oSIST prEN ISO 24211:2021

Vapour products - Determination of selected carbonyls in vapour product emissions (ISO/DIS 24211:2021)

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/DIS 24211:2021)

Produits de vapotage - Dosage de carbonyles sélectionnés dans les émissions de produits de vapotage (ISO/DIS 24211:2021)

Hlapni proizvodi - Ugotavljanje deleža izbranih karbonilov v emisijah hlapnih proizvodov (ISO/DIS 24211:2021)

General Information

• Status: Not Published
• Public Enquiry End Date: 30-Nov-2021
• ICS: 65.160 - Tobacco, tobacco products and related equipment
• Technical Committee: I13 - Imaginarni 13
• Current Stage: 4020 - Public enquire (PE) (Adopted Project)
• Start Date: 29-Sep-2021
• Due Date: 16-Feb-2022
• Ref Project: prEN ISO 24211 - Vapour products - Determination of selected carbonyls in vapour product emissions (ISO/DIS 24211:2021)

Standards Content (sample)

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

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: [phone]
Email: [e-mail]
Website: www.iso.org
Published in Switzerland
ii © ISO 2021 – All rights reserved
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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.
iv © ISO 2021 – All rights reserved
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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
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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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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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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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

...