fobnd In stoute from plain cl;at<rtes sunu- factured from the stngle c e gradeo, ss •,ell ae ahose ebe.rved for the comerclnl cigarrctes, will be reported. - 11 - Pn..NI1M-710 IN t•ue4:vRC:A1. EIt:ARETfL SynrE Cut:....s5ATE5. L_•:. .arrt , a. R. 9rtn Stokely, and N. R, r.urrtn• Tob-.rco Snoke Resear•h Pregram, uak RldgerNaaon.tl ]aboratoT/. ua. Rldge. Itt 328 20 rnlnnlnn-?In tn nx oralls • rring rodloacc Wc c d( rt n.[rn of wba.n., uhl<h h s bren uf rrtvnt fntere'tt ur dcveloped, te•sted, and uclllee -a thed fer delrrmination of "'Pe In tobacco +moke -.ondrnaat:. The method tnvolvtc dl•_lutlan of the cnnJen„te to nrrl, and u rehlar/: actJw vlth wddN hydroAOn perawtd•, ~ ' 1~J"eonCovs electraJepont- tlontuf the 11CV•. n nlckel, end lnu level alpl•., countlnR. A7otrac,'r t added tu the conJ•wsate samele before J/gestfon to corrett for losara tn dissolutinn nd eleetro- derosltion. The •eethwt v reed to dvtetmtne u.e `oPn cont,nt of coum4t'rial c1RarCtte snake [nn- dcna.'tt es. Tt•e condunsatcn vrte sclccted tu rerrosent a eref.•n nf the most p^p- •tlar hranda, both flltercd +nd non-IlltcreJ. TI•e 2ibPO Ce~.tentc nf the ,ondenc.[te nam- plea v c found te be Iuw•r than rspccted, based nn recent:y publt,.hed data by oth.r 1.•ve<tlRators. The =roPO cuntent of the eondensate•a wrire by as mnch n a factor of cfght and did not appanr tn be n f(netton of filtrat/on, a:rhortgh [ne hlghest 7•oPo valuae. vare fooM (n n n-flltered cigaretto condensate. Potonlurtl0 content per gram of ve6 condenaate varled from U.8 to 7.5 dpm. After a sufficient deray perla,J, repeat analyses of 7iJPo vera performed on the aondensates to est,blloh the degree of radio- active equilibr/um vith the 'tOPb precursor of 710Po. 25
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J TUESOAY MORNING - SECTION g TUESDRY MORNING - SECTION D T¢A.~SrFJr Or ADn1t1 AND NAT'YRALLV-OGCLRRIN[. NYDNUr.ARSnNS TO MAINSTRIAM AHg a q:49 SIDESTREA.y CIr.ARETTE SMUgE. R. U. gale M. Ikeda and F. L ~ _ , . Daylur, Jr., Phtllp Ftorrle Rcsearcn Lcntt•r, RlchmotW, VA 23261 . - 36 CAS CIISUMATnCRAPHIC DERLRMINATIDY OP HYDF.~GEN CYA.vIDE A:4O Cyn.vnLtv IN 1U=50 TUgACCU SHUNE. K. D. gcunnemann, L. Tu, and D. Hoffmann, Amcrltan Nealth Tr.e P-pnse nf this eMel str.iv vas to der,•rmine rhr effr,[ nf vo1+t111ty of Iydro- I Foundatinn, Valtslla, NY 10595 +r n ehelr transfer xn malna[rram IMS/ •nd nld.•strc•,a fStl enukr. A ml>ture of ula rared hydeorarbona, der e t~ Jnros•+ne, r aprnYCd .. . ctal rlgaraeCe filtrr.savenltltered 85-mm cigdrettr+ v n rreparrd and analyzrdntorrthern,:da< and naturaity-orcm ting hydrocarbons. Nydrorarhuns vcn~ analyred by rxtrarting t[e r ret r. vl[h h<xanr, separating the rsmerl by siilclc axld column rhromatofraphy, and nelyting for the tndlvldual hydrorarban by gas chrom+tngr..r•hy. The loo nf e~e hvdr- arhuns durtng appl,<atlen and ciR,aset[e_prrpaeat.lon -1s shovn.- Gtg.trsttes vete-amoked- .nd tl•e dts[rtbvtton of tha hydrocarhens ta n5 and 55 smokc and butt vas deteewlned. ~ sulta thoo that tAe iover the aelecul+e velght, the highar the trensfrr t.. 53 sa.ker a+e 6utts vere aUAt.[ly depteted of the lover molerutar vetqh[ hydroc.rbons. Pentadccane v s found eo havr the maxluum transfer to MS smoke- Three-us aect/one of ene-tobecco-rod-behl,rd-the.chat- line-were-analvzed-lust-prtor-to-and-lust-atr.r tna fourth puft• A considerable 9uanti[y of [he lover molecular velght t.ydrocarbaaa vea Preaent even tn rhe three-® eections behlnd the char Iine. These results indtcate e eety sharp teeperature gradlent Sn the ttller behind he caat. I:SE OF PAUIUACTIyL 70RAf111 TSn1.AT:5 FrrR SfnDYINL TNE FnRFtATInN DF SELEr.-Tf.p S+rUeE C~.MPONFMY. [. Scheoitr, A_ Yv^P.er, and n. ttvffnann, Amerr:an Health Fr•undatlun, Velhalla, Ny l0595 anJ T. (`. Tso, ARS, USDA, Bel[svflle 77n5 Agrttutrvral Reaearrr, Cr:ntee , E e llav f7 l e. NO 0 fr+rtlnns eonraining radi•.artive neuphytadtone, f•+tty uc415. sternls, anvrlr:•afk..l..Id. anJ others vore tsolated from grecn tnbacrn grovn 1. t'•W;- F'rartlnnaU,•n .,, arhlrved b• soivent-partltl- , Sephadcx and r:as and thln layer chrnmatogeaphy. t.•mpt+c~r tJ.-MS vas ,~sri cn rharartarite the f•~nt m.~loe tobacco sterols• palmltic and steart; ac,d», and .al nrc..t-a-rela[ed conPounds (nicotine, myosmine. an.baslne, ntrotsrinr, 6tp.rtdylr. An o a tertred nikslutd of mass 190 vas also obtalncd. fhe aprr/fte r.•It~ortlvity of eteab.,ruve cpuundn wn rrlatively low; only 42 of the cutal radlo- rcttvltv vas inr•rr-~cetcd-Into n+e fie..ne•sr.I,+blea: tha remainder resided tr the nore pular e[hannl-s.olubles. A s nsltive and rapld m.•[hnd for tne gas chronstographlc determinatton of hydrogen cyaulde rn cotr:,c[u snuke vlll be presented. it to baeed upon the c nverslon of cyanldr to ryanugen chlorlJe with chloramine-T. Cyanogen elloride, desmolved fn n-he.anr, Is analyzed by r.C vith an E60. Thc parctculate rmttar and the gas phase er naly:ed sepererely. The cocfflctent of variatton of tutrl F'N ts less than 52 torthe areoke-of- eommercfa i -clttarvuee. The m4/nntream +eoke of the Igl acandard cigarotce ontatnsJ [79 ,.g NCS. The e..lnsttea.n srcnke of regular cigarettes, filter ciRarettes and tlttle cigsrs contained between 219 and 551 ug of NCN. The sidestream smoke of cigarlr..es-and-lictle-clgara-centatnedfroo- -87-to 191 vg HCU. To evaluate the contrlbutlon of cyanogen to NCN val,.,n, ve devcloDed a se,,a:ate C.C wethnd for Cyanogen• [n clgarett! amoke, eyanegen [unt(tbutcs 3 to ): to the gCa found in the mslnatreaw amoke. C[A.r swoke aheued an even areater percent.ge of :yanegen pre- aent. - 17 - 11:1f1 Isarr,aT1UN a tnrNrtv[CAT[tW or 1,t,6-TttMrTNYL-4-PIPrR1IX,~F, A.1 ARTIfaC1 PROUDCF.tl g9 ,111 E REAGTTON OF CIGARETTE 5'.OKE CONOENSATE ANU ArET..6E. W. N. Ffnalf, R. N. FerRUSOn and I. F. Hhldhy. Philip Norris Rr•search Center P.O. gun 2658;. Rtchnond, VA 23.61 An unknovn cnmpcnent vlll, a molecular vaight (fDf) of 141 Yaa found In tbr proressad smoke condensate of a hurley cigarette but ves abser" t+ pro<assed emoMe condensate from a flur•cured ctgarette. The compound v.s nnt_frr.ent-.In_burlcy-ffller• Fartherstudy revealeJ that the MN 141 unknovn v s preeent vtthln the Itmlta of d•tcctlnn only if aretone was used ae e solvent for processtng the fresh burley smoke condensate. The unknovn hae been td:nttfled as 2,2,6-trimethyl-4 pipa•rldnne by spoctroscopic tech- niqucs (IR, MS, IN and ; tC NMRJ nnd by comparlaon W h all authentl< saople. Levcls of the conponent tn prorvssed condensate vary from a raatmum of 0,26 mg1 clgt froe a burley eigarette u/th added nitrate to levels beluv :,e limlc of eetectfon frow flue- cvred tobacco clgarettes. yoanlhle methanfsms sre sr.poeed far the formation of thra eralrac[ during proceasing of the smoke condensate. These lovolve the [eacslon of solvent acetone vlth ameonla and acetaid(hyde vhlch-are presant tn the fresh cigarette smoke condensate. - thr fabcled materlals v se put Into ttgate[[4a, snd trrelr fate during tobsc,s rnmbna- tlun vas investlgated. A svhstontlnl pnrtton of the tvC07 lncorporated lntr plnnt oa:rrlals during pi~etosynthasls vas reconverted to ''C0, dueing tobocco coot.rstlon, rtng praduatnanily !n atdestfeam smoke- Polatlle organlls vere alsa prafervaal.ily dtstribvted rnto the stdescream vbile non-voisttle organtcs were dintr(bute! more r less equally betveen both streates. Conversion of labeled precucsors to sainstream PAN unwlly amounted to less than 12. .'r I - 1124 iNTERYISGION 27 26
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/ V TUESDAy NCRNtNC - SECTION B Amerlcan Nealeh ro°ndatlun, Valnalla. NY 10595 tNIRMA:. E6ttt:! ANAtY/lR. r. D. er..nnrm.ynn. S. S. Heeht and D. tloffinepr, A- ISIS OF N.hl(e.:SO•ta1C IN Te,eAr,'O A9D TOIIACtY) SMCIeE Y1TN THE nID Cr TIIE Thr Thc-n..i r^rray Analvarr (TrA) I, a hiphly lrnaltlve and selective detector 1<.- nttr~so c•~mF~unds fFlnr el a/.• Anal. Ct,vm• L1:1188. 19151. 'onbtnacton ot ge. cnrwutnArav^v and TEA permits the an.,lyafs of tobacco and tob vco s'•.r tnr trace annunts •+/ nittosamtnes and both volattle and nonvolatile nttrosn dnes ean be drtentned vithln a reagunab)c el.e. Fur Iht gnalvsts of velatlle N.nitrnsxmtnes 50 rig.arettes vrre sm°ked on a rotatt.g avt+..,ttr ea•:ker. Evrrv •.Ihrr channrl of the re•t.atinF held vas connrctcd to a nl rngc•n tt•.r,e to pftvfnt artlf.,• tual (••tm,.t/on af nltr••namineo, Thn snnkv v.a led t..t•• <arute yuterr [pM s.5) <ontatnlnR 5 Y a otbic aC1J and dfne[hylni[rnsaslnt-~`C a In[e nel st c^:ard. Tt•e solution v v r.tracted vtth CN"I;- and the pnnlyd ectr.,<es vore c•acen- tr.•trd to 5 m/. A(0-.l e+nvle ,. sed t••r lhe r{/TF.A analyatn. Aarnt the vola ile N.^1[t°aaminet ve lound l0-Ii0 ngrotodfinett•yl nitrunan/nc per rlgarorte• ea va•I1 is vet:.yletnyl-, dierl,yl-. methylpropyl nltrosaatneg and also N-nltrosopyrrolidlne. The an:,Iysls of nonvnlatlle N-nltrosamineet tn tobacco and tobnc<u anpkv vtll also be discu.sed. - ry A(ION :,F PNEgOLS At1D PfIFNni.tC ACIDS FpOM CIt:AR¢T7F. SMORL C:+NDyh~tTl . t1:50 J, Cn.._b.riaen- M. t;. snovk, 0. B• 4.,lters. and 0. T. C;+nrtyk, T.,b.cco L.b-.rrtory, AArI<ultvral Reararal, Setvice. USbA, P.O. bee 5677, Atnt•ns. GA ln6OL inr s=yar..t,.•n anJ quancteaclon of thr phenols or a<lda ^f <tgarrtte amosr conacns.ce fc5c1 have alw.s bern aJuereety affected by losses during aqueous ac/d-baso oatraettons. Rerrnr;y, our radtnactl,•c trarci s[,u11es ahoved large losses (75S) of catcchoi dur:ng a rr•.rtne C;C ce~ara[te° to e•bta(n a pbenollc tractlon. Thuos losses of other pherslg alsn sreeed Ilielv. To correct lhe proble.m. v have dweloped an ton-e.change mett rd ror rcuttne trucrtonatlor. ot snail qwntlcies (I g) of CSC, and thig pr°cedure v111 ba descrlbed. The aecond preblea oe<vr. tn the g.. ch<omecoKraDr,y (GC) of theee eeape~ands• Er:esslve blteding of the carbovax TPA talulttls h.s prohibited their usa in KS idMtl(leatlon gtudles on nev phenols. The use of chs substrates. Tensa CC and SP-2401. (ar asobe pheaate vill be dteeasaed. 32.1E S.urON 7:Ag TEBRNICAL SESSION= SEBTFdM 0- or. NiINa. d. 6balepNblbr Frsslllsg -r,G- TUESOAY AFTERN00k ryh:wtur.'•IS Or Sl'CCIgIC ACID AND DIMLT(fyUtaLFIC ANIISDRIbL feuv AcPAaTIC ACID. iaA A. v. Fort, 1. N. Patterson. R. Small, b. _. banditah and Y r. Smr[h, ]r., bry.artmenl n/ cnrmlatry. itnloeretey of etn vcky. Lase°gton:'1cY 4uiun Aspartlc ac1c1 tr•t, pyrolyiru under a glnu gtream of nit ogsn at tomperat°res renqtnR from )50° - 6Srr', . u. c Intc ac 1J v..e thv ma)or nonvv1at11a actd prnduced, ulth matlm•va fSyle.d f1)Z) nccurring sat 650°. At Sn0° sapartle ac(d-6-Ilt i.sve succlnle acid with ,.nrlunged t'F. enrichment. euetarir an,l mlialc acids are possible lntorttedfates ln thls tran.forma- tlon. When +vm..ric ncid v.,s mlaed vlth slan/ne snd pr'olreed. le vas parrrelty convert<.f te avr.:inlc r..td. A m1n••e prnJ•,•t ffnn pYrnlysle r.f aoparrlc acid v s direlhylmalelc anhydrtdl. Alanlne rnvr nrgllf.lble a unts or dtmnthylaulele anhydrlde, b,t misturr,• °f alanfne and +spartlc acid t:ave a s,v nPtnld mcrc•ale 1. the y/eld of dlmethvlmaltle anhydrfde. The resulte of arbon-i) trntc•r e<rlnente establlahed the stolchlomrtry of the miat•d pyr.1yn1/ rtactlDn leading t.odlmrthylmalc/c anhydrlJe and also t:.oved that the <arbo.yt <arbon atose of aspartl< a:id bc•nec equivalent at some strNn af the res.tlon. A close rctatlon vh[p bcweon the formaelon of dtneehr~:^al•t< anhydrtdv fcee alanine and aspartJc acid or fumsr!< acid and ehe rrJvction at fvmric acld tc sucefarc attd by alantne fe /ndtcated. gesct/on echeaes are presented to account f°r the 7tC dtstrlbutlvn in the ptodv<ta. - 41 S1.aUTATtON br SMORttk. cONnIT(Ox5-by PyROLl--tS. C. br i¢. e: i.-;eva.ee, - :: zo R. P. Arrendala, ane n. T- Chertyk, Tobac o Inboratory, egricultural Reeearch Rervice, USDA• P.O. gn. 5677, Ath:ns, CA )0604 The ob)ectlve of thlt v°rk uas to develop a,ryrnlytfc ?rccedure to dvpl(ca:e the cnndl- ttnnc tn a bvrnini cigarette. rn th.n .v , to6nc<o s.,n~lc. •ou70 r'.e evalu- a[ed (nr ncl~rtrd ,al smpke aonetfluents, vlthn•~r (obric.r. +nJ am..ting of f,.,rvtees. rhe m,.ehn.f ,.ttland a„ntrnlled pyrnlygtb paratus ~..m[ldr 'o Urat dr•rLlyd by Smlth and P_,ttersnn ITnh. Srl. xlr: $0. 1975). With [t:ts np..,ratus• tt vas po•,>Ihie to •~pu:ae " the mov.•mc•nt of fhr n, and tt:e carrier Raa fto,< 10 -.n.,tete a clgarc,er pvff. or to h•,vc .,stant K- fl°v and nren m°vemcnt. This appara•nv prrmittoa dlstlllarton e( volet u r c°mpnunes obrad ot ehe awvtng hot z°ne and c:~nJ,nsau on and repyrolyefs o[ felnttvrly uo•wulatilr c.npnunde• thereby ste.ulatrng „twl ttearett. <..natelen.. 7Yrnlytic conaitl.•~.e to prodv^.e PN/ dlattih„tinna ' c.+cly reet•nhting .yYe Conderreate PAg Palternv vere detrnntncd VEfh 1R1 tigarottea aadt.-ba.ru. The resulting pvrvlysates e frpcttonated by •.•.tv.nt Porttttoni.ng-erv4pN-ad)us6ernta-into ntarals; bases, aclde• nnd phenols• Neutr.,ls .. chrowtogrept:ed o sllltlc acld vlth PAH bring t:°ted in the bc•nacne-petr°lcum cther (ractlen. The PAH vere than /:rther <oneeneratoJ by gei frl- trattvn enro,.ategraphy and ehen onelyzed by e_ •aroma ography, Th1b proredure repra duaed smoke PAH dlstrlbucione owre olosely than prevto uly descrlled methoda. ITe ugs- fulnesa of thlg pyrolytlc metMdf°r the avaiuatLom an+ <haracter[zacton of vartovs tobsccoe will be dlacuased. ' 29 28

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