ISO 23919:2020

Cigarettes - Determination of ammonia in cigarette mainstream smoke using ion chromatography

This document specifies a method for the quantification of ammonia by ion chromatography in mainstream smoke using ISO 3308 smoking parameters. This method is applicable to cigarettes with ammonia yields between 1 µg/cigarette and 30 µg/cigarette. It is not applicable for the determination of ammonia in dark-air cured cigarettes.

Cigarettes — Dosage de l'ammoniac dans le courant principal de la fumée de cigarette par chromatographie par échange d’ions

General Information

• Status: Published
• Publication Date: 15-Apr-2020
• ICS: 65.160 - Tobacco, tobacco products and related equipment
• Technical Committee: ISO/TC 126 - Tobacco and tobacco products
• Drafting Committee: ISO/TC 126 - Tobacco and tobacco products
• Current Stage: 9060 - Close of review
• Completion Date: 02-Dec-2030

Relations

• Consolidated By: ISO 6806:2024 - Rubber hoses and hose assemblies for use in oil burners - Specification
• Effective Date: 28-Jan-2023

Overview

ISO 23919:2020 - "Cigarettes - Determination of ammonia in cigarette mainstream smoke using ion chromatography" specifies a validated laboratory method to quantify ammonia in cigarette mainstream smoke. The procedure uses ISO 3308 smoking parameters and ion chromatography analysis. It applies to cigarettes with ammonia yields of 1 µg/cigarette to 30 µg/cigarette and is explicitly not applicable to dark‑air cured cigarettes. The method is based on a CORESTA recommended method (CRM 83) and includes interlaboratory validation and statistical evaluation.

Key topics and technical requirements

• Sampling & smoking regime
  • Machine smoking performed on an ISO 3308–compliant analytical smoking machine.
  • Guidance on tobacco product preparation, sampling and smoking-machine setup.
• Trapping systems (two validated alternatives)
  • Trapping system 1: Glass fibre filter pad followed by series impinger traps containing dilute sulphuric acid.
  • Trapping system 2: Impregnated glass fibre filter pad followed by an untreated glass fibre filter pad.
  • Both systems were shown to give equivalent results in the collaborative study.
• Extraction & analysis
  • Extraction of ammonia from filter pads/impingers using specified dilute acid solutions (sulphuric or hydrochloric).
  • Analysis by ion chromatography with conductivity detection and conductivity suppression.
  • Use of a cation exchange analytical column (example: Dionex IonPac CS16) and external standard calibration.
• Reagents & preparations
  • Includes preparation details for eluents and standards: sulphuric acid eluents, methanesulphonic acid (MSA) eluent, hydrochloric acid impregnation/extraction solutions, and primary ammonium stock from ammonium sulfate.
• Quality and performance
  • Calibration, calculation, and reporting requirements.
  • Repeatability and reproducibility data from a 2015 collaborative study are included.
• Safety note
  • The standard warns about hazardous materials and laboratory safety responsibilities.

Applications and users

ISO 23919:2020 is intended for:

• Analytical laboratories performing tobacco product emission testing.
• Regulatory bodies and standards organizations requiring standardized ammonia emission data.
• Product development and quality control teams in the tobacco industry.
• Research groups studying cigarette smoke chemistry and product hazard assessment.

Practical uses include characterizing ammonia emissions for design, regulatory compliance, method comparison, and controlled laboratory studies. Users should note that machine smoking data are not direct measures of human exposure or risk and should be interpreted accordingly.

Related standards

• ISO 3308 - routine analytical cigarette-smoking machine (definitions & standard conditions)
• ISO 3402 - conditioning and testing atmosphere for tobacco
• ISO 4387 - determination of particulate matter using a routine smoking machine
• ISO 8243 - cigarettes - sampling

Keywords: ISO 23919:2020, ammonia determination, cigarette mainstream smoke, ion chromatography, ISO 3308, trapping system, impinger, impregnated filter pad, analytical method.

Standards Content (Sample)

INTERNATIONAL ISO
STANDARD 23919
First edition
2020-04
Cigarettes — Determination of
ammonia in cigarette mainstream
smoke using ion chromatography
Cigarettes — Dosage de l'ammoniac dans le courant principal de la
fumée de cigarette par chromatographie par échange d’ions
Reference number
©
ISO 2020
© ISO 2020
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: [phone]
Fax: [phone]
Email: [e-mail]
Website: www.iso.org
Published in Switzerland
ii © ISO 2020 – All rights reserved

Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Apparatus . 2
6 Reagents . 2
7 Preparation . 2
7.1 General . 2
7.2 Preparation of solutions . 3
7.2.1 Sulphuric acid, 0,01 M — Impinger solution (trapping system 1) . 3
7.2.2 Sulphuric acid, 0,1 M — Solution C (Ion chromatography eluent) . 3
7.2.3 MSA 0,003 M — Solution A (Ion chromatography eluent) . 3
7.2.4 Sulphuric acid, 0,01 M — Ammonium standards preparation . 3
7.2.5 Hydrochloric acid, 0,05 M — Solution for glass fibre filter pad
impregnation (trapping system 2) . 3
7.2.6 Hydrochloric acid, 0,01 M — Extraction solution (trapping system 2) . 3
7.3 Preparation of standards. 3
7.3.1 Primary ammonium stock solution . 3
7.3.2 Calibration standards . 3
8 Sampling . 4
9 Tobacco product preparation . 4
10 Sample generation — Smoking of cigarettes . 4
10.1 General . 4
10.2 Smoking machine setup . 4
10.2.1 Trapping system 1 — Glass fibre filter pad and impinger traps . 4
10.2.2 Trapping system 2 — Impregnated glass fibre filter pad . 5
10.3 Smoking . 6
11 Sample analysis . 6
11.1 Preparation of sample. 6
11.1.1 Extraction of glass fibre filter pad — Trapping system 1 . 6
11.1.2 Extraction of glass fibre filter pad — Trapping system 2 . 6
11.2 Determination . 6
11.2.1 Ion chromatography operating conditions . 6
11.2.2 Calibration . 7
11.2.3 Calculation . 8
12 Repeatability and reproducibility . 8
12.1 General . 8
12.2 Results of the 2015 collaborative study . 9
13 Report . 9
Annex A (informative) Examples of chromatograms .10
Bibliography .11
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.
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 2020 – All rights reserved

Introduction
1)
The CORESTA Smoke Analytes Sub-Group conducted a survey among its members and determined
that most laboratories used a method involving ion chromatography for the determination of ammonia
in cigarette mainstream smoke. Two alternative trapping systems were used, either with a combination
of glass fibre filter pad followed by impinger traps or with an impregnated glass fibre filter pad followed
by a glass fibre filter pad.
[1]
A CORESTA recommended method (CRM) was written on the basis of the results obtained in an
interlaboratory study conducted in 2015 involving 17 laboratories from 8 countries using cigarettes
[2]
manufactured from a range of blend styles . The results demonstrated equivalency of the data
obtained by using both trapping systems. It was observed that the method is not applicable to dark-air
cured blended cigarettes.
This document is based upon the CRM 83 and includes statistical evaluations carried out according to
ISO 5725-1 and ISO 5725-2.
No machine smoking regime can represent all human smoking behaviour.
— 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 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.
1)  Until 2017, the sub-group has been previously known as CORESTA Special Analytes Sub-Group.
INTERNATIONAL STANDARD ISO 23919:2020(E)
Cigarettes — Determination of ammonia in cigarette
mainstream smoke using ion chromatography
WARNING — The use of this document involves 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 quantification of ammonia by ion chromatography in
mainstream smoke using ISO 3308 smoking parameters.
This method is applicable to cigarettes with ammonia yields between 1 µg/cigarette and 30 µg/
cigarette. It is not applicable for the determination of ammonia in dark-air cured cigarettes.
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 3308, Routine analytical cigarette-smoking machine — Definitions and standard conditions
ISO 3402, Tobacco and tobacco products — Atmosphere for conditioning and testing
ISO 4387, Cigarettes — Determination of total and nicotine-free dry particulate matter using a routine
analytical smoking machine
ISO 8243, Cigarettes — Sampling
3 Terms and definitions
No terms and definitions are listed in this document.
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/
4 Principle
Ammonia is collected by passing the mainstream smoke of cigarettes through either
a) a glass fibre filter pad as specified in ISO 3308 followed by impinger traps containing dilute
sulphuric acid (trapping system 1 in the document), or
b) an impregnated glass fibre filter pad followed by an untreated glass fibre filter pad (trapping
system 2 in the document).
The glass fibre filter pad is extracted either with the impinger solutions (trapping system 1) or with
dilute hydrochloric acid (trapping system 2). The obtained solutions are analysed by ion chromatography
using an external standard calibration.
5 Apparatus
The usual laboratory apparatus for use in preparation of samples, solutions and standards and, in
particular, the following.
5.1 Routine analytical cigarette-smoking machine, complying with the requirements of ISO 3308.
5.2 Impinger trapping system, capable of being connected in series.
5.3 High performance liquid chromatography system, consisting of a conductivity detector and
conductivity suppressor, an eluent degassing unit, a gradient pump, an autosampler with sampling loop
and cooling unit, a data collection system.
TM 2)
5.4 Cation exchange analytical column, e.g. Dionex IonPac CS16 IC or equivalent.
TM 2)
5.5 Disposable guard column, e.g. Dionex IonPac CG16 or equivalent.
5.6 Analytical balance, suitable for measuring to the nearest 0,1 mg.
5.7 Glassware, Erlenmeyer fl
...