Ambient air - Application of EN 16909 for the determination of elemental carbon (EC) and organic carbon (OC) in PM10 and PMcoarse

This document describes procedures to assess the applicability of the standard method EN 16909 (determination of OC and EC deposited on filters) to particle size fractions up to 10 µm in aerodynamic diameter (50 % cut off).

Außenluft - Anwendung der EN 16909 zur Bestimmung von elementarem Kohlenstoff (EC) und organischem Kohlenstoff (OC) in PM10 und PMcoarse

Dieses Dokument beschreibt Verfahren zur Einschätzung der Anwendbarkeit des Standardverfahrens EN 16909 (Bestimmung von auf Filtern abgeschiedenen OC und EC) für Korngrößenfraktionen von bis zu 10 μm aerodynamischem Durchmesser (50 % Abscheidegrad).

Air ambiant - Mesurage (ou Détermination) du carbone élémentaire (CE) et du carbone organique (OC) dans les fractions PM10 et grossières

Le présent document décrit les modes opératoires permettant d’évaluer l’applicabilité de la méthode normalisée EN 16909 (dosage du carbone élémentaire et du carbone organique prélevés sur filtre) pour des fractions granulométriques de diamètre aérodynamique allant jusqu’à 10 μm (efficacité de coupure de 50 %).

Zunanji zrak - Uporaba standarda EN 16909 za določevanje elementarnega ogljika (EC) in organskega ogljika (OC) v frakcijah PM10 in grobih delcev

General Information

Status
Published
Public Enquiry End Date
01-Oct-2020
Publication Date
06-Dec-2020
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
23-Nov-2020
Due Date
28-Jan-2021
Completion Date
07-Dec-2020

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SLOVENSKI STANDARD
SIST-TP CEN/TR 17554:2021
01-januar-2021
Zunanji zrak - Uporaba standarda EN 16909 za določevanje elementarnega ogljika
(EC) in organskega ogljika (OC) v frakcijah PM10 in grobih delcev

Ambient air - Application of EN 16909 for the determination of elemental carbon (EC)

and organic carbon (OC) in PM10 and PMcoarse
Außenluft - Anwendung der EN 16909 zur Bestimmung von elementarem Kohlenstoff
(EC) und organischem Kohlenstoff (OC) in PM10 und PMcoarse

Air ambiant - Mesurage (ou Détermination) du carbone élémentaire (CE) et du carbone

organique (OC) dans les fractions PM10 et grossières
Ta slovenski standard je istoveten z: CEN/TR 17554:2020
ICS:
13.040.20 Kakovost okoljskega zraka Ambient atmospheres
SIST-TP CEN/TR 17554:2021 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST-TP CEN/TR 17554:2021
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SIST-TP CEN/TR 17554:2021
CEN/TR 17554
TECHNICAL REPORT
RAPPORT TECHNIQUE
November 2020
TECHNISCHER BERICHT
ICS 13.040.20
English Version
Ambient air - Application of EN 16909 for the
determination of elemental carbon (EC) and organic
carbon (OC) in PM10 and PMcoarse

Air ambiant - Application de la norme EN 16909 pour Außenluft - Anwendung der EN 16909 zur

le dosage du carbone élémentaire (EC) et du carbone Bestimmung von elementarem Kohlenstoff (EC) und

organique (OC) dans les fractions PM10 et PMgrossière organischem Kohlenstoff (OC) in PM10 und PMcoarse

This Technical Report was approved by CEN on 9 November 2020. 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, Turkey 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

© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TR 17554:2020 E

worldwide for CEN national Members.
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Contents Page

European foreword ....................................................................................................................................................... 3

Introduction .................................................................................................................................................................... 4

1 Scope .................................................................................................................................................................... 5

2 Normative references .................................................................................................................................... 5

3 Terms and definitions ................................................................................................................................... 5

4 Symbols and abbreviations ......................................................................................................................... 6

5 Principle ............................................................................................................................................................. 6

6 Previous studies on interferences from inorganic components .................................................... 7

6.1 General ................................................................................................................................................................ 7

6.2 Carbonate carbon ............................................................................................................................................ 7

6.3 Metal oxides ...................................................................................................................................................... 8

6.4 Inorganic salts .................................................................................................................................................. 8

7 Information from the data obtained during the EN 16909 field validation campaigns ........ 9

8 Procedures for evaluating the applicability of EN 16909 to PM and PM ...................... 14

10 coarse

8.1 General ............................................................................................................................................................. 14

8.2 Materials, instruments and analysis ..................................................................................................... 15

8.3 Sampling .......................................................................................................................................................... 15

8.4 Procedures...................................................................................................................................................... 15

8.4.1 General ............................................................................................................................................................. 15

8.4.2 Comparison of OC and EC concentrations in different PM size fractions ................................. 15

9 Assessment of the effect of coarse PM constituents on OC and EC determination ............... 16

9.1 Carbonate carbon ......................................................................................................................................... 16

9.2 Analytical artefacts in PM filter samples spiked with PM constituents that
2,5 coarse

contain no EC or OC ..................................................................................................................................... 16

9.2.1 Spiking material preparation .................................................................................................................. 16

9.2.2 Test sample preparation and measurements .................................................................................... 16

9.2.3 Test evaluation .............................................................................................................................................. 17

9.3 Analytical artefacts in PM filters spiked with known amounts of OC and/or EC .......... 17

coarse

9.3.1 Spiking material preparation .................................................................................................................. 17

9.3.2 Test sample preparation and measurements .................................................................................... 17

9.3.3 Test evaluation .............................................................................................................................................. 17

Annex A (informative) Details of PM and PM filters included in the laboratory
2,5 10

comparison exercise ................................................................................................................................... 18

Annex B (informative) Estimation of the uncertainty of EC and OC ....................................... 19

coarse coarse

Bibliography ................................................................................................................................................................. 20

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European foreword

This document (CEN/TR 17554:2020) has been prepared by Technical Committee CEN/TC 264 “Air

quality”, the secretariat of which is held by DIN.

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent

rights.
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Introduction

The standard method EN 16909 provides guidance for the determination of organic carbon (OC) and

elemental carbon (EC) in airborne particulate matter deposited on filters. It has been developed following

the requirement for the EU member states to measure OC and EC in the PM size fraction (less than 2,5

2,5

μm in aerodynamic diameter) at background sites [5]. EN 16909 standard states: “The same analysis

method may also be used for smaller size fractions than PM . Any possible additional artefacts for larger

2,5

particles, e.g. pyrolysis or higher concentrations of carbonates, should be assessed.”

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1 Scope

This document describes procedures to assess the applicability of the standard method EN 16909

(determination of OC and EC deposited on filters) to particle size fractions up to 10 µm in aerodynamic

diameter (50 % cut off).
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.

EN 16909, Ambient air - Measurement of elemental carbon (EC) and organic carbon (OC) collected on filters

3 Terms and definitions

For the purposes of this document, the terms and definitions given in EN 16909 and the following 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

particulate matter suspended in air which is small enough to pass through a size-selective inlet with a

50 % efficiency cut-off at x µm aerodynamic diameter
[SOURCE: EN 12341:2014 [1], definition 3.1.14]
3.2
PM fraction
coarse
the PM fraction excluding the PM fraction
10 2,5
3.3
organic carbon component of PM
3.4
elemental carbon component of PM
3.5
pyrolytic carbon component of PM
3.6
Total carbon component of PMx
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4 Symbols and abbreviations
TC total carbon
CC carbonate carbon
EC elemental carbon
OC organic carbon
OC organic carbon in spiked samples
OC ambient organic carbon
EC elemental carbon in spiked samples
EC ambient elemental carbon
OC organic carbon in spiked blank filters
EC elemental carbon in spiked blank filters
PC pyrolytic carbon as defined by the thermal-optical method

EBC equivalent black carbon measured by optical absorption at 658 nm within the OC-EC

analyser
CPM calculated PM mass concentration (PM calculated as PM – PM )
coarse coarse coarse 10 2,5
COC calculated OC mass concentration (OC calculated as OC – OC )
coarse coarse coarse 10 2,5
CEC calculated EC mass concentration (EC calculated as EC – EC )
coarse coarse coarse 10 2,5
CPC calculated PC mass concentration (PC calculated as PC – PC )
coarse coarse coarse 10 2,5
CTC calculated TC mass concentration (TC calculated as TC – TC )
coarse coarse coarse 10 2,5

EUSAAR2 thermal-optical analytical protocol for determining OC and EC, from EN 16909

5 Principle

The principle of these procedures is to compare the results of the analytical protocol described in

EN 16909, for the analysis of OC and EC deposited on filters in particulate matter, on samples containing

different amounts of coarse particles (aerodynamic diameter > 2,5 µm) or different amounts of species

that are predominantly in the PM fraction (e.g. sea salt, carbonates, silicates, metal oxides, primary

coarse

biogenic matter). These comparisons aim at determining the range of mass concentrations of possibly

interfering material(s) (or the range of PM mass concentration, as an indicator of those) for which

coarse

EN 16909 is applicable for the determination of OC and EC concentrations in PM or PM deposited

10 coarse
on filters.

Certain procedures in this document make use of ambient aerosol samples of different size fractions that

have been collected simultaneously. They are based on the simple principle that for any PM constituent

(including OC and EC), its concentration in PM shall be less than or equal to its concentration in PM ,

2,5 10

and its concentration in PM10 is equal to the sum of its concentrations in PM2,5 and PMcoarse (within

combined uncertainties).
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Other procedures involve the spiking of loaded filters with well-characterized synthetic or natural

material. OC, EC or OC:EC mixtures can be spiked onto coarse PM filter sample aliquots (punches). The

applicability of EN 16909 is assessed on the recovery of OC and/or EC. Alternatively, species known to be

major constituents of PM but which contain no OC or EC (e. g. sea salt, carbonates, silicates, metal

coarse

oxides) can be spiked on PM ambient filter sample aliquots. In this case, the applicability of EN 16909

2,5

is assessed on the consistency of OC and EC loadings in the spiked and non-spiked aliquots.

A robust estimation of the measurement uncertainties is needed to make it possible to draw conclusions

from these tests.

Considering the diversity of the aerosol particle compositions (both in the coarse and the fine fraction),

the procedures listed in this document can rigorously only give “negative” results (i.e. a conclusion that

EN 16909 is not applicable above a certain level of interfering material). If none of these tests gave

negative results, it could only be stated that there is no evidence that EN 16909 cannot be applied for the

cases that have been tested.
6 Previous studies on interferences from inorganic components
6.1 General

The optically-determined split point between OC and EC in the analysis could be shifted by the presence

of coarse material. This will affect the determination of EC and OC only if the assumptions on PC and EC

absorption cross-sections become invalid, so that the optical correction for charring is inconsistent with

the EC and OC analysis in PM . Certain inorganic compounds might interfere with OC and EC

2,5

determination in this way. These include carbonate carbon, mineral oxides and salts [6]. Carbonates can

evolve during thermal-optical analysis and be detected as either OC or EC. Metal oxides and inorganic

salts can oxidise EC or catalyse EC oxidation in an inert atmosphere [7]. Carbonate carbon, CC is of

primary origin, making usually only a minor contribution to the total carbonaceous matter in the fine

fraction. It has been shown to represent less than 5 % of TC in PM2,5 mass concentration [6]. However, CC

may be an important constituent of PM coarse fractions; e.g. [27] reported high CC concentrations in PM

due to sandstorms (up to 8 % in PM mass concentration in extreme events). Thus, CC interferences in

thermal-optical analysis are more relevant for PM and PM than for PM . Similarly, interferences

10 coarse 2,5

from mineral oxides on the OC and EC determination, typically from soil, are expected to be high in coarse

aerosol particles. Concerning inorganic salts, their effect is relevant for all size fractions because they

have different size distribution patterns. Alkali and alkaline-earth metal salts are mostly found in the

coarse size fraction, while transition metal salts can be present in all particle size modes [8].

6.2 Carbonate carbon

The lack of information regarding CC content of PM samples may significantly affect OC and EC

determination, especially in certain areas (such as sites affected by construction works or resuspended

road dust, or at coastal sites), and/or under specific meteorological conditions, e.g. during desert dust

intrusions. The overestimation of OC or EC due to CC interference might be negligible for fine particulate

matter, since the contribution of CC in PM is usually below 5 % of TC, but it could be significant for PM

2,5 10
or PM fractions if the CC is measured as EC [7].
coarse

The decomposition temperature of carbonate during thermal-optical analysis may vary depending on a

number of factors such as: the chemical composition of the carbonate compound (e.g. CaCO vs.

CaMg(CO ) ), the presence of other minerals (e.g. hematite), the crystal form (e.g. calcite vs. aragonite),

3 2

the grain size, and the temperature protocol used [9]. [10] demonstrated that natural calcite decomposes

at 650 °C in the helium mode of the EUSAAR2 protocol. However, evolution temperatures may vary

substantially depending on the mixture of CC with other materials. For example, the presence of NaCl

decreased the decomposition temperature of dolomite from 735 °C to 560 °C when pure dolomite was

analysed by thermal analysis [11].
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EN 16909 described several methods for the determination of CC in PM samples. Jankowski et al.

2,5

(2008) recommended a thermal treatment of aerosol-loaded filters at 460 °C for 60 min in an O

atmosphere to remove OC and EC, and a subsequent determination of TC. This TC would then be

completely attributed to CC. [10] suggested a separate analysis for CC by directly determining the amount

of CO produced by acidifying the sample. Some researchers ([12], [13], [14]) used acid pretreatment and

infrared spectroscopy measurements to identify CC presence in the sample and fitted a Gaussian function

to the FID signal to determine CC, EC, and OC levels. [9] compared the HCl acidification method, the

manual integration of the sharp peak appearing in the last step of the inert mode of a NIOSH-like protocol,

and the acidification of the sample with phosphoric acid. The peak integration method provided higher

CC concentrations than the acidification method [9], and therefore the determination of CC with an

independent method (e.g. by acidic decomposition of carbonate and subsequent detection of CO ) is

recommended if other parts of the filter are available.
6.3 Metal oxides

The presence of certain minerals in aerosol samples can complicate the optical correction for pyrolysis.

[15] and [16] report that mineral oxides like iron oxide might provide oxygen and oxidize some EC at

high temperatures in the helium mode. For samples that contain large fractions of resuspended soil,

demolition dust, desert dust, sea salt, or samples from sites close to railways, trams, subways, where a

high content of Fe oxides is expected, the split point between OC and EC might be moved relative to the

position when the minerals are not present [17], [18], [19].
6.4 Inorganic salts

The presence of certain elements (Na, K, Pb, Mn, V, Cu, Ni, Co, and Cr), existing either as contaminants in

the filters, or as part of the deposited material, has been shown to catalyse the oxidation of EC at lower

temperatures [20]. Such catalysis would affect the distribution of carbon between the peaks during

thermal-optical analysis.

In the study reported in [21], metal salt particles generated in the laboratory, including alkali (NaCl, KCl,

Na SO ), alkaline-earth (MgCl , CaCl ) and transition metal salts (CuCl , FeCl , FeCl , CuCl, ZnCl , MnCl ,

2 4 2 2 2 2 3 2 2

CuSO , Fe (SO ) ), were deposited on a layer of diesel particles to investigate their effect on EC and OC

4 2 4 3

quantification with thermal-optical analysis using the NIOSH5040 protocol. The measurements showed

that metal salts lowered the split time, reduced the oxidation temperature of EC and enhanced charring.

The split point was more affected by changes in EC oxidation temperature than it was by charring. The

resulting EC/OC ratio was reduced by between 0 % and 80 % in the presence of the salts. Transition

metals were more active than alkali and alkaline-earth metals; copper was the most active. Copper and

iron chlorides were more active than sulphates. The melting point of the metal salts was strongly

correlated with the increase of OC charring, but not with the reduction of EC oxidation temperature. [22]

analysed mixtures of industrial carbon black and NaCl by thermal-optical analysis and concluded that Na

lowers the combustion temperature of EC from 870 °C to approximately 800 °C. An older study [23]

+ +

reported that high concentrations of the ions Na and K in biomass burning aerosol samples catalyse the

combustion of EC material at lower temperatures.

Inorganic constituents that coexist with carbonaceous materials in ambient aerosol samples such as

(NH ) SO and NH HSO can enhance charring of insoluble OC (Yu et al., 2002). Moreover, the presence

4 2 4 4 4

of the oxygen in (NH ) SO could affect the OC and EC concentrations by releasing oxygen in the helium

4 2 4
mode and therefore allowing some of the EC to evolve [22].
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7 Information from the data obtained during the EN 16909 field validation
campaigns

A laboratory comparison exercise was performed during the field tests for the preparation of EN 16909

in order to provide an initial insight on the comparability of EC and OC between PM and PM samples.

2,5 10

The laboratory comparison exercise approach followed the procedure detailed in [24]. Briefly, punches

of 22 high volume filters (11 PM and 11 PM samples taken in parallel), 4 blank filters, one sucrose

10 2,5,

solution and one blank solution were distributed to the four participating laboratories. Filters were

analyzed in duplicate, and solutions in triplicate, applying the EUSAAR2 temperature protocol. Filter

details and gravimetric analysis results are summarized in Annex A. Following ISO 5725-2 [3], 3 Cochran

outliers were identified for TC and 2 Cochran outliers for EC. Outliers were not removed for the later

presentation. The z-scores were calculated for TC and EC according to ISO 5725-2 [3] using values of

standard deviations for proficiency analysis of 5 % and 10 % for TC and EC, respectively. No data were

identified outside the action limits, indicating satisfactory performance for the four laboratories.

Figures 1 to 4 present the pooled results obtained from the averages of duplicate analysis from all

participants, for TC, EC, PC and EBC – as determined by the OC-EC analysers – plotted on PM against

2,5

PM charts. TC and TC are very well correlated (Figure 1), and the regression slope (0,87±0,02)

10 2,5 10

shows that about 87 % of the TC in the PM size fraction belongs to the PM size fraction. Purely optical

10 2,5

measurements (658 nm) of EBC also show a very good correlation between EBC and EBC (Figure 2).

2,5 10

The slope of the regression (0,96±0,02) indicates that 96% of the light absorbing material in PM comes

from PM . This is consistent with the regression between EC and EC (Figure 3) when samples B1 and

2,5 2,5 10

D1 are excluded (slope = 0,96±0,03, R = 0,96). For most samples, there is therefore no immediately

obvious evidence that the optical-thermal method described in the standard EN 16909 cannot accurately

measure EC in PM .

However, the ratio EC /EC (Figure 3) is much less than 0.96 for the measurements on sample B1

2,5 10

obtained by all 4 laboratories, which suggests that thermal-optical analyses have detected as EC in the

PM samples some material that does not absorb visible light (and therefore cannot be EC). The bias in

EC determination could be up to +45 % for the “worst” B1 PM analysis.
10 10

Figure 5 shows a shift in the split point determined in the analysis of B1 PM compared to B1 PM , due

10 2,5

to the fact that from t = 520 s the laser signal increases much faster in the analysis of the PM sample

than for the PM sample. This could result from the presence of material in the coarse fraction leading

2,5

to the oxidation of PC or EC at lower temperatures. The shift of the split point leads to a greater EC value

for the PM sample, probably due to the fact that mainly EC evolves at that time of the analysis while PC

has not totally evolved yet. The optical correction of charring indeed assumes that PC evolves before EC,

or that PC and EC have the same absorption cross-section. These two assumptions are generally not met

[4].

Such an overestimation of EC caused by PC failing to be interpreted as OC was observed in samples

containing primary biological aerosol particles (PBAP). Some PBAPs contain OC that chars and evolves

as EC during thermal-optical analysis [2].

in the B1 samples could also be due to the presence of CC in the coarse fraction,

The overestimation of EC10

which would contribute to the EC peaks without contributing to the laser signal variations. However, the

superposition of B1 PM and PM sample thermograms shows only a slight increase of the EC2 peak in

10 2,5

the PM sample relatively to the PM sample, contributing for about 20 % to the increase of EC

10 2,5 10

compared to EC . Therefore carbonate could account for only a minor fraction of the difference observed

2,5
between EC and EC .
10 2,5

Another analytical artefact is clearly indicated by the determination of nil or negative PC loadings, when

thermograms show that charring actually occurred during the analysis. Negative PC values

2 2

(-0,2 µg/cm to -0,4 µg/cm ) were determined by one of the laboratories in the analysis of PM and PM

2,5 10

sample D2 (Figure 4), and are observed when the split point occurs before the carrier gas shifts from He

to He:O (Figure 6). Negative PC values lead to overestimations of EC. In the particular analysis mentioned

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above, the error in EC determination reached 10 % and 23 % for the PM and the PM D2 samples,

2,5 10

respectively. As a consequence, the greatest negative value of CEC (-0,5 µg/cm ) was found by this

coarse

one laboratory for sample D2. However, this negative value is probably not statistically significant, and

for no sample was EC found consistently negative by all 4 laboratories.
coarse

The results derived from this comparison exercise suggest that potential artefacts may occur during EC

and OC analysis of PM samples with the method described in EN 16909. The impact of these analytical

artefacts on the determination of EC were up to 45 %. However, the samples analysed were limited in

number and could not represent the whole range of air masses experienced across Europe. Additional

field tests are encouraged. Pairs of PM and PM samples selected to represent a wide range of e.g.

10 2,5

mineral dust concentrations should be collected and analysed. In addition to the quantitative evaluation

described in Clause 8, the following questions could be investigated:
1) Evaluation of PC formation and EC pre-combustion in PM and PM
10 2,5
2) Comparison of the various carbon peaks (OC 1-4, EC 1-4) in PM and PM
10 2,5
3) Comparison of the correlation between EBC and EC in PM and PM
10 2,5
Key
X TC , in μg/cm
Y TC , in μg/cm
2,5
B 1 Sample ID
D 1 Sample ID
Figure 1 — TC comparison between PM and PM EUSAAR2 (y = 0,87x – 0,26; R = 0,98)
2,5 10
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CEN/TR 17554:2020 (E)
Key
X EBC in PM10, in μg/cm
Y EBC in PM , in μg/cm
2,5
Figure 2 — EBC comparison between PM and PM (y = 0,96x+0,05; R = 0,99)
2,5 10
Key
X EC PM10, in μg/cm
Y EC PM2,5, in μg/cm
B 1 Sample ID
D 1 Sample ID

Figure 3 — EC comparison between PM and PM (y = 0,96x-0,02; R = 0,96) excluding B 1 and

2,5 10
D1 points, (y = 0,82x+0,18; R = 0,94) including all points.
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Key
X PC10, in μg/cm
Y PC , in μg/cm
2,5
B 1 Sample ID
D 1 Sample ID
Figure 4 — PC comparison between PM and PM EUSAAR2 (y = 0,90x + 0,09; R = 0,71).
2,5 10
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Key
X Time, in s
Y1 FID and laser transmittance signals, in arbitrary units
Y2 Temperature, in ˚C
1 FID, PM2,5 sample, in arbitrary units
2 FID, PM sample, in arbitrary units
3 Laser transmittance, sample PM , in arbitrary units
2,5
4 Laser transmittance, sample PM10, in arbitrary units
5 Split point, PM2,5 sample, in s
6 Split point, PM sample, in s
7 Desired temperature, in ˚C
NOTE FID signals have been scaled to identical calibration peak areas.
Figure 5 — Thermogram of samples B 1 - PM and B 1 - PM
10 2,5.
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Key
X Time, in s
Y1 FID and laser transmittance signals, in arbitrary units
Y2 Temperature, in˚C
1 Laser transmittance, in arbitrary units
2 FID, in arbitrary units
3 Split point, in s
4 Desired temperature, in ˚C
Figure 6 — Thermogram of sample D 2 - PM .
8 Procedures for evaluating the applicability of EN 16909 to PM and PM
10 coarse
8.1 General

The principle of the procedures described below is to determine the conditions (e.g. high concentrations

of species mainly present in the PM fraction) in which EN 16909 cann
...

SLOVENSKI STANDARD
kSIST-TP FprCEN/TR 17554:2020
01-september-2020
Zunanji zrak - Uporaba standarda EN 16909 za določevanje elementarnega ogljika
(EC) in organskega ogljika (OC) v PM10 in grobih frakcijah

Ambient air - Application of EN 16909 for the determination of elemental carbon (EC)

and organic carbon (OC) in PM10 and PMcoarse
Außenluft - Anwendung der EN 16909 zur Bestimmung von elementarem Kohlenstoff
(EC) und organischem Kohlenstoff (OC) in PM10 und PMcoarse

Air ambiant - Mesurage (ou Détermination) du carbone élémentaire (CE) et du carbone

organique (OC) dans les fractions PM10 et grossières
Ta slovenski standard je istoveten z: FprCEN/TR 17554
ICS:
13.040.20 Kakovost okoljskega zraka Ambient atmospheres
kSIST-TP FprCEN/TR 17554:2020 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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kSIST-TP FprCEN/TR 17554:2020
FINAL DRAFT
TECHNICAL REPORT
FprCEN/TR 17554
RAPPORT TECHNIQUE
TECHNISCHER BERICHT
July 2020
ICS
English Version
Ambient air - Application of EN 16909 for the
determination of elemental carbon (EC) and organic
carbon (OC) in PM10 and PMcoarse

Air ambiant - Mesurage (ou Détermination) du carbone Außenluft - Anwendung der EN 16909 zur

élémentaire (CE) et du carbone organique (OC) dans Bestimmung von elementarem Kohlenstoff (EC) und

les fractions PM10 et grossières organischem Kohlenstoff (OC) in PM10 und PMcoarse

This draft Technical Report 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, Turkey 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 Report. It is distributed for review and comments. It is subject to change without

notice and shall not be referred to as a Technical Report.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. FprCEN/TR 17554:2020 E

worldwide for CEN national Members.
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Contents Page

European foreword ....................................................................................................................................................... 3

Introduction .................................................................................................................................................................... 4

1 Scope .................................................................................................................................................................... 5

2 Normative references .................................................................................................................................... 5

3 Terms and definitions ................................................................................................................................... 5

4 Symbols and abbreviations ......................................................................................................................... 6

5 Principle ............................................................................................................................................................. 6

6 Previous studies on interferences from inorganic components .................................................... 7

6.1 General ................................................................................................................................................................ 7

6.2 Carbonate carbon ............................................................................................................................................ 7

6.3 Metal oxides ...................................................................................................................................................... 8

6.4 Inorganic salts .................................................................................................................................................. 8

7 Information from the data obtained during the EN 16909 field validation campaigns ........ 9

8 Procedures for evaluating the applicability of EN 16909 to PM and PM ...................... 14

10 coarse

8.1 General ............................................................................................................................................................. 14

8.2 Materials, instruments and analysis ..................................................................................................... 15

8.3 Sampling .......................................................................................................................................................... 15

8.4 Procedures...................................................................................................................................................... 15

8.4.1 General ............................................................................................................................................................. 15

8.4.2 Comparison of OC and EC concentrations in different PM size fractions ................................. 15

9 Assessment of the effect of coarse PM constituents on OC and EC determination ............... 16

9.1 Carbonate carbon ......................................................................................................................................... 16

9.2 Analytical artefacts in PM filter samples spiked with PM constituents that
2,5 coarse

contain no EC or OC ..................................................................................................................................... 16

9.2.1 Spiking material preparation .................................................................................................................. 16

9.2.2 Test sample preparation and measurements .................................................................................... 16

9.2.3 Test evaluation .............................................................................................................................................. 17

9.3 Analytical artefacts in PM filters spiked with known amounts of OC and/or EC .......... 17

coarse

9.3.1 Spiking material preparation .................................................................................................................. 17

9.3.2 Test sample preparation and measurements .................................................................................... 17

9.3.3 Test evaluation .............................................................................................................................................. 17

Annex A (informative) Details of PM and PM filters included in the laboratory
2,5 10

comparison exercise ................................................................................................................................... 18

Annex B (informative) Estimation of the uncertainty of EC and OC ....................................... 19

coarse coarse

Bibliography ................................................................................................................................................................. 20

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European foreword

This document (FprCEN/TR 17554:2020) 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 TR.
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Introduction

The standard method EN 16909 provides guidance for the determination of organic carbon (OC) and

elemental carbon (EC) in airborne particulate matter deposited on filters. It has been developed following

the requirement for the EU member states to measure OC and EC in the PM size fraction (less than 2,5

2,5

μm in aerodynamic diameter) at background sites [1]. EN 16909 standard states: “The same analysis

method may also be used for smaller size fractions than PM . Any possible additional artefacts for larger

2,5

particles, e.g. pyrolysis or higher concentrations of carbonates, should be assessed.”

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1 Scope

This document describes procedures to assess the applicability of the standard method EN 16909

(determination of OC and EC deposited on filters) to particle size fractions up to 10 µm in aerodynamic

diameter (50 % cut off).
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.

EN 16909, Ambient air - Measurement of elemental carbon (EC) and organic carbon (OC) collected on filters

3 Terms and definitions

For the purposes of this document, the terms and definitions given in EN 16909 and the following 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

particulate matter suspended in air which is small enough to pass through a size-selective inlet with a

50 % efficiency cut-off at x µm aerodynamic diameter
[SOURCE: EN 12341:2014 [27], definition 3.1.14]
3.2
PM fraction
coarse
the PM fraction excluding the PM fraction
10 2,5
3.3
organic carbon component of PM
3.4
elemental carbon component of PM
3.5
pyrolytic carbon component of PM
3.6
Total carbon component of PMx
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4 Symbols and abbreviations
TC total carbon
CC carbonate carbon
EC elemental carbon
OC organic carbon
OC organic carbon in spiked samples
OC ambient organic carbon
EC elemental carbon in spiked samples
EC ambient elemental carbon
OC organic carbon in spiked blank filters
EC elemental carbon in spiked blank filters
PC pyrolytic carbon as defined by the thermal-optical method

EBC equivalent black carbon measured by optical absorption at 658 nm within the OC-EC

analyser
CPM calculated PM mass concentration (PM calculated as PM – PM )
coarse coarse coarse 10 2,5
COC calculated OC mass concentration (OC calculated as OC – OC )
coarse coarse coarse 10 2,5
CEC calculated EC mass concentration (EC calculated as EC – EC )
coarse coarse coarse 10 2,5
CPC calculated PC mass concentration (PC calculated as PC – PC )
coarse coarse coarse 10 2,5
CTC calculated TC mass concentration (TC calculated as TC – TC )
coarse coarse coarse 10 2,5

EUSAAR2 thermal-optical analytical protocol for determining OC and EC, from EN 16909

5 Principle

The principle of these procedures is to compare the results of the analytical protocol described in

EN 16909, for the analysis of OC and EC deposited on filters in particulate matter, on samples containing

different amounts of coarse particles (aerodynamic diameter > 2,5 µm) or different amounts of species

that are predominantly in the PM fraction (e.g. sea salt, carbonates, silicates, metal oxides, primary

coarse

biogenic matter). These comparisons aim at determining the range of mass concentrations of possibly

interfering material(s) (or the range of PM mass concentration, as an indicator of those) for which

coarse

EN 16909 is applicable for the determination of OC and EC concentrations in PM or PM deposited

10 coarse
on filters.

Certain procedures in this document make use of ambient aerosol samples of different size fractions that

have been collected simultaneously. They are based on the simple principle that for any PM constituent

(including OC and EC), its concentration in PM shall be less than or equal to its concentration in PM ,

2,5 10

and its concentration in PM10 is equal to the sum of its concentrations in PM2,5 and PMcoarse (within

combined uncertainties).
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Other procedures involve the spiking of loaded filters with well-characterized synthetic or natural

material. OC, EC or OC:EC mixtures can be spiked onto coarse PM filter sample aliquots (punches). The

applicability of EN 16909 is assessed on the recovery of OC and/or EC. Alternatively, species known to be

major constituents of PM but which contain no OC or EC (e. g. sea salt, carbonates, silicates, metal

coarse

oxides) can be spiked on PM ambient filter sample aliquots. In this case, the applicability of EN 16909

2,5

is assessed on the consistency of OC and EC loadings in the spiked and non-spiked aliquots.

A robust estimation of the measurement uncertainties is needed to make it possible to draw conclusions

from these tests.

Considering the diversity of the aerosol particle compositions (both in the coarse and the fine fraction),

the procedures listed in this document can rigorously only give “negative” results (i.e. a conclusion that

EN 16909 is not applicable above a certain level of interfering material). If none of these tests gave

negative results, it could only be stated that there is no evidence that EN 16909 cannot be applied for the

cases that have been tested.
6 Previous studies on interferences from inorganic components
6.1 General

The optically-determined split point between OC and EC in the analysis could be shifted by the presence

of coarse material. This will affect the determination of EC and OC only if the assumptions on PC and EC

absorption cross-sections become invalid, so that the optical correction for charring is inconsistent with

the EC and OC analysis in PM . Certain inorganic compounds might interfere with OC and EC

2,5

determination in this way. These include carbonate carbon, mineral oxides and salts [2]. Carbonates can

evolve during thermal-optical analysis and be detected as either OC or EC. Metal oxides and inorganic

salts can oxidise EC or catalyse EC oxidation in an inert atmosphere [3]. Carbonate carbon, CC is of

primary origin, making usually only a minor contribution to the total carbonaceous matter in the fine

fraction. It has been shown to represent less than 5 % of TC in PM2,5 mass concentration [2]. However, CC

may be an important constituent of PM coarse fractions; e.g. [26] reported high CC concentrations in PM

due to sandstorms (up to 8 % in PM mass concentration in extreme events). Thus, CC interferences in

thermal-optical analysis are more relevant for PM and PM than for PM . Similarly, interferences

10 coarse 2,5

from mineral oxides on the OC and EC determination, typically from soil, are expected to be high in coarse

aerosol particles. Concerning inorganic salts, their effect is relevant for all size fractions because they

have different size distribution patterns. Alkali and alkaline-earth metal salts are mostly found in the

coarse size fraction, while transition metal salts can be present in all particle size modes [4].

6.2 Carbonate carbon

The lack of information regarding CC content of PM samples may significantly affect OC and EC

determination, especially in certain areas (such as sites affected by construction works or resuspended

road dust, or at coastal sites), and/or under specific meteorological conditions, e.g. during desert dust

intrusions. The overestimation of OC or EC due to CC interference might be negligible for fine particulate

matter, since the contribution of CC in PM is usually below 5 % of TC, but it could be significant for PM

2,5 10
or PM fractions if the CC is measured as EC [2].
coarse

The decomposition temperature of carbonate during thermal-optical analysis may vary depending on a

number of factors such as: the chemical composition of the carbonate compound (e.g. CaCO vs.

CaMg(CO ) ), the presence of other minerals (e.g. hematite), the crystal form (e.g. calcite vs. aragonite),

3 2

the grain size, and the temperature protocol used [5]. [6] demonstrated that natural calcite decomposes

at 650 °C in the helium mode of the EUSAAR2 protocol. However, evolution temperatures may vary

substantially depending on the mixture of CC with other materials. For example, the presence of NaCl

decreased the decomposition temperature of dolomite from 735 °C to 560 °C when pure dolomite was

analysed by thermal analysis [7].
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EN 16909 described several methods for the determination of CC in PM samples. Jankowski et al.

2,5

(2008) recommended a thermal treatment of aerosol-loaded filters at 460 °C for 60 min in an O

atmosphere to remove OC and EC, and a subsequent determination of TC. This TC would then be

completely attributed to CC. [6] suggested a separate analysis for CC by directly determining the amount

of CO produced by acidifying the sample. Some researchers ([8], [9], [10]) used acid pretreatment and

infrared spectroscopy measurements to identify CC presence in the sample and fitted a Gaussian function

to the FID signal to determine CC, EC, and OC levels. [5] compared the HCl acidification method, the

manual integration of the sharp peak appearing in the last step of the inert mode of a NIOSH-like protocol,

and the acidification of the sample with phosphoric acid. The peak integration method provided higher

CC concentrations than the acidification method [5], and therefore the determination of CC with an

independent method (e.g. by acidic decomposition of carbonate and subsequent detection of CO ) is

recommended if other parts of the filter are available.
6.3 Metal oxides

The presence of certain minerals in aerosol samples can complicate the optical correction for pyrolysis.

[11] and [12] report that mineral oxides like iron oxide might provide oxygen and oxidize some EC at

high temperatures in the helium mode. For samples that contain large fractions of resuspended soil,

demolition dust, desert dust, sea salt, or samples from sites close to railways, trams, subways, where a

high content of Fe oxides is expected, the split point between OC and EC might be moved relative to the

position when the minerals are not present [13], [14], [15].
6.4 Inorganic salts

The presence of certain elements (Na, K, Pb, Mn, V, Cu, Ni, Co, and Cr), existing either as contaminants in

the filters, or as part of the deposited material, has been shown to catalyse the oxidation of EC at lower

temperatures [16]. Such catalysis would affect the distribution of carbon between the peaks during

thermal-optical analysis.

In the study reported in [17], metal salt particles generated in the laboratory, including alkali (NaCl, KCl,

Na SO ), alkaline-earth (MgCl , CaCl ) and transition metal salts (CuCl , FeCl , FeCl , CuCl, ZnCl , MnCl ,

2 4 2 2 2 2 3 2 2

CuSO , Fe (SO ) ), were deposited on a layer of diesel particles to investigate their effect on EC and OC

4 2 4 3

quantification with thermal-optical analysis using the NIOSH5040 protocol. The measurements showed

that metal salts lowered the split time, reduced the oxidation temperature of EC and enhanced charring.

The split point was more affected by changes in EC oxidation temperature than it was by charring. The

resulting EC/OC ratio was reduced by between 0 % and 80 % in the presence of the salts. Transition

metals were more active than alkali and alkaline-earth metals; copper was the most active. Copper and

iron chlorides were more active than sulphates. The melting point of the metal salts was strongly

correlated with the increase of OC charring, but not with the reduction of EC oxidation temperature. [18]

analysed mixtures of industrial carbon black and NaCl by thermal-optical analysis and concluded that Na

lowers the combustion temperature of EC from 870 °C to approximately 800 °C. An older study [19]

+ +

reported that high concentrations of the ions Na and K in biomass burning aerosol samples catalyse the

combustion of EC material at lower temperatures.

Inorganic constituents that coexist with carbonaceous materials in ambient aerosol samples such as

(NH ) SO and NH HSO can enhance charring of insoluble OC (Yu et al., 2002). Moreover, the presence

4 2 4 4 4

of the oxygen in (NH ) SO could affect the OC and EC concentrations by releasing oxygen in the helium

4 2 4
mode and therefore allowing some of the EC to evolve [18].
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7 Information from the data obtained during the EN 16909 field validation
campaigns

A laboratory comparison exercise was performed during the field tests for the preparation of EN 16909

in order to provide an initial insight on the comparability of EC and OC between PM and PM samples.

2,5 10

The laboratory comparison exercise approach followed the procedure detailed in [20]. Briefly, punches

of 22 high volume filters (11 PM and 11 PM samples taken in parallel), 4 blank filters, one sucrose

10 2,5,

solution and one blank solution were distributed to the four participating laboratories. Filters were

analyzed in duplicate, and solutions in triplicate, applying the EUSAAR2 temperature protocol. Filter

details and gravimetric analysis results are summarized in Annex A. Following ISO 5725-2 [21], 3 Cochran

outliers were identified for TC and 2 Cochran outliers for EC. Outliers were not removed for the later

presentation. The z-scores were calculated for TC and EC according to ISO 5725-2 [21] using values of

standard deviations for proficiency analysis of 5 % and 10 % for TC and EC, respectively. No data were

identified outside the action limits, indicating satisfactory performance for the four laboratories.

Figures 1 to 4 present the pooled results obtained from the averages of duplicate analysis from all

participants, for TC, EC, PC and EBC – as determined by the OC-EC analysers – plotted on PM against

2,5

PM charts. TC and TC are very well correlated (Figure 1), and the regression slope (0,87±0,02)

10 2,5 10

shows that about 87 % of the TC in the PM size fraction belongs to the PM size fraction. Purely optical

10 2,5

measurements (658 nm) of EBC also show a very good correlation between EBC and EBC (Figure 2).

2,5 10

The slope of the regression (0,96±0,02) indicates that 96% of the light absorbing material in PM comes

from PM . This is consistent with the regression between EC and EC (Figure 3) when samples B1 and

2,5 2,5 10

D1 are excluded (slope = 0,96±0,03, R = 0,96). For most samples, there is therefore no immediately

obvious evidence that the optical-thermal method described in the standard EN 16909 cannot accurately

measure EC in PM .

However, the ratio EC /EC (Figure 3) is much less than 0.96 for the measurements on sample B1

2,5 10

obtained by all 4 laboratories, which suggests that thermal-optical analyses have detected as EC in the

PM samples some material that does not absorb visible light (and therefore cannot be EC). The bias in

EC determination could be up to +45 % for the “worst” B1 PM analysis.
10 10

Figure 5 shows a shift in the split point determined in the analysis of B1 PM compared to B1 PM , due

10 2,5

to the fact that from t = 520 s the laser signal increases much faster in the analysis of the PM sample

than for the PM sample. This could result from the presence of material in the coarse fraction leading

2,5

to the oxidation of PC or EC at lower temperatures. The shift of the split point leads to a greater EC value

for the PM sample, probably due to the fact that mainly EC evolves at that time of the analysis while PC

has not totally evolved yet. The optical correction of charring indeed assumes that PC evolves before EC,

or that PC and EC have the same absorption cross-section. These two assumptions are generally not met

[22].

Such an overestimation of EC caused by PC failing to be interpreted as OC was observed in samples

containing primary biological aerosol particles (PBAP). Some PBAPs contain OC that chars and evolves

as EC during thermal-optical analysis [23].

in the B1 samples could also be due to the presence of CC in the coarse fraction,

The overestimation of EC10

which would contribute to the EC peaks without contributing to the laser signal variations. However, the

superposition of B1 PM and PM sample thermograms shows only a slight increase of the EC2 peak in

10 2,5

the PM sample relatively to the PM sample, contributing for about 20 % to the increase of EC

10 2,5 10

compared to EC . Therefore carbonate could account for only a minor fraction of the difference observed

2,5
between EC and EC .
10 2,5

Another analytical artefact is clearly indicated by the determination of nil or negative PC loadings, when

thermograms show that charring actually occurred during the analysis. Negative PC values

2 2

(-0,2 µg/cm to -0,4 µg/cm ) were determined by one of the laboratories in the analysis of PM and PM

2,5 10

sample D2 (Figure 4), and are observed when the split point occurs before the carrier gas shifts from He

to He:O (Figure 6). Negative PC values lead to overestimations of EC. In the particular analysis mentioned

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above, the error in EC determination reached 10 % and 23 % for the PM and the PM D2 samples,

2,5 10

respectively. As a consequence, the greatest negative value of CEC (-0,5 µg/cm ) was found by this

coarse

one laboratory for sample D2. However, this negative value is probably not statistically significant, and

for no sample was EC found consistently negative by all 4 laboratories.
coarse

The results derived from this comparison exercise suggest that potential artefacts may occur during EC

and OC analysis of PM samples with the method described in EN 16909. The impact of these analytical

artefacts on the determination of EC were up to 45 %. However, the samples analysed were limited in

number and could not represent the whole range of air masses experienced across Europe. Additional

field tests are encouraged. Pairs of PM and PM samples selected to represent a wide range of e.g.

10 2,5

mineral dust concentrations should be collected and analysed. In addition to the quantitative evaluation

described in Clause 8, the following questions could be investigated:
1) Evaluation of PC formation and EC pre-combustion in PM and PM
10 2,5
2) Comparison of the various carbon peaks (OC 1-4, EC 1-4) in PM and PM
10 2,5
3) Comparison of the correlation between EBC and EC in PM and PM
10 2,5
Key
X TC10, in μg/cm
Y TC , in μg/cm
2,5
B 1 Sample ID
D 1 Sample ID
Figure 1 — TC comparison between PM and PM EUSAAR2 (y = 0,87x – 0,26; R = 0,98)
2,5 10
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Key
X EBC in PM10, in μg/cm
Y EBC in PM2,5, in μg/cm
Figure 2 — EBC comparison between PM and PM (y = 0,96x+0,05; R = 0,99)
2,5 10
Key
X EC PM10, in μg/cm
Y EC PM2,5, in μg/cm
B 1 Sample ID
D 1 Sample ID

Figure 3 — EC comparison between PM and PM (y = 0,96x-0,02; R = 0,96) excluding B 1 and

2,5 10
D1 points, (y = 0,82x+0,18; R = 0,94) including all points.
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Key
X PC10, in μg/cm
Y PC2,5, in μg/cm
B 1 Sample ID
D 1 Sample ID
Figure 4 — PC comparison between PM and PM EUSAAR2 (y = 0,90x + 0,09; R = 0,71).
2,5 10
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Key
X Time, in s
Y1 FID and laser transmittance signals, in arbitrary units
Y2 Temperature, in ˚C
1 FID, PM2,5 sample, in arbitrary units
2 FID, PM sample, in arbitrary units
3 Laser transmittance, sample PM , in arbitrary units
2,5
4 Laser transmittance, sample PM10, in arbitrary units
5 Split point, PM2,5 sample, in s
6 Split point, PM sample, in s
7 Desired temperature, in ˚C
NOTE FID signals have been scaled to identical calibration peak areas.
Figure 5 — Thermogram of samples B 1 - PM and B 1 - PM
10 2,5.
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Key
X Time, in s
Y1 FID and laser transmittance signals, in arbitrary units
Y2 Temperature, in˚C
1 Laser transmittance, in arbitrary units
2 FID, in arbitrary units
3 Split point, in s
4 Desired temperature, in ˚C
Figure 6 — Thermogram of sam
...

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