SIST ISO 4387:2000
(Main)Cigarettes -- Determination of total and nicotine-free dry particulate matter using a routine analytical smoking machine
Cigarettes -- Determination of total and nicotine-free dry particulate matter using a routine analytical smoking machine
Cigarettes -- Détermination de la matière particulaire totale et de la matière particulaire anhydre et exempte de nicotine au moyen d'une machine à fumer analytique de routine
La présente Norme internationale spécifie des méthodes de détermination de la matière particulaire totale et de détermination ultérieure de la matière particulaire anhydre et exempte de nicotine, présente dans la fumée de cigarette, produite et recueillie au moyen d'une machine à fumer analytique de routine.
Cigarete - Določevanje celotne in nikotina proste suhe snovi z uporabo rutinsko analiznega cigaretnega dimnega stroja
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INTERNATIONAL ISO
STANDARD 4387
Third edition
2000-04-01
Cigarettes — Determination of total and
nicotine-free dry particulate matter using a
routine analytical smoking machine
Cigarettes — Détermination de la matière particulaire totale et de la
matière particulaire anhydre et exempte de nicotine au moyen d'une
machine à fumer analytique de routine
Reference number
ISO 4387:2000(E)
©
ISO 2000
---------------------- Page: 1 ----------------------
ISO 4387:2000(E)
PDF disclaimer
This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but shall not
be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In downloading this
file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat accepts no liability in this
area.
Adobe is a trademark of Adobe Systems Incorporated.
Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation parameters
were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In the unlikely event
that a problem relating to it is found, please inform the Central Secretariat at the address given below.
© ISO 2000
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic
or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISO's member body
in the country of the requester.
ISO copyright office
Case postale 56 � CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 734 10 79
E-mail copyright@iso.ch
Web www.iso.ch
Printed in Switzerland
ii © ISO 2000 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 4387:2000(E)
Contents Page
Foreword.iv
Introduction.v
1 Scope .1
2 Normative references .1
3 Terms, definitions and abbreviated terms .1
4 Principle.2
5 Apparatus .3
6 Sampling.3
7 Determination of total particulate matter .3
7.1 Preparation of the cigarettes for smoking .3
7.2 Marking the butt length.5
7.3 Selection of cigarettes .5
7.4 Conditioning.5
7.5 Preliminary tests before smoking.6
7.6 Smoking and collection of particulate matter.6
7.7 Determination of total particulate matter .8
7.8 Calculation of total particulate matter .8
7.9 Treatment of total particulate matter .8
8 Test report .9
9 Repeatability and reproducibility.11
Annex A (informative) Smoking plans.12
Bibliography.17
© ISO 2000 – All rights reserved iii
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ISO 4387:2000(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO
member bodies). The work of preparing International Standards is normally carried out through ISO 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, governmental and non-governmental, in
liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical
Commission (IEC) on all matters of electrotechnical standardization.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3.
Draft International Standards adopted by the technical committees are circulated to the member bodies for voting.
Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this International Standard may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights.
International Standard ISO 4387 was prepared by Technical Committee ISO/TC 126, Tobacco and tobacco
products.
This third edition cancels and replaces the second edition (ISO 4387:1991), which has been editorially revised.
Annex A of this International Standard is for information only.
iv © ISO 2000 – All rights reserved
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ISO 4387:2000(E)
Introduction
Cigarettes are manufactured to close tolerances using strict quality control procedures. However, all the
constituents involved in the manufacture are derived from natural products (tobacco, cigarette paper, tipping, etc.)
and this results in a final product which is intrinsically variable. The complexity does not finish here because the
cigarette is converted during smoking to cigarette smoke.
Cigarette smoke is a complex mixture consisting of many individual chemical constituents. These compounds exist
as gases, vapours and condensed aerosol particles. Additionally, various ageing processes, together with
diffusional and intersolubility effects, start occurring immediately after the formation of the smoke which further
complicate its composition.
The quantitative measurement of nicotine-free dry particulate matter (NFDPM, sometime referred to as "tar") is,
therefore, dependent on its arbitrary definition.
From the time that scientists have attempted to determine a value for NFDPM, many different methods have been
used. However, experience has shown some procedures to be more reliable and, with these factors in mind, during
1988 and 1989, collaborative studies by Task Forces composed of members of the Cooperation Centre for
Scientific Research Relative to Tobacco (CORESTA) Smoke and Technology groups have been made on the
repeatability and reproducibility of the determination of total and dry particulate matter from cigarettes.
The studies show that improvements in repeatability and reproducibility result when some restrictions are placed on
the wide variety of methods and practices permitted by existing standard methods. Thus, this International
Standard, and the others which together form a complete set for the sampling, conditioning and determination of
nicotine, water and particulate matter from cigarettes, have been produced after much cooperation and
collaborative experimentation by many laboratories in many countries.
CORESTA first published an International Standard for the machine smoking of cigarettes in 1968, and since that
time many improvements in equipment as well as in procedure have been suggested.
This International Standard incorporates these improvements and consequently represents the state of the art on
this subject and provides one set of procedures accepted as reference methods.
This method is a machine method and allows cigarettes to be smoked using a strictly controlled set of parameters.
Thus, it enables the NFDPM and nicotine from cigarettes, when smoked by this procedure, to be compared and
ranked on the basis of machine yield.
© ISO 2000 – All rights reserved v
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INTERNATIONAL STANDARD ISO 4387:2000(E)
Cigarettes — Determination of total and nicotine-free dry
particulate matter using a routine analytical smoking machine
1 Scope
This International Standard specifies methods for the determination of total particulate matter and for the
subsequent determination of nicotine-free dry particulate matter present in the smoke from cigarettes generated
and collected using a routine analytical smoking machine.
2 Normative references
The following normative documents contain provisions which, through reference in this text, constitute provisions of
this International Standard. For dated references, subsequent amendments to, or revisions of, any of these
publications do not apply. However, parties to agreements based on this International Standard are encouraged to
investigate the possibility of applying the most recent editions of the normative documents indicated below. For
undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC
maintain registers of currently valid International Standards.
ISO 2971, Cigarettes and filter rods — Determination of nominal diameter —Method using a laser beam measuring
apparatus.
ISO 3308:2000, Routine analytical cigarette-smoking machine — Definitions and standard conditions.
ISO 3402, Tobacco and tobacco products — Atmosphere for conditioning and testing.
ISO 6488-1, Tobacco — Determination of water content — Part 1: Karl Fischer method.
ISO 6565, Tobacco and tobacco products — Draw resistance of cigarettes and pressure drop of filter rods —
Standard conditions and measurement.
ISO 8243, Cigarettes — Sampling.
ISO 10315, Cigarettes — Determination of nicotine in smoke condensates — Gas-chromatographic method.
ISO 10362-1, Cigarettes — Determination of water in smoke condensates — Part 1: Gas-chromatographic method.
ISO 16055, Tobacco and tobacco products — Monitor test piece — Requirements and application.
3 Terms, definitions and abbreviated terms
For the purposes of this International Standard, the following terms, definitions and abbreviated terms apply.
3.1
total particulate matter
crude smoke condensate
TPM
that portion of the mainstream smoke which is trapped in the smoke trap, expressed as milligrams per cigarette
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ISO 4387:2000(E)
3.2
dry particulate matter
dry smoke condensate
DPM
total particulate matter after deduction of its water content, expressed as milligrams per cigarette
3.3
nicotine-free dry particulate matter
nicotine-free dry smoke condensate
NFDPM
dry particulate matter after deduction of its nicotine content, expressed as milligrams per cigarette
3.4
smoking process
use of a smoking machine to smoke cigarettes from lighting to final puff
3.5
smoking run
specific smoking process to produce such smoke from a sample of cigarettes as is necessary for the determination
of the smoke components
3.6
laboratory sample
sample intended for laboratory inspection or testing and which is representative of the gross sample or the sub-
period sample
3.7
test sample
cigarettes for test taken at random from the laboratory sample and which are representative of each of the
increments making up the laboratory sample
3.8
conditioning sample
cigarettes selected from the test sample for conditioning prior to tests
3.9
test portion
group of cigarettes prepared for a single determination and which is a random sample from the test sample or
conditioned sample, as appropriate
3.10
monitor test piece
cigarette taken from a batch specially fabricated under controlled manufacturing conditions
NOTE The cigarettes of such a batch show the greatest possible homogeneity with regard to their physical and chemical
characteristics.
4Principle
The test cigarettes are sampled then conditioned. The test cigarettes are smoked on an automatic smoking
machine with simultaneous collection of total particulate matter in a glass fibre filter trap. If used, the consistency of
the laboratory smoking process and subsequent analytical procedures are controlled by using monitor test pieces
specified in ISO 16055. The mass of the total particulate matter so collected is determined gravimetrically. The total
particulate matter is extracted from the trap for determination of the water and nicotine contents by gas
chromatography.
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ISO 4387:2000(E)
NOTE In the countries that are not in a position to use gas-chromatographic methods, reference should be made to
ISO 3400 for the determination of total nicotine alkaloids, and the determination of water in smoke condensate should be
performed by the method described in ISO 10362-2. In such cases, values obtained for nicotine and water in smoke condensate
may be used with the addition of a note made in the expression of the result.
5 Apparatus
Normal laboratory apparatus and, in particular, the following items.
5.1 Routine analytical cigarette-smoking machine, complying with the requirements of ISO 3308.
5.2 Soap bubble flow meter, graduated at 35 ml to an accuracy of � 0,2 ml and with a resolution of 0,1 ml.
5.3 Apparatus for the determination of puff duration and frequency.
5.4 Analytical balance, suitable for measuring to the nearest 0,1 mg.
The weighing of filter pad holders may be affected by static electricity, necessitating the use of an antistatic device.
5.5 Conditioning enclosure, carefully maintained under the conditions specified in ISO 3402.
5.6 Length-measuring device, suitable for measuring to the nearest 0,5 mm.
5.7 Device for the determination of diameter, in accordance with ISO 2971.
If such apparatus is not available, the diameter may be determined from the circumference by slitting the cigarette
longitudinally, removing and flattening the paper then measuring its width.
5.8 Smoke trap sealing device, end caps made from a non-hygroscopic and chemically inert material.
5.9 Gloves, made of cotton, or the non-talc surgical type.
6 Sampling
A laboratory sample (3.6) shall be taken by a sampling scheme such as one of those given in ISO 8243.
This sample will normally contain cigarettes taken from different parts of the population. Make up the test sample
(3.7) required for the test by randomly selecting cigarettes from the different parts of the population represented in
the laboratory sample.
7 Determination of total particulate matter
7.1 Preparation of the cigarettes for smoking
7.1.1 General
If N cigarettes of a given type are to be smoked, C� N cigarettes shall be prepared from Q cigarettes for
conditioning and butt marking.
The symbols used in this clause are as follows:
N is the number of cigarettes of a given type to be smoked, resulting from sampling at one point in time or
from a sub-period sample;
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ISO 4387:2000(E)
C is a multiplying factor, of value greater than 1, to allow for loss due to damage or selection procedures
between initial sampling and smoking;
Q is the total number of cigarettes available (laboratory sample, see 3.6);
n is the number of replicate determinations of total particulate matter;
q is the number of cigarettes smoked into the same trap;
P is the total number of packets of cigarettes available.
NOTE The multiplier C is usually at least 1,2 to provide extra cigarettes in case some are damaged and for optional tests
which may be required (see 7.5). If selection by mass or draw resistance (or any other parameter) is necessary, C will have to
be much larger (experience suggests 2 to 4) depending on the selection process.
The precision normally required generally demands that 80uu 100. This number may be considerably
augmented if the variability of the sample is high; on the contrary, in certain comparisons made of homogeneous
samples, this number may be reduced. It can also be reduced when N represents a sub-period sample. N shall
never be less than 40 when 20 cigarettes are smoked per trap, or less than 20 when 5 cigarettes are smoked per
trap.
It is necessary for 40 cigarettes to be smoked when 20 cigarettes are smoked per trap, thus providing a replicate
analysis and data replication.
The N cigarettes to be smoked will be tested in n = N/q determinations if q cigarettes are smoked into one trap. As far
as possible these n determinations should correspond to different test portions of the test sample. Selection of each
test portion will depend upon the form of the test sample.
7.1.2 Selection of test portions from a bulk of Q cigarettes
If the test sample is in the form of a single bulk, consisting of Q cigarettes, C� N cigarettes shall be selected at
random so that every cigarette has an equal probability of being selected.
7.1.3 Selection of test portions from P packets
If the test sample consists of P packets, the selection procedure depends upon the number of cigarettes in each
packet (Q/P) compared with q.
If Q/PW C� q, select a test portion by choosing a single packet at random, then randomly select C � q cigarettes
from that packet.
If Q/P � C� q, select the smallest number of packets (k) such that
Qk�
WCq�
P
and randomly choose an equal (or as near equal as possible) number of cigarettes from each packet to form the
test portion of C� q cigarettes.
7.1.4 Duplicate test portions
Provided that the test sample is sufficiently large (W 2C� N), a duplicate set of n test portions should be reserved.
In this event the parallel selection of a test portion and its duplicate would seem sensible. In this case the two
selection conditions of 7.1.3 would need to be changed to Q/PW 2C� q and Q/P� 2C� q.
4 © ISO 2000 – All rights reserved
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ISO 4387:2000(E)
7.2 Marking the butt length
7.2.1 Standard butt length
The standard butt length to which cigarettes shall be marked shall be the greatest of the following three lengths:
� 23 mm,
� length of filter� 8mm, or
� length of overwrap� 3 mm,
where the overwrap is defined as any wrapper applied to the mouth end of the cigarette, and the length of the filter
is defined as the total length of the cigarette minus the length of the tobacco portion.
NOTE Butt length is defined in ISO 3308 as the length of unburnt cigarette remaining at the moment when smoking is
stopped.
7.2.2 Measurement of length of filter
The length of filter as defined in 7.2.1 shall be the mean value of 10 cigarettes taken from the laboratory sample,
measured to an accuracy of 0,5 mm. Express the mean to the nearest 0,5 mm.
NOTE In some instances it may be necessary to measure more than 10 cigarettes, but when the variation in filter length
can be demonstrated to be well controlled, a smaller number of measurements may be sufficient.
7.2.3 Measurement of length of overwrap
The length of overwrap as defined in 7.2.1 shall be the mean value of 10 overwraps taken from the laboratory
sample, measured to an accuracy of 0,5 mm. Express the mean to the nearest 0,5 mm.
NOTE In some instances it may be necessary to measure more than 10 cigarettes, but when the variation in overwrap
length can be demonstrated to be well controlled, a smaller number of measurements may be sufficient.
7.2.4 Butt length to be marked on the cigarettes before conditioning
Draw a line, using a fine soft-tipped marker, at the standard butt length, to an accuracy of 0,5 mm, from the mouth
end for the particular cigarette type.
Care should be taken to avoid damaging the cigarettes during butt marking. Any cigarettes accidentally torn or
punctured during marking, or any found during marking to be defective, shall be discarded and replaced with spare
cigarettes from the test portion.
If cigarettes are to be smoked on a smoking machine on which the butt length in accordance to 7.2.1 can be pre-
set, it is not necessary to mark the butt lengths on the cigarettes themselves.
7.3 Selection of cigarettes
If a selection by mass or draw resistance (or any other parameter) is necessary because of the nature of the
problem being studied, the selection shall not be considered as a method of reducing the number of cigarettes to
be smoked.
7.4 Conditioning
Condition all the test portions in the conditioning atmosphere specified in ISO 3402 for a minimum of 48 h and a
maximum of 10 days.
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ISO 4387:2000(E)
If for any reason test samples are to be kept for longer than 10 days before conditioning, store them in original
packaging or in airtight containers just large enough to contain the sample.
The testing atmosphere in the laboratory where the smoking is to be carried out shall also be in accordance with
ISO 3402.
Transfer the test portions to the smoking location in airtight containers (just large enough to contain the portions)
unless the smoking location and the conditioning location are adjoining and have identical atmospheres.
7.5 Preliminary tests before smoking
The following data may be required in the test report:
a) total length of the cigarette;
b) nominal diameter, determined in accordance with ISO 2971;
c) draw resistance of the cigarette, determined in accordance with ISO 6565;
d) average mass of the conditioned cigarettes selected for the smoking operation (in milligrams per cigarette);
e) water content (as a mass fraction) of the conditioned cigarettes, determined in accordance with ISO 6488-1.
7.6 Smoking and collection of particulate matter
7.6.1 Smoking plan
Choose a smoking plan; examples of plans are given in informative annex A.
The plan shall show the number of cigarettes to be smoked into each trap (q) and the number in the conditioning
sample (C� N).
The plan should include the use of a test portion of monitor test pieces. The test pieces are included in the plan as
if they were a type of cigarette and prepared and smoked as in 7.6.4, 7.7, 7.8 and 7.9.
7.6.2 Preparation of smoke traps and cigarette holders
For all operations, the operator shall prevent contamination from the fingers by wearing gloves of a suitable
material (5.9).
Insert filter discs which have been conditioned in the test atmosphere for at least 12 h into their holders, and
assemble, placing the rough side of the filter disc so that it will face the oncoming smoke. After assembly, examine
the filter holders to ensure that the discs have been properly fitted. If the smoke trap is designed to contain the
perforated disc (washer), insert it and fit the sealing devices (end caps). If the cigarette holder is designed to
contain a perforated disc, insert it into the cigarette holder before attaching the labyrinth seals (see ISO 3308:2000,
4.8). Weigh the assembled smoke traps to the nearest 0,1 mg.
Because of absorption of water by smoke traps and solvent, it is necessary to determine a value for the sample
blank. Prepare sample blanks by treating additional smoke traps (at least 2 per 100 cigarettes) in the same manner
as that used for smoke collection.
7.6.3 Setting up the smoking machine
7.6.3.1 General
If necessary, replace any protective filters on the machine. Switch on the machine and allow it to warm up on
automatic cycling for at least 20 min.
6 © ISO 2000 – All rights reserved
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ISO 4387:2000(E)
With the machine warmed up, check that the puff duration and puff frequency on each channel are in accordance
with the standard conditions.
The puff volume should be checked if it is suspected that the smoking machine is subject to a large change in
temperature during use.
7.6.3.2 Measurement of puff duration
A timer, working with reference to a crystal-controlled oscillator, shall be used to measure the period of time which
elapses between the triggering operations which begin and end a puffing action of the smoking machine. The
accuracy of the timing device shall be such as to ensure that a 1 % error in the puff duration can be detected. The
timer should be coupled directly to the triggering circuits.
NOTE It is not possible to specify the method of measurement beyond a statement of principle because of the variety of
types of suitable timers and smoking machines available.
7.6.3.3 Checking of puff frequency
Measure the period of time which elapses between the triggering operations which begin successive puffing actions
of the smoking machine, thus determining the puff frequency. The timer used shall be suitable for measuring to the
nearest 0,1 s and should, preferably, be coupled directly to the triggering circuits.
7.6.3.4 Measurement of puff volume
The displacement of the bubble in a soap bubble flow meter (5.2) gives a direct measurement of puff volume and
also provides a check for leaks in the system. A suitable indicator graduated at 35 ml shall have a resolution of
0,1 ml. It shall be connected through a standard pressure drop device of 1 kPa� 5 % to the cigarette holder of the
smoking machine channel under test. Before use for a series of measurements, wet the instrument twice with
detergent solution and then allow it to drain for a period of between 30 s and 45 s.
The bubble flow meter shall contain a mass fraction of 15 % aqueous solution of a surface active agent.
1)
Teepol L ® has been found to be satisfactory. The concentration of Teepol as purchased must be known before
carrying out further dilution.
Fit the prepared smoking trap or traps and cigarette holders onto the machine. Attach a plastic insert of an
appropriate size for the labyrinth seals in the cigarette holder to the resistance in the tube from the soap bubble
flow meter indicator. Prepare the soap bubble flow meter by wetting the inside of the tube with the detergent
solution to above the top graduation mark. Connect the indicator to the cigarette holder in port 1 and determine the
puff volume; adjust if necessary to (35,0� 0,3) ml. Repeat for all remaining ports in turn.
Repeat the determinations until the necessary precision of measurement is obtained. If the number of replicates
exceeds three, continue until the correct precision is obtained but replace the pad before smoking, reweigh the
smoke trap and recheck the puff volume with the new pad in place. Measure the temperature and relative humidity
of the air surrounding the smoking machine and note the atmospheric pressure.
7.6.4 Procedure for smoking run
Insert the conditioned cigarettes from the test portion into the cigarette holders so that the butt end impinges upon
the perforated disc (washer) fitted within the filter trap. Avoid any leaks or deformations. Any cigarettes found to
have obvious defects, or which have been damaged during insertion, shall be discarded and replaced with spare,
conditioned cigarettes.
1)
Teepol L is the trade name of a product supplied by Shell. This information is given for the convenience of users of this
International Standard and does not constitute an endorsement by ISO of this product. Equivalent products may be used if they
canbeshowntoleadtothesameresults.
© ISO 2000 – All rights reserved 7
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ISO 4387:2000(E)
Ensure that the cigarettes are positioned correctly so that the axes of the cigarettes coincide with the axes of the
ports. Adjust the position of each cigarette so that when the burning coal reaches the butt mark, the puff termination
device is activated. If the burning through of 100 % cotton thread of (48� 4) tex is used to terminate smoking at the
butt mark, the cotton shall just touch the cigarette at the butt mark, without modifying the cigarette positioning.
Zero the puff counters and light each cigarette at the beginning of its first puff. Should it be necessary to relight a
cigarette, a hand-held electrical lighter may be used. When each butt mark has been reached, remove the burning
coal from the cigarette and note the final reading of the puff counters. After the smoking process is complete, leave
the cigarette butt in place for at least 30 s to enable deposition of any residual smoke in the trap.
Avoid disturbanc
...
SLOVENSKI STANDARD
SIST ISO 4387:2000
01-september-2000
&LJDUHWH'RORþHYDQMHFHORWQHLQQLNRWLQDSURVWHVXKHVQRYL]XSRUDERUXWLQVNR
DQDOL]QHJDFLJDUHWQHJDGLPQHJDVWURMD
Cigarettes -- Determination of total and nicotine-free dry particulate matter using a
routine analytical smoking machine
Cigarettes -- Détermination de la matière particulaire totale et de la matière particulaire
anhydre et exempte de nicotine au moyen d'une machine à fumer analytique de routine
Ta slovenski standard je istoveten z: ISO 4387:2000
ICS:
65.160 7REDNWREDþQLL]GHONLLQ Tobacco, tobacco products
RSUHPD and related equipment
SIST ISO 4387:2000 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST ISO 4387:2000
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SIST ISO 4387:2000
INTERNATIONAL ISO
STANDARD 4387
Third edition
2000-04-01
Cigarettes — Determination of total and
nicotine-free dry particulate matter using a
routine analytical smoking machine
Cigarettes — Détermination de la matière particulaire totale et de la
matière particulaire anhydre et exempte de nicotine au moyen d'une
machine à fumer analytique de routine
Reference number
ISO 4387:2000(E)
©
ISO 2000
---------------------- Page: 3 ----------------------
SIST ISO 4387:2000
ISO 4387:2000(E)
PDF disclaimer
This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but shall not
be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In downloading this
file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat accepts no liability in this
area.
Adobe is a trademark of Adobe Systems Incorporated.
Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation parameters
were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In the unlikely event
that a problem relating to it is found, please inform the Central Secretariat at the address given below.
© ISO 2000
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic
or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISO's member body
in the country of the requester.
ISO copyright office
Case postale 56 � CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 734 10 79
E-mail copyright@iso.ch
Web www.iso.ch
Printed in Switzerland
ii © ISO 2000 – All rights reserved
---------------------- Page: 4 ----------------------
SIST ISO 4387:2000
ISO 4387:2000(E)
Contents Page
Foreword.iv
Introduction.v
1 Scope .1
2 Normative references .1
3 Terms, definitions and abbreviated terms .1
4 Principle.2
5 Apparatus .3
6 Sampling.3
7 Determination of total particulate matter .3
7.1 Preparation of the cigarettes for smoking .3
7.2 Marking the butt length.5
7.3 Selection of cigarettes .5
7.4 Conditioning.5
7.5 Preliminary tests before smoking.6
7.6 Smoking and collection of particulate matter.6
7.7 Determination of total particulate matter .8
7.8 Calculation of total particulate matter .8
7.9 Treatment of total particulate matter .8
8 Test report .9
9 Repeatability and reproducibility.11
Annex A (informative) Smoking plans.12
Bibliography.17
© ISO 2000 – All rights reserved iii
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SIST ISO 4387:2000
ISO 4387:2000(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO
member bodies). The work of preparing International Standards is normally carried out through ISO 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, governmental and non-governmental, in
liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical
Commission (IEC) on all matters of electrotechnical standardization.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3.
Draft International Standards adopted by the technical committees are circulated to the member bodies for voting.
Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this International Standard may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights.
International Standard ISO 4387 was prepared by Technical Committee ISO/TC 126, Tobacco and tobacco
products.
This third edition cancels and replaces the second edition (ISO 4387:1991), which has been editorially revised.
Annex A of this International Standard is for information only.
iv © ISO 2000 – All rights reserved
---------------------- Page: 6 ----------------------
SIST ISO 4387:2000
ISO 4387:2000(E)
Introduction
Cigarettes are manufactured to close tolerances using strict quality control procedures. However, all the
constituents involved in the manufacture are derived from natural products (tobacco, cigarette paper, tipping, etc.)
and this results in a final product which is intrinsically variable. The complexity does not finish here because the
cigarette is converted during smoking to cigarette smoke.
Cigarette smoke is a complex mixture consisting of many individual chemical constituents. These compounds exist
as gases, vapours and condensed aerosol particles. Additionally, various ageing processes, together with
diffusional and intersolubility effects, start occurring immediately after the formation of the smoke which further
complicate its composition.
The quantitative measurement of nicotine-free dry particulate matter (NFDPM, sometime referred to as "tar") is,
therefore, dependent on its arbitrary definition.
From the time that scientists have attempted to determine a value for NFDPM, many different methods have been
used. However, experience has shown some procedures to be more reliable and, with these factors in mind, during
1988 and 1989, collaborative studies by Task Forces composed of members of the Cooperation Centre for
Scientific Research Relative to Tobacco (CORESTA) Smoke and Technology groups have been made on the
repeatability and reproducibility of the determination of total and dry particulate matter from cigarettes.
The studies show that improvements in repeatability and reproducibility result when some restrictions are placed on
the wide variety of methods and practices permitted by existing standard methods. Thus, this International
Standard, and the others which together form a complete set for the sampling, conditioning and determination of
nicotine, water and particulate matter from cigarettes, have been produced after much cooperation and
collaborative experimentation by many laboratories in many countries.
CORESTA first published an International Standard for the machine smoking of cigarettes in 1968, and since that
time many improvements in equipment as well as in procedure have been suggested.
This International Standard incorporates these improvements and consequently represents the state of the art on
this subject and provides one set of procedures accepted as reference methods.
This method is a machine method and allows cigarettes to be smoked using a strictly controlled set of parameters.
Thus, it enables the NFDPM and nicotine from cigarettes, when smoked by this procedure, to be compared and
ranked on the basis of machine yield.
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SIST ISO 4387:2000
INTERNATIONAL STANDARD ISO 4387:2000(E)
Cigarettes — Determination of total and nicotine-free dry
particulate matter using a routine analytical smoking machine
1 Scope
This International Standard specifies methods for the determination of total particulate matter and for the
subsequent determination of nicotine-free dry particulate matter present in the smoke from cigarettes generated
and collected using a routine analytical smoking machine.
2 Normative references
The following normative documents contain provisions which, through reference in this text, constitute provisions of
this International Standard. For dated references, subsequent amendments to, or revisions of, any of these
publications do not apply. However, parties to agreements based on this International Standard are encouraged to
investigate the possibility of applying the most recent editions of the normative documents indicated below. For
undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC
maintain registers of currently valid International Standards.
ISO 2971, Cigarettes and filter rods — Determination of nominal diameter —Method using a laser beam measuring
apparatus.
ISO 3308:2000, Routine analytical cigarette-smoking machine — Definitions and standard conditions.
ISO 3402, Tobacco and tobacco products — Atmosphere for conditioning and testing.
ISO 6488-1, Tobacco — Determination of water content — Part 1: Karl Fischer method.
ISO 6565, Tobacco and tobacco products — Draw resistance of cigarettes and pressure drop of filter rods —
Standard conditions and measurement.
ISO 8243, Cigarettes — Sampling.
ISO 10315, Cigarettes — Determination of nicotine in smoke condensates — Gas-chromatographic method.
ISO 10362-1, Cigarettes — Determination of water in smoke condensates — Part 1: Gas-chromatographic method.
ISO 16055, Tobacco and tobacco products — Monitor test piece — Requirements and application.
3 Terms, definitions and abbreviated terms
For the purposes of this International Standard, the following terms, definitions and abbreviated terms apply.
3.1
total particulate matter
crude smoke condensate
TPM
that portion of the mainstream smoke which is trapped in the smoke trap, expressed as milligrams per cigarette
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ISO 4387:2000(E)
3.2
dry particulate matter
dry smoke condensate
DPM
total particulate matter after deduction of its water content, expressed as milligrams per cigarette
3.3
nicotine-free dry particulate matter
nicotine-free dry smoke condensate
NFDPM
dry particulate matter after deduction of its nicotine content, expressed as milligrams per cigarette
3.4
smoking process
use of a smoking machine to smoke cigarettes from lighting to final puff
3.5
smoking run
specific smoking process to produce such smoke from a sample of cigarettes as is necessary for the determination
of the smoke components
3.6
laboratory sample
sample intended for laboratory inspection or testing and which is representative of the gross sample or the sub-
period sample
3.7
test sample
cigarettes for test taken at random from the laboratory sample and which are representative of each of the
increments making up the laboratory sample
3.8
conditioning sample
cigarettes selected from the test sample for conditioning prior to tests
3.9
test portion
group of cigarettes prepared for a single determination and which is a random sample from the test sample or
conditioned sample, as appropriate
3.10
monitor test piece
cigarette taken from a batch specially fabricated under controlled manufacturing conditions
NOTE The cigarettes of such a batch show the greatest possible homogeneity with regard to their physical and chemical
characteristics.
4Principle
The test cigarettes are sampled then conditioned. The test cigarettes are smoked on an automatic smoking
machine with simultaneous collection of total particulate matter in a glass fibre filter trap. If used, the consistency of
the laboratory smoking process and subsequent analytical procedures are controlled by using monitor test pieces
specified in ISO 16055. The mass of the total particulate matter so collected is determined gravimetrically. The total
particulate matter is extracted from the trap for determination of the water and nicotine contents by gas
chromatography.
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NOTE In the countries that are not in a position to use gas-chromatographic methods, reference should be made to
ISO 3400 for the determination of total nicotine alkaloids, and the determination of water in smoke condensate should be
performed by the method described in ISO 10362-2. In such cases, values obtained for nicotine and water in smoke condensate
may be used with the addition of a note made in the expression of the result.
5 Apparatus
Normal laboratory apparatus and, in particular, the following items.
5.1 Routine analytical cigarette-smoking machine, complying with the requirements of ISO 3308.
5.2 Soap bubble flow meter, graduated at 35 ml to an accuracy of � 0,2 ml and with a resolution of 0,1 ml.
5.3 Apparatus for the determination of puff duration and frequency.
5.4 Analytical balance, suitable for measuring to the nearest 0,1 mg.
The weighing of filter pad holders may be affected by static electricity, necessitating the use of an antistatic device.
5.5 Conditioning enclosure, carefully maintained under the conditions specified in ISO 3402.
5.6 Length-measuring device, suitable for measuring to the nearest 0,5 mm.
5.7 Device for the determination of diameter, in accordance with ISO 2971.
If such apparatus is not available, the diameter may be determined from the circumference by slitting the cigarette
longitudinally, removing and flattening the paper then measuring its width.
5.8 Smoke trap sealing device, end caps made from a non-hygroscopic and chemically inert material.
5.9 Gloves, made of cotton, or the non-talc surgical type.
6 Sampling
A laboratory sample (3.6) shall be taken by a sampling scheme such as one of those given in ISO 8243.
This sample will normally contain cigarettes taken from different parts of the population. Make up the test sample
(3.7) required for the test by randomly selecting cigarettes from the different parts of the population represented in
the laboratory sample.
7 Determination of total particulate matter
7.1 Preparation of the cigarettes for smoking
7.1.1 General
If N cigarettes of a given type are to be smoked, C� N cigarettes shall be prepared from Q cigarettes for
conditioning and butt marking.
The symbols used in this clause are as follows:
N is the number of cigarettes of a given type to be smoked, resulting from sampling at one point in time or
from a sub-period sample;
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C is a multiplying factor, of value greater than 1, to allow for loss due to damage or selection procedures
between initial sampling and smoking;
Q is the total number of cigarettes available (laboratory sample, see 3.6);
n is the number of replicate determinations of total particulate matter;
q is the number of cigarettes smoked into the same trap;
P is the total number of packets of cigarettes available.
NOTE The multiplier C is usually at least 1,2 to provide extra cigarettes in case some are damaged and for optional tests
which may be required (see 7.5). If selection by mass or draw resistance (or any other parameter) is necessary, C will have to
be much larger (experience suggests 2 to 4) depending on the selection process.
The precision normally required generally demands that 80uu 100. This number may be considerably
augmented if the variability of the sample is high; on the contrary, in certain comparisons made of homogeneous
samples, this number may be reduced. It can also be reduced when N represents a sub-period sample. N shall
never be less than 40 when 20 cigarettes are smoked per trap, or less than 20 when 5 cigarettes are smoked per
trap.
It is necessary for 40 cigarettes to be smoked when 20 cigarettes are smoked per trap, thus providing a replicate
analysis and data replication.
The N cigarettes to be smoked will be tested in n = N/q determinations if q cigarettes are smoked into one trap. As far
as possible these n determinations should correspond to different test portions of the test sample. Selection of each
test portion will depend upon the form of the test sample.
7.1.2 Selection of test portions from a bulk of Q cigarettes
If the test sample is in the form of a single bulk, consisting of Q cigarettes, C� N cigarettes shall be selected at
random so that every cigarette has an equal probability of being selected.
7.1.3 Selection of test portions from P packets
If the test sample consists of P packets, the selection procedure depends upon the number of cigarettes in each
packet (Q/P) compared with q.
If Q/PW C� q, select a test portion by choosing a single packet at random, then randomly select C � q cigarettes
from that packet.
If Q/P � C� q, select the smallest number of packets (k) such that
Qk�
WCq�
P
and randomly choose an equal (or as near equal as possible) number of cigarettes from each packet to form the
test portion of C� q cigarettes.
7.1.4 Duplicate test portions
Provided that the test sample is sufficiently large (W 2C� N), a duplicate set of n test portions should be reserved.
In this event the parallel selection of a test portion and its duplicate would seem sensible. In this case the two
selection conditions of 7.1.3 would need to be changed to Q/PW 2C� q and Q/P� 2C� q.
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7.2 Marking the butt length
7.2.1 Standard butt length
The standard butt length to which cigarettes shall be marked shall be the greatest of the following three lengths:
� 23 mm,
� length of filter� 8mm, or
� length of overwrap� 3 mm,
where the overwrap is defined as any wrapper applied to the mouth end of the cigarette, and the length of the filter
is defined as the total length of the cigarette minus the length of the tobacco portion.
NOTE Butt length is defined in ISO 3308 as the length of unburnt cigarette remaining at the moment when smoking is
stopped.
7.2.2 Measurement of length of filter
The length of filter as defined in 7.2.1 shall be the mean value of 10 cigarettes taken from the laboratory sample,
measured to an accuracy of 0,5 mm. Express the mean to the nearest 0,5 mm.
NOTE In some instances it may be necessary to measure more than 10 cigarettes, but when the variation in filter length
can be demonstrated to be well controlled, a smaller number of measurements may be sufficient.
7.2.3 Measurement of length of overwrap
The length of overwrap as defined in 7.2.1 shall be the mean value of 10 overwraps taken from the laboratory
sample, measured to an accuracy of 0,5 mm. Express the mean to the nearest 0,5 mm.
NOTE In some instances it may be necessary to measure more than 10 cigarettes, but when the variation in overwrap
length can be demonstrated to be well controlled, a smaller number of measurements may be sufficient.
7.2.4 Butt length to be marked on the cigarettes before conditioning
Draw a line, using a fine soft-tipped marker, at the standard butt length, to an accuracy of 0,5 mm, from the mouth
end for the particular cigarette type.
Care should be taken to avoid damaging the cigarettes during butt marking. Any cigarettes accidentally torn or
punctured during marking, or any found during marking to be defective, shall be discarded and replaced with spare
cigarettes from the test portion.
If cigarettes are to be smoked on a smoking machine on which the butt length in accordance to 7.2.1 can be pre-
set, it is not necessary to mark the butt lengths on the cigarettes themselves.
7.3 Selection of cigarettes
If a selection by mass or draw resistance (or any other parameter) is necessary because of the nature of the
problem being studied, the selection shall not be considered as a method of reducing the number of cigarettes to
be smoked.
7.4 Conditioning
Condition all the test portions in the conditioning atmosphere specified in ISO 3402 for a minimum of 48 h and a
maximum of 10 days.
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If for any reason test samples are to be kept for longer than 10 days before conditioning, store them in original
packaging or in airtight containers just large enough to contain the sample.
The testing atmosphere in the laboratory where the smoking is to be carried out shall also be in accordance with
ISO 3402.
Transfer the test portions to the smoking location in airtight containers (just large enough to contain the portions)
unless the smoking location and the conditioning location are adjoining and have identical atmospheres.
7.5 Preliminary tests before smoking
The following data may be required in the test report:
a) total length of the cigarette;
b) nominal diameter, determined in accordance with ISO 2971;
c) draw resistance of the cigarette, determined in accordance with ISO 6565;
d) average mass of the conditioned cigarettes selected for the smoking operation (in milligrams per cigarette);
e) water content (as a mass fraction) of the conditioned cigarettes, determined in accordance with ISO 6488-1.
7.6 Smoking and collection of particulate matter
7.6.1 Smoking plan
Choose a smoking plan; examples of plans are given in informative annex A.
The plan shall show the number of cigarettes to be smoked into each trap (q) and the number in the conditioning
sample (C� N).
The plan should include the use of a test portion of monitor test pieces. The test pieces are included in the plan as
if they were a type of cigarette and prepared and smoked as in 7.6.4, 7.7, 7.8 and 7.9.
7.6.2 Preparation of smoke traps and cigarette holders
For all operations, the operator shall prevent contamination from the fingers by wearing gloves of a suitable
material (5.9).
Insert filter discs which have been conditioned in the test atmosphere for at least 12 h into their holders, and
assemble, placing the rough side of the filter disc so that it will face the oncoming smoke. After assembly, examine
the filter holders to ensure that the discs have been properly fitted. If the smoke trap is designed to contain the
perforated disc (washer), insert it and fit the sealing devices (end caps). If the cigarette holder is designed to
contain a perforated disc, insert it into the cigarette holder before attaching the labyrinth seals (see ISO 3308:2000,
4.8). Weigh the assembled smoke traps to the nearest 0,1 mg.
Because of absorption of water by smoke traps and solvent, it is necessary to determine a value for the sample
blank. Prepare sample blanks by treating additional smoke traps (at least 2 per 100 cigarettes) in the same manner
as that used for smoke collection.
7.6.3 Setting up the smoking machine
7.6.3.1 General
If necessary, replace any protective filters on the machine. Switch on the machine and allow it to warm up on
automatic cycling for at least 20 min.
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With the machine warmed up, check that the puff duration and puff frequency on each channel are in accordance
with the standard conditions.
The puff volume should be checked if it is suspected that the smoking machine is subject to a large change in
temperature during use.
7.6.3.2 Measurement of puff duration
A timer, working with reference to a crystal-controlled oscillator, shall be used to measure the period of time which
elapses between the triggering operations which begin and end a puffing action of the smoking machine. The
accuracy of the timing device shall be such as to ensure that a 1 % error in the puff duration can be detected. The
timer should be coupled directly to the triggering circuits.
NOTE It is not possible to specify the method of measurement beyond a statement of principle because of the variety of
types of suitable timers and smoking machines available.
7.6.3.3 Checking of puff frequency
Measure the period of time which elapses between the triggering operations which begin successive puffing actions
of the smoking machine, thus determining the puff frequency. The timer used shall be suitable for measuring to the
nearest 0,1 s and should, preferably, be coupled directly to the triggering circuits.
7.6.3.4 Measurement of puff volume
The displacement of the bubble in a soap bubble flow meter (5.2) gives a direct measurement of puff volume and
also provides a check for leaks in the system. A suitable indicator graduated at 35 ml shall have a resolution of
0,1 ml. It shall be connected through a standard pressure drop device of 1 kPa� 5 % to the cigarette holder of the
smoking machine channel under test. Before use for a series of measurements, wet the instrument twice with
detergent solution and then allow it to drain for a period of between 30 s and 45 s.
The bubble flow meter shall contain a mass fraction of 15 % aqueous solution of a surface active agent.
1)
Teepol L ® has been found to be satisfactory. The concentration of Teepol as purchased must be known before
carrying out further dilution.
Fit the prepared smoking trap or traps and cigarette holders onto the machine. Attach a plastic insert of an
appropriate size for the labyrinth seals in the cigarette holder to the resistance in the tube from the soap bubble
flow meter indicator. Prepare the soap bubble flow meter by wetting the inside of the tube with the detergent
solution to above the top graduation mark. Connect the indicator to the cigarette holder in port 1 and determine the
puff volume; adjust if necessary to (35,0� 0,3) ml. Repeat for all remaining ports in turn.
Repeat the determinations until the necessary precision of measurement is obtained. If the number of replicates
exceeds three, continue until the correct precision is obtained but replace the pad before smoking, reweigh the
smoke trap and recheck the puff volume with the new pad in place. Measure the temperature and relative humidity
of the air surrounding the smoking machine and note the atmospheric pressure.
7.6.4 Procedure for smoking run
Insert the conditioned cigarettes from the test portion into the cigarette holders so that the butt end impinges upon
the perforated disc (washer) fitted within the filter trap. Avoid any leaks or deformations. Any cigarettes found to
have obvious defects, or which have been damaged during insertion, shall be discarded and replaced with spare,
conditioned cigarettes.
1)
Teepol L is the trade name of a product supplied by Shell. This information is given for the convenience of use
...
NORME ISO
INTERNATIONALE 4387
Troisième édition
2000-04-01
Cigarettes — Détermination de la matière
particulaire totale et de la matière
particulaire anhydre et exempte de nicotine
au moyen d'une machine à fumer
analytique de routine
Cigarettes — Determination of total and nicotine-free dry particulate matter
using a routine analytical smoking machine
Numéro de référence
ISO 4387:2000(F)
©
ISO 2000
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ISO 4387:2000(F)
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ii © ISO 2000 – Tous droits réservés
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ISO 4387:2000(F)
Sommaire Page
Avant-propos.iv
Introduction.v
1 Domaine d'application.1
2 Références normatives .1
3 Termes, définitions et termes abrégés.2
4 Principe.3
5 Appareillage .3
6 Échantillonnage .3
7 Détermination de la matière particulaire totale .4
7.1 Préparation des cigarettes pour le fumage.4
7.2 Marquage de la longueur du mégot.5
7.3 Sélection des cigarettes.6
7.4 Conditionnement .6
7.5 Essais préliminaires avant le fumage.6
7.6 Fumage et piégeage du condensat.6
7.7 Détermination de la matière particulaire totale .8
7.8 Calcul de la masse de la matière particulaire totale .9
7.9 Traitement de la matière particulaire totale .9
8 Rapport d'essai .10
9 Répétabilité et reproductibilité.11
Annexe A (informative) Plans de fumage.13
Bibliographie .18
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ISO 4387:2000(F)
Avant-propos
L'ISO (Organisation internationale de normalisation) est une fédération mondiale d'organismes nationaux de
normalisation (comités membres de l'ISO). L'élaboration des Normes internationales est en général confiée aux
comités techniques de l'ISO. Chaque comité membre intéressé par une étude a le droit de faire partie du comité
technique créé à cet effet. Les organisations internationales, gouvernementales et non gouvernementales, en
liaison avec l'ISO participent également aux travaux. L'ISO collabore étroitement avec la Commission
électrotechnique internationale (CEI) en ce qui concerne la normalisation électrotechnique.
Les Normes internationales sont rédigées conformément aux règles données dans les Directives ISO/CEI, Partie 3.
Les projets de Normes internationales adoptés par les comités techniques sont soumis aux comités membres pour
vote. Leur publication comme Normes internationales requiert l'approbation de 75 % au moins des comités
membres votants.
L’attention est appelée sur le fait que certains des éléments de la présente Norme internationale peuvent faire
l’objet de droits de propriété intellectuelle ou de droits analogues. L’ISO ne saurait être tenue pour responsable de
ne pas avoir identifié de tels droits de propriété et averti de leur existence.
La Norme internationale ISO 4387 a été élaborée par le comité technique ISO/TC 126, Tabac et produits du tabac.
Cette troisième édition annule et remplace la deuxième édition (ISO 4387:1991), laquelle a fait l'objet d'une révision
rédactionnelle.
L’annexe A de la présente Norme internationale est donnée uniquement à titre d’information.
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ISO 4387:2000(F)
Introduction
Les cigarettes sont fabriquées en respectant des tolérances étroites et des procédés rigoureux de contrôle de la
qualité. Toutefois, tous les constituants utilisés dans la fabrication dérivent de produits naturels (tabac, papier à
cigarette, manchette d'assemblage, etc.), ce qui entraîne une variabilité intrinsèque du produit fini. La complexité
ne s'arrête pas là car, au cours du fumage, la cigarette est transformée en fumée.
La fumée de cigarette est un mélange complexe d'une multitude de constituants chimiques individuels, présents en
phase gazeuse, en vapeur et en aérosol de particules condensées. Cette composition est rendue encore plus
complexe par des altérations chimiques, accompagnées d'effets de diffusion et d'intersolubilité, qui prennent effet
dès la formation de la fumée.
La détermination quantitative de la matière particulaire anhydre et exempte de nicotine (MPAEN, parfois appelée
«goudrons») découle en dernière instance de sa définition, nécessairement arbitraire.
Depuis que les chercheurs du tabac s'efforcent de déterminer une valeur pour la MPAEN, diverses méthodes ont
été utilisées. L'expérience a toutefois montré que certaines méthodes sont plus fiables que d'autres, et c'est en
tenant compte de ces facteurs que durant les années 1988 et 1989 des équipes de travail ad hoc composées de
membres des Groupes «Fumée» et «Technologie» du Centre de coopération pour les recherches scientifiques
relatives au tabac (CORESTA) ont conduit des études collectives portant sur la répétabilité et la reproductibilité des
déterminations de la matière particulaire totale et anhydre de la fumée de cigarettes.
Il ressort de ces études que des améliorations en répétabilité et reproductibilité sont effectivement possibles si on
limite le large éventail de méthodes et pratiques encore autorisées par les méthodes normalisées existantes. Il en
est résulté la présente Norme internationale ainsi que d'autres, qui forment un ensemble complet couvrant
l'échantillonnage, le conditionnement et la détermination de la nicotine, de l'eau et de la matière particulaire des
cigarettes, ceci grâce à la coopération et l'expérimentation en commun d'un grand nombre de laboratoires
originaires de nombreux pays différents.
La première méthode normalisée CORESTA pour le fumage mécanique de cigarettes remonte à 1968. Depuis,
bien des améliorations ont été proposées tant pour l'équipement d'essai que pour la méthodologie.
La présente Norme internationale inclut ces améliorations et représente donc le dernier état de la technique en la
matière. Elle fournit un ensemble de modes opératoires acceptés comme méthodes de référence.
Il s'agit d'une méthode sur machine permettant le fumage des cigarettes selon un jeu de paramètres étroitement
contrôlés. Ceci permet de comparer et de classer, sur la base d’un fumage mécanique, la MPAEN et la nicotine de
cigarettes fumées selon le mode opératoire décrit.
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NORME INTERNATIONALE ISO 4387:2000(F)
Cigarettes — Détermination de la matière particulaire totale et de
la matière particulaire anhydre et exempte de nicotine au moyen
d'une machine à fumer analytique de routine
1 Domaine d'application
La présente Norme internationale spécifie des méthodes de détermination de la matière particulaire totale et de
détermination ultérieure de la matière particulaire anhydre et exempte de nicotine, présente dans la fumée de
cigarette, produite et recueillie au moyen d'une machine à fumer analytique de routine.
2 Références normatives
Les documents normatifs suivants contiennent des dispositions qui, par suite de la référence qui y est faite,
constituent des dispositions valables pour la présente Norme internationale. Pour les références datées, les
amendements ultérieurs ou les révisions de ces publications ne s’appliquent pas. Toutefois, les parties prenantes
aux accords fondés sur la présente Norme internationale sont invitées à rechercher la possibilité d'appliquer les
éditions les plus récentes des documents normatifs indiqués ci-après. Pour les références non datées, la dernière
édition du document normatif en référence s’applique. Les membres de l'ISO et de la CEI possèdent le registre des
Normes internationales en vigueur.
ISO 2971, Cigarettes et bâtonnets-filtres — Détermination du diamètre nominal — Méthode utilisant un instrument
de mesure à faisceau laser.
ISO 3308:2000, Machine à fumer analytique de routine pour cigarettes — Définitions et conditions normalisées.
ISO 3402, Tabac et produits du tabac — Atmosphère de conditionnement et d’essai.
ISO 6488-1, Tabac — Détermination de la teneur en eau — Partie 1: Méthode de Karl Fischer.
ISO 6565, Tabac et produits du tabac — Résistance au tirage des cigarettes et perte de charge des bâtonnets-
filtres — Conditions normalisées et mesurage.
ISO 8243, Cigarettes — Échantillonnage.
ISO 10315, Cigarettes — Dosage de la nicotine dans les condensats de fumée — Méthode par chromatographie
en phase gazeuse.
ISO 10362-1, Cigarettes — Dosage de l’eau dans les condensats de fumée — Partie 1: Méthode par
chromatographie en phase gazeuse.
ISO 16055, Tabac et produits du tabac — Éprouvette de contrôle — Exigences et application.
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ISO 4387:2000(F)
3 Termes, définitions et termes abrégés
Pour les besoins de la présente Norme internationale, les termes, définitions et termes abrégés suivants
s'appliquent.
3.1
matière particulaire totale
condensat brut de fumée
MPT
partie de la fumée du courant principal qui est retenue dans le piège à fumée, exprimée en milligrammes par
cigarette
3.2
matière particulaire anhydre
condensat anhydre de fumée
MPA
condensat brut de fumée après déduction de sa teneur en eau, exprimé en milligrammes par cigarette
3.3
matière particulaire anhydre et exempte de nicotine
condensat de fumée anhydre et exempt de nicotine
MPAEN
condensat anhydre de fumée après déduction de sa teneur en nicotine, exprimé en milligrammes par cigarette
3.4
opération de fumage
utilisation d'une machine à fumer pour fumer des cigarettes depuis l'allumage jusqu'à la bouffée finale
3.5
série de fumages
ensemble spécifique d'opérations de fumage en vue de produire, à partir d'un échantillon de cigarettes, la quantité
de fumée nécessaire à la détermination des composants de la fumée
3.6
échantillon pour laboratoire
échantillon destiné à être utilisé pour un contrôle ou pour des essais en laboratoire et qui est représentatif de
l'échantillon brut ou de sous-période
3.7
échantillon pour essai
cigarettes pour essai prélevées de façon aléatoire sur l'échantillon pour laboratoire et qui sont représentatives de
chacun des échantillons élémentaires constituant ce dernier
3.8
échantillon à conditionner
cigarettes sélectionnées à partir de l'échantillon pour essai et à conditionner préalablement aux essais
3.9
prise d’essai
ensemble de cigarettes préparées pour un mesurage unique et qui est prélevé de façon aléatoire sur l'échantillon
pour essai ou l'échantillon conditionné, selon ce qui est approprié
3.10
éprouvette de contrôle
cigarette prélevée sur un lot spécialement fabriqué dans des conditions de production contrôlées
NOTE Les cigarettes d’un tel lot présentent la plus grande homogénéité possible en ce qui concerne leurs caractéristiques
physiques et chimiques.
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ISO 4387:2000(F)
4Principe
Échantillonnage des cigarettes pour essai. Conditionnement des cigarettes pour essai. Fumage des cigarettes pour
essai sur une machine à fumer automatique et piégeage simultané de la matière particulaire totale dans un piège
en fibre de verre. Le cas échéant, contrôle de la conformité des opérations de fumage en laboratoire et des
méthodes analytiques consécutives à l’aide d’éprouvettes de contrôle, spécifiées dans l’ISO 16055. Détermination
gravimétrique de la masse de matière particulaire totale ainsi obtenue. Extraction du piège de la matière
particulaire totale en vue de la détermination des teneurs en eau et en nicotine par chromatographie en phase
gazeuse.
NOTE Dans les pays qui ne sont pas en mesure d'utiliser la chromatographie en phase gazeuse, il convient de se référer à
l’ISO 3400 pour le dosage des alcaloïdes nicotiniques totaux et d’effectuer le dosage de l'eau dans le condensat de fumée
selon la méthode décrite dans l’ISO 10362-2. Dans ce cas, les valeurs obtenues pour la nicotine et l'eau dans le condensat de
fumée peuvent être utilisées moyennant une note ajoutée à l'expression des résultats.
5 Appareillage
Appareillage courant de laboratoire et, en particulier, ce qui suit.
5.1 Machine à fumer analytique de routine, conforme aux exigences de l’ISO 3308.
5.2 Débitmètre à bulle de savon, portant une marque à 35 ml, d’une précision de � 0,2 ml, et ayant une
résolution de 0,1 ml.
5.3 Appareillage pour la détermination de la durée de l'aspiration et de la fréquence des bouffées.
5.4 Balance analytique, permettant d’effectuer des mesurages à 0,1 mg près.
L’électricité statique peut influer sur le pesage des porte-filtres, nécessitant l’utilisation d’un dispositif antistatique.
5.5 Enceinte de conditionnement, soigneusement maintenue dans les conditions spécifiées dans l’ISO 3402.
5.6 Dispositif de mesure de la longueur, permettant d'effectuer des mesurages à 0,5 mm près.
5.7 Dispositif pour la mesure du diamètre, conformément à l’ISO 2971.
Si un tel dispositif n'est pas disponible, le diamètre peut être déterminé à partir de la circonférence en fendant
longitudinalement la cigarette, et en prélevant et aplatissant le papier pour en mesurer la largeur.
5.8 Capuchons étanches pour piège à fumée, faits d'un matériau non hygroscopique et chimiquement inerte.
5.9 Gants, en coton ou de type chirurgical sans talc.
6 Échantillonnage
Constituer un échantillon pour laboratoire (3.6) selon un plan d’échantillonnage tel que l’un de ceux donnés dans
l’ISO 8243.
Cet échantillon comportera normalement des cigarettes prélevées sur des parties distinctes de la population.
Constituer l’échantillon pour essai (3.7) requis pour cette détermination en effectuant une sélection au hasard à
partir des parties distinctes de la population représentée dans l’échantillon pour laboratoire.
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ISO 4387:2000(F)
7 Détermination de la matière particulaire totale
7.1 Préparation des cigarettes pour le fumage
7.1.1 Généralités
Pour fumer N cigarettes d'un type donné, on devra, à partir des Q cigarettes disponibles, préparer C � N cigarettes
pour conditionnement et marquage du mégot.
Dans le présent article, les symboles suivants sont utilisés:
N est le nombre de cigarettes d'un type donné destinées à être fumées et résultant d'un échantillonnage à
un moment donné ou de sous-période;
C est un facteur multiplicatif, d'une valeur supérieure à 1, qui permet de tenir compte les pertes dues aux
cigarettes endommagées, ou résultant des procédures de sélection entre l'échantillonnage initial et le
fumage;
Q est le nombre total de cigarettes disponibles (échantillon pour laboratoire, voir 3.6);
n est le nombre de répétitions de la détermination de la matière particulaire totale;
q est le nombre de cigarettes fumées à travers un même piège;
P est le nombre total de paquets de cigarettes disponibles.
NOTE Le facteur multiplicatif C est en général égal au moins à 1,2 pour permettre, le cas échéant, le remplacement de
cigarettes endommagées et la réalisation des essais facultatifs susceptibles d’être requis (voir 7.5). Si une sélection selon la
masse ou la résistance au tirage (ou tout autre paramètre) est nécessaire, C devra être beaucoup plus grand (l'expérience
suggère 2 à 4), en fonction du mode de sélection.
L’exactitude habituellement requise nécessite généralement que 80uu 100. Ce nombre peut être
considérablement augmenté si la dispersion de l'échantillon est élevée; en revanche, dans certaines comparaisons
effectuées sur échantillons homogènes, ce nombre peut être réduit. Il peut également être réduit quand N
représente un échantillon de sous-période. N ne doit jamais être inférieur à 40 lorsque 20 cigarettes sont fumées
par piège, ou inférieur à 20 lorsque 5 cigarettes sont fumées par piège.
Il est nécessaire de fumer 40 cigarettes lorsque 20 cigarettes sont fumées par piège, ce qui permet d'obtenir des
résultats de l'analyse et des données en double.
Les N cigarettes à fumer donneront lieu à n = N/q déterminations, si l'on fume q cigarettes par piège. Dans la
mesure du possible, il convient que ces n déterminations correspondent aux différentes prises d’essai de
l'échantillon pour essai. La constitution de chaque prise d’essai dépendra de la forme de l'échantillon pour essai.
7.1.2 Sélection des prises d’essai à partir de Q cigarettes en vrac
Si l'échantillon pour essai se présente sous la forme de Q cigarettes en vrac, on doit y prélever au hasard C � N
cigarettes de telle manière que chaque cigarette ait une probabilité égale d'être choisie.
7.1.3 Sélection des prises d’essai à partir de P paquets
Si l'échantillon pour essai est constitué de P paquets, la procédure de sélection dépend du nombre de cigarettes
par paquet (Q/P) comparé à q.
Si Q/PW C � q, constituer chaque prise d’essai en choisissant un paquet au hasard et en prélevant au hasard C � q
cigarettes de ce paquet.
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ISO 4387:2000(F)
Si Q/P� C� q, sélectionner le plus petit nombre de paquets (k)telque
Qk�
W C · q
P
et prélever au hasard dans chaque paquet un nombre égal (ou aussi voisin que possible) de cigarettes, de façon à
constituer la prise d’essai de C� q cigarettes.
7.1.4 Duplication des prises d’essai
Si l'échantillon pour essai est de taille suffisante (W 2C� N), il convient de prévoir une deuxième série de n prises
d’essai. Il sera alors judicieux de constituer en parallèle la prise d’essai et son homologue dupliqué. Dans ce cas,
les deux conditions de sélection de 7.1.3 devront être transformées en Q/PW 2C� q et Q/P� 2C� q.
7.2 Marquage de la longueur du mégot
7.2.1 Longueur de mégot normalisée
La longueur de mégot à respecter lors du fumage doit être la plus grande des trois longueurs suivantes:
� 23 mm,
� longueur de filtre + 8 mm,
� longueur de la manchette d'assemblage + 3 mm,
où la manchette d'assemblage est définie comme toute enveloppe entourant l'extrémité bouche de la cigarette, et
la longueur de filtre est définie comme la longueur totale de la cigarette diminuée de la longueur du boudin de
tabac.
NOTE La longueur du mégot est définie dans l’ISO 3308 comme la longueur de la partie non consumée de la cigarette
subsistant à l'instant où le fumage est arrêté.
7.2.2 Mesurage de la longueur du filtre
La longueur du filtre, définie en 7.2.1, doit être la valeur moyenne pour 10 cigarettes prélevées sur l'échantillon
pour laboratoire, mesurée avec une précision de 0,5 mm. Exprimer cette moyenne à 0,5 mm près.
NOTE Dans certains cas, il peut être nécessaire de mesurer plus de 10 cigarettes, mais lorsqu'il est établi que la variabilité
de la longueur du filtre est bien contrôlée, un nombre de mesurages plus faible peut être suffisant.
7.2.3 Mesurage de la longueur de la manchette d'assemblage
La longueur de la manchette d'assemblage, définie en 7.2.1, doit être la valeur moyenne de 10 manchettes prises
dans l'échantillon pour laboratoire, mesurée avec une précision de 0,5 mm. Exprimer cette moyenne à 0,5 mm
près.
NOTE Dans certains cas, il peut être nécessaire de mesurer plus de 10 cigarettes, mais lorsqu'il est établi que la variabilité
de la longueur de la manchette est bien contrôlée, un nombre de mesurages plus faible peut être suffisant.
7.2.4 Longueur de mégot à marquer sur les cigarettes avant conditionnement
À l’aide d’un marqueur à pointe fine et souple, tracer une ligne à la longueur normalisée de mégot, prise à partir de
l'extrémité bouche de la cigarette du type concerné, avec une précision de 0,5 mm.
Il faut veiller à ne pas endommager les cigarettes pendant le marquage. Les cigarettes accidentellement percées
ou déchirées pendant le marquage, ou trouvées défectueuses à cette occasion, doivent être rejetées et
remplacées par des cigarettes prélevées à partir de la prise d’essai.
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ISO 4387:2000(F)
Il n'est pas nécessaire de procéder à ce marquage dans le cas d'une machine à fumer sur laquelle la longueur de
mégot peut être préréglée conformément à 7.2.1.
7.3 Sélection des cigarettes
Si une sélection selon la masse ou la résistance au tirage (ou tout autre paramètre) est nécessaire en raison de la
nature du problème à étudier, cette sélection ne doit pas être considérée comme une méthode destinée à réduire
le nombre des cigarettes à fumer.
7.4 Conditionnement
Conditionner toutes les prises d’essai dans l'atmosphère de conditionnement spécifiée dans l’ISO 3402 pendant
48 h au moins et 10 jours au plus.
Si, pour une raison quelconque, des échantillons à tester doivent être gardés plus de 10 jours préalablement à leur
conditionnement, les conserver dans leur emballage original ou dans des récipients hermétiques à peine plus
grands que les échantillons.
L'atmosphère d'essai du laboratoire de fumage doit également être conforme à l’ISO 3402.
Transférer les prises d’essai au laboratoire de fumage dans des récipients étanches à l'air et à peine plus grands
que le volume des lots, à moins que les locaux de conditionnement et de fumage ne soient contigus et dotés
d'atmosphères identiques.
7.5 Essais préliminaires avant le fumage
Les paramètres suivants peuvent être exigés dans le rapport d'essai:
a) la longueur totale de la cigarette;
b) le diamètre nominal, déterminé conformément à l’ISO 2971;
c) la résistance au tirage de la cigarette, déterminée conformément à l’ISO 6565;
d) la moyenne arithmétique de la masse des cigarettes conditionnées destinées au fumage (en milligrammes par
cigarette);
e) la teneur en eau (en fraction massique) des cigarettes conditionnées, déterminée conformément à
l’ISO 6488-1.
7.6 Fumage et piégeage du condensat
7.6.1 Plan de fumage
Choisir un plan de fumage; des exemples sont donnés à titre indicatif dans l'annexe A.
Le plan doit indiquer le nombre de cigarettes à fumer par piège (q) et leur nombre dans l'échantillon pour
conditionnement (C � N).
Il convient d'inclure dans le plan l’utilisation d’une prise d’essai composée d’éprouvettes de contrôle. Les
éprouvettes figurent dans le plan comme si elles constituaient un type de cigarette et sont préparées et fumées
commeen7.6.4,7.7,7.8et7.9.
7.6.2 Préparation des pièges à fumée et des porte-cigarettes
Pour toutes les opérations, l'opérateur doit éviter la contamination par les doigts en portant des gants d'un matériau
approprié (5.9).
6 © ISO 2000 – Tous droits réservés
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ISO 4387:2000(F)
Insérer dans leurs supports les disques filtrants, préalablement conditionnés dans l'atmosphère d'essai pendant
12 h au moins, et les assembler, en s'assurant que la face rugueuse des disques est tournée vers l'arrivée de la
fumée. Après assemblage, examiner les porte-filtres pour vérifier que les disques ont été correctement ajustés. Si
le piège à fumée est conçu pour contenir un disque perforé, l'insérer et ajuster les capuchons étanches. Si le porte-
cigarettes est conçu pour contenir un disque perforé, l'insérer avant de fixer les joints-labyrinthe (voir
l’ISO 3308:2000, 4.8). Peser, à 0,1 mg près, les pièges à fumée ainsi assemblés.
En raison de l'absorption d'eau par les pièges à fumée et le solvant, il est nécessaire de déterminer une valeur
pour le blanc. Préparer des blancs en préparant des pièges additionnels (au moins 2 pour 100 cigarettes) de la
même manière que ceux utilisés pour la récupération de la fumée.
7.6.3 Réglage de la machine à fumer
7.6.3.1 Généralités
Si nécessaire, remplacer les filtres de protection pouvant équiper la machine. Mettre sous tension et laisser
chauffer en cycle automatique pendant 20 min au moins.
Quand la machine est en régime, vérifier que la durée de l'aspiration et la fréquence des bouffées sur chaque
canal sont conformes aux conditions normalisées.
Il convient de contrôler le volume de la bouffée si l’on pense que la machine à fumer est sujette à une variation
importante de la température pendant son utilisation.
7.6.3.2 Mesurage de la durée de l'aspiration
Un minuteur, étalonné par rapport à un oscillateur à cristal, doit être utilisé pour mesurer la période de temps qui
s'écoule entre les déclenchements qui commencent et terminent une action d'aspiration de la machine à fumer.
L’exactitude du dispositif de mesure doit cependant être telle qu'une erreur de 1 % dans la durée de l'aspiration
puisse être décelée. Il convient de coupler le dispositif de mesure du temps directement au circuit de
déclenchement.
NOTE Il n'est pas possible de spécifier la méthode de mesure autrement que par une indication de principe, en raison de
la diversité des types d'appareils de mesure du temps et des machines à fumer disponibles.
7.6.3.3 Vérification de la fréquence des bouffées
Mesurer la période de temps qui s'écoule entre les déclenchements qui commencent les actions d'aspiration
successives de la machine à fumer, ce qui détermine la fréquence des bouffées. Le minuteur utilisé doit être
capable de mesurer le temps à 0,1 s près, et il convient qu'il soit, de préférence, couplé directement au circuit de
déclenchement.
7.6.3.4 Mesurage du volume de la bouffée
Le déplacement de la bulle dans un débitmètre à bulle de savon (5.2.) donne une mesure directe du volume de la
bouffée et permet aussi de vérifier les fuites du système. Un indicateur adéquat gradué à 35 ml doit avoir une
précision de 0,1 ml. Il doit être relié par un dispositif de perte de charge normalisé de 1 kPa�5% au porte-
cigarettes du canal de la machine à fumer à vérifier. Avant utilisation pour une série de mesurages, mouiller
l'instrument deux fois avec une solution de détergent puis laisser égoutter pendant 30 s à 45 s.
Le débitmètre à bulle doit contenir une solution aqueuse d'une concentration de 15 % (fraction massique) d'un
�1)
agent de surface. Le Teepol L s'est avéré satisfaisant
...
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