Revenrch & Develoymnt Zfft&b1i9bM~ntV
GOU111AITTON.
;.1fith April, 1956
H-VI!,,FD pROp0!:Ajj% InR r,-r)x, AIA-1-:110
1. Pitin' Aim
The initiql aim ,112. be to -.anln,~# prinarilyr
the neputral
fraction of tho ron-Tolatiles In tObnccO moke.
There way be fl.":P90ted
to c-~nuist of polycyclic hydroearbone mud tivir
doriTatillep high
moleculer we'uht, raraffirls an" their
derivativort certain riterelp (if
prcoont) ruid hirh noleculAr velpht alechyder,
ketcres and alcoholp If
thece are rroduced. There n:~y elso be
contevninntion from unrenoved
acide and Iw-eq. Vicotine ard Its treni-cloi-rn
prolucte appenr from
reports to hn-nd to be very pcTrintent In
ciparette tars.
One* Vie annlytical pro,~cfl,jre hnn teen firrIly
ral-ated nrd
an Van -f tho rrrl-c of e-rnwines nrd Vinir
qunnttty hns been deternine%lp
tho rrer!eduro -III be applim] t,) virt-aft brrnen
or ric-tratte, rradve of
x7 M tobneco -ind tobacco-types nnd s,),reerp a.r.
flue-nireA, burl-71 etc.
2. 14--Wi,0 to rwdo,itnd
1 hin znirt nceerrarily bo e-n-0,nt rch---c-Qe rt
t hiv rt-re.
InMilly, It In -rer-oned to ure thn I.T.Co. (-urlt
r!1ttcrrck,_r in the
rwirer dercribed in tho Irstru,)Urn rimet, i.e.
Lbe rnnhe nwrorol "411
be pred!1tnted in et r1are tul:s by an
vlectrort,~Qc I!J.Fh tertrion
rrecipitator. Liter, thin r!,y 1-a no,11find to
en-Oln th-9 v-eh" 0 be
coUceted in a rolvont.
Ihn rrcke coneertrnts tl,u,) bt-tn-d -Ill 1-i
diarolv-d In a
rolvmt, rrol-031y ne!tIqlPre ehlcrida ritir,3
Ternrnr~!_ r-!qtn.!'.n Co. rtate
that V,in e-eq not react vtth polycycile
1?y0r-ocnr!--rr1 in the 1-!'Y enrbon
tetrneldcrit!o ertl chloroform i1c. Di r,,Ixztion
of t!,e a-.wkn t?,re vill
th--n be thorou.-,Toy extracted vith diluto neld
(to rcr-~Ye bmrie ccrTanentri)
euit! ther., mftcr varbing vi.'h wnt,cr, thr-
rerltlu-tl. orimnlo plrir,!v Mll be
7 `7" rxtrnotod vl.th alkali. This eccond
ertraction inf,;# l1th n,!T,-ntrjrey
be roplaced 1,y a tvo-part o~-trnetloni-
(I) t1th redium ekib-)nqto r-lutlen, t,3 r,~-)Ys
acldR
(U) with andiim hj-,Irm-ide rf,lutien, to rr-:owe
ph-~r,~ls
01 ch t-M n,~t retet with podium carborate. After
a fir.,ql tvtch vith
water, the orr-nic phiss %1U conatet of reutral
tmrp..
It "y prove nererfrry nt st Inter ata-q to enrry
vit all the
initit,2 ort,rations In the nbrrtice -f lirlit or
in r-cn-acttnic T-FtAlnttion
(rot!-yel,lo-.- fJ-Itcr) in order to mirimiro
rhoto-o7ldntinn of th"
1 wx1rowrb,?r.n.
The rnttr:,_I t" 1-1.11 1,9 rcenTern,' frcn 0-t
nothy-lene eh1critle
r.n,l thrn it till he redivelved in Fk rcn-ral,.ir
rolvt-ntp e-r.- rntrolet.".
or cyclohv~rnr!. It vill then 1~o fri-eticwited by
elution chrcv-ritegrrrtq
on colurra nf netivated nluntri or rilit-a. gel
(1-ith -drcrb~.-rtr hnve been
urod in thin typo of unrit), ur-irFp volvmitr! nf
rr.-t00 dnrerptl,~n pet:-r.
The e-.)arvo cf Vie fractlerition vill nerA V) 1,9
elnr,,Jy chrehetl
t-.y rc. rn -.f flitcrod ultrn-T.1,31at li-lit.
Tha var.1-:is hytlror-rb-~rm 01
fl,w,rerco -Ith Olfferent cnlourr, rrl thtn fcv-a
a uroful qur_ltt'~UT-9
Irlicition of the mtent of re,-&rntI^n nr~?ievoe.
It vill rrob,!My 1-9
rreorcn:y V3 nvild c%-perure of -tho c~.,br!" to
31rht P~r Ionf, ,Ti,l n .rmall CJ;;
dnr!~-rvrn r-y Nq re. juirad.
BATCo document for Province of British Columbia 2
November 1999


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The fractions obtnined In the Initial
fractionation will
havo to be taken to dryness to obt-tin rL rough
qu&ntit&'t1T9 balance
of the procedure. They will then require
reebtromatographing to
effect further separation of the roir-h fractions.
3- Ider'" ficatt-
The method of identification to be adopted will be
determined
by the oocp=Ms present* Polycyolle arawtis
sompiands eon, In
gone-ralp be detected by their ultra-violet
absorptirn Mmetra.
Hovevers it appears that with 3s4-benspyrera and
perluWs with other
tbeproperes of Impurities can ve distort the UV
absorption
curve as to dIrguirs the true nature of the
Components prevent. In
thl- enno the fluorescence "..-trun may I-* utted
(r"v belov,
Apparatual, 314-Bonspyrene can apparently be
annoyed on a microeren
level by means of the fluorevernev Ppectru-1,
(Rw,-lort of wyrk carried
out by X.T.Co. (of G.B. & I.) ).
Fanor chromatograpb;r of the firal frar4ir- f.,
eliitton
chromatographl was, used by e9 Sousa for the
detection of bearpyrene
follovInr a roeedure mhlirhel bv Tarbell at..Pl.
7 L M, 1ho revultri u--re nel:%tive, %tich m-y be
Oixo to the
method being In-vifficiently sersitive. It I a
-orth bosri-rr, In mind
ard an early attenOt nay be rndo to of-11-Ate the
f,!ftrillility of the
methnd.
4- &L-XAtYJt
for tho r-casurement of ultza-violet abrorption
sy,,~etrj,
rhoto-el,~~ctrlc spectrophot4meter of tbe Vilver
Uvl7mek tr-s A.s
Irdispeneil-as. Houvver, all designed, this tyne
of instrument cannot
meneuro fluorescence spectrap although ly the ure
of filtn" it ~s
porsible to meauura the intensity of fluoroeetnco
at a particulpr
wavelmigthj In thin procedure tho monochrom-itor
ir tot urr~.
T
Mu orly Instrument ilhich does record
fl,2-,rora-m,?-9 r-r-etra
is the Cary rtteording Ultra-violet
spectrophotometer, OM Amorlemn
instrummt Jh1ch used photo-mvItiplier tutex in a
chmppod d~-ble-heam
optical assanbly, the difference bet-reon the
rofer~,nes becyt PTA the
an-ple berm being amplified and red to it
recorder. It M be merible
to modify a Itilger Uvi"k so as to ure a
photomatiplivr je-%rerAs)
tube In Place of the norm-al photoelectric
datect-r tube. Joi-M the
momclu-ccator could be uLod WW a Iluotericence
spectra obtnti-W.
From i4tat krowledee I have of the HUFar
inwtrum~nt I thirk the
rwidificaLimi would Imv#3 to be drastic, since us
it otrmde at present,
the va~ple and solvent 00119 OLre situated
Imerlint-sly lit front !-T the
detcetor call and the beam of lig;tt parsing
throub+ is alrraeT rono-
chromstic. Circe the fluorescence Id.11 crivinsto
in tho the
fluorepcont lirht (at right ark:los to the paih of
the exciting
radittion) wU-l need to pnes through a
ronochromator between thm call
and tLu p1wtczultipl1er tube. Howu"r, eKptrt
advice an thts MIF-.ht
be scuCht.
A accord possibility ariver. In Ch&-airtry nr.1
'(rA,,Rt-v7
(A-1.21F.t i-rae)# Unican Ltd. of CambridFo have
advertired a now
Roolirdirs Ultra-violet rpeetrophotometer
(dmud,le-bew-t,
optical ry.-ten) -jh!ch they vill be showifg at
Vis Fb7sical goojoty
rxhibition in Lon-ion an 14th - 17th May. This
would app-ar to 1,o 0
elorely sk-2113,r to the Cary inctrument, vith
inazoved revolution, end C,
It should be porrible to ncffeL" fluorercence
PPeetra and record the
regults vith this. '"i
BATCO document for Province of BritiSh Columbia 2
November 1999


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If it In ad porAble to mdIfy a Uvispok Imtrurtrut
to nespure
fluorvrof-ace rr".trz Men ronriderntinn rICK vn11
he gim V3 tbo
Valcon ree-yrdirg ultra-violet vatrophotometer
vinen, If an anticipated
this is VInOor to the Amorier-'a Cery Ltrw;a' it
;111 .,arnw. both
ultra-vidle't absorption and fluorescence spectra.
An alternative
pr*poral vould require tv* inrtruments, a Hilger
Vvisp*k and a photographic
opectrograph for fluoraecemet meantrements only,
with e-011-7
4"'Jual-ttion and photographic equipment.
Together with this inw-rumental roquiramentp an
ultraaviolet
lw:P idll be rapired for visual warAnotion of
varlow fractions and/or
abrormitograw.
5. Solvents and, Che"ic-la
The initial Polvente alreody ordered will probably
mt be
mifficient, in qtutntity and will certainly be of
lore than the reTLIred
purity. All the reports available refer to
solverts purified to I p.p.m.
polynualear hydrocarbono, and I.T.Oo. (of G.D. &
1.) state that rigorous
storage and handling precautions are alro
required. It voidd be
valuable to Itnow, their methods of volvent
purification, the storage
precautions finally adopted nnd their moth,)d of
purity assay.
Since the sapdrations or-MaTed on P-lumins, eolwws
are AnpmAent
upon the tretre-stnent ani qunlity grado of the
alumina ureti, It W be
rieearr--ry to try eaveral so-areas for thiv. It
rty be rorrible to
recowr ard reactivate the urW. alumina.
Informi4tion as to the I.T.Co.
p-ocedure would be ur-ofti in P"rtenirg the tine
of rxroriment on this,
too.
Ba-MrIGE of Tnrlolav of the rol7eyelle,
b1drocarbone -All be
rsquirod. for eon-rkrieon purpores and for dot".
in-!tlon of their Y~ectra
ote. There My be purchaced from stirrIlers of
rerearch ehe-icalpt e.g.
L. Lls~,ht & Co.1 1-ut It rzy not be thought
der1raMe for the GoTmW to
Purchase N4-bonrpyrone for example. A decision an
the onijrEe to be
ndonied here vould be valeme.
6 e Smokinp RpOva
There appears to be no uniformity In th,~ solecti=
of factors
Wch gayern the ter-)erature of the pyrolyrte, 9.g.
volume .1 puff, tine
of puff and interval betveen ruffs. The length rf
cirnrette tuttleft
will have an effect an the producte distilled -
the longer the butt,
the better filtering action on high molecular
usipht comp, ounao. The
regimen given In three report@ are, tabulated
belous
Labarat." Val. of Daff Puff tine Fo.of T"Iff" Mt
le"Pth
Cos. seen. /min. Me
Tomorres ?hatnon ? ? 3 2
I.T.Co. (G-inada) 35 2 1 Z3
I.T.Co. (of G.B. & 1.) 15 2 J. 19
The I.T.Co. Autoovoker in ftPigred to givt A PUffn
per minute,
the puff volume being adjurtable up to 3o can.
Aspiration of a large
Volufte of' air through a gloUng clearette 4 times
a minute P-rq well
rnise the t "rerature of th I t u-turally high
levall so that CD
the volume choren by I.T Co J
rr,". appear. . reaponable fi.L-uro
up= which to stnndardiaeo A butt longtb of 19 me
(equivaltInt to
CO
BATCO document for Province of BritiSh Columbia 2
November 1999


- J, 40
is also ress-,oWle. Modification of the Autcamoker
to prodww f~9
Lwgw puffs per mi=te sbould be sonrldered for
future work. A simple
goar box thotad bv suffialtnt for this pa"oso
7.
required$
oolim - RavIrLes hmm been made ftm
Baird Tatlock Ltd. re=rdiag a q!iatiftm for the
wipply of them.
Quicktit A Quartz Ltd, an alternative NMPUWS#
although the nags of
sisev'is IL&Itod. A decision Y111 be taken as socs
an the qm&MMow
(b) Brectrometers - It vould be very desirable to
visit,
Magarle, particularly to too vheher the Uviw4k
instrwant cow be
m6 dified to meama-9 flucresow" epee . tba Unions
instrument
~wti=d idn 1-9 on 0-ow at the Pliqvical Society
2zhibition in London
I;OrA May 11,+.'a - 17th, tickets for Aich w7 be
obtained im Woes. It
wad be derirable to see the Unifts instrumeat and
see the povalbilities
of this f ", thft job In viev, in the event that
the HIlger lnetruwnt
oa=wt be riodified.
(a) Ul Ian - A catalogue of UT lo" has boon
requested from
Hanavia, LU., "laugh.
(e) F-iner M n-a-ntn"nrbY - Proll-tinary
enerimants an the
feasibtlity of thi!? analytical viethod for bens;7
no can protably be
carried out vith emixting arm, Rntus. Tf the
method in vorkable, then
at a War eat* a comercial chormatograpb7 tank
var.1d be r"ared.
Littron wjWjT.C,3. (,)t c.p. e- it).. Briffta - If
a vialt to
thane lelt"tortsi% ern be arrem?eAl it vould
greatly facilitate an *aAy
start tn %cft. The rrthaAn of nurification and
stwAarde of purity of
the solvents are obviously of crucial importance
In order to avoid
spurious results. 1.7.0o. have apparently a
otan4ard procoduve, th2
adoptirn of %tt~eh 1~y B-A.T. vould onable direct
coc:parison of results
on different tobftecce.
CD
BATCo document for Province of BritiSh Columbia 2
November 1999