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

Status
Published
Publication Date
26-May-2020
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
19-May-2020
Due Date
24-Jul-2020
Completion Date
27-May-2020

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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 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
Ta 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.

---------------------- Page: 1 ----------------------
SIST ISO 4387:2020
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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
---------------------- Page: 3 ----------------------
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
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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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SIST ISO 4387:2020
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
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SIST ISO 4387:2020
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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 apparatus

ISO 3308, Routine analytical cigarette-smoking machine — Definitions and standard conditions

ISO 3402, Tobacco and tobacco products — Atmosphere for conditioning and testing

ISO 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 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 use

3 Terms and definitions
For 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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SIST ISO 4387:2020
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 components
3.6
clearing puff

any puff taken after a cigarette has been extinguished or removed from the cigarette holder

3.7
laboratory sample

sample intended for laboratory inspection or testing and which is representative of the gross sample or

the sub-period sample
3.8
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 sample
3.9
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 appropriate
3.11
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
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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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SIST ISO 4387:2020
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 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/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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SIST ISO 4387:2020
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 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 + 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.

© ISO 2019 – All rights reserved 5
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SIST ISO 4387:2020
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 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.

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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SIST ISO 4387:2020
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 holders
For 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
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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.
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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 apparatus

ISO 3308, Routine analytical cigarette-smoking machine — Definitions and standard conditions

ISO 3402, Tobacco and tobacco products — Atmosphere for conditioning and testing

ISO 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 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 use

3 Terms and definitions
For 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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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 components
3.6
clearing puff

any puff taken after a cigarette has been extinguished or removed from the cigarette holder

3.7
laboratory sample

sample intended for laboratory inspection or testing and which is representative of the gross sample or

the sub-period sample
3.8
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 sample
3.9
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 appropriate
3.11
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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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.
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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 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/P ≥ C × q, select a test portion by choosing a single packet at random, then randomly select C × q

cigarettes from that packet.
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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 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 + 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 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.

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.
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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 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 3308:2012, 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)
DOCUMENT PROTÉGÉ PAR COPYRIGHT
© ISO 2019

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publication ne peut être reproduite ni utilisée sous quelque forme que ce soit et par aucun procédé, électronique ou mécanique,

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Publié en Suisse
ii © ISO 2019 – Tous droits réservés
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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

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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
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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 contact

ISO 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'essai

ISO 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 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 la matière particulaire totale du courant principal de

fumée — Partie 1: Méthode par chromatographie en phase gazeuse

ISO 16055, Tabac et produits du tabac — Éprouvette de contrôle — Exigences et utilisation

3 Termes et définitions

Pour 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

3.5
série 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

3.6
bouffée de balayage

toute bouffée tirée après qu’une cigarette ait été éteinte ou retirée du porte-cigarettes

3.7
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
3.8
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 dernier
3.9
échantillon à conditionner

cigarettes sélectionnées à partir de l’échantillon pour essai (3.7) et à conditionner préalablement aux essais

3.10
prise 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

3.11
éprouvette 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.
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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 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 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 paquets

Si 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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