CEN/TS 18044:2024

Ambient air - Determination of the concentration of levoglucosan - Chromatographic method

This document specifies a chromatographic method for the determination of levoglucosan in aqueous or organic extracts of filter samples collected in accordance with EN 12341:2023 [5]. The method has been tested for concentrations of ca. 10 ng/m3 up to ca. 3 000 ng/m3 with a sampling duration of 24 h. The procedure is also suitable for the determination of galactosan and mannosan.
Depending on the analysis instrumentation used, the carbohydrates inositol, glycerol, threitol/erythritol, xylitol, arabitol, sorbitol, mannitol, threalose, mannose, glucose, galactose and fructose can also be determined. However, no performance characteristics are given for these compounds in this document.

Außenluft - Bestimmung der Konzentration von Levoglucosan - Chromatographisches Verfahren

Dieses Dokument legt ein chromatographisches Verfahren zur Bestimmung von Levoglucosan in wässrigen oder organischen Extrakten von nach EN 12341:2023 [5] gesammelten Filterproben fest. Das Verfahren wurde für Konzentrationen von etwa 10 ng/m3 bis etwa 3 000 ng/m3 bei einer Probenahmedauer von 24 h geprüft. Das Verfahren ist auch zur Bestimmung von Galactosan und Mannosan geeignet.
Je nach verwendetem Analytikinstrumentarium können auch die Kohlenhydrate Inositol, Glycerol, Threitol/Erythritol, Xylitol, Arabitol, Sorbitol, Mannitol, Threalose, Mannose, Glucose, Galactose und Fructose bestimmt werden. In diesem Dokument werden jedoch keine Leistungskenngrößen für diese Verbindungen angegeben.

Air ambiant - Détermination de la concentration de lévoglucosan - Méthode chromatographique

Le présent document spécifie une méthode chromatographique pour la détermination du lévoglucosan dans des extraits aqueux ou organiques d’échantillons de filtres collectés conformément à l’EN 12341:2023 [5]. La méthode a été soumise à essai pour des concentrations d’environ 10 ng/m3 jusqu’à environ 3 000 ng/m3 avec une durée de prélèvement de 24 h. Le mode opératoire convient également pour la détermination du galactosan et du mannosan.
Selon les instruments d’analyse utilisés, il est également possible de déterminer les hydrates de carbone inositol, glycérol, thréitol/érythritol, xylitol, arabitol, sorbitol, mannitol, tréhalose, mannose, glucose, galactose et fructose. Cependant, le présent document ne spécifie aucune caractéristique de performance pour ces composés.

Zunanji zrak - Določanje koncentracije levoglukozana - Kromatografska metoda

General Information

• Status: Published
• Publication Date: 02-Jul-2024
• ICS: 13.040.20 - Ambient atmospheres
• Technical Committee: CEN/TC 264 - Air quality
• Drafting Committee: CEN/TC 264/WG 21 - Measurement method for B(a)P in Ambient Air
• Current Stage: 6060 - Definitive text made available (DAV) - Publishing
• Start Date: 03-Jul-2024
• Due Date: 03-Dec-2024
• Completion Date: 03-Jul-2024
• Ref Project: kSIST-TS FprCEN/TS 18044:2024 - Ambient air - Determination of the concentration of levoglucosan - Chromatographic method

Standards Content (Sample)

SLOVENSKI STANDARD
01-marec-2024
Zunanji zrak - Določanje koncentracije levoglukozana - Kromatografska metoda
Ambient air - Determination of the concentration of levoglucosan - Chromatographic
method
Außenluft - Bestimmung der Konzentration von Levoglucosan - Chromatographisches
Verfahren
Air ambiant - Détermination de la concentration de lévoglucosan - Méthode
chromatographique
Ta slovenski standard je istoveten z: FprCEN/TS 18044
ICS:
13.040.20 Kakovost okoljskega zraka Ambient atmospheres
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

FINAL DRAFT
TECHNICAL SPECIFICATION
FprCEN/TS 18044
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
January 2024
ICS 13.040.20
English Version
Ambient air - Determination of the concentration of
levoglucosan - Chromatographic method
Air ambiant - Détermination de la concentration de Außenluft - Bestimmung der Konzentration von
lévoglucosan - Méthode chromatographique Levoglucosan - Chromatographisches Verfahren

This draft Technical Specification is submitted to CEN members for Vote. It has been drawn up by the Technical Committee
CEN/TC 264.
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.
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.

Warning : This document is not a Technical Specification. It is distributed for review and comments. It is subject to change
without notice and shall not be referred to as a Technical Specification.

EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2024 CEN All rights of exploitation in any form and by any means reserved Ref. No. FprCEN/TS 18044:2024 E
worldwide for CEN national Members.

FprCEN/TS 18044:2023 (E)
Contents Page
European foreword . 4
Introduction . 5
1 Scope . 6
2 Normative references . 6
3 Terms and definitions . 6
4 Symbols and abbreviations . 6
5 Principle . 7
6 Equipment . 7
6.1 Sampling . 7
6.1.1 Sampling device . 7
6.1.2 Particle filter . 7
6.2 Apparatus for sample preparation . 7
6.3 Analytical equipment . 7
6.3.1 IC-PAD . 7
6.3.2 GC-MS . 8
6.4 Chemicals and accessories . 8
7 Sampling . 9
8 Sample preparation and analysis . 9
8.1 General. 9
8.2 IC-PAD method . 9
8.2.1 Sample preparation . 9
8.2.2 Eluent preparation . 9
8.2.3 Analysis . 9
8.2.4 Calibration . 9
8.3 GC-MS method . 10
8.3.1 Sample preparation . 10
8.3.2 Analysis . 10
8.3.3 Calibration . 10
9 Calculation of results . 10
10 Measurement uncertainty . 11
10.1 General. 11
10.2 Evaluation according to ISO 5725-2 . 11
10.3 Evaluation of laboratory data according to ISO Guide 98-3 . 12
11 Limit of detection and limit of quantification . 13
12 Interferences . 14
12.1 General. 14
12.2 IC-PAD . 14
12.3 GC-MS . 15
13 Quality assurance and quality control . 15
FprCEN/TS 18044:2023 (E)
Annex A (informative) Application examples of the IC-PAD method . 16
Annex B (informative) Application example of the GC-MS method . 28
Annex C (informative) Calculation of the measurement uncertainty using results of a laboratory
intercomparison . 32
Annex D (informative) Possible requirements for the uncertainty of single steps in work up and
analysis for an overall uncertainty of 40 % . 37
Annex E (informative) Calculation of the limit of detection from the calibration function . 39
Annex F (informative) Illustrative chromatograms . 40
Bibliography . 42

FprCEN/TS 18044:2023 (E)
European foreword
This document (FprCEN/TS 18044:2023) has been prepared by Technical Committee CEN/TC 264 “Air
quality”, the secretariat of which is held by DIN.
This document is currently submitted to the Vote on TS.
FprCEN/TS 18044:2023 (E)
Introduction
Emissions from the combustion of biomass (e.g. wood firing) contribute to particulate air pollution (PM ,
PM ). Under inversion weather conditions in winter, the contribution of biomass combustion to the
2,5
particulate load can increase up to 50 % of the PM average daily value. As levoglucosan originates by
pyrolysis of materials containing cellulose, it is a suitable tracer for biomass combustion [1 to 4].
The formation of levoglucosan from cellulose proceeds as follows: The cellulose polymer is thermally
split into oligomers. Conformation change of β-D-glucose units, followed by dehydration leads to
levoglucosan as shown in Figure 1.

Key
1 Conformation change
2 Levoglucosan
3 β-D-Glucose
Figure 1 — Formation of levoglucosan from β-D-glucose
In a similar way, units of galactose and mannose, which also occur in hemicellulose, can be converted to
galactosan and mannosan.
Laboratory-scale wood combustion studies and also estimates derived from ambient air measurements,
can be used to estimate the contribution of biomass combustion to the fine particulate load on the basis
of the levoglucosan concentration. Conversion factors of 8 to 20 were obtained for calculation of the PM
concentration attributable to wood combustion from the levoglucosan concentration.
FprCEN/TS 18044:2023 (E)
1 Scope
This document specifies a chromatographic method for the determination of levoglucosan in aqueous or
organic extracts of filter samples collected in accordance with EN 12341:2023 [5]. The method has been
3 3
tested for concentrations of ca. 10 ng/m up to ca. 3 000 ng/m with a sampling duration of 24 h. The
procedure is also suitable for the determination of galactosan and mannosan.
Depending on the analysis instrumentation used, the carbohydrates inositol, glycerol, threitol/erythritol,
xylitol, arabitol, sorbitol, mannitol, threalose, mannose, glucose, galactose and fructose can also be
determined. However, no performance characteristics are given for these compounds in this document.
2 Normative references
There are no normative references in this document.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— IEC Electropedia: available at https://www.electropedia.org/
— ISO Online browsing platform: available at https://www.iso.org/obp/
3.1
internal standard solution
solution of a known substance of known concentration, added to the sample before chromatographic
analysis
[SOURCE: EN 15549:2008, 3.5 [6]]
3.2
surrogate standard solution
solution of a known substance and of known concentration, used to spike filters before extraction in order
to check the recovery efficiency
[SOURCE: EN 15449:2008, 3.10]
4 Symbols and abbreviations
GC-MS Gas Chromatography – Mass Spectrometry
HPLC-MS High Performance Liquid Chromatography – Mass Spectrometry
IC-PAD Ion Chromatography – Pulsed Amperometric Detection
BSTFA N,O-Bis(trimethylsilyl)trifluoroacetamide
FprCEN/TS 18044:2023 (E)
5 Principle
Fine particulate samples are collected on filters in accordance with EN 12341:2023. Subsamples are
extracted with water (for IC-PAD analysis) or with an organic solvent (e.g. methanol or
methanol/dichloromethane mixtures, for GC-MS analysis). After a method-specific sample preparation
the extract is analysed by IC-PAD or by GC-MS after silylation.
NOTE Levoglucosan can also be analysed by HPLC-MS [7; 8; 9]. This method is not validated.
6 Equipment
6.1 Sampling
6.1.1 Sampling device
A particle sampler equipped with a particle selective sampling head (e.g. for PM and PM ), a filter
10 2,5
holder and a volume regulated pump. Appropriate sampler types are specified in EN 12341:2023. High
volume samplers (sampling volume 700 m /d, filter diameter 150 mm) and low volume samplers
(
...