Cigarettes — Determination of total and dry particulate matter using a routine analytical cigarette-smoking machine — Glass fibre filter smoke trap method

Cigarettes — Détermination du condensat de fumée brut et anhydre au moyen d'une machine à fumer analytique de routine pour cigarettes — Méthode par piégeage sur disque en fibre de verre

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Status
Withdrawn
Publication Date
08-Apr-1987
Withdrawal Date
08-Apr-1987
Current Stage
9599 - Withdrawal of International Standard
Completion Date
17-Oct-1991
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ISO 4387:1987 - Cigarettes — Determination of total and dry particulate matter using a routine analytical cigarette-smoking machine — Glass fibre filter smoke trap method Released:4/9/1987
French language
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Standards Content (Sample)

IS0
INTERNATIONAL STANDARD 4387
First edition
1987-04-15
INTERNATIONAL ORGANIZATION FOR STANDARDIZATION
ORGANISATION INTERNATIONALE DE NORMALISATION
MEXAYHAPOAHAR OPrAHM3AL(MR il0 CTAHAAPTMSAUMM
Cigarettes - Determination of total and dry particulate
matter using a routine analytical cigarette-smoking
machine - Glass fibre filter smoke trap method
Cigarettes - Détermination du condensat de fumée brut et anhydre au moyen d'une machine à
fumer analytique de routine pour cigarertes - Méthode par piégeage sur disque en fibre de verre
Reference number
IS0 4387 : 1987 (E)

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Foreword
IS0 (tye International Organization for Standardization) is a worldwide federation of
national standards bodies (IS0 member bodies). The work of preparing International
Standards is normally carried out through IS0 technical committees. Each member
body interested in a subject for which a technical committee has been established has
the right to be represented on that committee. International organizations, govern-
mental and non-governmental, in liaison with ISO, also take part in the work.
Draft International Standards adopted by the technical committees are circulated to
the me ber bodies for approval before their acceptance as International Standards by
the IS Council. They are approved in accordance with IS0 procedures requiring at
least 7, B % approval by the member bodies voting.
IS0 4387 was prepared by Technical Committee ISO/TC 126,
International Standard
Tobacco and tobacco products.
Users should note that all International Standards undergo revision from time to time
and that any reference made herein to any other International Standard implies its
latest ecition, unless otherwise stated.
0 International Organization for Standardization, 1987 0
,
Printed in^ Switzerland
!

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IS0 4387: 1987 (E)
INTERNATIONAL STANDARD
Cigarettes - Determination of total and dry particulate
matter using a routine analytical cigarette-smoking
machine - Glass fibre filter smoke trap method
O Introduction 3 Definitions
The procedure specified in this International Standard is ap-
For the purposes of this International Standard, the following
plicable to all types of cigarettes; however, the results obtained
definitions apply.
of certain types of cigarettes may not be
from machine smoking
suitable for ranking or consumer information and may reveal
(I)
the need for further and more adequate information to be made
3.1 total particulate matter; crude smoke condensate :
available.
That portion of the mainstream smoke which is trapped in the
smoke trap, expressed as milligrams per cigarette (mg/cig.).
ISO/TC 126 is studying this problem and will try to find a solu-
tion which will be taken into account in a future revision of this
International Standard.
3.2 dry particulate matter; dry smoke condensate : The
total particulate matter after deduction of its water content,
1 Scope and field of application expressed as milligrams per cigarette (mg/cig.).
This International Standard specifies a method for determining
the total and dry particulate matter present in the smoke from
3.3 nicotine-free dry particulate matter; nicotine-free
cigarettes generated and collected using a routine analytical
dry smoke condensate : The dry particulate matter after
cigarette-smoking machine equipped with glass fibre filter
deduction of its nicotine alkaloids content, expressed as
smoke traps.
milligrams per cigarette (mg/cig.).
2 References
3.4 clearing puff : Any puff taken after a cigarette has been
extinguished.
IS0 760, Determination of water - Karl Fischer method
(General method).
3.5 smoking process : The use of a smoking machine to
IS0 2971, Tobacco and tobacco products - Cigarettes and
smoke one cigarette per port from lighting to final puff.
filters - Determination of nominal diameter.
IS0 3308, Cigarettes - Routine analytical cigarette-smoking
machine - Definitions and standard conditions. 3.6 smoking run : A combination of smoking processes to
produce such smoke from a sample of cigarettes as is
IS0 3400, Tobacco and tobacco products - Determination of
necessary for the determination of the smoke components.
alkaloids in cigarette smoke condensates - Spectro-
photometric method.
3.7 laboratory sample: The cigarettes Sent to the
IS0 3402, Tobacco and tobacco products - Atmospheres for
laboratory for testing.
conditioning and testing.
IS06488, Tobacco - Determination of water content
3.8 test sample; conditioning sample : The cigarettes
(Reference method).
selected from the laboratory sample for conditioning prior to
tests for particulate matter yield.
IS0 6565, Tobacco and tobacco products - Draw resistance
of cigarettes and filer rods - Definitions, standard conditions
and general aspects.
3.9 test portion : The conditioned cigarettes smoked for
particulate matter yield tests.
IS0 8243, Cigarettes - Sampling. 1)
~~
1) At present at the stage of draft.
1

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IS0 4387: 1987 (E)
set of calipers, one leg of which is in the horizontal plane while
4 Ptinciple
the other is adjustable so as to be parallel to the cigarettes in-
Smoking of the test cigarettes in an automatic smoking
serted in the cigarette holders on the smoking machine. By us-
machihe and collection of the mainstream smoke by a glass
ing a protractor, it will be possible to ensure that the cigarette
fibre filter smoke trap. Gravimetric determination of the mass of position with respect to the horizontal plane is in agreement
total particulate matter SO collected. Extraction of the total par-
with the standard conditions.
ticulate matter from the trap and determination of the water
content by Karl Fischer or gas chromatographic methods.
Length-measuring device, suitable for measuring to
5.10
the nearest 0.5 mm.
5 Apparatus
5.11 Apparatus for the determination of diameter.
Normal laboratory apparatus and in particular the following
items : ,
6 Sampling
5.1 Routine analytical cigarette-smoking machine,
complying with the requirements of IS0 3308.
A laboratory sample, representative of the cigarette type to be
sampled, shall be provided by a sampling scheme such as one
Soap bubble flow meter, range O to 50 ml, graduated
5.2
of those in IS0 8243. This sample will normally contain cigar-
in 0,l ml divisions.
ettes taken from different parts of the population.
5.3 hpparatus for the determination of puff duration
For any particular test, for example determination of total par-
and frèquency.
ticulate matter, it should then be possible to make up the test
sample required for the test by randomly selecting cigarettes
from the different parts of the population represented in the
5.4 Analytical balance.
laboratory sample.
5.5 Pressure drop testing equipment.
7 Determination of total particulate matter
5.6 Conditioning enclosure, maintained accurately in
accordance with the conditions specified in IS0 3402.
In 7.1 and 7.6 below, the following symbols are used :
dquipment for the determination of water content.
5.7
, N is the number of cigarettes of a given type to be smoked;
This ca'n be either Karl Fischer equipment in accordance with
C is a multiplying factor, value greater than 1, to allow for loss
IS0 760 or a suitable gas chromatograph (see 8.1 or 8.2).
due to damage or selection procedures between initial sampling
and smoking;
Glass fibre filter smoke trap, comprising :
5.8
n is the number of replicate determinations of total particulate
- Filter holders made of an airtight non-hygroscopic
matter;
and chemically inert material, preferably transparent, able to
con ain a filter disc of glass fibre material 1 to 2 mm thick
q is the number of cigarettes smoked into the same trap;
and with a diameter of at least 44 mm. The rough filter sur-
1
face) shall face the oncoming smoke.
P is the total number of packets of cigarettes available;
- Filter material which shall retain at least 99,9 % of all
particles having a diameter equal to or greater than 0,3 pm Q is the total number of cigarettes available (test sample).
of a dioctyl phthalate aerosol at a linear air velocity of
140 mm/s. The pressure drop of the filter assembly shall not
7.1 Preparation of the cigarettes for smoking
exceed 900 Pa (9 mbar) at this air velocity. The content of
polyiicrylate binder shall not exceed 5 % (rn/rn).
If N cigarettes of a given type are to be smoked, C x N
cigarettes should be prepared from Q for conditioning and butt
The filt r assembly shall be capable of quantitatively retaining
marking. The multiplier Cis usually at least 1,2 to provide extra
all the ainstream smoke produced by the cigarette without:
cigarettes in case some are damaged. If selection by mass or
loss of a articulate matter. In addition, the filter assembly shall
draw resistance (or any other parameter) is necessary, C will
be chosen SO that the increase in pressure drop of the assembly
have to be much larger (experience suggests 2,O to 4,0), de-
does not exceed 250 Pa (2,5 mbar), at a flow rate of 17,5 ml/s
pending on the selection process.
when measured after the smoking run.
The precision normally required generally demands that
Apparatus for measuring the angular position of the
5.9 80 4 N < 100. This number may be substantially
augmented if the variability of the sample is high; on the
cigarettes.
contrary, in certain comparisons made of homogeneous
samples, this number may be reduced. As a precaution it is rec-
This insirument shall rest on a horizontal plane of the smoking
machind at the level of the smoking ports. It shall consist of a ommended that N should never be less than 40.
2

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IS0 43W: 1987 (E)
It is recommended that the testing atmosphere in the
The N cigarettes to be smoked will be tested in n = N/q deter-
minations if q cigarettes are smoked into one trap. As far as laboratory where the smoking is to be carried out is as close as
possible to the conditioning atmosphere. If the testing
possible these n determinations should correspond to different
atmosphere is different, place the conditioned test sample in
test portions of the test sample. Selection of each test portion
an airtight container (just large enough to contain the portion)
will depend upon the form of the test sample.
it from the container until just before the
and do not remove
smoking.
7.1.1 Selection of test portions from a bulk of Q
cigarettes
7.5 Preliminary tests for physical parameters
If the test sample is in the form of a single bulk, consisting of Q
cigarettes, C x N cigarettes should be selected at random so
that every cigarette has an equal probability of being chosen. The following data which may be required in the test repoi
should be determined :
7.1.2 Selection of test portions from P packets
7.5.1 Total length of the cigarette.
If the test sample consists of P packets, the selection pro-
cedure depends upon the number of cigarettes in each packet
7.5.2 Nominal diameter determined according to IS0 2971.
(QlP) compared with q.
If QIP > C x q, select a test portion by choosing a single
7.5.3 Length of filter and tipping paper.
0
packet at random, then randomly choose C x q cigarettes
from that packet.
7.5.4 Draw resistance of the cigarette determined according
If QIP < C x q, select the smallest number of packets (k) to IS0 6565.
such that
7.6 Smoking and collection of particulate matter
QXk
>cxq
P
7.6.1 Smoking plan
and randomly choose an equal (or as near equal as possible)
number of cigarettes from each packet to form the test portion
A smoking plan shall be chosen; examples are given in the
of C x q cigarettes.
annex to this International Standard.
7.1.3 Duplicate test portions
The plan shall show the number of cigarettes to be smoked into
each trap (q) and the number in the test sample for condition-
Provided that the test sample is sufficiently large
ing (C x N).
( > 2 C x N), it would be prudent to reserve a duplicate set of
n test portions. In this event the parallel selection of a test por-
tion and its duplicate would seem sensible. In this case the two 7.6.2 Preparation of glass fibre filter discs
selection conditions of 7.1.2 would need to be changed to
QIP > 2 C x q and QIP < 2 C x q. For all operations the operator shall prevent contamination
from the fingers by wearing gloves of a suitable material.
7.2 Butt marking
Insert the filter discs into their holders and assemble the
holders. If the filter disc material has a rough and a smooth
The butt length should be marked on the cigarettes in accord-
side, place the rough side facing the cigarettes. After assembly,
ance with 4.9 of IS0 3308 before conditioning.
examine the filter holders to ensure that the discs have been
properly fitted and then expose them to the air in the laboratory
Care should be taken to avoid damaging the cigarettes during
for at least 12 h. Weigh the assembled filter holders to the
butt marking. Any cigarettes accidentally torn or punctured
nearest 0,l mg.
during marking, or any found during marking to be defective,
shall be discarded.
7.6.3 Setting up the smoking machine
7.3 Selection of cigarettes
If necessary replace any protective filters on the machine.
If a selection by mass or draw resistance (or any other
Switch on and allow to warm up on automatic cycling for at
parameter) is necessary because of the nature of the problem
least 20 min.
being studied, the selection is not to be considered as a method
of reducing the number of cigarettes to be smoked.
If draught screens are needed to achieve the standard ambient
conditions (see 5.4 of IS0 3308) set them in place.
7.4 Conditioning
With the machine warmed up, check that the puff duration and
Condition all the test portions in conditioning atmosphere A of puff frequency on each channel are in accordance with the
IS0 3402 for a minimum of 48 h and for a maximum of 1 week. standard conditions.
3

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IS0 4387: 1987 (E)
7.6.3.1 Measurement of puff duration Adjust the position of each cigarette SO that when the burning
coal reaches the butt mark, the puff termination device is
A timir working with reference to a crystal-controlled oscillator activated. If the burning through of cotton threads (30 to 40
shall E,e used to measure the period of time which elapses be- denier) is used to terminate smoking at the butt mark, the cot-
tween the triggering operations which begin and end a puffing ton shall just touch the cigarettes at the butt mark, without
action of the smoking machine. The accuracy of the timing modifying the cigarette positioning.
device shall be such as to ensure that a 1 % error in the puff
Zero the puff counters and light each cigarette at the beginning
duration can be detected. The timer should be coupled directly
of its first puff. When each butt mark has been reached,
to the triggering circuits.
remove the burning coal from the cigarette, and note the final
reading of the puff counters. Take at least one clearing puff im-
NOTE L It is not possible to specify the method of measurement
beyondl a statement of principle because of the variety of types of mediately the smoking process is complete and remove the
suitable( timers and smoking machines available.
cigarette butt.
NOTE - Avoid disturbance of the smoking by artificial removal of ash.
7.6.3.2 Checking of puff frequency
New cigarettes shall be inserted immediately and the smoking
Measure the period of time which elapses between the trigger-
process repeated until the predetermined number of cigarettes,
ing operations which begin successive puffing actions of the
according to the smoking plan, has been smoked into the
smoking machine. This will determine the puff frequency. The
smoke trap. Begin the determination of total particulate matter
timer used shall be suitable for measuring to the nearest 0,l s.
as described in 7.7 immediately.
It should be coupled directly to the triggering circuits.
7.7 Determination of total particulate matter
7.6.3.31 Measurement of puff volume
Remove the smoke traps from the smoking machine. Where
Fit the prepared smoking trap or traps and cigarette holders
necessary, remove the cigarette holder from the smoke trap. It
onto the machine.
is recommended, particularly when plain cigarettes have been
smoked, that this latter operation be conducted with the smoke
For each channel attach a resistance equal
...

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