IWK/CAW46C 28th MAY 1965
STANDARDTSATTON OF SMOKING PROCEDURES
There Is considerable attraction in any form of
standardieation
of smoking procedures which might be used
throughout the B-A.T.
laboratories, and indeed on a smaller scale R. &
D.E. has been,
and In, actively involved in various collaborative
tests with
the T.R.C. and the Analytical Methods Committee of
the Tobacco
Chemists' Conference.
The various laboratories are becoming more and
more
concerned with the routine measurement of
deliveries of a number
of individual components In cigarette smoke, and
with the more
extensive evaluation of filter performance. Within
each laboratory
various methods are being used for such
investigations, and by and
large each laboratory has probably spent time and
effort on
methods development which might have been devoted
to other work
if a Procedure for methods standardisation had
been In existence.
Certainly in the future the number of problems
common to all
laboratories will increase, but only when standard
methods are
In use can one hope for inter-laboratory agreement
and good sub-
division of work.
Consequently, there does seem to be a good case
for accepting
the principle of standardisation and considering
where practical
steps can be taken to reach this end.
In this context It might be pertinent to define
where pos Ible
those smoke components which are of immediate
Interest and th:se
of possible future interest to the Group. In terms
of the first
requirement, It in suggested that smoke indices
which will need to
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be measured routinely In the near future will be:-
tar, nicotine,
acrolein, formaldehyde, hydrogen cyanide,
phenol(s), oxides of
nitrogen, individual acids (?) and menthol.
Some of the above, tar and nicotine, are to some
extent
already routinely measured, albeit by different
methods. However,
with the collaborative tests that have been under
way in the past
year it is likely that the use of the Cambridge
filter and the
measurement of total particulate matter and
nicotine may become a
standardised procedure; this method might well
form the basis
for a B-A.T. standard also. For the other
components the
situation is a little more confused in that each
laboratory
appears to be using methods which are either
similar or different,
and certainly there is considerable scope here for
valuable
standardisation following the use of well-designed
collaborative
tests.
If such an approach is acceptable, then other
features
e.g. smoking parameters, collection technique,
will automatically
be considered.
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APPENDIX I
The standardization of smoking procedures can be
considered
logically under three headings.
I Smoking parameters
II Smoke collection
III Assay methods
1. SMOKTNG PARAMETERS
Here It is necessary to consider smoking machine
design as
well as puff volu , duration and frequency.
Suggestions on smoking
machine design can be summarized as follows!
I) For routine smoke delivery measurements - the
existing
R. & D.E. (bellows type) smoking engine.
ii) For routine selective filtration work - it Is
intended
to use a 12 port R. & D.E. type smoking engine.
The
Increased smoking output is necessary to take up
the
auto analyzer facilities to full advantage.
III) For research purposeso a design of machine
ban not yet
been finalized. but it is hoped to have available
soon:
a) a "free" B-A.T. machine
b) a "free' 'square puff' machine to give
flexibility of puffing parameters and
co-ordinate with biological work.
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For puffing parameters, there are two sets in use
IR-A.T./R. & D.E. T.R.C.
puff volume (ml) 35 25
puff duration (see) 2 2
puff frequency (per min) 1 1
Butt ler:gth (mm)
plain cigarette 2.3 20
filtered cigarette a) length of filter filter plus
+ 8 mm tobacco rod 8 mm
b) length of filter tobacco rod
+ 2_3 mm tobacco rod
For plain cigarettes, the 2_3 mm butt used
internally in
R. & D.E. was fixed some considerable time ago to
fit in with
the earlier Foster D. Sn*ll requirements.
For filter evaluation, most of the R. & D.E. work
is
restricted to a butt length comprising the filter
+ 2.3 mm of
tobacco rod. There are principally two reasons for
this choice
of butt lengths:
a) the need to measure the filtration of the
smoke, when
the smoke In at ambient temperature, and
b) avoidance of butt lengths at which marked
changes In
the filtration coefficient values occuri this
leads
to better reproducibility and hence economy of
sample.
Another important factor In smoking in the
standardination
of cigarettes. The conditions are
Moisture Equilibration 56-58. R.H. and 700F
Selection average weight (:t 20 mg)
average pressure drop (t 4-~) at
a flow rate of 1050 ml/mIn.
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11. SMOKE COLLECTION
The methods of smoke collection are to a high
degree
dependent upon the component in smoke which is to
be assayed.
So far, tar and nicotine are the two indices which
have
received the greatest "public interest", and the
two standard
collection techniques in use are the Cambridge
filter and the
Foster D. Snell train.
The R. & D.E. method of collection for measuring
tar,
nicotine and phenola is the 221 In diameter
Cambridge filter.
For other smoke components, various trapping
systems are
used in R. & D.E., for example:-
benzpy,rene
low temperature trap aldehydes
nitrosamines
land other trace compounds
',furfuraldehyde
solvent trap oxides of nitrogen
.acrolein
,aldehydes
chemical trap hydrogen cyanide
~hydrogen sulphide
For filtration studies, Louisville use a high
pressure drop
carbon bed for collection of the whole vapour
phase. The carbon
In eluted with a solvent which In then used for
multiple assay
with the auto-analyser.
111. ASSAY METHODS
The various methods In use In R. & D.E. are given
below:-
Tar and Nicotine see Appendix II
Benzpyrene see RD-314-R
Phenol(s) see L-64-R and L-72-R
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Volatile Acids see L-8~3-R
Cyanides (Organic & rnorsanic) son L-144-R &
L-145-R
Acrolein report In preparation
Hydrogen Sulphido
Carbon MonoxId* no* L.131-F
Water see L.146-R
From the various reports available, and djacusSlon
dUrjAg
visits *to, it would appear that the methods In
use at the
various laboratories are as follows-
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0
(D
0
0
0
E
3
40 b
z
0
(D
3
Cr
CD
W
W
to
668990001
Tar
Nicotine
Phenol(s)
Aldehydes
AorolaIn
H,,drogen Cianlde
Hydrogen Sulphide
Penzpyrone
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R. & D.E. Laut4vtlle Montreal Australia C*rmany
(t ) Total Particulate (I ) Total Particulate (1)
Colartmetric Foster D Snail Total Particulate
Matter Matter Mat'.er
(11) Baked weight (it) Foster D.Sn*ll (it) Poster
D.Snell Foster D Snell
Spectrophotometer Colortmeter Spectrophotometer
Spe~trophotomet*r Spe trophotometer
Colorimeter Colorimetor Same as R. & D.E. Same an
R. D F. Same an R D.E.
Colortmeter C.L.C. Same an R. & D.E. r. L.C. r
L.C.
Colorlmeter
Colortmeter Same as R. & D.E. ? Same an A. & D r
Colorimeter Colortmeter Colortmeter Sa,,.~ asR D
E.
Colortnister
(1) as Montreal (1) Radioactive spike Done by
C-rimmer
(11) G.L.C. assay
Acids (1) Titrometer
(11) G.L.C.
& Speotrophotometer
assay
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APPENDTX 11
DETERMTNATrON OF "TAR AND NTCOTTNE"
The term ttar' refers to that weight of smoke
which
survives baking In an oven at 1000C for 16 hours.
Nicotine
refers to total nicotine alkaloids an determined
by U.V.
spectroscopy.
APPARATUS
B-A.T. smoking engine.
Cambridge filter holders (21") complete with pads.
Ventilated oven.
Steam distillation apparatus (Note 1.)
UV spectrophotometer.
REAGENTS
Methanol (free of pyridine).
2 N sulphuric acid.
Sodium hydroxide/aodium chloride solution prepared
by
dissolving sodium hydroxide (300 9) and sodium
chloride
(133 S) in water and making up to one litre.
2 N hydrochloric acid.
PROCEDURE
1. Smoke five cigarettes (Note 2) through each
Cambridge filter.
2. Extract the Cambridge filter by shaking with
methanol and
filter into 100 ml volumetric flask. Wash the
Cambridge
holder with methanol and add to the flask. Make up
to
volume. This solution Is used for the
determination of both
tar and nicotine.
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Tar estimation
3. Pipette 2 x 20 ml aliquot$ Into weighed 100 ml
beakers.
4. Evaporate the methanol on a water bath.
5. Bake the residue in a ventilated oven at 100oC
for 16 hours.
6. Allow beakers to cool In a desiccator over
silica Sol.
7. Weigh the beakers and calculate the delivery of
tar per
cigarette (Note 3).
Nicotine estimation
8. Pipette 2 x 20 ml aliquots Into 100 ml beakers.
9. Add water (5 ml) and 2N sulphuria acid (10 ml)
and evaporate
the methonol on a water bath.
10. Transfer the contents of the beaker into a
boiling tube of
the steam-distillation apparatus and steam distil.
11. The distillate (100 - 120 ml) is rejected.
12. Add sodium hydroxide/sodium chloride solution
(15 ml) to the
residue in the boiling tube from the first
distillation.
Steam distil and collect the distillate (200 - 220
ml) In a
250 ml volumetric flask containing 2N hydrochlorio
acid (6 ml).
13. Make the distillate up to volume and determine
the optical
density of the solution using 1 cm calls and water
as a
reagent blank, at 2.36, 259 and 282 mg.
14. Calculate the weight of nicotine alkaloids per
cigarette,
W mg from the formula
D (D + D
W - .30-87 1 259 - 2 236 282)] 1000
whore D259' D236 and D282 are the optical
densities at
wavelengths 259, 2.36 and 282 mp respectively.
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Note I
The distillation apparatus consists of 12" boiling
tubes
carrying a B.34 ground glass joint, fitted with an
efficient
splash-head and water-condensor. The delivery tube
dips below
the surface of the acid in the receiving flank.
Note ?
In all smoke analysis, the cigarettes are
conditioned and
selected on a basis of weight and draw resistance
an detailed
below.
Cizarette ConditionInx
The cigarettes are conditioned for at least 72
hours at
70 OF and a relative humidity of 58'--
Welaht Selection
The cigarettes are selected on the basis of
average weight
.t 20 mg.
Selection for Draw Resistance
The pressure drop of a cigarette Is determined at
a flow rate
of 1050 ml per minute. The basis of draw
resistance selectior
is average pressure drop t 4--s.
Claarette Smokinx
The cigarettes are smoked to a 23 mm butt at one
puff a
minute, each puff of .35 ml volume and 2 seconds
duration.
A tar and nicotine estimation in normally based on
the
smoke from at least 4 x 5 cigarettes.
Note 3
The weight of residue In the beaker is usually
between 10 and
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20 mg and Suitable adjustment of the number of
cigarettes
smoked or the size of the aliquot taken may be
necessary
to keep within this range.
There is a small weight blank from the Cambridge
pad
which is determined using the same batch of
solvent and filters
as are used in the smcke estimation.
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