SIST ISO 4387:2020
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
This document 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.
Cigarettes - Détermination de la teneur en matière particulaire totale et en matière particulaire anhydre et exempte de nicotine au moyen d'une machine à fumer analytique de routine
Le présent document spécifie des méthodes de détermination de la teneur en matičre particulaire totale et de détermination ultérieure de la teneur en matičre particulaire anhydre et exempte de nicotine, présente dans la fumée de cigarette, produite et recueillie au moyen d'une machine ŕ fumer analytique de routine.
Cigarete - Določevanje celotne in suhe snovi brez nikotina z uporabo rutinsko analiznega cigaretnega dimnega stroja
General Information
RELATIONS
Buy Standard
Standards Content (sample)
SLOVENSKI STANDARD
SIST ISO 4387:2020
01-julij-2020
Nadomešča:
SIST ISO 4387:2000
Cigarete - Določevanje celotne in suhe snovi brez nikotina z uporabo rutinsko
analiznega cigaretnega dimnega stroja
Cigarettes - Determination of total and nicotine-free dry particulate matter using a
routine analytical smoking machineCigarettes - Détermination de la teneur en matière particulaire totale et en matière
particulaire anhydre et exempte de nicotine au moyen d'une machine à fumer analytique
de routineTa slovenski standard je istoveten z: ISO 4387:2019
ICS:
65.160 Tobak, tobačni izdelki in Tobacco, tobacco products
oprema and related equipment
SIST ISO 4387:2020 en,fr
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST ISO 4387:2020
INTERNATIONAL ISO
STANDARD 4387
Fourth edition
2019-09
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 4387:2019(E)
ISO 2019
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SIST ISO 4387:2020
ISO 4387:2019(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2019
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting
on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address
below or ISO’s member body in the country of the requester.ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2019 – All rights reserved
---------------------- Page: 4 ----------------------
SIST ISO 4387:2020
ISO 4387:2019(E)
Contents Page
Foreword ........................................................................................................................................................................................................................................iv
Introduction ..................................................................................................................................................................................................................................v
1 Scope ................................................................................................................................................................................................................................. 1
2 Normative references ...................................................................................................................................................................................... 1
3 Terms and definitions ..................................................................................................................................................................................... 1
4 Principle ........................................................................................................................................................................................................................ 2
5 Apparatus ..................................................................................................................................................................................................................... 3
6 Sampling ........................................................................................................................................................................................................................ 3
7 Determination of total particular matter ................................................................................................................................... 4
7.1 Preparation of the cigarettes for smoking ....................................................................................................................... 4
7.1.1 General...................................................................................................................................................................................... 4
7.1.2 Selection of test portions from a bulk of Q cigarettes ...................................................................... 4
7.1.3 Selection of test portions from P packets ................................................................................................... 4
7.1.4 Duplicate test portions ............................................................................................................................................... 5
7.2 Marking the butt length ................................................................................................................................................................... 5
7.2.1 Standard butt length ..................................................................................................................................................... 5
7.2.2 Measurement of length of filter .......................................................................................................................... 5
7.2.3 Measurement of length of overwrap .............................................................................................................. 6
7.2.4 Butt length to be marked on the cigarettes before conditioning ........................................... 6
7.3 Selection of cigarettes ....................................................................................................................................................................... 6
7.4 Conditioning .............................................................................................................................................................................................. 6
7.5 Preliminary tests before smoking .......................................................................................................................................... 6
7.6 Smoking and collection of particular matter ................................................................................................................ 7
7.6.1 Smoking plan ...................................................................... ................................................................................................. 7
7.6.2 Preparation of smoke traps and cigarette holders ............................................................................. 7
7.6.3 Setting up the smoking machine ........................................................................................................................ 7
7.6.4 Procedure for smoking run ..................................................................................................................................... 8
7.7 Determination of total particulate matter ....................................................................................................................... 9
7.8 Calculation of total particulate matter ............................................................................................................................... 9
7.9 Treatment of total particulate matter ................................................................................................................................. 9
7.9.1 Extraction procedure ................................................................................................................................................... 9
7.9.2 Determination of water ...........................................................................................................................................10
7.9.3 Determination of nicotine .....................................................................................................................................10
8 Test report ................................................................................................................................................................................................................10
9 Repeatability and reproducibility ...................................................................................................................................................12
Annex A (informative) Smoking plans .............................................................................................................................................................13
Bibliography .............................................................................................................................................................................................................................19
© ISO 2019 – All rights reserved iii---------------------- Page: 5 ----------------------
SIST ISO 4387:2020
ISO 4387:2019(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.The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www .iso .org/patents).Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.For an explanation on the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following
URL: www .iso .org/iso/foreword .html.This document was prepared by Technical Committee ISO/TC 126, Tobacco and tobacco products.
This fourth edition cancels and replaces the third edition (ISO 4387:2000), which has been
technically revised. It also incorporates the Amendments ISO 4387:2000/Amd.1:2008 and
ISO 4387:2000/Amd.2:2017.The main change compared to the previous edition is as follows:
— in 7.6.4, smoking and collecftion of particular matter has been modified by moving wording from
ISO 8454 into ISO 4387.Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www .iso .org/members .html.iv © ISO 2019 – All rights reserved
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Introduction
Cigarettes are manufactured to close tolerances using strict quality control procedures. However, all
the constituents involved in the manufacture (such as tobacco, cigarette paper, tipping, etc.) are derived
from natural products and this result in a final product which is intrinsically variable. The complexity
does not end 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 complicates its composition.The quantitative measurement of nicotine-free dry particulate matter (NFDPM, sometimes referred to
as “tar”) is, therefore, dependent on its arbitrary definition.From the time that scientists have attempted to determine a value for NFDPM, a number of 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 document, 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 document 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.No machine smoking regime can represent all human smoking behaviours.
— It is recommended that cigarettes also be tested under conditions of a different intensity of machine
smoking than those specified in this document.— Machine smoking testing is useful to characterize cigarette emissions for design and regulatory
purposes, but communication of machine measurements to smokers can result in misunderstandings
about differences in exposure and risk across brands.— Smoke emission data from machine measurements may be used as inputs for product hazard
assessment, but they are not intended to be nor are they valid as measures of human exposure or
risks. Communicating differences between products in machine measurements as differences in
exposure or risk is a misuse of testing using ISO standards.© ISO 2019 – All rights reserved v
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SIST ISO 4387:2020
INTERNATIONAL STANDARD ISO 4387:2019(E)
Cigarettes — Determination of total and nicotine-
free dry particulate matter using a routine analytical
smoking machine
1 Scope
This document 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 documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 2971, Cigarettes and filter rods — Determination of nominal diameter — Method using a non-contact
optical measuring apparatusISO 3308, Routine analytical cigarette-smoking machine — Definitions and standard conditions
ISO 3402, Tobacco and tobacco products — Atmosphere for conditioning and testingISO 6488, Tobacco and tobacco products — Determination of water content — Karl Fischer method
ISO 6565, Tobacco and tobacco products — Draw resistance of cigarettes and pressure drop of filter
rods — Standard conditions and measurementISO 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 methodISO 16055, Tobacco and tobacco products — Monitor test piece — Requirements and use
3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https: //www .iso .org/obp— IEC Electropedia: available at http: //www .electropedia .org/
3.1
total particulate matter
crude smoke condensate
TPM
portion of the mainstream smoke which is trapped in the smoke trap
Note 1 to entry: It is expressed as milligrams per cigarette.
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3.2
dry particulate matter
dry smoke condensate
DPM
total particulate matter (3.1) after deduction of its water content
Note 1 to entry: It is expressed as milligrams per cigarette.
3.3
nicotine-free dry particulate matter
nicotine-free dry smoke condensate
NFDPM
dry particulate matter (3.2) after deduction of its nicotine content
Note 1 to entry: It is 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 (3.4) to produce such smoke from a sample of cigarettes as is necessary for the
determination of the smoke components3.6
clearing puff
any puff taken after a cigarette has been extinguished or removed from the cigarette holder
3.7laboratory sample
sample intended for laboratory inspection or testing and which is representative of the gross sample or
the sub-period sample3.8
test sample
cigarettes for test taken at random from the laboratory sample (3.6) and which are representative of
each of the increments making up the laboratory sample3.9
conditioning sample
cigarettes selected from the test sample (3.7) for conditioning prior to tests
3.10
test portion
group of cigarettes prepared for a single determination and which is a random sample from the test
sample (3.7) or conditioned sample, as appropriate3.11
monitor test piece
cigarette taken from a batch specially fabricated under controlled manufacturing conditions
Note 1 to entry: The cigarettes of such a batch show the greatest possible homogeneity with regard to their
physical and chemical characteristics.4 Principle
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
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SIST ISO 4387:2020
ISO 4387:2019(E)
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.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 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 required for the test by randomly selecting cigarettes from the different parts of the
population represented in the laboratory sample.© ISO 2019 – All rights reserved 3
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7 Determination of total particular 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;C is a multiplying factor, of value greater than 1, to allow for loss due to damage or selection proce-
dures 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.
NOTE The multiplier C is usually at least 1,2 to provide extra cigarettes in case some are damaged and
for optional tests which are possibly required (see 7.5). If selection by mass or draw resistance (or any other
parameter) is necessary, C is likely to be much larger (experience suggests 2 to 4) depending on the selection
process.The precision normally required generally demands that 80 ≤ N ≤ 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.
Where q is the number of cigarettes smoked into the same trap.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 packetsIf 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/P ≥ C × q, select a test portion by choosing a single packet at random, then randomly select C × q
cigarettes from that packet.4 © ISO 2019 – All rights reserved
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ISO 4387:2019(E)
If Q/P < C × q, select the smallest number of packets (k) as shown in Formula (1):
Qk×≥×Cq (1)
where
Q is the total number of cigarettes available (laboratory sample, see 3.6)
k is the smallest number of packets;
P is the total number of packets of cigarettes available;
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 number of cigarettes smoked into the same trap.
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 (≥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/P ≥ 2C × q and Q/P < 2C × q.
7.2 Marking the butt length7.2.1 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 + 8 mm, 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 might 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 is sufficient.
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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 might 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 is sufficient.
7.2.4 Butt length to be marked on the cigarettes before conditioningDraw 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 cigarettesIf 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.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 6488.6 © ISO 2019 – All rights reserved
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7.6 Smoking and collection of particular matter
7.6.1 Smoking plan
Choose a smoking plan. Examples of plans are given in 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 holdersFor all operations, the operator shall prevent con
...
INTERNATIONAL ISO
STANDARD 4387
Fourth edition
2019-09
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 4387:2019(E)
ISO 2019
---------------------- Page: 1 ----------------------
ISO 4387:2019(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2019
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting
on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address
below or ISO’s member body in the country of the requester.ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2019 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 4387:2019(E)
Contents Page
Foreword ........................................................................................................................................................................................................................................iv
Introduction ..................................................................................................................................................................................................................................v
1 Scope ................................................................................................................................................................................................................................. 1
2 Normative references ...................................................................................................................................................................................... 1
3 Terms and definitions ..................................................................................................................................................................................... 1
4 Principle ........................................................................................................................................................................................................................ 2
5 Apparatus ..................................................................................................................................................................................................................... 3
6 Sampling ........................................................................................................................................................................................................................ 3
7 Determination of total particular matter ................................................................................................................................... 4
7.1 Preparation of the cigarettes for smoking ....................................................................................................................... 4
7.1.1 General...................................................................................................................................................................................... 4
7.1.2 Selection of test portions from a bulk of Q cigarettes ...................................................................... 4
7.1.3 Selection of test portions from P packets ................................................................................................... 4
7.1.4 Duplicate test portions ............................................................................................................................................... 5
7.2 Marking the butt length ................................................................................................................................................................... 5
7.2.1 Standard butt length ..................................................................................................................................................... 5
7.2.2 Measurement of length of filter .......................................................................................................................... 5
7.2.3 Measurement of length of overwrap .............................................................................................................. 6
7.2.4 Butt length to be marked on the cigarettes before conditioning ........................................... 6
7.3 Selection of cigarettes ....................................................................................................................................................................... 6
7.4 Conditioning .............................................................................................................................................................................................. 6
7.5 Preliminary tests before smoking .......................................................................................................................................... 6
7.6 Smoking and collection of particular matter ................................................................................................................ 7
7.6.1 Smoking plan ...................................................................... ................................................................................................. 7
7.6.2 Preparation of smoke traps and cigarette holders ............................................................................. 7
7.6.3 Setting up the smoking machine ........................................................................................................................ 7
7.6.4 Procedure for smoking run ..................................................................................................................................... 8
7.7 Determination of total particulate matter ....................................................................................................................... 9
7.8 Calculation of total particulate matter ............................................................................................................................... 9
7.9 Treatment of total particulate matter ................................................................................................................................. 9
7.9.1 Extraction procedure ................................................................................................................................................... 9
7.9.2 Determination of water ...........................................................................................................................................10
7.9.3 Determination of nicotine .....................................................................................................................................10
8 Test report ................................................................................................................................................................................................................10
9 Repeatability and reproducibility ...................................................................................................................................................12
Annex A (informative) Smoking plans .............................................................................................................................................................13
Bibliography .............................................................................................................................................................................................................................19
© ISO 2019 – All rights reserved iii---------------------- Page: 3 ----------------------
ISO 4387:2019(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.The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www .iso .org/patents).Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.For an explanation on the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following
URL: www .iso .org/iso/foreword .html.This document was prepared by Technical Committee ISO/TC 126, Tobacco and tobacco products.
This fourth edition cancels and replaces the third edition (ISO 4387:2000), which has been
technically revised. It also incorporates the Amendments ISO 4387:2000/Amd.1:2008 and
ISO 4387:2000/Amd.2:2017.The main change compared to the previous edition is as follows:
— in 7.6.4, smoking and collecftion of particular matter has been modified by moving wording from
ISO 8454 into ISO 4387.Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www .iso .org/members .html.iv © ISO 2019 – All rights reserved
---------------------- Page: 4 ----------------------
ISO 4387:2019(E)
Introduction
Cigarettes are manufactured to close tolerances using strict quality control procedures. However, all
the constituents involved in the manufacture (such as tobacco, cigarette paper, tipping, etc.) are derived
from natural products and this result in a final product which is intrinsically variable. The complexity
does not end 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 complicates its composition.The quantitative measurement of nicotine-free dry particulate matter (NFDPM, sometimes referred to
as “tar”) is, therefore, dependent on its arbitrary definition.From the time that scientists have attempted to determine a value for NFDPM, a number of 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 document, 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 document 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.No machine smoking regime can represent all human smoking behaviours.
— It is recommended that cigarettes also be tested under conditions of a different intensity of machine
smoking than those specified in this document.— Machine smoking testing is useful to characterize cigarette emissions for design and regulatory
purposes, but communication of machine measurements to smokers can result in misunderstandings
about differences in exposure and risk across brands.— Smoke emission data from machine measurements may be used as inputs for product hazard
assessment, but they are not intended to be nor are they valid as measures of human exposure or
risks. Communicating differences between products in machine measurements as differences in
exposure or risk is a misuse of testing using ISO standards.© ISO 2019 – All rights reserved v
---------------------- Page: 5 ----------------------
INTERNATIONAL STANDARD ISO 4387:2019(E)
Cigarettes — Determination of total and nicotine-
free dry particulate matter using a routine analytical
smoking machine
1 Scope
This document 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 documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 2971, Cigarettes and filter rods — Determination of nominal diameter — Method using a non-contact
optical measuring apparatusISO 3308, Routine analytical cigarette-smoking machine — Definitions and standard conditions
ISO 3402, Tobacco and tobacco products — Atmosphere for conditioning and testingISO 6488, Tobacco and tobacco products — Determination of water content — Karl Fischer method
ISO 6565, Tobacco and tobacco products — Draw resistance of cigarettes and pressure drop of filter
rods — Standard conditions and measurementISO 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 methodISO 16055, Tobacco and tobacco products — Monitor test piece — Requirements and use
3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https: //www .iso .org/obp— IEC Electropedia: available at http: //www .electropedia .org/
3.1
total particulate matter
crude smoke condensate
TPM
portion of the mainstream smoke which is trapped in the smoke trap
Note 1 to entry: It is expressed as milligrams per cigarette.
© ISO 2019 – All rights reserved 1
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ISO 4387:2019(E)
3.2
dry particulate matter
dry smoke condensate
DPM
total particulate matter (3.1) after deduction of its water content
Note 1 to entry: It is expressed as milligrams per cigarette.
3.3
nicotine-free dry particulate matter
nicotine-free dry smoke condensate
NFDPM
dry particulate matter (3.2) after deduction of its nicotine content
Note 1 to entry: It is 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 (3.4) to produce such smoke from a sample of cigarettes as is necessary for the
determination of the smoke components3.6
clearing puff
any puff taken after a cigarette has been extinguished or removed from the cigarette holder
3.7laboratory sample
sample intended for laboratory inspection or testing and which is representative of the gross sample or
the sub-period sample3.8
test sample
cigarettes for test taken at random from the laboratory sample (3.6) and which are representative of
each of the increments making up the laboratory sample3.9
conditioning sample
cigarettes selected from the test sample (3.7) for conditioning prior to tests
3.10
test portion
group of cigarettes prepared for a single determination and which is a random sample from the test
sample (3.7) or conditioned sample, as appropriate3.11
monitor test piece
cigarette taken from a batch specially fabricated under controlled manufacturing conditions
Note 1 to entry: The cigarettes of such a batch show the greatest possible homogeneity with regard to their
physical and chemical characteristics.4 Principle
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
2 © ISO 2019 – All rights reserved---------------------- Page: 7 ----------------------
ISO 4387:2019(E)
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.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 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 required for the test by randomly selecting cigarettes from the different parts of the
population represented in the laboratory sample.© ISO 2019 – All rights reserved 3
---------------------- Page: 8 ----------------------
ISO 4387:2019(E)
7 Determination of total particular 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;C is a multiplying factor, of value greater than 1, to allow for loss due to damage or selection proce-
dures 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.
NOTE The multiplier C is usually at least 1,2 to provide extra cigarettes in case some are damaged and
for optional tests which are possibly required (see 7.5). If selection by mass or draw resistance (or any other
parameter) is necessary, C is likely to be much larger (experience suggests 2 to 4) depending on the selection
process.The precision normally required generally demands that 80 ≤ N ≤ 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.
Where q is the number of cigarettes smoked into the same trap.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 packetsIf 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/P ≥ C × q, select a test portion by choosing a single packet at random, then randomly select C × q
cigarettes from that packet.4 © ISO 2019 – All rights reserved
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ISO 4387:2019(E)
If Q/P < C × q, select the smallest number of packets (k) as shown in Formula (1):
Qk×≥×Cq (1)
where
Q is the total number of cigarettes available (laboratory sample, see 3.6)
k is the smallest number of packets;
P is the total number of packets of cigarettes available;
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 number of cigarettes smoked into the same trap.
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 (≥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/P ≥ 2C × q and Q/P < 2C × q.
7.2 Marking the butt length7.2.1 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 + 8 mm, 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 might 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 is sufficient.
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ISO 4387:2019(E)
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 might 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 is sufficient.
7.2.4 Butt length to be marked on the cigarettes before conditioningDraw 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 cigarettesIf 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.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 6488.6 © ISO 2019 – All rights reserved
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ISO 4387:2019(E)
7.6 Smoking and collection of particular matter
7.6.1 Smoking plan
Choose a smoking plan. Examples of plans are given in 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 holdersFor 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 3308:2012, 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 smoke traps 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.With the machine warmed up
...
NORME ISO
INTERNATIONALE 4387
Quatrième édition
2019-09
Cigarettes — Détermination de la
teneur en matière particulaire totale
et en 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 4387:2019(F)
ISO 2019
---------------------- Page: 1 ----------------------
ISO 4387:2019(F)
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Publié en Suisse
ii © ISO 2019 – Tous droits réservés
---------------------- Page: 2 ----------------------
ISO 4387:2019(F)
Sommaire Page
Avant‑propos ..............................................................................................................................................................................................................................iv
Introduction ..................................................................................................................................................................................................................................v
1 Domaine d’application ................................................................................................................................................................................... 1
2 Références normatives ................................................................................................................................................................................... 1
3 Termes et définitions ....................................................................................................................................................................................... 1
4 Principe .......................................................................................................................................................................................................................... 3
5 Appareillage .............................................................................................................................................................................................................. 3
6 Échantillonnage ..................................................................................................................................................................................................... 3
7 Détermination de la teneur en matière particulaire totale ..................................................................................... 4
7.1 Préparation des cigarettes pour le fumage ..................................................................................................................... 4
7.1.1 Généralités ............................................................................................................................................................................ 4
7.1.2 Sélection de prises d’essai à partir de Q cigarettes en vrac ........................................................ 4
7.1.3 Sélection de prises d’essai à partir de P paquets ................................................................................. 4
7.1.4 Duplication des prises d’essai .............................................................................................................................. 5
7.2 Marquage de la longueur du mégot ...................................................................................................................................... 5
7.2.1 Longueur de mégot normalisée .......................................................................................................................... 5
7.2.2 Mesurage de la longueur du filtre ..................................................................................................................... 5
7.2.3 Mesurage de la longueur de la manchette d’assemblage .............................................................. 6
7.2.4 Longueur de mégot à marquer sur les cigarettes avant conditionnement .................... 6
7.3 Sélection des cigarettes ................................................................................................................................................................... 6
7.4 Conditionnement .................................................................................................................................................................................. 6
7.5 Essais préliminaires avant le fumage .................................................................................................................................. 6
7.6 Fumage et collecte de la matière particulaire .............................................................................................................. 7
7.6.1 Plan de fumage .................................................................................................................................................................. 7
7.6.2 Préparation des pièges à fumée et des porte-cigarettes................................................................ 7
7.6.3 Réglage de la machine à fumer ............................................................................................................................ 7
7.6.4 Mode opératoire pour la série de fumage .................................................................................................. 8
7.7 Détermination de la teneur en matière particulaire totale .............................................................................. 9
7.8 Calcul de la masse de la matière particulaire totale ............................................................................................... 9
7.9 Traitement de la matière particulaire totale ................................................................................................................. 9
7.9.1 Mode opératoire d’extraction ............................................................................................................................... 9
7.9.2 Détermination de la teneur en eau ...............................................................................................................10
7.9.3 Détermination de la teneur en nicotine ....................................................................................................10
8 Rapport d’essai ....................................................................................................................................................................................................10
9 Répétabilité et reproductibilité .........................................................................................................................................................12
Annexe A (informative) Plans de fumage ......................................................................................................................................................13
Bibliographie ...........................................................................................................................................................................................................................19
© ISO 2019 – Tous droits réservés iii---------------------- Page: 3 ----------------------
ISO 4387:2019(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 (IEC) en ce qui
concerne la normalisation électrotechnique.Les procédures utilisées pour élaborer le présent document et celles destinées à sa mise à jour sont
décrites dans les Directives ISO/IEC, Partie 1. Il convient, en particulier de prendre note des différents
critères d’approbation requis pour les différents types de documents ISO. Le présent document a été
rédigé conformément aux règles de rédaction données dans les Directives ISO/IEC, Partie 2 (voir www
.iso .org/directives).L’attention est attirée sur le fait que certains des éléments du présent document 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. Les détails concernant
les références aux droits de propriété intellectuelle ou autres droits analogues identifiés lors de
l’élaboration du document sont indiqués dans l’Introduction et/ou dans la liste des déclarations de
brevets reçues par l’ISO (voir www .iso .org/brevets).Les appellations commerciales éventuellement mentionnées dans le présent document sont données
pour information, par souci de commodité, à l’intention des utilisateurs et ne sauraient constituer un
engagement.Pour une explication de la nature volontaire des normes, la signification des termes et expressions
spécifiques de l’ISO liés à l’évaluation de la conformité, ou pour toute information au sujet de l’adhésion
de l’ISO aux principes de l’Organisation mondiale du commerce (OMC) concernant les obstacles
techniques au commerce (OTC), voir le lien suivant: www .iso .org/iso/fr/avant-propos.
Le présent document a été élaboré par le comité technique ISO/TC 126, Tabac et produits du tabac.
Cette quatrième édition annule et remplace la troisième édition (ISO 4387:2000), qui a fait l’objet
d’une révision technique. Elle intègre également les Amendements ISO 4387:2000/Amd.1:2008 et
ISO 4387:2000/Amd.2:2017.La principale modification par rapport à l’édition précédente est la suivante:
— en 7.6.4, le fumage et la collecte de matière particulaire ont été modifiés en intégrant l’énoncé de
l’ISO 8454 dans l’ISO 4387.Il convient que l’utilisateur adresse tout retour d’information ou toute question concernant le présent
document à l’organisme national de normalisation de son pays. Une liste exhaustive desdits organismes
se trouve à l’adresse www .iso .org/fr/members .html.iv © ISO 2019 – Tous droits réservés
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ISO 4387:2019(F)
Introduction
Les cigarettes sont fabriquées en respectant des tolérances strictes s’appuyant sur des modes
opératoires rigoureux de contrôle de la qualité. Toutefois, tous les constituants utilisés dans la
fabrication (tabac, papier à cigarette, manchette d’assemblage, etc.) dérivent de produits naturels, 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. La complexité de cette
composition est accrue par différents processus de vieillissement, accompagnés d’effets de diffusion et
d’intersolubilité, qui prennent effet dès la formation de la fumée.Le mesurage quantitatif 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 s’efforcent de déterminer une valeur pour la MPAEN, diverses méthodes
ont été utilisées. L’expérience démontre toutefois que certains modes opératoires sont plus fiables
que d’autres. C’est en tenant compte de ces facteurs que, durant les années 1988 et 1989, des groupes
d’étude composés 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 de la détermination de la teneur en matière particulaire totale et
anhydre des cigarettes.Il ressort de ces études que des améliorations en répétabilité et reproductibilité sont effectivement
possibles lorsque des limites sont définies au sein du large éventail de méthodes et pratiques autorisées
par les méthodes normalisées existantes. Il en résulte le présent document ainsi que d’autres, qui
forment un ensemble complet couvrant l’échantillonnage, le conditionnement et la détermination de
la teneur en nicotine, en eau et en 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.Le CORESTA a d’abord publié une Norme internationale pour le fumage mécanique de cigarettes
en 1968. Depuis, bien des améliorations ont été proposées tant pour l’équipement d’essai que pour le
mode opératoire.Le présent document inclut ces améliorations et représente donc l’état de la technique en la matière. Il
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.Aucun régime de fumage mécanique ne peut reproduire parfaitement le comportement des fumeurs.
— Il est recommandé que les cigarettes soient aussi soumises à essai sous les conditions d’une différente
intensité de fumage mécanique que celles spécifiées dans le présent document.— L’essai de fumage mécanique permet de caractériser les émissions des cigarettes pour des besoins
de conception et de réglementation, mais communiquer aux fumeurs les résultats de mesures sur
machine peut susciter des malentendus sur les niveaux d’exposition et de risques selon les marques.
— Les données concernant l’émission de fumées obtenues par des mesurages mécaniques peuvent
être utilisées comme des données d’entrée pour l’évaluation des dangers du produit, mais elles ne
constituent pas des mesures valables de l’exposition des individus ou des risques, et ce n’est pas
leur objectif. C’est faire un usage impropre des essais réalisés conformément aux normes ISO que de
communiquer que les différences de mesures mécaniques entre différents produits correspondent
à des différences de niveaux d’exposition ou de risque.© ISO 2019 – Tous droits réservés v
---------------------- Page: 5 ----------------------
NORME INTERNATIONALE ISO 4387:2019(F)
Cigarettes — Détermination de la teneur en matière
particulaire totale et en matière particulaire anhydre et
exempte de nicotine au moyen d'une machine à fumer
analytique de routine
1 Domaine d’application
Le présent document spécifie des méthodes de détermination de la teneur en matière particulaire totale
et de détermination ultérieure de la teneur en 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 suivants sont cités dans le texte de sorte qu’ils constituent, pour tout ou partie de leur
contenu, des exigences du présent document. Pour les références datées, seule l’édition citée s’applique.
Pour les références non datées, la dernière édition du document de référence s’applique (y compris les
éventuels amendements).ISO 2971, Cigarettes et bâtonnets-filtres — Détermination du diamètre nominal — Méthode utilisant un
instrument de mesure optique sans contactISO 3308, Machine à fumer analytique de routine pour cigarettes — Définitions et conditions normalisées
ISO 3402, Tabac et produits du tabac — Atmosphère de conditionnement et d'essaiISO 6488, Tabac et produits du tabac — Détermination de la teneur en eau — 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 mesurageISO 8243, Cigarettes — Échantillonnage
ISO 10315, Cigarettes — Dosage de la nicotine dans les condensats de fumée — Méthode par
chromatographie en phase gazeuseISO 10362-1, Cigarettes — Dosage de l'eau dans la matière particulaire totale du courant principal de
fumée — Partie 1: Méthode par chromatographie en phase gazeuseISO 16055, Tabac et produits du tabac — Éprouvette de contrôle — Exigences et utilisation
3 Termes et définitionsPour les besoins du présent document, les termes et définitions suivants s’appliquent.
L’ISO et l’IEC tiennent à jour des bases de données terminologiques destinées à être utilisées en
normalisation, consultables aux adresses suivantes:— ISO Online browsing platform: disponible à l’adresse https: //www .iso .org/obp;
— IEC Electropedia: disponible à l’adresse http: //www .electropedia .org/.© ISO 2019 – Tous droits réservés 1
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ISO 4387:2019(F)
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
Note 1 à l'article: Valeur exprimée en milligrammes par cigarette.
3.2
matière particulaire anhydre
condensat anhydre de fumée
MPA
matière particulaire totale (3.1) après déduction de sa teneur en eau
Note 1 à l'article: Valeur exprimée en milligrammes par cigarette.
3.3
matière particulaire anhydre et exempte de nicotine
condensat de fumée anhydre et exempt de nicotine
MPAEN
matière particulaire anhydre (3.2) après déduction de sa teneur en nicotine
Note 1 à l'article: Valeur exprimée 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
3.5série de fumages
ensemble spécifique d’opérations de fumage (3.4) en vue de produire, à partir d’un échantillon de
cigarettes, la quantité de fumée nécessaire à la détermination des composants de la fumée
3.6bouffée de balayage
toute bouffée tirée après qu’une cigarette ait été éteinte ou retirée du porte-cigarettes
3.7échantillon 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-période3.8
échantillon pour essai
cigarettes pour essai prélevées de façon aléatoire sur l’échantillon pour laboratoire (3.6) et qui sont
représentatives de chacun des échantillons élémentaires constituant ce dernier3.9
échantillon à conditionner
cigarettes sélectionnées à partir de l’échantillon pour essai (3.7) et à conditionner préalablement aux essais
3.10prise d’essai
ensemble de cigarettes préparées pour une détermination unique et qui est prélevé de façon aléatoire
sur l’échantillon pour essai (3.7) ou l’échantillon conditionné, selon ce qui est approprié
3.11éprouvette de contrôle
cigarette prélevée sur un lot spécialement fabriqué dans des conditions de production contrôlées
Note 1 à l'article: Les cigarettes d’un tel lot présentent la plus grande homogénéité possible en ce qui concerne
leurs caractéristiques physiques et chimiques.2 © ISO 2019 – Tous droits réservés
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ISO 4387:2019(F)
4 Principe
Les cigarettes pour essai ont été échantillonnées, puis conditionnées. Les cigarettes pour essai sont
fumées sur une machine à fumer automatique avec piégeage simultané de la matière particulaire totale
dans un piège à disque filtrant en fibre de verre. Le cas échéant, la conformité des opérations de fumage
en laboratoire et les modes opératoires analytiques consécutifs sont contrôlés à l’aide des éprouvettes
de contrôle spécifiées dans l’ISO 16055. La masse de matière particulaire totale ainsi obtenue est
déterminée de manière gravimétrique. La matière particulaire totale est extraite du piège en vue de la
détermination de la teneur en eau et en nicotine par chromatographie en phase gazeuse.
5 AppareillageAppareillage 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 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 exigé pour l’essai 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 4387:2019(F)
7 Détermination de la teneur en matière particulaire totale
7.1 Préparation des cigarettes pour le fumage
7.1.1 Généralités
Pour fumer N cigarettes d’un type donné, préparer C × N cigarettes à partir des Q cigarettes disponibles
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 échantillon-
nage à un moment donné ou de sous-période;C est un facteur multiplicatif, d’une valeur supérieure à 1, qui permet de tenir compte des pertes
dues aux cigarettes endommagées, ou résultant des modes opératoires de sélection entre l’échan-
tillonnage 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 teneur en matière particulaire totale.
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 nécessaires
(voir 7.5). Si une sélection selon la masse ou la résistance au tirage (ou tout autre paramètre) est nécessaire,
C sera susceptible d’être beaucoup plus grand (l’expérience suggère 2 à 4), en fonction du mode de sélection.
L’exactitude habituellement exigée nécessite généralement que 80 ≤ N ≤ 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 q cigarettes sont fumées 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.Où q est le nombre de cigarettes fumées sur le même piège.
7.1.2 Sélection de 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, C × N cigarettes doivent y
être prélevées au hasard de telle manière que chaque cigarette ait une probabilité égale d’être choisie.
7.1.3 Sélection de prises d’essai à partir de P paquetsSi l’échantillon pour essai est constitué de P paquets, le mode opératoire de sélection dépend du nombre
de cigarettes par paquet (Q/P) comparé à q.Si Q/P ≥ C × q, constituer chaque prise d’essai en choisissant un paquet au hasard et en prélevant au
hasard C × q cigarettes de ce paquet.4 © ISO 2019 – Tous droits réservés
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ISO 4387:2019(F)
Si Q/P < C × q, sélectionner le plus petit nombre de paquets (k) tel qu’illustré dans la Formule (1):
Qk×≥×Cq (1)
Q est le nombre total de cigarettes disponibles (échantillon pour laboratoire, voir 3.6);
k est le plus petit nombre de paquets;P est le nombre total de paquets de cigarettes disponibles;
C est un facteur multiplicatif, d’une valeur supérieure à 1, qui permet de tenir compte des pertes
dues aux cigarettes endommagées, ou résultant des modes opératoires de sélection entre
l’échantillonnage initial et le fumage;q est le nombre de cigarettes fumées sur le même piège.
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 (≥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/P ≥ 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 est suffisant.
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ISO 4387:2019(F)
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 d’assemblage est bien contrôlée, un nombre de mesurages plus faible
est 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 convient de 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.
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 pour essai doivent être gardés plus de 10 jours
préalablement à leur conditionnement, les conserver dans leur em...
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