LABOV,\WRY IO-TOrT %. 51, 1.
COPY till.
I SEP1968
DIPERIAL TOBACCO COMPANY OF CANADA LIMITED
RESEARCH LABORATORY
MONTREAL
SIMULTANEOUS DETERMINATION OF TOTAL ALIPHATIC
ALDEHYDES, HYDROGEN CYANIDE, ACROLZIN, PHENOL,
NICOTINE
AND STEAM-VOLATILE ACIDS IN WHOLE SMOKE.
PROJECT NO. 0331-01
_A,
AUTHORS:
WORK DONE BY:
ISSUED 37: DR. V. C. RUNECKLES
DISTRIBU-1--0:
Copy No. I . Library
2. Mr. L. C. Laporte
3. Mr. R. S. Wade
4. Dr. V. C. Runeckles
5. Dr. T. A. Smith
6. Mr. E. R. Freiesleben
7. Mr. M. Scherbak
8. Miss R.R. Smith
9. Dr. S.J. Green
E.R. PREIESLrBFN & T.A. SMITH
L. DOUCET AND E.R. FrEIESLEBEN
DATE ISSUED: MAY 31, 1968
10. Dr. S. J. Green
11. Dr. S. J. Green
12. Dr. S. J. Green
13. Dr. S. J. Green
14. Dr. S. J. Green
15. Dr. S. J. Green
16. Dr. S. J. Green
17. Dr. R. B. Griffith
18. Mr. G. A. P-.e$Lon
(j,
CID
BATCo document for Province of British Columbia 5
November 1999


A method has been developed for the simultaneous
determination
of scroLain, aldehydes, hydrogen cyanide, phenol,
nicotine and *team
volatile acids. Greater accuracy is obtained by
applying the established
procedures to aliquots of the whole smoke
condensate from ten cigarettes,
rather than by using the smoke condensate from a
separate set of five
cigarettas for each analysis.
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BATCo document for Province of British Columbia 5
November 1999


INMDUCTION
In the previous standard method@ for the
determination of
hydrogen cyanide, total aliphatic aldehydes,
acrolein, total particulate
matter (T.P.M.) %otineoenditotal phanols in
cigarette smoke (procedure,
November 19, 190) 6at f f ve cigarettes was
smoked, TFN, nicotine and
phouals being determined from Cambridge filters,
and oldehydes, scrolein
and BCX from the "vapour phase". It has since been
shown that such dater-
minations of vapour phase components are erroneous
due to absorption in
the particulate phase an the filter (1).
Procedures have subsequently
boon developed for the determination of 9CW (1),
total aliphatic aldehydes
(1) and scrolsin (2) in whole cigarette smoke. it
was felt that those,
:rd,orlwod1fi*d::thodo for nicotint (3) and
phenol*
t0 h1swtheorldwilb.satan! fu ato rua tvchosee to
the above, except that the
smoking of 15 cigarettes for each not of
determinations would be necessary,
compared with 5 previously. In addition the
stesse-volatile acids in whole
cigarette smoke could be determined by smoking a
further 5 cigarette@ (5).
In the present work a method has been developed by
which hydrogen cyanide,
aliphatic aldthydes, scroloin, phenol, nicotine
and steam-valstile acids
can be determined In whole cigarette smoke using
the whole smoke condensate
from only 10 cigarettes. An outlLn* of this
modified procedure to given
in the appendix.
Comparative analyses using separate smoke
condensate# and a
sLoglo condensate were obtained using conditioned
74 mm. plair Check
cigarettes, selected at 1095115 mg. The cigarettes
were smoked under
standard I.T. Co. conditions to a 23 ass. butt.
A. Determinations usins Separate Smoke Condensates
The smoke from four sets of five cigarettes was
trapped in the
normal way, and the condensate* used separately to
analyse for the follow-
ing components by the established procedures (a)
total aliphatic oldehydes
sod HCH; (b) acrolain; (c) phenol and nicotine;
(d) steam-volatile acids.
S. Determinations usLuz a Sinale Smoke Condensate
The smoke from ton cigarettes was trapped in a
cooled spiral,
coated with 9:1 v/v methanol:water, and an aqueous
mothonclic solution of
this condensate prepared. Aliquots of this
solution were then analysed an
described in the appendix.
IRSULTS AND DISCUSSION
Check 14o. 7 cigarettes were used in the first
study (Tables I
and 11)~ while for later analyses, Check No. 8
cigarettes were used
(Table@ III end IV). The standard deviations for
individual ounlysee were
smallest when aliquots of the same whole smoke
condensate were used for
each analysis. Thus although fewer cigarettes were
smoked for the combined
analyses, greater accuracy was obtained,, possibly
through the reduction of
cigarette variability as a source of error.
CD
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\41
BATCo document for Province of British Columbia 5
November 1999


R9 Fw9ItNCzS
1. X. Schorbak 4 J. R. do Sousat I.T. CO. RL
Report No. 80, April 13, 1965.
2. N. Scharbak & J. 1. do Souzap I.T. Co. &L
Report No. 90, August 1, 1966.
3. J. 1. do Sousa & W. D. Stephenson, I.T. Co. IL
Report No. 46, February
25, 1963.
4. W. D. Stephenson, M. Scharbak & J. Z. do Sousap
I.T. Co. IL Report No. 51~
June 12, 1963.
5. 1. IL. Froisslabon, I.T. Co. &L Report No. 93,
October 310 1966.
XI'
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BATCo document for Province of British Columbia 5
November 1999


0
0
CL
0
0
TABLE I
MTKIMMATIONS, IN SIPARATS SHM CONDINSAT9 S FROM
FIVE C.R. 7 CIGMMS
0
M
I
0 Set Mo. Acrolain Aldehydes Hydrogen Cyanide
Phenol Nicotine Steam-Volatile Acids
/cigt. psm/cist. AUICLgt. S./cist. Mg/cist.
Mg/cf8t.
CD 1 87.2 1158.3 324-T 234 1.70 1.02
0
2 85.8 1230.8 305.0 240 1.69 1.11
5 80.8 1204.1 338.2 212 1.62 1.13
4 95.8 331.9 204 1.62 t.04
0 5 305.0 1.06
0
6 328.1
7 353.2
z x 87.4 1197.7 326.6 223 1.66 1.07
0
(D
3 Standard 6.2 36.6 17.4 17.2 0.044 0.047
Cr Dovistion
CD
Coefficient of
Variation % 7.14 3.06 5.5 7.73 2.63 h.39
to
16 SZ6~~O~


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0
CL
0
0
(D
0
0
0
Cr
CA
z
0
Cr
CD
CO
TABLE II
!)ETERMNATIONS IN OITF SMOKI CONDENSATE Fl.OE TEN
C. 14 7 CIGAI:Err.-,S
Set No. A~rolein Aldehydes Hydrogen Cyanide Phenol
Ni-otine I Stea.-Volatile Acids
-/cigt
pgm/cigt.
ardcict.
I,g"/Cigt.
"'g /c j ft. C.1
I
g/cil.t.
1 79.7 267
1 332.5 202 1.65 1.09
2 100.0 1
348 339.7 210 1.70 1.02
3 90.7 1276 340.0 203 1.66 0.96
x 90.1 1297 337.4 205 1.67
Standard
Deviation 10.2 44.4 4.3 4.4 0.03 0.065
Coefficient
of 11.3 3.42 1.26 2.13 1.58 6.37
Variation X
~6(-;Z6ROp


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F
:3
Cr
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Cn
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Cr
TA511 III
DETZRNMTIONS IN SEPAILATZ SMOKE CONDENSATES FROM
FIVE C.K. 8 CIGMTTZS
Set No. l
Acrol Aldehydes Hydrogen Cyanide Phenol Nicotine
:
;t.
~,gm/ I pan/cist, pga/cigt. pgn/cigt. me/cist.
1 102.8 1267.5 520.1 250 1. 69
2 139.8 1378.2 468.8 222 1.57
3 125.8 1240.7 545.7 206 1.68
4 118.0 1308.2 541.3 254 1. 69
1 5 108.0 1058.0 490.6 270 1.74
1 6 107.8 1544.0 522.8 278 1.72
7 127.8 1260.0 525.0 286 1.72
a 120.0 1316.0 562.5 289 1.72
9 io4.8 1.72
x
Standard
Deviation
coefficient of
Variation
Steam Volatile Acids
mg/cigt.
1.27
1.17
1.18
1.19
1.27
1.19
117.2 ivi. 6 522.1 257 1.69 1.21
12.5 97.6 30.3 29.7 0.026 0.046
io.6 7.67 5.79 11.5 1.51 3.80


0
0
CL
0
3
0
M.
-ft
0
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3
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3
Cr
CD
to
TARLI IV
DgT-MIUTIONS IV M SMn OoNDIgNSATE F&M TO C.R. 8
CIGAUTrES
set No Acrolein
I Aldebydes Hydrogen Cyanide Phenol Nicotine Steam
Volatile Acids
.
pwcigt
pgm/cLgt.
pgm/cigt.
p ga/cigt.
mg/cigt.- mg/cist.
1
124.0
14 W
528
212
1.75 1.22
2 126.7 1565 557 246 1.78 1.22
3 uh.6 14W 558 248 IM 1.27
4 105.2 1418 530 262 1.71 1.2T
5 119.0 1455 56T 2% 1.72 1.33
6 u6.0 lh45 565 248 1.73 1.27
--
117.6 1462 547.5 242 1.74 1.26
standard
Deviation 7.6 38.1 17.6 16.9 0.028 0.04
Coefficient
-99 Variation 6.49 2.60 5.22 6.98 1.61 3.17
P 6 ~ Z 6 ~ e 0


6 PPZNDT'r
PROCOURE FOR DIT19RHIMATION OF ACROLZIN. ALDSHYDgS
HYDROGEN CYANID9. PKINOL. NICOTINE AND
STRAH-VOLATILZ
ACIDS FROM ONE SMIS CONDRNSATZ
1. Smoke ton cigarettes, each conditioned and
selected at their
average or target weight t 15 mg. to a 23 sm. or
specified butt
length under standard or specified smoking
conditions.
2. Collect the smoke in a spiral trap which is
internally coated with
a 1:9 (v/v) water: me thanol mixture and cooled by
immersion in solid
carbon dioxide and acetone.
3. Wash the spiral, containin the smoke solution,
successively with
several portions of a 1:9 1-1/v) water-methanol
mixture, transfer the
washing@ to a 100 mL. volunatric flask, and make
up to volume with
water:uethanol mixture.
Determination of Aldehydes and Hydrozen Cyanide
4. Pipette a 25 aL. aliquot, (paragraph 3), into a
dry, clean Claise"
flask and steam distil.
5. Collect approximately 180 ml. of distillate in
a 200 u1. volumstric
flask containing 20 al. of a 1:9 (v/v)
wat*r:methanol mixture, and
adjust to the correct volume.
6. Use sLiquots (h mL.) for the aldehyde and
hydrogen cyanide determine-
tions following the established procedures.
V*ter-4nation of Acrolsia
7. Transfer 20 mL. of 95% ethanol into a 200 ml.
volumstric flask and
reserve as distillate receiver.
8. Pipette a 25 al. aliquot, (paragraph 3), Into a
dry, clean Clateen flask.
9. Connect the Claiven flask to the distillation
apparatus start the
ethanol vapour generator and distil, collecting
about 160 L. of
distillate and adjusting to volume.
10. Use aliquots (1 al.) for the determination of
scrolein following the
established procedure.
peter"Instion of Phenol and Nicotine
11. Transfer 10 al. of saturated sodium
bicarbonate solution Into a
200 =L. volumstric flask, and use as distillate
receiver.
12. Pipette a 25 uLL. aliquot, (paragraph 3), into
a clean Claisen flask
containing 20 al. of 5% sodium hydroxide solution.
13. Add 10 ml. of 20% sulphuric acid oolution.
Connect limsedLatel t
the disti.11stion apparatus and steam distiL.
collecting about 1900.11.
and adjusting to the mark. Do not discard
distilland after distillation.
Un
110
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BATCo document for Province of British Columbia 5
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14. Determine the phenol In a 25 al. aliquot of
distillate by the
established proctdurs.
15. Cool the phenol dlatilland (paragraph 13) In
ice water and add
10 al. of a solution which consists of 30~ sodium
hydroxide in
saturated sodLuu chloride solution.
16. Repast stems distillation, collecting
approximately 480 al. of
diatillate in a 500 al. volumetric flask
containing 18 al. 1.2W
aqueous hydrochloric acid, and adjust to volume
with water.
17. Determine the nicotine by the established
procedure.
18. Determine a phenol blank In the same
apparatus, by distilling 25 ftL-
of 1:9 (v/v) water:mthanol mixture, to which 20
al. of 5% sodium
hydroxide and 10 al. of 20% sulphuric meld
solution have baten added.
Stema-Volatilo Acid Determination
19. Transfer a 20 al. aliquot (paragraph 3) into a
125 al. separstory
funnel.
20. Add 60 al. of peroxLde-froo other and 10 al.
of 0.02 N sodium
bicarbonate. Shake and allow the layers to
separate.
21. Transfer the aqueous layer Into a 50 al.
BrIenneyer flask.
22. Repeat the extraction with 5 al. of 0.02 N
sodium bicarbonate.
23. Proceed with the acid determination on the
combined aqueous layers
using the established procedure.
BATCo document for Province of British Columbia 5
November 1999