SIST EN 15980:2011

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
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

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

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

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

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

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

Collectors used in the field trial A.1 General The 3 different types of collectors which were used in the field trial are illustrated in Figures A.1 to A.5. Figures A.1, A.2, A.3 and A.4 illustrate the funnel-bottle bulk collector, Figure A.5 illustrates the cylindrical gauge (Bergerhoff collector) and Figure A.6 illustrates the wet-only collector. A.2 Funnel-bottle bulk collector
Key 1 protective basket 2 tube, 190 mm diameter 3 stopper to fix funnel and bottle 4 post Figure A.1 — Housing and protective basket SIST EN 15980:2011

Key 1 funnel (brown glass) 2 connector 3 bottle (brown glass) Dimensions: Diameter of funnel and bottle:
165 mm Height of the vertical section of the funnel:
200 mm Height of the complete collector: 700 mm Figure A.2 — Funnel and bottle
Key 1 funnel with thread GL 45 2 screw caps with thread GL 45 3 ferrules, coated with PTFE 4 glass liner 5 bottle with thread GL 45 Dimensions: Glass liner Inner diameter:
22 mm Diameter of capillary section:
3 mm Length: 125 mm Inner diameter of bottleneck:
28 mm Figure A.3 — Detailed illustration of the connector SIST EN 15980:2011

Figure A.4 — Glass liner (left) and glass liner within the screw caps (right) A.3 Cylindrical gauge (Bergerhoff collector)
Key 1 deposition gauge 2 protective basket
Dimensions: Total height: ca. 150 cm Diameter of deposition gauge:
110 mm Height of deposition gauge:
190 mm Diameter of protective basket:
350 mm Figure A.5 — Cylindrical gauge (Bergerhoff collector) SIST EN 15980:2011

Dimensions: Total height: ca. 150 cm Diameter of the funnel: 252 mm Height of the vertical section of the funnel: 250 mm Figure A.6 — Wet-only collector SIST EN 15980:2011

Work-up of deposition samples for PAH analysis B.1 Schematic representation Figure B.1 shows the schematic representation of the sample work-up procedure.
Figure B.1 — Flow-chart of sample processing (adapted from [4]) SIST EN 15980:2011

B.2.1.4 Bergerhoff collector  4 Bergerhoff collectors with lids made of glass NOTE 4 collectors are recommended for one monthly sample in order to obtain sufficient sample amount. B.2.2 For use in the laboratory B.2.2.1 General  High purity solvents, e.g. toluene, cyclohexane, DCM, acetonitrile, n-hexane and water  Anhydrous sodium sulphate, high purity  Sodium chloride, high purity  Ultrasonic bath  Internal standard, e.g. 6-methylchrysene or perylene-d12 (approximately 100 µg/ml in the appropriate solvent)  Vials, volume e.g. 2 ml SIST EN 15980:2011

 Extraction station containing: extraction disk holder, reservoir for extraction medium, collection chambers, flask adapter  Reversed phase or hydrophilic extraction disk  1 l flasks B.3 Work to be done in the field B.3.1 Bulk collectors Handle the collector according to the manufacturer’s instructions, if commercially purchased. The following example is given for the funnel-bottle bulk collector described in A.2.  Remove one screw from the stopper.  Hold the complete glassware deposition sampling equipment and lift it a few millimetres.  Pull out the stopper.  Remove the glassware downwards carefully.  Use tweezers to remove coarse impurities (e.g. insects, leaves) from the funnel and rinse them carefully with high purity water, collect the rinsing water into a bottle, close and store the bottle, discard the impurities.  Disconnect the screw cap from the collector.  Close the collector.  Connect the funnel to a clean 500 ml bottle.  Clean the funnel with approximately 150 ml of e.g. acetone and wiping material (use gloves) and collect the solvent in the 500 ml bottle.  Store the wiping material in the bottle, disconnect the bottle and close it tightly.  Connect the funnel with an empty 4 l collecting bottle.  Put the bottle and the funnel into the tube. SIST EN 15980:2011

15 min, repeat the procedure once.  Dry the combined solutions with anhydrous sodium sulphate, filter, rinse the bottle and rinse the filter three times with toluene or DCM, evaporate (using a round bottom flask) in order to obtain a concentrated solution of 2 ml to 3 ml, finally fill this concentrated solution into a vial and complete the evaporation to dryness.  If sampling is on a weekly basis combine 4 weekly extracts to one sample. Combine the extracts with those of the water samples, if separate analysis is not required. NOTE If separate analysis of funnel and bottle is required, e.g. 1 µg of surrogate standard is added to the bottle with the rinsing solutions before the extraction. B.4.4 Bergerhoff collectors: treatment of collected deposition using liquid–liquid extraction or SPE  Add e.g. 0,25 µg of surrogate standard (e.g. 6-methylchrysene (for HPLC) or perylene-d12 (for GC/MS) in 1 ml of appropriate solvent) to each collector.  Filter the water of all the four collectors as described for the funnel-bottle and wet-only collectors. Use one filter and one separation funnel for the 4 collectors.  Rinse the collectors as described for the bottles of the funnel-bottle and wet-only collectors, use only
ca. 5 ml of solvent per collector. Filter the rinsing solutions with the same filter as it was used for the rain water. SIST EN 15980:2011

1 ml of appropriate solvent) to the bottles or 0,25 µg of surrogate standard to each of the Bergerhoff collectors. Add 200 ml of water (50 ml to each of the Bergerhoff collectors) and treat the sample as usual. SIST EN 15980:20
...