SIST EN ISO 24211:2022
(Main)Vapour products - Determination of selected carbonyls in vapour product emissions (ISO 24211:2022)
Vapour products - Determination of selected carbonyls in vapour product emissions (ISO 24211:2022)
This document specifies a method for the determination of selected carbonyl compounds in e-vapor product emissions.
Selected carbonyl compounds are:
• Acetaldehyde
• Formaldehyde
• Acrolein (potentially)
• Crotonaldehyde (potentially)
Dampfprodukte - Bestimmung von ausgewählten Carbonylen in Emissionen von Dampfprodukten (ISO 24211:2022)
Dieses Dokument legt ein Verfahren für die Bestimmung der Menge ausgewählter Carbonylverbindungen (Formaldehyd und Acetaldehyd) als ihre 2,4-Dinitrophenylhydrazine in den Emissionen von Dampfprodukten mittels Umkehrphasen-Flüssigkeitschromatographie in Verbindung mit einem Ultraviolett- oder Diodenarray-Detektor (LC-UV oder LC-DAD) fest.
Die Analyse anderer Carbonylverbindungen wie Acrolein und Crotonaldehyd ist nicht Teil dieses Dokuments, da frühere Arbeiten auf Probleme im Zusammenhang mit der Stabilität dieser Verbindungen in den E Liquid-Lösungen hinwiesen, die zur Bewertung der Leistungsfähigkeit des Verfahrens verwendet wurden [4].
WARNUNG — Mit der Anwendung dieses Dokuments kann der Einsatz gefährlicher Stoffe, Arbeitsgänge und Geräte einhergehen. Dieses Dokument erhebt nicht den Anspruch, alle mit seiner Anwendung einhergehenden Sicherheitsprobleme zu behandeln. Es liegt in der Verantwortung des Anwenders dieses Dokumentes, vor der Anwendung angemessene Maßnahmen in Bezug auf den Gesundheits- und Arbeitsschutz zu ergreifen und die Anwendbarkeit anderer Beschränkungen zu bestimmen.
Produits de vapotage - Dosage de carbonyles sélectionnés dans les émissions de produits de vapotage (ISO 24211:2022)
Le présent document spécifie une méthode de dosage de composés carbonylés sélectionnés (formaldéhyde et acétaldéhyde) sous la forme de leurs 2,4-dinitrophénylhydrazones dans les émissions de produits de vapotage par chromatographie liquide en phase inverse couplée à un détecteur UV ou à barrette de diodes (CL-UV ou CL-DBD).
Le présent document n'inclut pas l'analyse d'autres composés carbonylés, tels que l'acroléine et le crotonaldéhyde, en raison de problèmes d’instabilité de ces composés dans les solutions d’e-liquides qui ont été utilisées pour évaluer la performance de la méthode[4], problèmes signalés lors de travaux antérieurs.
Hlapni proizvodi - Ugotavljanje deleža izbranih karbonilov v emisijah hlapnih proizvodov (ISO 24211:2022)
Ta dokument določa metodo za ugotavljanje deleža izbranih karbonilnih spojin v emisijah e-hlapnih proizvodov.
Izbrane so naslednje karbonilne spojine:
• acetaldehid
• formaldehid
• akrolein (potencialno)
• krotonaldehid (potencialno)
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 24211:2022
01-november-2022
Hlapni proizvodi - Ugotavljanje deleža izbranih karbonilov v emisijah hlapnih
proizvodov (ISO 24211:2022)
Vapour products - Determination of selected carbonyls in vapour product emissions (ISO
24211:2022)
Dampfprodukte - Bestimmung von ausgewählten Carbonylen in Emissionen von
Dampfprodukten (ISO 24211:2022)
Produits de vapotage - Dosage de carbonyles sélectionnés dans les émissions de
produits de vapotage (ISO 24211:2022)
Ta slovenski standard je istoveten z: EN ISO 24211:2022
ICS:
65.160 Tobak, tobačni izdelki in Tobacco, tobacco products
oprema and related equipment
SIST EN ISO 24211:2022 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 24211:2022
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SIST EN ISO 24211:2022
EN ISO 24211
EUROPEAN STANDARD
NORME EUROPÉENNE
September 2022
EUROPÄISCHE NORM
ICS 65.160
English Version
Vapour products - Determination of selected carbonyls in
vapour product emissions (ISO 24211:2022)
Produits de vapotage - Dosage de carbonyles Dampfprodukte - Bestimmung von ausgewählten
sélectionnés dans les émissions de produits de Carbonylen in Emissionen von Dampfprodukten (ISO
vapotage (ISO 24211:2022) 24211:2022)
This European Standard was approved by CEN on 30 August 2022.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 24211:2022 E
worldwide for CEN national Members.
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SIST EN ISO 24211:2022
EN ISO 24211:2022 (E)
Contents Page
European foreword . 3
2
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SIST EN ISO 24211:2022
EN ISO 24211:2022 (E)
European foreword
This document (EN ISO 24211:2022) has been prepared by Technical Committee ISO/TC 126 "Tobacco
and tobacco products" in collaboration with Technical Committee CEN/TC 437 “Electronic cigarettes
and e-liquids” the secretariat of which is held by AFNOR.
This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by March 2023, and conflicting national standards shall
be withdrawn at the latest by March 2023.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
Any feedback and questions on this document should be directed to the users’ national standards
body/national committee. A complete listing of these bodies can be found on the CEN website.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,
Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of
North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and the
United Kingdom.
Endorsement notice
The text of ISO 24211:2022 has been approved by CEN as EN ISO 24211:2022 without any modification.
3
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SIST EN ISO 24211:2022
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SIST EN ISO 24211:2022
INTERNATIONAL ISO
STANDARD 24211
First edition
2022-08
Vapour products — Determination of
selected carbonyls in vapour product
emissions
Produits de vapotage — Dosage de carbonyles sélectionnés dans les
émissions de produits de vapotage
Reference number
ISO 24211:2022(E)
© ISO 2022
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SIST EN ISO 24211:2022
ISO 24211:2022(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2022
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
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Phone: +41 22 749 01 11
Email: copyright@iso.org
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Published in Switzerland
ii
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SIST EN ISO 24211:2022
ISO 24211:2022(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 2
5 Reagents . 2
5.1 General . 2
5.2 Solution preparation . 3
5.3 Preparation of standards . 3
5.3.1 General . 3
5.3.2 HPLC calibration standards and working solutions . 3
5.3.3 Primary carbonyl standards . 3
5.3.4 Secondary carbonyl standards . 4
5.3.5 Carbonyl working standards . 4
6 Apparatus . 4
7 Procedure .5
7.1 Preparation of test samples . 5
7.2 Glass fibre filter pads handling . 5
7.3 Aerosol collection and sample preparation . 5
7.4 Determination of aerosol collected mass (ACM) and e-liquid vaporised mass (EVM) . 6
7.5 Test portion . 6
7.6 Setting up the apparatus . 7
7.7 Calibration of the HPLC system . 8
7.8 Determination . 8
8 Expression of the results .8
9 Repeatability and reproducibility .9
9.1 General . 9
9.2 Results of an interlaboratory study . 9
10 Test report .11
Annex A (informative) DNPH solution (prepared with DNPH containing approximately
30 % water) .12
Annex B (informative) Example of calibration standards preparation .14
Annex C (informative) HPLC chromatogram of a typical aerosol sample containing
carbonyls .15
Bibliography .16
iii
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SIST EN ISO 24211:2022
ISO 24211:2022(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 of 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
www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 126, Tobacco and tobacco products,
Subcommittee SC 3, Vape and vapour products, in collaboration with the European Committee for
Standardization (CEN) Technical Committee CEN/TC 437, Electronic cigarettes and e-liquids, in
accordance with the Agreement on technical cooperation between ISO and CEN (Vienna Agreement).
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
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SIST EN ISO 24211:2022
ISO 24211:2022(E)
Introduction
In many countries, regulation of vapour products requires reporting for carbonyl compounds in
emissions. Therefore, there is a necessity to have an International Standard in place to get reliable/
comparable data for selected carbonyls in vapour product emissions.
[1]
The method in this document is based upon the CORESTA recommended method CRM 96 which was
written on the basis of the results obtained in an interlaboratory study conducted in 2019 involving 11
laboratories.
Carbonyl compounds are known to be derived from the thermal degradation of the base ingredients
[2],[3]
of the e-liquid formulations. The experimental design parameters used to collect the aerosolised
vapour should be evaluated and documented for each analysis.
v
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SIST EN ISO 24211:2022
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SIST EN ISO 24211:2022
INTERNATIONAL STANDARD ISO 24211:2022(E)
Vapour products — Determination of selected carbonyls in
vapour product emissions
WARNING — The use of this document can involve hazardous materials, operations and
equipment. This document does not purport to address all the safety problems associated with
its use. It is the responsibility of the user of this document to establish appropriate safety and
health practices, and determine the applicability of any other restrictions prior to use.
1 Scope
This document specifies a method for the determination of the amount of selected carbonyl compounds
(formaldehyde and acetaldehyde) as their 2,4-dinitrophenylhydrazones in vapour product emissions
using reversed phase liquid chromatography coupled with ultraviolet or diode array detector (LC-UV
or LC-DAD).
This document does not include the analysis of other carbonyl compounds, such as acrolein and
crotonaldehyde, due to previous work indicated issues associated with stability of these compounds in
[4]
the e-liquid solutions that were used to evaluate method performance .
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 3696, Water for analytical laboratory use — Specification and test methods
ISO 20768, Vapour products — Routine analytical vaping machine — Definitions and standard conditions
1)
ISO 24197:— , Vapour products — Determination of e-liquid vaporised mass and aerosol collected mass
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 https:// www .electropedia .org/
3.1
aerosol collected mass
ACM
mass of aerosol collected on a glass fibre filter pad resulting from the operation of a vapour product by
a routine analytical vaping machine after a defined number of puffs
Note 1 to entry: Routine analytical vaping machine is covered by ISO 20768.
1) Under preparation. Stage at the date of publication: ISO/FDIS 24197:2022.
1
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SIST EN ISO 24211:2022
ISO 24211:2022(E)
3.2
e-liquid vaporised mass
EVM
mass of e-liquid transferred from the vapour product to the aerosol
Note 1 to entry: The term “vapour product mass loss” or “mass loss” refers to the e-liquid vaporised mass.
[SOURCE: ISO 24197:—, 3.3]
3.3
puff block
finite series of sequential puffs as defined by the user or by the test request
EXAMPLE Puff block: 1: puffs 1 to 50, puff block 2: puffs 51 to 100, puff block 3: puffs 101 to 150.
3.4
aerosol trapping system
system for collecting the aerosol from vapour products
Note 1 to entry: For this method the aerosol trapping system consists of a filter trap (pad + holder) and an
impinger in series.
3.5
reagent blank
solution that is evaluated to check the level of contamination introduced by the reagents
3.6
aerosol blank
sample from a port that is attached to an aerosol trapping system (3.4) that contains no vapour product
and is carried through the same collection, preparation and analysis steps as the test samples
4 Principle
The vapour product emissions are generated and collected on a vaping machine according to
ISO 20768. The trapping system that is used to trap carbonyls consists of a pad holder containing a
glass fibre filter pad according to ISO 24197, in series with an impinger containing an acidified
solution of 2,4-dinitrophenylhydrazine (DNPH) in 1:1 acetonitrile: water. Post-vaping, the glass fibre
filter pad is combined with the impinger solution and shaken mechanically for 20 min. An aliquot of
the sample extract is subsequently neutralised with pyridine and analysed by reversed phase liquid
chromatography with ultra violet or diode array detector (RPLC-UV or RPLC-DAD). The carbonyl
content in the vapour product emissions is calculated based on an external calibration curve containing
the prederivatized DNPH carbonyl compounds. Results are expressed as the weight of carbonyl per
puff, per aerosol collected mass (ACM) or per puff block as warranted.
5 Reagents
5.1 General
Use only reagents of recognized analytical grade.
NOTE Alternative reagents can be used provided the suitability and equivalence is verified.
5.1.1 Acetonitrile, ACN, HPLC grade.
5.1.2 Ethanol, HPLC grade.
5.1.3 Phosphoric acid, (H PO , a mass fraction of 85 %, or a volume fraction of 10 % aqueous
3 4
solution).
2
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SIST EN ISO 24211:2022
ISO 24211:2022(E)
5.1.4 Water, grade 1 according to ISO 3696 or equivalent.
5.1.5 Pyridine, minimum purity 99 %.
5.1.6 Formaldehyde-DNPH, minimum purity 99 %.
5.1.7 Acetaldehyde-DNPH, minimum purity 99 %.
5.1.8 2,4-Dinitrophenylhydrazine hydrochloride (DNPH-HCL) or 2,4-dinitrophenylhydrazine
(DNPH)(containing approximately 30 % water).
5.2 Solution preparation
5.2.1 General
Prepare appropriately proportioned amounts of the solutions listed below. All solutions shall be
equilibrated to room temperature prior to use. Use graduated cylinders and calibrated pipettes to
combine components.
5.2.2 10 % H PO
3 4
Prepare by bringing 118 ml of 85 % H PO (5.1.3) to 1 l water (5.1.4). Vendor prepared 10 % H PO may
3 4 3 4
be used instead. Store at room temperature.
5.2.3 DNPH trapping solution, prepared with DNPH-HCL (5.1.8)
Dissolve 1,0 g DNPH-HCl (5.1.8) in 500 ml of ACN (5.1.1), combine with 40 ml of 10 % H PO (5.2.2) and
3 4
bring to 1 l with water (5.1.4). Mix solution to ensure all the DNPH-HCl dissolves and no crystals remain.
Solution should be prepared fresh weekly, stored at room temperature and protected from light.
NOTE Alternative preparation of trapping solution with DNPH containing 30 % water is provided in Annex A.
5.2.4 Neutralised DNPH trapping solution (if dilutions are required)
Transfer 50 ml of DNPH trapping solution to a suitable size glass bottle and add 2,5 ml of pyridine. Mix
solution thoroughly.
5.3 Preparation of standards
5.3.1 General
All solutions shall be equilibrated to room temperature prior to use.
5.3.2 HPLC calibration standards and working solutions
The calibration should cover the concentration range of interest. Annex B provides a suitable
concentration range that can be used for the analysis, however, it can be adjusted depending on the
level of carbonyls detected in the samples. The user shall ensure the low calibration standard has a
sufficient signal to noise ratio for accurate quantitation (≥10:1) and that the calibration curve is linear.
5.3.3 Primary carbonyl standards
Weigh the hydrazones as described in Annex B into individual 25 ml volumetric flasks and dissolve in
acetonitrile. Record the concentrations of the free aldehyde equivalents in µg/ml.
3
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SIST EN ISO 24211:2022
ISO 24211:2022(E)
5.3.4 Secondary carbonyl standards
Pipette predetermined volumes (see Annex B) of each primary hydrazone standard into a 25 ml
volumetric flask and dilute to the mark with acetonitrile.
NOTE Stock solutions of the individual DNPH derivatized carbonyls can be purchased at the required levels.
5.3.5 Carbonyl working standards
Take appropriate volumes (0,05 ml to 5 ml) of the secondary carbonyl standard (5.3.4) and dilute to
10 ml with acetonitrile to prepare calibration standards with approximate carbonyl concentrations
(see Annex B).
Transfer to auto-sampler vials and cap.
Stability and storage time should be evaluated by the laboratory.
6 Apparatus
Usual laboratory apparatus and, in particular, the following items.
6.1 HPLC system, equipped with UV and/or DAD detector and a suitable data handling system.
6.2 HPLC columns.
— Disposable guard column: Reversed phase (RP) C18, and
— Analytical column: Reversed phase (RP) C18: 4,6 mm x 15 cm, 1,8 µm, or 2,5 µm or equivalent.
6.3 Vaping machine.
The aerosol is generated on a vaping machine, which follows the specifications specified in ISO 20768.
The standard conditions for puff duration and the puff profile are specified in ISO 20768; other
parameters may also be used.
6.4 Aerosol trapping system.
6.4.1 44 mm glass fibre filter pads.
6.4.2 Filter pad holder.
6.4.3 Impingers for trapping emissions from vapour products.
6.4.4 Stem: Bubbler insert.
NOTE A coarse fritted tip impinger has been shown to be fit for purpose, alternative bubble insert can be
used if demonstrated that the trapping efficiency is equivalent.
6.5 Analytical balance, minimum of 1 mg, which can be read to the nearest 0,1 mg.
6.6 Syringe filter (PTFE: 0,45 µm) and disposable syringe.
6.7 Autosampler vials, caps and PTFE faced septa.
4
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SIST EN ISO 24211:2022
ISO 24211:2022(E)
7 Procedure
7.1 Preparation of test samples
All the vapour products to be tested shall be stored according to ISO 20768. Vapour products with
rechargeable batteries shall be fully charged before the test. The aerosols are generated on a vaping
machine which follows the specifications specified in ISO 20768.
7.2 Glass fibre filter pads handling
Glass fibre filter pads shall be stored in the test atmosphere for a minimum of 24 h prior to determination
of pre-testing weights.
For all operations, the operator shall prevent contamination from the fingers by wearing gloves of a
proper material (powder free). Between operations, a glass fibre filter pad holder cap, if available, may
be installed to prevent water loss or uptake. Glass fibre filter pads shall be processed as quickly after
collection as is feasible to prevent uptake or loss of water.
7.3 Aerosol collection and sample preparation
The tested vapour product shall be operated in accordance with the manufacturer recommendations.
Samples shall be collected under the conditions specified in ISO 20768. The vaping machine shall be set
up to collect aerosol onto the glass fibre filter pad connected in series with an impinger (Figure 1).
Add 35 ml of DNPH trapping solution (5.2.3) to a separate impinger with an insert for each sample to be
collected.
Assemble trapping system of the vaping machine in the following order (see Figure 1):
— pre-weighed 44 mm filter pad/holder;
— impinger;
— optional backup filter pad (not included in analysis);
— vaping machine.
Prior to collecting aerosol samples, the trapping system should be evaluated to ensure there are no
leaks in the system and to ensure the puff volume is correct.
— Leak check: To determine whether a leak has occurred in the vaping machine impinger setup, use a
leak tester.
— Puff volume check: Check and adjust the puff volume drawn by the vaping machine at all channels
at the product insertion end of the port with the filter pad/holder and impinger and in line.
5
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SIST EN ISO 24211:2022
ISO 24211:2022(E)
Key
1 e-vapour product
2 pre-weighed 44 mm filter pad/holder
3 glass impinger with 35 ml of DNPH
4 optional backup filter pad (not included in analysis)
5 vaping machine
Figure 1 — Aerosol collection setup for carbonyls analysis
Collect aerosol under standard conditions for aerosol generation as specified in ISO 20768.
Since there is no standard impinger design, trapping efficiency shall be verified when validating this
method. Ensure the end of the bubbler tube is completely submerged in the trapping solution and that
the impinger can adequately hold 35 ml of trapping solution. The trapping system should effectively
trap 95 % of the analytes of interest. To check the trapping efficiency of the method, add an additional
impinger after the impinger and analyse the contents separately according to the method. If less than
5 % of the compounds are detected in the backup impinger, then only one impinger is required to trap
all the carbonyls effectively. Breakthrough or poor trapping efficiency can be due to the size of the
impinger, or bubbler tube or due to products with high carbonyl yields.
7.4 Determination of aerosol collected mass (ACM) and e-liquid vaporised mass (EVM)
Aerosol collected mass (ACM) and e-liquid vaporised mass (EVM) shall be determined gravimetrically
according to ISO 24197.
7.5 Test portion
Post collection, for each glass fibre filter pad, open the holder and remove glass fibre filter pad with
forceps. Fold the pad twice with the aerosol side toward the inside of the folds, being careful to
handle only the edge of the glass fibre filter pad. Wipe the inside of the filter holder with the filter pad
to ensure all residue is captured. Transfer the glass fibre filter pad to a suitable size glass vial with
screw cap. Transfer the entire contents of impinger to the glass vial containing the filter pad and cap.
6
© ISO 2022 – Al
...
SLOVENSKI STANDARD
oSIST prEN ISO 24211:2021
01-november-2021
Hlapni proizvodi - Ugotavljanje deleža izbranih karbonilov v emisijah hlapnih
proizvodov (ISO/DIS 24211:2021)
Vapour products - Determination of selected carbonyls in vapour product emissions
(ISO/DIS 24211:2021)
Dampfprodukte - Bestimmung von ausgewählten Carbonylen in Emissionen von
Dampfprodukten (ISO/DIS 24211:2021)
Produits de vapotage - Dosage de carbonyles sélectionnés dans les émissions de
produits de vapotage (ISO/DIS 24211:2021)
Ta slovenski standard je istoveten z: prEN ISO 24211
ICS:
65.160 Tobak, tobačni izdelki in Tobacco, tobacco products
oprema and related equipment
oSIST prEN ISO 24211:2021 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN ISO 24211:2021
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oSIST prEN ISO 24211:2021
DRAFT INTERNATIONAL STANDARD
ISO/DIS 24211
ISO/TC 126/SC 3 Secretariat: AFNOR
Voting begins on: Voting terminates on:
2021-09-21 2021-12-14
Vapour products — Determination of selected carbonyls in
vapour product emissions
ICS: 65.160
THIS DOCUMENT IS A DRAFT CIRCULATED
This document is circulated as received from the committee secretariat.
FOR COMMENT AND APPROVAL. IT IS
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS
ISO/CEN PARALLEL PROCESSING
BEING ACCEPTABLE FOR INDUSTRIAL,
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 24211:2021(E)
RECIPIENTS OF THIS DRAFT ARE INVITED
TO SUBMIT, WITH THEIR COMMENTS,
NOTIFICATION OF ANY RELEVANT PATENT
RIGHTS OF WHICH THEY ARE AWARE AND TO
©
PROVIDE SUPPORTING DOCUMENTATION. ISO 2021
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oSIST prEN ISO 24211:2021
ISO/DIS 24211:2021(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2021
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oSIST prEN ISO 24211:2021
ISO/DIS 24211:2021(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 2
5 Reagents . 2
6 Apparatus . 3
7 Procedure. 4
7.1 Preparation of test samples . 4
7.2 Glass fibre filter pads handling . 4
7.3 Aerosol collection and sample preparation . 4
7.4 Determination of aerosol collected mass . 6
7.5 Test portion . 6
7.6 Setting up the apparatus. 6
7.7 Calibration of the HPLC system . 7
7.8 Determination . 7
8 Expression of the results . 8
9 Repeatability and reproducibility . 8
10 Test report .10
Annex A (informative) DNPH solution (prepared with DNPH containing approximately
30 % water) .11
Annex B (informative) Example of calibration standards preparation .13
Annex C (informative) HPLC chromatogram of a typical combined carbonyl calibration
standard .14
Bibliography .15
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oSIST prEN ISO 24211:2021
ISO/DIS 24211:2021(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 of 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 www .iso .org/
iso/ foreword .html.
This document was prepared by Technical Committee ISO/TC 126, Tobacco and tobacco products,
Subcommittee SC 3, Vape and vapour products.
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.
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oSIST prEN ISO 24211:2021
ISO/DIS 24211:2021(E)
Introduction
In many countries regulation of vapour products require reporting for carbonyl compounds in
emissions. Therefore, there is a necessity to have an International Standard in place to get reliable/
comparable data for selected carbonyls in vapour product emissions.
[3]
The method in this document is based upon the CORESTA recommended method CRM 96 (Draft)
which was written on the basis of the results obtained in an interlaboratory study conducted in 2019
involving 11 laboratories
Carbonyl compounds are known to be derived from the thermal degradation of the base ingredients
[4][5]
of the e-liquid formulations. Therefore, the experimental design parameters used to collect the
aerosolised vapour should be evaluated and documented for each analysis.
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oSIST prEN ISO 24211:2021
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oSIST prEN ISO 24211:2021
DRAFT INTERNATIONAL STANDARD ISO/DIS 24211:2021(E)
Vapour products — Determination of selected carbonyls in
vapour product emissions
WARNING — The use of this document can involve hazardous materials, operations and
equipment. This document does not purport to address all the safety problems associated with
its use. It is the responsibility of the user of this document to establish appropriate safety and
health practices, and determine the applicability of any other restrictions prior to use.
1 Scope
This document specifies a method for the determination of the amount of selected carbonyl compounds
(formaldehyde and acetaldehyde) as their 2,4-dinitrophenylhydrazones in vapour product emissions
using reversed phase liquid chromatography coupled with Ultraviolet or Diode Array detector (LC-UV
or LC-DAD).
This document does not include the analysis of other carbonyl compounds, such as acrolein and
crotonaldehyde, due to previous work indicated issues associated with stability of these compounds
[6]
and inconsistencies in deliveries of these compounds in emissions from vapour products .
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 20768, Vapour products — Routine analytical vaping machine — Definitions and standard conditions
ISO 24197, Vapour products — Determination of e-liquid vaporised mass and aerosol collected mass
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 https:// www .electropedia .org/
3.1
Aerosol collected mass
ACM
mass of aerosol collected on an aerosol trapping system from the operation of a vapour product by a
routine analytical vaping machine after a defined number of puffs
Note 1 to entry: Routine analytical vaping machine is covered by ISO 20768.
3.2
e-liquid vaporised mass
EVM
Mass of e-liquid transferred from the vapour product to the aerosol
Note 1 to entry: The term “vapour product mass loss” or “mass loss” refers to the e-liquid vaporised mass.
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oSIST prEN ISO 24211:2021
ISO/DIS 24211:2021(E)
3.3
puff block
finite series of sequential puffs
EXAMPLE Puff block: 1: puffs 1 to 50, puff block 2: puffs 51 to 100, puff block 3: puffs 101 to 150.
3.4
aerosol trapping system
system for collecting the aerosol from vapour products
Note 1 to entry: For this method the aerosol trapping system consists of a filter trap (pad + holder) or an impinger
in series
3.5
reagent blank
solution that is evaluated to ensure that no contamination is introduced by the reagents
3.6
aerosol blank
port that is attached to an aerosol trapping system that contains no vapour product and is carried
through the same collection, preparation and analysis steps as the samples
4 Principle
The vapour product emissions are generated and collected on a vaping machine according to
ISO 20768. The trapping system that is used to trap carbonyls consists of a pad holder containing a
Glass fibre filter pad (as specified in ISO 24197) in series with an impinger containing an acidified
solution of 2,4-dinitrophenylhydrazine (DNPH) in 1:1 acetonitrile: water. Post-vaping, the glass fibre
pad is combined with the impinger solution and shaken mechanically for 20 minutes. An aliquot of
the sample extract is subsequently neutralised with pyridine and analysed by reversed phase liquid
chromatography with Ultra Violet or Diode Array detector (LC-UV or LC-DAD). The carbonyl content
in the vapour product emissions is calculated based on an external calibration curve containing the
prederivatized DNPH carbonyl compounds. Results are expressed as the weight of carbonyl per puff,
per aerosol collected mass (ACM) or per puff block as warranted.
5 Reagents
Use only reagents of recognized analytical grade.
5.1 Acetonitrile, ACN, HPLC grade.
5.2 Ethanol, HPLC grade.
5.3 Phosphoric acid, (H PO , a mass fraction of 85 %, or a volume fraction of 10 % Aqueous Solution).
3 4
5.4 Water, HPLC grade or Deionized or equivalent.
5.5 Pyridine, minimum purity 99 %.
5.6 Formaldehyde-DNPH, minimum purity 99 %.
5.7 Acetaldehyde-DNPH, minimum purity 99 %.
5.8 2,4-Dinitrophenylhydrazine Hydrochloride (DNPH-HCL) or 2,4-Dinitrophenylhydrazine
(DNPH)(containing approximately 30 % water).
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oSIST prEN ISO 24211:2021
ISO/DIS 24211:2021(E)
5.9 Solution Preparation: Prepare appropriately proportioned amounts of the solutions listed
below. All solutions must be equilibrated to room temperature prior to use. Use graduated cylinders and
calibrated pipettes to combine components.
5.9.1 10 % H PO
3 4
Prepare by bringing 118 ml of 85 % H PO (5.3) to 1 l water. Vendor prepared 10 % H PO may be used
3 4 3 4
instead. Store at room temperature.
5.9.2 DNPH Trapping solution, prepared with DNPH-HCL (5.8)
Dissolve 1,0 g DNPH-HCl (5.8) in 500 ml of ACN (5.1), combine with 40 ml of 10 % H PO (5.9.1) and
3 4
bring to 1 l with water. Mix solution to ensure all the DNPH-HCl dissolves and no crystals remain.
Solution should be prepared fresh weekly, stored at room temperature and protected from light.
NOTE Alternative preparation of trapping solution with DNPH containing 30 % water is provided in Annex A.
5.9.3 DNPH Neutralised trapping solution (if dilutions are required)
Transfer 50 ml of DNPH trapping solution to a suitable size glass bottle and add 2,5 ml of pyridine. Mix
solution thoroughly.
5.10 Preparation of Standards
All solutions shall be equilibrated to room temperature prior to use.
5.10.1 HPLC calibration standards and working solutions
The calibration should cover the concentration range of interest. Annex B provides a suitable
concentration range that can be used for the analysis, however, it can be adjusted depending on the
level of carbonyls detected in the samples. The user shall ensure the low calibration standard has a
sufficient signal to noise ratio for accurate quantitation (≥10:1) and that the calibration curve is linear.
5.10.2 Primary carbonyl standards
Weigh the hydrazones as described in Annex B into individual 25 ml volumetric flasks and dissolve in
acetonitrile. Record the concentrations of the free aldehyde equivalents in µg/ml.
5.10.3 Secondary carbonyl standards
Pipette predetermined volumes (Annex B) of each primary hydrazone standard into a 25 ml volumetric
flask and dilute to the mark with acetonitrile.
NOTE Stock solutions of the individual DNPH derivatized carbonyls can be purchased at the required levels.
5.10.4 Carbonyl working standards
Take appropriate volumes (0,05 ml to 5 ml) of the secondary carbonyl standard (5.10.3) and dilute to
10 ml with acetonitrile to prepare calibration standards with approximate carbonyl concentrations
(see Annex B).
Transfer to auto-sampler vials and cap.
Stability and storage time should be evaluated by the laboratory.
6 Apparatus
Usual laboratory apparatus and, in particular, the following items.
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oSIST prEN ISO 24211:2021
ISO/DIS 24211:2021(E)
6.1 HPLC system, equipped with UV and/or DAD detector and a suitable data handling system.
6.2 HPLC columns
— Disposable Guard Column: Reversed Phase (RP) C18 and
— Analytical Column: Reversed Phase (RP) C18: 4,6 mm x 15 cm, 1,8 µm, or 2,5 µm or equivalent.
6.3 Vaping machine
The aerosol are generated on a vaping machine, which follows the specifications described in ISO 20768.
The standard conditions for puff duration and the puff profile are describe in ISO 20768, other
parameters may also be used.
6.4 Aerosol trapping system.
6.4.1 44 mm glass fibre filter pads.
6.4.2 Filter pad holder.
6.4.3 Impingers for trapping emissions from vapour products.
6.4.4 Stem: Bubbler insert with course fritted tip.
6.5 Analytical balance, minimum of 1 mg, which can be read to the nearest 0,1 mg.
6.6 Syringe filter (PTFE: 0,45 µm) and disposable syringe.
6.7 Autosampler vials, caps and PTFE faced septa.
7 Procedure
7.1 Preparation of test samples
All the vapour products to be tested shall be stored according to ISO 20768. Vapour products with
rechargeable batteries shall be fully charged before the test. The aerosols are generated on a vaping
...
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