Air quality - Standard method for the measurement of the concentration of benzo[a]pyrene in ambient air

This document describes a measurement method for the determination of particulate Benzo[a]pyrene (B[a]P) in ambient air, which can be used in the framework of the Council Directive 96/62/EC and the Directive 2004/107/EC. This document specifies performance characteristics and performance criteria to which the method shall comply when it is used as reference method.

Luftbeschaffenheit - Messverfahren zur Bestimmung der Konzentration von Benzo[a]pyren in Luft

Dieses Dokument legt ein Messverfahren zur Bestimmung von partikelgebundenem Benzo[a]pyren (BaP) in Luft fest, das im Zusammenhang mit der Richtlinie 96/62/EG [1] und der Richtlinie 2004/107/EG [2] ange¬wendet werden kann. Dieses Dokument legt Verfahrenskenngrößen und Leistungskriterien für das Mess¬verfahren fest, wenn es als Referenzverfahren eingesetzt wird. Die Verfahrenskenngrößen beruhen auf einer Probenahmedauer von 24 h.
Dieses Dokument beschreibt ein Messverfahren, das die Probenahme von BaP als Bestandteil der PM10-Partikel, die Probenextraktion und die Analyse mit Hochleistungs-Flüssigkeitschromatographie (HPLC) in Kombination mit einem Fluoreszenzdetektor (FLD) oder mit Gaschromatographie in Kombination mit massen¬spektro¬metrischer Detektion (GC/MS) umfasst. Das Verfahren ist anwendbar für die Messung von BaP im Konzentrationsbereich von etwa 0,04 ng/m3 bis etwa 20 ng/m3.
Die untere Grenze des Anwendungsbereichs hängt vom Rauschpegel des Detektors und der Streubreite des Laborfilterblindwerts ab.
ANMERKUNG   Falls die BaP-Konzentration den Kalibrierbereich übersteigt, kann der Extrakt verdünnt werden.

Méthode de mesurage de la concentration du benzo [a] pyrene dans l'air ambiant

Le présent document spécifie une méthode de mesure permettant de déterminer la concentration de benzo[a]pyrène (BaP) particulaire dans l’air ambiant, qui peut être utilisée dans le cadre de la Directive 96/62/CE du Conseil [1] et de la Directive 2004/107/CE [2]. Le présent document spécifie des caractéristiques de performance et des critères de performance pour la méthode de mesure lorsque celle-ci est utilisée comme une méthode de référence. Les caractéristiques de performance de la méthode de mesure sont basées sur une période de prélèvement de 24 h.
Le présent document décrit une méthode de mesure comprenant l’échantillonnage du BaP faisant partie intégrante des particules PM10, l’extraction et l’analyse d’échantillons par chromatographie liquide à haute performance (CLHP) avec un détecteur de fluorescence (FLD) ou par chromatographie en phase gazeuse avec détection par spectrométrie de masse (CG/SM). La méthode est applicable au mesurage du BaP dans la plage de concentration comprise approximativement entre 0,04 ng/m3 et 20 ng/m3.
La limite inférieure de la plage applicable dépend du niveau de bruit de fond du détecteur et de la variabilité de la valeur des blancs des filtres de laboratoire.
NOTE   Si la concentration de BaP dépasse la plage d’étalonnage, l’extrait peut être dilué.

Kakovost zraka - Standardna metoda za določevanje koncentracije benzo[a]pirena (B[a]P) v zunanjem zraku

General Information

Status
Published
Publication Date
08-Jun-2008
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
04-Jun-2008
Due Date
09-Aug-2008
Completion Date
09-Jun-2008

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SLOVENSKI STANDARD
SIST EN 15549:2008
01-julij-2008
.DNRYRVW]UDND6WDQGDUGQDPHWRGD]DGRORþHYDQMHNRQFHQWUDFLMHEHQ]R>D@SLUHQD
%>D@3 Y]XQDQMHP]UDNX

Air quality - Standard method for the measurement of the concentration of benzo[a]

pyrene in ambient air
Luftbeschaffenheit - Messverfahren zur Bestimmung der Konzentration von Benzo[a]
pyren in Luft
Méthode de mesurage de la concentration du benzo [a] pyrene dans l'air ambiant
Ta slovenski standard je istoveten z: EN 15549:2008
ICS:
13.040.20 Kakovost okoljskega zraka Ambient atmospheres
SIST EN 15549:2008 en,fr,de

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

---------------------- Page: 1 ----------------------
EUROPEAN STANDARD
EN 15549
NORME EUROPÉENNE
EUROPÄISCHE NORM
March 2008
ICS 13.040.20
English Version
Air quality - Standard method for the measurement of the
concentration of benzo[a]pyrene in ambient air

Qualité de l'air - Méthode normalisée pour le mesurage de Luftbeschaffenheit - Messverfahren zur Bestimmung der

la concentration de benzo[a]pyrène dans l'air ambiant Konzentration von Benzo[a]pyren in Luft

This European Standard was approved by CEN on 2 February 2008.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European

Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national

standards may be obtained on application to the CEN Management Centre or to any CEN member.

This European Standard exists in three official versions (English, French, German). A version in any other language made by translation

under the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as the

official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,

France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,

Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels

© 2008 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 15549:2008: E

worldwide for CEN national Members.
---------------------- Page: 2 ----------------------
EN 15549:2008 (E)
Contents Page

Foreword..............................................................................................................................................................3

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

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

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

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

4 Symbols and abbreviations..................................................................................................................7

5 Principle of the method.........................................................................................................................8

6 Requirements.........................................................................................................................................9

7 Reagents and gases............................................................................................................................11

8 Apparatus .............................................................................................................................................12

9 Sampling...............................................................................................................................................13

10 Sample preparation .............................................................................................................................14

11 Analysis ................................................................................................................................................15

12 Quantification.......................................................................................................................................17

13 Quality control .....................................................................................................................................21

14 Determination of measurement uncertainty .....................................................................................23

15 Interferences ........................................................................................................................................25

16 Reporting of results.............................................................................................................................26

Annex A (informative) Sampling systems ......................................................................................................27

Annex B (informative) Extraction methods (examples of experimental conditions) .................................30

Annex C (informative) Example for clean-up procedure...............................................................................32

Annex D (informative) Parameters for analysis (examples) .........................................................................33

Annex E (informative) Assessment of performance indicators and uncertainty contributions ...............35

Annex F (informative) Results of laboratory and field tests .........................................................................44

Bibliography......................................................................................................................................................50

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EN 15549:2008 (E)
Foreword

This document (EN 15549:2008) has been prepared by Technical Committee CEN/TC 264 “Air quality”, the

secretariat of which is held by DIN.

This European Standard shall be given the status of a national standard, either by publication of an identical

text or by endorsement, at the latest by September 2008, and conflicting national standards shall be

withdrawn at the latest by September 2008.

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.

This document has been prepared under a mandate given to CEN by the European Commission and the

European Free Trade Association, and supports essential requirements of EU Directive(s).

According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following

countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech

Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,

Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain,

Sweden, Switzerland and the United Kingdom.
---------------------- Page: 4 ----------------------
EN 15549:2008 (E)
Introduction

The European Directive 2004/107/EC prescribes the reference methodology for the measurement of

benzo[a]pyrene (BaP) in ambient air and states that the method shall be a method based on manual PM10

sampling systems described in EN 12341 or equivalent.

Hence, this European Standard describes a method in which the sampling systems fulfil this requirement.

However, in the course of drafting this European Standard it became clear that in certain circumstances, in the

presence of oxidants such as ozone, BaP may be degraded. In specific situations this may result in losses of

BaP of > 50 %. It has been shown that the degradation due to ozone can be substantially reduced by

including an ozone denuder in the sampling system.

To date only a limited number of experiments has been performed in order to evaluate the particular

conditions under which the denuder systems can be efficiently used. Consequently, the application of ozone

denuders lacks sufficient validation to be a normative part of this European Standard.

In order to have a complete picture of the performance of ozone denuder systems further information is

required on:
• efficiency under variable atmospheric conditions,
• regeneration time after exposure to high humidity,
• maximum capacity for ozone,
• maximum sample volume and maximum sampling period,
• stability of catalyst,
• maximum period of use,
• particle losses.
Examples of sampling using an ozone denuder are given in Annex A.
The experimental evidence collected so far is presented in Annex F.

It is recommended that further work is undertaken to provide data of BaP comparisons with and without ozone

denuders.
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EN 15549:2008 (E)
1 Scope

This document specifies a measurement method for the determination of particulate benzo[a]pyrene (BaP) in

ambient air, which can be used in the framework of the Council Directive 96/62/EC [1] and the Directive

2004/107/EC [2]. This document specifies performance characteristics and performance criteria for the

measurement method when it is used as a reference method. The performance characteristics of the

measurement method are based on a sampling period of 24 h.

This document describes a measurement method which comprises sampling of BaP as part of the PM10

particles, sample extraction and analysis by high performance liquid chromatography (HPLC) with

fluorescence detector (FLD) or by gas chromatography with mass spectrometric detection (GC/MS). The

method is applicable for the measurement of BaP in the concentration range from approx. 0,04 ng/m to

approximately 20 ng/m .

The lower limit of the applicable range depends on the noise level of the detector and the variability of the

laboratory filter blank.

NOTE If the BaP concentration exceeds the calibration range the extract can be diluted.

2 Normative references

The following referenced documents are indispensable for the application 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 12341:1998, Air quality – Determination of the PM 10 fraction of suspended particulate matter – Reference

method and field test procedure to demonstrate reference equivalence of measurement methods

ENV 13005:1999, Guide to the expression of uncertainty in measurement

ISO 8258, Shewhart control charts (including ISO 8258:1993 Technical Corrigendum 1)

3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
calibration solution

solution used for calibration of the analytical instrument, containing the analyte of interest at a suitable

concentration, prepared by dilution of the stock standard solution
3.2
certified reference material (CRM)

reference material one or more of whose property values are certified by a technically valid procedure,

accompanied by or traceable to a certificate or other documentation that is issued by a certifying body

3.3
external standard solution
solution of the analyte of known concentration
3.4
field blank filter

filter that is taken through the same procedure as a sample, except that no air is drawn through it

3.5
internal standard solution

solution of a known substance of known concentration, added to the sample before chromatographic analysis

---------------------- Page: 6 ----------------------
EN 15549:2008 (E)
3.6
laboratory blank filter

unused filter that does not leave the laboratory and is taken through the same analytical procedure as the

sample
3.7
PM10
target specification for sampling the thoracic particles
[EN 12341:1998]
3.8
reagent blank solution

solution that contains all the reagents used during analysis of the sample, but without the sample and filter

matrix
[EN 14902:2005] [27]
3.9
stock standard solution

solution used for preparing calibration solutions, containing the analyte of interest at a concentration traceable

to national or international standards
3.10
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
3.11
target value

concentration in the ambient air fixed with the aim of avoiding, preventing or reducing harmful effects on

human health and the environment, as a whole, to be attained where possible over a given period

NOTE This definition originates from [2]. The current value for BaP is 1 ng/m for the total content in the PM10

fraction averaged over a calendar year.
3.12
uncertainty (of measurement)

parameter associated with the result of a measurement, that characterises the dispersion of the values that

could reasonably be attributed to the measurand
[ENV 13005:1999]
---------------------- Page: 7 ----------------------
EN 15549:2008 (E)
4 Symbols and abbreviations
4.1 Symbols
a is the slope of linear calibration function;

A is the peak area or peak height of BaP or of its characteristic ion in the chromatogram of the

calibration solution;

A is the peak area or peak height of BaP or of its characteristic ion in the chromatogram of the sample

extract;

A is the peak area or peak height of the internal standard or of its characteristic ion in the chromatogram

of the calibration solution;

A is the peak area or peak height of the internal standard or of its characteristic ion in the chromatogram

ISE
of the sample extract;
b is the intercept of the linear calibration function;
C is the concentration of BaP in ambient air in ng/m³;
D is the detection limit, expressed in ng/m³;
D is the absolute detection limit in the sample in ng;
f is the response factor of BaP;
m is the mean of laboratory filter blanks in ng;
m is the mass of BaP in the calibration solution in ng;
m is the certified mass in the CRM in ng;
CRM
m is the mass of BaP in the sample extract in ng;
m is the mass of BaP on the filter sample in ng;
m is the individual filter blank in ng;
m is the mass of the internal standard in the calibration solution in ng;
m is the mass of the internal standard in the sample extract in ng;
ISE

m is the mass of BaP calculated from the regression equation at the level of the calibration standard in

reg
ng;
m is the mass of the surrogate standard in the sample extract in ng;
SSE
m is the mass of the surrogate standard added to the filter in ng;
SSF
m/z is the mass-to-charge ratio;
---------------------- Page: 8 ----------------------
EN 15549:2008 (E)
n is the number of analysed filters;
R is the recovery efficiency of BaP in %;
R is the peak resolution;
S is the standard deviation of laboratory filter blanks in ng;
lfb

s(m ) is the standard deviation of the replicate measurement results of the mass determined in ng;

t is the sampling time in h;
t is the Student factor for n measurements and a 95 % confidence interval;
n-1;0,95
t is the retention time for peak 1 in min;
t is the retention time for peak 2 in min;
VE is the volume of the extract in ml;
V is the volume of air sampled in m ;
V is the nominal daily sampling volume in m³;
w is the peak width of peak 1 in min;
w is the peak width of peak 2 in min;
X is the measured mass fraction of BaP in mg/kg;
X is the certified mass fraction of BaP in mg/kg.
4.2 Abbreviations
BaP Benzo[a]pyrene
CRM Certified reference material
DAD Diode array detector
FLD Fluorescence detector
GC Gas chromatography
HPLC High performance liquid chromatography
MS Mass spectrometry
5 Principle of the method

The method is divided into two main parts: first the sampling in the field and second the analysis in the

laboratory. During sampling, particles are collected on a filter by sampling a measured volume of air by means

of a sampler equivalent to one of those described in EN 12341.

The sampling time is 24 h. The filter is transported to the laboratory. BaP is extracted using an organic

solvent. If necessary, the extract is cleaned up. The resulting solution is analysed by HPLC/FLD or GC/MS.

---------------------- Page: 9 ----------------------
EN 15549:2008 (E)
6 Requirements
6.1 Siting requirements

Specific siting requirements depend on the objectives of the measurements. For measuring in compliance with

Directive 2004/107/EC then the instructions for siting samplers given in [2] shall be followed.

6.2 Sampling requirements
The sampling system shall be equivalent to EN 12341 (see [2]).

NOTE 1 Equivalence can be demonstrated by performing a side-by-side comparison of the system with a PM10

reference sampler. Guidance for the performance of such comparisons is given in [3].

NOTE 2 In the presence of ozone BaP may degrade. In specific situations this may lead to losses of BaP of > 50 %.

Whenever these effects are expected to be significant, the PM10 sampler may be equipped with an ozone denuder (see

Annex A). The experimental evidence collected so far is presented in Annex F. However, the application of ozone

denuders lacks sufficient validation to be a normative part of this European Standard.

NOTE 3 Examples of sampling systems with and without denuder are presented in Annex A.

6.3 Analysis
6.3.1 Recovery efficiency

Using the external or internal standard method for quantification check the recovery efficiency periodically by

spiking laboratory blank filters with a known amount of BaP and process them as usual. The recovery

efficiency shall be between 80 % and 120 %, otherwise the surrogate standard method shall be used. The

recovery efficiency shall be checked with a frequency to ensure that 95 % probability for a correct

measurement is maintained (see 12.1.1).

Using the surrogate standard method (see 12.1.3) this initial recovery check is not necessary. The surrogate

recovery for field samples shall not be less than 50 %, otherwise the sample shall be discarded.

NOTE 1 If the surrogate recovery is constantly less than 70 %, this indicates problems with the sample preparation

procedure. These problems should be eliminated.

Check the recovery efficiency of the method for BaP in certified reference material (e. g. NIST 1649a) using

equation (1).
R = × 100
(1)
where
R is the recovery efficiency of BaP in %;
X is the measured mass fraction of BaP in mg/kg;
X is the certified mass fraction of BaP in mg/kg.
The recovery efficiency shall be between 80 % and 120 %.

NOTE 2 A certified reference material containing the same matrix as ambient PM10 particles collected on filters is not

available at the moment. Interferences occurring to field samples, e. g. chemical reactions of BaP during extraction, can

be identified, for example, by

• Repeating the extraction step with a different method and comparing the results;

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EN 15549:2008 (E)

• Comparing the ratio of BaP to at least one more stable and high-boiling PAH like benzo[e]pyrene or

benzo[k]fluoranthene: an indication for problems occurring during the sample preparation procedure is that deviations

(lower ratios) with respect to previous measurements at the same location and in the same season are observed.

Changing the sample preparation procedure (different extraction solvent, different purification procedure) can verify

the problem.
6.3.2 Detection limit
6.3.2.1 General
The detection limit shall be less than 0,04 ng/m³.
6.3.2.2 Determination based on laboratory filter blanks

Determine the detection limit from the standard deviation of at least ten laboratory filter blanks using equation

(2).
(m − m )
∑ i
i=1
S =
(2)
lfb
n−1
where
S is the standard deviation of laboratory filter blanks in ng;
lfb
m is the mean of laboratory filter blanks in ng;
m is the individual filter blank in ng;
n is the number of analysed filters.
The minimal detectable mass of BaP is calculated using equation (3).
D = t × S
(3)
M n−1;0,95 lfb
where
D is the minimal detectable mass of BaP in ng;
t is the Student factor for n measurements and a 95 % confidence interval;
n-1;0,95
S is the standard deviation of laboratory filter blanks in ng.
lfb
6.3.2.3 Determination based on the signal-to-noise ratio

Perform a chromatographic analysis without injecting any solution. Keep the chromatographic parameters as

used for the calibration and the detection of BaP. Calculate the detection limit as three times the average of

the height of the noise at the retention time of BaP ± 10 times the peak width at half peak height at the lowest

calibration level.
6.3.2.4 Calculation of the detection limit

The detection limit, expressed in ng/m³, is calculated introducing the nominal daily sampling volume according

to equation (4).
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EN 15549:2008 (E)
D = (4)
where
D is the detection limit, expressed in ng/m³;
D is the minimal detectable mass of BaP in ng;
V is the nominal daily sampling volume in m³.

For the nominal daily sampling volume data shall be used which are usually obtained during sampling.

NOTE The volume is, for example, approximately 1 630 m³ for the sampler type, which has been used in the field test

(see Annex F.2), or approximately 64 m³ for cuts of 50 mm diameter of the filter samples, collected with this sampler type.

6.4 Oven temperature for HPLC
The temperature of the HPLC column oven shall kept constant to at least ± 1 °C.
7 Reagents and gases
7.1 Solvents

High purity solvents (see 13.1), e.g. toluene, cyclohexane, dichloromethane, acetonitrile and water.

7.2 Gases

Helium (purity 99,999 %) used as carrier gas for GC/MS and for degasification of solvents of the HPLC

method.
7.3 External standard
BaP, e.g. a dilution of the stock standard solution (7.6).
7.4 Internal standard
 Methylated or halogenated PAH, e.g. 6-methylchrysene (for HPLC/FLD);
 deuterated or carbon-13-labelled PAH, e. g. perylene-d12 (for GC/MS).
Make sure that the standards contain less than 1 % (relative) of the native BaP.
7.5 Surrogate standard
 Methylated or halogenated PAH, e.g. 7-methylbenzo[a]pyrene (for HPLC/FLD);
 deuterated or carbon-13-labelled 5-ring PAH, e. g. BaP -d12 (for GC/MS).
Make sure that the standards contain less than 1 % (relative) of the native BaP.
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EN 15549:2008 (E)
7.6 Stock standard solution

Dilution of a solution of BaP with a concentration traceable to internationally accepted standards, e.g. NIST

1647e.
7.7 Certified reference material

Containing a certified concentration of BaP, in a matrix similar to PM 10 particles, e.g. NIST 1649a.

8 Apparatus
8.1 Sampling equipment
8.1.1 PM10 sampler
The sampling system shall be equivalent to EN 12341 (see [2]).

8.1.2 Greasing agent, if required, suitable for greasing the sampler impaction plate (see manufacturer's

instructions).

8.1.3 Quartz fibre or glass fibre filters, of a diameter suitable for use with the samplers (8.1.1), with a

separation efficiency of at least 99,5 % at an aerodynamic diameter of 0,3 µm. This criterion has also to be

met after pre-treatment of filters according to NOTE 1 in 13.6.
The purity of the filters shall be checked according to 13.7.

NOTE It is recommended that filter manufacturers determine the filter separation efficiency according to standard

methods such as EN 13274-7 [4] or EN 1822-1 [5].

8.1.4 Flow meter, with a measurement uncertainty that is sufficient to enable the volumetric flow rate of

the samplers (8.1.1) to be measured within ± 5 %. The calibration of the flow meter shall be traceable to

internationally accepted standards.
8.2 Sample preparation/extraction
The following apparatus is required:
• round-bottomed flask with reflux condenser; or
• Soxhlet assembly; or
• microwave digestion system; or
• accelerated solvent extraction apparatus; or
• sonication bath.
For examples or details of the procedure see Annex B.
8.3 Laboratory apparatus
8.3.1 HPLC/FLD apparatus

Liquid chromatograph fitted with injection system, a reverse phase column suitable for PAH analysis, a

temperature controlled oven, a pump system and a FLD (see also D.1). Furthermore a system for solvent

degassing (internal or external) is required.
---------------------- Page: 13 ----------------------
EN 15549:2008 (E)

NOTE If the BaP concentration in the extract is high enough a DAD can be used (see 15.2).

8.3.2 GC/MS apparatus

Gas chromatograph with split/splitless injector or on column injector, capillary column suitable for PAH

analysis, and a mass selective detector (see also D.2).
9 Sampling
9.1 Preparation of the equipment before sampling

Consult the manufacturer's instruction manual to determine the minimum voltage and power requirements of

the sampler and ensure that an adequate power supply is available at the sampling site.

Clean the sampler inlet, suction pipe, and all other parts of the sampler, such as filter a change mechanism

and filter cassettes, which may come in contact with the filter before use according to the manufacturer's

specifications. Similarly, inspect greased parts like impaction plates before use, clean them if necessary and

grease them again.

A leak test and flow rate calibration shall be carried out before deploying the sampler in the field in order to

identify problems with the sampler in an early stage.
9.2 Handling of filters

Handle small filters with blunt tweezers, so as to avoid contamination and damage. For large filters this

procedure might not be practicable. In this case handle them carefully using gloves made of an appropriate

material, touching only the outside edges of the filters.
9.3 Preparation of filters

Filters that have visibly been contaminated, e.g. during packing and/or transport shall be rejected.

Inspect each filter before use for pin holes and other imperfections, such as chaffing, loose material,

dislocation and non-uniformity. For example, use a magnifying lens with a light or check in front of an area

light. Reject any filter if its integrity is suspect.

Assign each filter a unique identifier and place it in a labelled, sealed container for storage and transportation

to the field.
NOTE The container should be made of appropriate material (e. g. glass, PTFE).

If the filter has to be marked for identification purposes, do not mark it in an area that will be analysed.

Establish a filter log (i.e. a chain of custody book/record) to document the use of each filter. Record the

number of filters in the filter log. If the sampler to be used is a sequential sampler that operates continuously

for a programmed period, load the required number of filters into a labelled filter cartridge and seal it ready for

transportation to the field. It shall be recorded which filter was located into which position in the cartridge.

Handle laboratory blank filters in the same way as real samples, but do not transport them and do not draw air

through them. Each batch of filters shall be checked before use by analysing one filter (see 13.6).

Prepare field blank filters and process them as far as possible as real samples. Transport them to the

sampling site, mount them into the sampler (without switching on the pump), dismount them, return them to

the laboratory and process them in the same way as real samples. At least one of every twenty filters shall be

analysed as field filter blank. If the field filter blank significantly exceeds the average laboratory filter blank, the

sources of contamination shall be investigated and eliminated. If the results of real samples are significantly

affected by the field filter blank, the samples shall be reanalysed, if possible.

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EN 15549:2008 (E)
9.4 Sample collection and storage

Set up the sampler in the field according to the manufacturer’s instructions, ensuring that the siting

requirements (see 6.1) are met. Then carry out a leak test and check the flow rate of the sampler using the

calibrated flow meter before use and at least every three months, following the manufacturer's instructions. If

the flow rate deviates from its nominal value by more than the deviation given by the manufacturer, calibrate

the sampler by adjusting the flow rate as necessary.

Take field filter blanks periodically at each site (at least once for every twenty filters used for sampling, see

9.3).

Load either an unexposed filter (for single filter devices) or a cartridge of unexposed filters (for sequential

samplers) into the sampler at the start of the sampling period. Program the sampler following the

manufacturer's instructions, start the timer and record the start time.
The sampling time is 24 h.

Collect the filter from the sampler at the end of the sampling period, replace it in its uniquely marked transport

container and seal the container for transportation to the laboratory (for single filter devices). For sequential

samplers, collect the used filters an
...

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