SIST EN 15980:2011
(Main)Air quality - Determination of the deposition of benz[a]anthracene, benzo[b]fluoranthene, benzo[j]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, dibenz[a,h]anthracene and indeno[1,2,3-cd]pyrene
Air quality - Determination of the deposition of benz[a]anthracene, benzo[b]fluoranthene, benzo[j]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, dibenz[a,h]anthracene and indeno[1,2,3-cd]pyrene
The Standard specifies methods for the determination of the atmospheric deposition of benz[a]anthracene, benzo[b]fluoranthene, benzo[j]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, indeno[1,2,3-cd]pyrene and dibenz[a,h]anthracene, that can be used in the framework of Council Directive 96/62/EC and Council Directive 2004/107/EC. The Standard specifies performance requirements with which the methods have to comply in order to meet the data quality objectives given in the Directives. Methods for sampling, sample preparation and analysis (GC/MS and (HPLC/FLD) are given. The method is applicable for deposition measurements in rural and remote areas, industrial areas and urban areas.
Luftqualität - Bestimmung der Deposition von Benz[a]anthracen, Benzo[b]fluoranthen, Benzo[j]fluoranthen, Benzo[k]fluoranthen, Benzo[a]pyren, Dibenz[a,h]anthracen und Indeno[1,2,3-cd]pyren
Dieses Dokument legt ein Verfahren zur Bestimmung der Bulk-Deposition von Benz[a]anthracen (BaA),
Benzo[b]fluoranthen (BbF), Benzo[ j ]fluoranthen (BjF), Benzo[k]fluoranthen (BkF), Benzo[a]pyren (BaP),
Dibenz[a,h]anthracen (DBahA) und Indeno[1,2,3-cd]pyren (INP) fest, das im Zusammenhang mit der
Richtlinie 2004/107/EG angewendet werden kann. Diese Europäische Norm legt die Leistungsanforderungen
fest, die das Verfahren erfüllen muss, um die Datenqualitätsziele dieser Richtlinie zu erreichen.
Das vorliegende Dokument legt Verfahren zur Probennahme, Probenaufbereitung und Analyse unter
Anwendung der Gaschromatographie mit massenspektrometrischer Detektion (GC/MS) oder Hochleistungsflüssigkeitschromatographie
mit Fluoreszenzdetektion (HPLC/FLD) fest. Der Bulk-Sammler vom Trichter-
Flasche-Typ ist der Standardsammler.
Das Verfahren ist anwendbar für Depositionsmessungen in
- ländlichen und entlegenen Gebieten;
- Industriegebieten;
- städtischen Gebieten.
Die Norm ist anwendbar im Bereich von einigen ng/(m2 . d) bis zu einigen Hundert ng/(m2 . d).
Qualité de l'air - Détermination du benzo[a]anthracène, benzo[b]fluoranthène, benzo[j]fluoranthène, benzo[k]fluoranthène, benzo[a]pyrène, dibenzo[a,h]anthracène et indeno[1,2,3-cd]pyrène dans les dépôts atmosphériques
Ce document spécifie une méthode de détermination du dépôt atmosphérique de benzo[a]anthracène (BaA), benzo[b]fluoranthène (BbF), benzo[j]fluoranthène (BjF), benzo[k]fluoranthène (BkF), benzo[a]pyrène (BaP), dibenzo[a,h]anthracène (DBahA) et indeno[1,2,3-cd]pyrène (INP), qui peut être utilisée dans le cadre de la Directive 2004/107/CE. La présente Norme européenne spécifie des prescriptions relatives aux performances auxquelles la méthode doit se conformer afin de répondre aux objectifs de qualité des données indiqués dans cette Directive. Les caractéristiques de performance de la méthode ont été déterminées lors d’essais comparatifs de validation sur le terrain réalisés dans quatre régions d’Europe.
Ce document spécifie des méthodes d’échantillonnage, de préparation des échantillons et d’analyse par chromatographie en phase gazeuse avec détection par spectroscopie de masse (CPG/SM) ou par chromatographique liquide à haute performance avec détection par fluorescence (CLHP/FLD).
La méthode s’applique aux mesures de dépôt dans :
- les zones rurales et reculées ;
- les zones industrielles ;
- les zones urbaines.
La norme s’applique dans la plage allant de quelques ng/(m2 d) à quelques centaines de ng/(m2 d).
Kakovost zraka - Določevanje usedanja benzo[a]antracena, benzo[b]fluorantena, benzo[j]fluorantena, benzo[k]fluorantena, benzo[a]pirena, dibenzo[a,h]antracena in indeno[1,2,3-cd]pirena
Standard določa metode za določevanje atmosferskega usedanja benz[a]antracena, benzo[b]fluorantena, benzo[j]fluorantena, benzo[k]fluorantena, benzo[a]pirena, indeno[1,2,3-cd]pirena in dibenz[a,h]antracena, ki se lahko uporabljajo v okviru Direktive Sveta 96/62/ES in Direktive Sveta 2004/107/ES. Ta standard določa zahteve za zmogljivost, ki jim morajo metode ustrezati, da dosegajo cilje kakovosti podatkov, podane v direktivah. Podane so metode za vzorčenje, pripravo in analizo vzorcev (GC/MS in (HPLC/FLD). Metoda velja za meritve usedlin na podeželju in oddaljenih območjih, v industrijskih območjih in v mestnih okoljih.
General Information
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.IOXRUDQWHQDLQGHQR>FG@SLUHQDLuftqualität - Bestimmung der Deposition von Benz[a]anthracen, Benzo[b]fluoranthen, Benzo[j]fluoranthen, Benzo[k]fluoranthen, Benzo[a]pyren, Dibenz[a,h]anthracen und Indeno[1,2,3-cd]pyrenQualité de l'air - Détermination du benzo[a]anthracène, benzo[b]fluoranthène, benzo[j]fluoranthène, benzo[k]fluoranthène, benzo[a]pyrène, dibenzo[a,h]anthracène et indeno[1,2,3-cd]pyrène dans les dépôts atmosphériquesAir quality - Determination of the deposition of benz[a]anthracene, benzo[b]fluoranthene, benzo[j]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, dibenz[a,h]anthracene and indeno[1,2,3-cd]pyrene13.040.01Kakovost zraka na splošnoAir quality in generalICS:Ta slovenski standard je istoveten z:EN 15980:2011SIST EN 15980:2011en,fr,de01-december-2011SIST EN 15980:2011SLOVENSKI
STANDARD
SIST EN 15980:2011
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15980
May 2011 ICS 13.040.01 English Version
Air quality - Determination of the deposition of benz[a]anthracene, benzo[b]fluoranthene, benzo[j]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, dibenz[a,h]anthracene and indeno[1,2,3-cd]pyrene
Qualité de l'air - Détermination du benzo[a]anthracène, benzo[b]fluoranthène, benzo[j]fluoranthène, benzo[k]fluoranthène, benzo[a]pyrène, dibenz[a,h]anthracène et indeno[1,2,3-cd]pyrène dans les dépôts atmosphériques
Luftqualität - Bestimmung der Deposition von Benz[a]anthracen, Benzo[b]fluoranthen, Benzo[j]fluoranthen, Benzo[k]fluoranthen, Benzo[a]pyren, Dibenz[a,h]anthracen und Indeno[1,2,3-cd]pyren This European Standard was approved by CEN on 21 April 2011.
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-CENELEC 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-CENELEC Management Centre has the same status as the official versions.
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, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2011 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15980:2011: ESIST EN 15980:2011
EN 15980:2011 (E) 2 Contents Page Foreword .3Introduction .41Scope .52Normative references .53Terms and definitions .54Symbols and abbreviations .74.1Symbols .74.2Abbreviations .85Principle .96Apparatus, reagents and materials .96.1Reagents .96.2Materials .96.3Sampling equipment .96.4Laboratory equipment . 107Sampling . 107.1General . 107.2Sampling location . 107.3Sampling requirements . 117.4Sample transport . 128Sample preparation and analysis. 128.1Sample storage . 128.2Extraction . 128.3Analysis . 128.4Interferences . 129Quality assurance . 1210Calculation of results . 1311Performance characteristics . 1312Uncertainty . 1413Reporting of results . 14Annex A (informative)
Collectors used in the field trial . 15Annex B (normative)
Work-up of deposition samples for PAH analysis . 19Annex C (normative)
Analytical conditions . 26Annex D (informative)
Performance characteristics determined in laboratory and field tests . 29Annex E (informative)
Relationship between this European Standard and the essential requirements of EU Directives . 43Bibliography . 44 SIST EN 15980:2011
EN 15980:2011 (E) 3 Foreword This document (EN 15980:2011) 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 November 2011, and conflicting national standards shall be withdrawn at the latest by November 2011. 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. 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, Croatia, 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.
SIST EN 15980:2011
EN 15980:2011 (E) 4 Introduction Directive 2004/107/EC [2] requires the measurement of the "total or bulk deposition" of benz[a]anthracene (BaA), benzo[b]fluoranthene (BbF), benzo[j]fluoranthene (BjF), benzo[k]fluoranthene (BkF), benzo[a]pyrene (BaP), dibenz[a,h]anthracene (DBahA) and indeno[1,2,3-cd]pyrene (INP) at background sites, one every
100 000 km². Wet-only sampling may be used instead of bulk sampling if it can be shown that the difference between their results is within 10 %. Where appropriate, monitoring shall be coordinated with the European Monitoring and Evaluation Programme (EMEP). The Directive uses "total deposition" and "bulk deposition" as synonyms and defines it as the total mass of pollutants which is transferred from the atmosphere to surfaces (e.g. soil, vegetation, water, buildings) in a given area within a given time. The considered polycyclic aromatic hydrocarbons (PAH) are predominantly bound to particles. The mass of PAH bound to non sedimenting particles is thought to be low compared to the mass of the compounds bound to sedimenting wet and dry particles. Consequently the sum of the deposition of sedimenting wet and dry particles (defined as "bulk deposition" in this European Standard) and total deposition has been considered as substantially equivalent for the purposes of this document. At sites far enough from obstacles like buildings and trees the influence of specific surface characteristics on the deposition of PAH can be neglected. This document describes the measurement of the deposition of PAH using collectors designed for bulk and wet-only deposition. The validation field test demonstrated that the funnel-bottle bulk collector provided the most reliable and robust results. Therefore this collector type has been chosen as standard collector. SIST EN 15980:2011
EN 15980:2011 (E) 5 1 Scope This document specifies a method for the determination of the bulk deposition of benz[a]anthracene (BaA), benzo[b]fluoranthene (BbF), benzo[j]fluoranthene (BjF), benzo[k]fluoranthene (BkF), benzo[a]pyrene (BaP), dibenz[a,h]anthracene (DBahA) and indeno[1,2,3-cd]pyrene (INP), which can be used in the framework of Directive 2004/107/EC. This European Standard specifies performance requirements with which the method has to comply in order to meet the data quality objectives given in this Directive. This document specifies methods for sampling, sample preparation and analysis using gas chromatography with mass spectroscopic detection (GC/MS) or high performance liquid chromatography with fluorescence detection (HPLC/FLD). The funnel-bottle bulk collector is used as the standard collector. The method is applicable for deposition measurements in rural and remote areas, industrial areas, urban areas. The standard is applicable in the range from a few ng/(m2⋅ d) to a few hundred ng/(m2⋅ d). 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 15549:2008, Air quality — Standard method for the measurement of the concentration of benzo[a]pyrene in ambient air 3 Terms and definitions For the purpose of this document, the following terms and definitions apply. 3.1 analysis all operations carried out after sample preparation to determine the amount or concentration of the polycyclic aromatic hydrocarbons of interest present in the sample 3.2 bulk collector equipment to collect bulk deposition, permanently open to the atmosphere NOTE In this document, two types of bulk collectors are described: a funnel-bottle bulk collector and a cylindrical gauge (Bergerhoff collector). 3.3 bulk deposition sum of the deposition of sedimenting wet and dry particles NOTE Bulk deposition does not contain gases and non-sedimenting particles. The bulk deposition of the polycyclic aromatic hydrocarbons is considered as substantially equivalent to total deposition. SIST EN 15980:2011
EN 15980:2011 (E) 6 3.4 detection limit lowest deposition rate of an analyte detectable using the specified procedure 3.5 expanded uncertainty quantity defining an interval about the result of a measurement that can be expected to encompass a large fraction of the distribution of values that could reasonably be attributed to the measurand [ISO/IEC Guide 98-3:2008 [9]] 3.6 field blank artificial sample (e.g. distilled water) transported to the sampling site, mounted in the sampling unit, but not left exposed to ambient air, returned to the laboratory and worked up in the same way as the deposition sample 3.7 laboratory blank artificial sample (e.g. distilled water) worked up in the same way as the deposition sample in the laboratory 3.8 precipitation rain, snow, sleet, graupel, hail and dew 3.9 sample extraction sample dissolution process to obtain a solution containing the analyte of interest in an organic solvent 3.10 sample preparation all operations carried out on a sample, after transportation and storage, to prepare it for analysis NOTE Such operations are, e.g. extraction, purification, evaporation, solvent exchange. 3.11 standard uncertainty uncertainty of the results of measurements expressed as a standard deviation [ISO/IEC Guide 98-3:2008 [9]] 3.12 uncertainty (of measurement) measurement uncertainty parameter associated with the result of a measurement that characterises the dispersion of the values that could reasonably be attributed to the measurement [ISO/IEC Guide 98-3:2008 [9]] 3.13 wet-only collector equipment to collect wet deposition, consisting of a funnel-bottle combination, open to the atmosphere only during precipitation events SIST EN 15980:2011
EN 15980:2011 (E) 7 4 Symbols and abbreviations 4.1 Symbols A area of the cross-section of the collector opening; c mean value of the concentration of a compound in a solution; ic mean value of the concentration of a compound, obtained by laboratory i; cj concentration of a compound in the solution j; d(1,j) deposition in collector 1; d(2,j) deposition in collector 2; Da deposition rate of compound a; DL,a detection limit of compound a; DM ,a minimal detectable mass of compound a; k coverage factor; ma mass of compound a; ma,d detected mass of compound a; am mean of laboratory blank value; ma,i
individual laboratory blank value for compound a; n number of measurements; rss residual sum of squares from the fit; si within-laboratory standard deviation; sL between-laboratory standard deviation; sd between-collector standard deviation; sR reproducibility standard deviation; sri standard deviation of repeated measurements of laboratory i; Sm mass of surrogate standard, added to the sample; Sd mass of surrogate standard detected in the sample extract; Slb,a standard deviation of laboratory blank value for compound a; t sampling duration; tn-1;0,95 Student factor for n measurements and a 95 % confidence interval; SIST EN 15980:2011
EN 15980:2011 (E) 8 ubc,j between-collector uncertainty for collector type j; uD uncertainty of measured depositions; uM standard uncertainty of the deposition measurement; Up(y) expanded uncertainty of the measured value y with a coverage probability p; wbc,j relative between-collector uncertainty for collector type j; wfit random relative uncertainty of the fits. 4.2 Abbreviations BaA Benz[a]anthracene BaP Benzo[a]pyrene BeP Benzo[e]pyrene BbF Benzo[b]fluoranthene BjF Benzo[j]fluoranthene BkF Benzo[k]fluoranthene CHR Chrysene CRM Certified reference material CPP Cyclopenta[cd]pyrene DAD Diode array detection DBacA Dibenz[a,c]anthracene DBahA Dibenz[a,h]anthracene DBajA Dibenz[a,j]anthracene DCM Dichloromethane EMEP Co-operative Programme for Monitoring and Evaluation of the Long-range Transmission of Air pollutants in Europe (European Monitoring and Evaluation Programme) FLD Fluorescence detection GC Gas chromatography HPLC High performance liquid chromatography INP Indeno[1,2,3-cd]pyrene MS Mass spectrometry PAH Polycyclic aromatic hydrocarbons SIST EN 15980:2011
EN 15980:2011 (E) 9 PTFE Polytetrafluoroethylene QA/QC Quality Assurance/Quality Control SOP Standard operating procedure SPE Solid phase extraction TRI Triphenylene WMO/GAW World Meteorological Organization / Global Atmosphere Watch 5 Principle Deposition samples for the determination of specified PAH compounds are taken in funnel-bottle bulk collectors for a measured period of time (see Clause 7). Samples are prepared using liquid-liquid or solid phase extraction with organic solvent (see 8.2). Identification and quantification of the substances are performed by either GC/MS or HPLC/FLD (see 8.3). 6 Apparatus, reagents and materials 6.1 Reagents High purity reagents: solvents: e.g. acetone, acetonitrile, cyclohexane, dichloromethane (DCM), methanol, toluene, water; solid substances: NaCl, anhydrous Na2SO4. 6.2 Materials Ordinary laboratory materials; wiping material, e.g. glass wool, quartz wool or pre-extracted cotton wool. 6.3 Sampling equipment Funnel-bottle bulk collectors consist of a cylindrical funnel and a sample collection vessel (see A.2). The vertical section of the funnel shall be at least as high as its diameter. The collection vessels shall have a cylindrical vertical section of sufficient height to avoid sampling losses resulting from splashing. The collector is permanently open to the atmosphere. The collector shall be equipped with a device for keeping birds off. The area of the cross-section of the funnel opening and the size of the sample collection vessel shall be adjusted to the precipitation amount which is expected in the chosen sampling period in order to avoid overflow. Typical sampling periods vary between one week and one month. The area of the cross-section of the funnel opening shall be large enough to provide sufficient sample for analysis at a minimum precipitation height of 1 mm per week. NOTE 1 The funnel diameter should be at least 15 cm. The funnel opening shall be at least 1,5 m above ground. For areas that receive high snowfall accumulations, the collector may be raised onto a platform above the snow. NOTE 2 An extra large and deep cylindrical collector may be used for snow sampling (see [1]). SIST EN 15980:2011
EN 15980:2011 (E) 10 Funnel and sample collection vessel shall be made of glass. If connectors, which come into contact with sampled material, are not made of glass, only PTFE or other fluoroelastomers are permissible. All parts shall be able to be easily cleaned. 6.4 Laboratory equipment 6.4.1 General Ordinary laboratory apparatus and the items given in 6.4.2 and 6.4.3 are required. 6.4.2 Apparatus for sample extraction Liquid-liquid or solid phase extraction apparatus (see B.2.2.2 and B.2.2.3). 6.4.3 Apparatus for sample analysis 6.4.3.1 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 an FLD. Furthermore a system for solvent degassing (internal or external) is required. NOTE If the amounts of PAH are high, also the HPLC/DAD technique can be used. 6.4.3.2 GC/MS apparatus Gas chromatograph with split/splitless injector or on-column injector, a capillary column suitable for PAH analysis, and a mass selective detector. 7 Sampling 7.1 General The validation field test was carried out using funnel-bottle bulk collectors, cylindrical gauges and wet-only collectors (see Annex A). The results showed that the deposition rates of PAH measured with the funnel-bottle bulk collector were in most cases higher than those measured with the cylindrical gauges or the wet-only collector. The between-collector uncertainty in general was the lowest for the funnel-bottle bulk collector (see D.4.2). Therefore the funnel-bottle bulk collector shall be used as the standard collector for the determination of the deposition of BaA, BbF, BjF, BkF, BaP, DBahA and INP. NOTE When the deposition rates were high and the climatic conditions moderate the results of cylindrical gauges were similar to those obtained with the funnel-bottle bulk collectors. When the precipitation was high and the climatic conditions were cold the results of wet-only and funnel bottle bulk collectors were similar. Therefore in special cases, if equivalence with the funnel-bottle bulk collector can be shown different types of collectors like wet-only collectors and cylindrical gauges can be used to measure the deposition of PAH. 7.2 Sampling location Macroscale and microscale siting shall follow the guidelines of Directive 2004/107/EC [2], which are harmonized with the guidelines from EMEP [1] and WMO/GAW [3] for deposition measurements in rural areas. The collector shall as far as possible not be exposed in areas where strong winds occur like shores, cliffs and top of hills, but it shall also not be sheltered by tall trees or buildings. The flow around the collector should be unrestricted, without any obstructions affecting the airflow in the vicinity of the collector. The criteria depend on the site characteristic: SIST EN 15980:2011
EN 15980:2011 (E) 11 rural site: as far as practicable no obstacles such as trees, buildings, hedges or topographical features above 30° (see Figure 1) from the rim of the collector, which may give rise to updraughts or downdraughts; urban and industrial site: as far as possible away from buildings, trees and other obstacles.
Key 1 collector 2 obstacle, acceptable 3 obstacle, too high Figure 1 — Position of obstacles which affect sampling 7.3 Sampling requirements Handle sampling equipment such that contamination is avoided. Avoid contact of skin with the glassware of the exposed side of the collector, e.g., by wearing cotton gloves during mounting and dismounting of the collector. The procedures used in the field test are described in B.3 and B.4. NOTE 1 In order to avoid breaking of glassware due to freezing 100 ml of a saturated NaCl solution may be added before sampling, if low temperatures are expected. If materials like leaves or insects clog the pipe of the funnel, remove them carefully with tweezers and rinse them with water. The rinsing water is added to the collected rain water. Also rinse the funnel carefully. Cleaning of the funnel can be done either at the sampling site or in the laboratory depending on local conditions. Parts of the collector which are transported to the laboratory shall be carefully wrapped, e.g. with aluminium foil. NOTE 2 The sampled water amount can be determined by weighing the collector before and after exposure. The precipitation rate can be calculated from the water amount, the cross-section of the funnel opening and the exposure time. These data can be compared with meteorological data to check the plausibility of the results. Store equipment in the field so that contamination is prevented, e.g. wrapped in aluminium foil, and kept it in an as clean and dust-free place as possible. Clean the funnel between exposures with wiping material moistened with acetone or methanol, followed by rinsing with water. Send the funnel to the laboratory for thorough cleaning, if necessary. The sampling duration shall not exceed 1 month. SOPs are given in Annex B. SIST EN 15980:2011
EN 15980:2011 (E) 12 7.4 Sample transport The sample consisting of deposited liquid and solid material and the solution of funnel rinsing shall be transported in suitable containers to the laboratory directly after the end of sampling. The samples shall be kept as cool as practically possible while avoiding exposure to sunlight and contaminants. NOTE 1 It is recommended to keep the temperature below 30 °C. NOTE 2 Possible sources of contamination are e.g. vehicle exhausts and tobacco smoke. 8 Sample preparation and analysis 8.1 Sample storage Store the samples cool and dark before processing. Sample preparation shall be carried out within 1 month after end of sampling. NOTE A degradation test as part of the method validation procedure demonstrated that the composition of a synthetic sample, CRM (urban dust) suspended in rain water, did not change during exposure in the field within a period of 1 month. 8.2 Extraction Both liquid-liquid extraction in combination with filtration and solid phase extraction (SPE) have been shown to be effective for the quantitative extraction of PAH in the laboratory test. These methods are specified in Annex B. 8.3 Analysis The analysis procedure is specified in Annex C. For BaP it is consistent with EN 15549. 8.4 Interferences Unusual results, peak forms or retention times of PAH may suggest that chromatographic interferences are present. Attention shall be given to interferences concerning BaA, BbF+BjF+BkF and DBahA in GC/MS and BjF in HPLC/FLD (see C.3). 9 Quality assurance The low ambient concentration of PAH can cause erroneous results unless strict precautions are taken to prevent contamination and other sources of errors. The laboratories collecting PAH data shall therefore have a QC procedure according to the relevant items of EN 15549:2008, Clause 13, which is designed for their sampling and analytical procedures. Laboratory equipment used for storage of samples shall be properly cleaned before use. Laboratory and field blanks shall be taken regularly to check for potential contamination. The check of the purity of reagents is part of the normal laboratory QA/QC programme. The laboratory blanks are used to identify potential contamination sources in the laboratory. The laboratory blanks shall be used to calculate the detection limit (see D.2). If the laboratory blank contributes significantly to the amount of deposition samples for the same period, necessary steps shall be taken to identify the contamination sources and correct the procedure accordingly. Laboratory blanks shall be analysed at least once in every set of extracted samples. SIST EN 15980:2011
EN 15980:2011 (E) 13 Field blanks shall be taken regularly, twice per year per site. In case of a laboratory being responsible for samples from more than one site the number of field blanks may be reduced. In any case, the minimum number of field blanks shall be 10 % of the number of the deposition samples. Results that are judged to be suspect based on the level of the field blanks shall be flagged. When reporting the results the reason for flagging shall be indicated. NOTE The interpretation of the results of the field blanks is a matter of expert judgement. As a rule of thumb, a blank value of twice the detection limit of a component or greater is an indication of contamination. If this blank value is ≥ 10 % of the level of a sample, the sample result should be flagged. If laboratories carry out routine analyses of PAH deposition samples it is recommended that they participate in a relevant external quality assessment scheme or proficiency testing scheme like laboratory and field intercomparisons. 10 Calculation of results The amount of PAH in depositions shall be given in ng, the deposition rate in ng/(m2⋅d). The deposition in the collectors shall be calculated according to Equation (1). tAmD×=aa (1) where Da
is the deposition rate of compound a in ng/(m2⋅d); ma
is the mass of compound a in ng; A
is the area of the cross-section of the collector opening in m²; t
is the sampling duration in d. The masses of the compounds shall be corrected by the recovery of the surrogate standard (see B.4.1) according to Equation (2). dmda,aSSmm×= (2) where ma,d is the detected mass of compound a in ng/(m2⋅d); Sm is the mass of surrogate standard added to the sample, in ng; Sd is the mass of surrogate standard detected in the sample extract, in ng. 11 Performance characteristics The performance characteristics of the method were determined from the data of the laboratory and field validation tests. The results are given in Annex D. SIST EN 15980:2011
EN 15980:2011 (E) 14 12 Uncertainty Sampling and between-laboratory differences provide the main contributions to the uncertainty of the measurement of PAH depositions (see Annex D). The uncertainty of sampling and analysis shall be assessed by the laboratory for all compounds to be measured. The laboratory shall perform tests to ensure that the requirements for the analytical uncertainty as defined in EN 15549 are met; the recovery of the surrogate standard added to the collected sample before extraction is ≥ 50 %
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