EN 16181:2018

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Boden, behandelter Bioabfall und Schlamm - Bestimmung von polycyclischen aromatischen Kohlenwasserstoffen (PAK) mittels Gaschromatographie (GC) und Hochleistungs-Flüssigkeitschromatographie (HPLC)Sols, biodéchets traités et boues - Dosage des hydrocarbures aromatiques polycycliques (HAP) par chromatographie en phase gazeuse et chromatographie liquide à haute performanceSoil, treated biowaste and sludge - Determination of polycyclic aromatic hydrocarbons (PAH) by gas chromatography (GC) and high performance liquid chromatography (HPLC)71.040.50Fizikalnokemijske analitske metodePhysicochemical methods of analysis13.080.10Chemical characteristics of soils13.030.20Liquid wastes. SludgeICS:Ta slovenski standard je istoveten z:EN 16181:2018SIST EN 16181:2018en,fr,de01-december-2018SIST EN 16181:2018SLOVENSKI
STANDARDSIST-TS CEN/TS 16181:20131DGRPHãþD

EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16181
June
t r s z English Version
Soilá treated biowaste and sludge æ Determination of Solsá biodéchets traités et boues æ Dosage des chromatographie en phase gazeuse et chromatographie liquide à haute performance
Bodená behandelter Bioabfall und Schlamm æ Bestimmung von polycyclischen aromatischen This European Standard was approved by CEN on
v April
t r s zä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
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t r s z CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s x s z sã t r s z ESIST EN 16181:2018

Repeatability and reproducibility data . 31 A.1 Materials used in the interlaboratory comparison study . 31 A.2 Interlaboratory comparison results . 31 Annex B (informative)
Examples of instrumental conditions and chromatograms . 34 B.1 Measurement of PAH with GC-MS . 34 B.2 Measurement of PAH with HPLC fluorescence . 39 Bibliography . 46
Key
difference in retention times of the two peaks a and b in seconds (s) Ya peak width at the base of peak a in seconds (s) Yb peak width at the base of peak b in seconds (s) Figure 1 — Example of a chromatogram of a critical pair 3.2 internal standard isotopically labelled PAH or PAH unlikely to be present in the sample, added to samples prior to extraction, against which the concentrations of native substances are calculated 3.3 injection standard PAH that is unlikely to be present in samples added to the sample extract before injection into the gas chromatograph, to monitor variability of instrument response and the recovery of the internal standards [SOURCE: EN 15527:2008, 3.5, modified – the wording of the definition was revised.] 3.4 Surrogate PAH that is unlikely to be present in samples added to the sample prior to analysis and used to correct for losses of the PAH analytes during sample extraction or clean-up 4 Principle Due to the multi matrix (horizontal) character of this European Standard, different procedures for different steps (modules) are allowed. Which modules should be used depends on the sample. A recommendation is given in this European Standard. Performance criteria are described and it is the responsibility of the laboratories applying this European Standard to show that these criteria are met. Using of spiking standards (internal standards) allows an overall check on the efficiency of a specific combination of modules for a specific sample. But it does not necessarily give the information upon the extensive extraction efficiency of the native PAH bonded to the matrix. SIST EN 16181:2018

1) Bio-Beads® is an example of a suitable product available commercially. This information is given for the convenience of this document and does not constitute an endorsement by CEN of this product. Equivalent products may be used if they can be shown to lead to the same results. SIST EN 16181:2018

Indeno[1,2,3-cd]pyrene (CAS-RN 193-39-5) Indeno[1,2,3-cd]pyrene-d12 (CAS-RN 203578-33-0) Dibenz[a,h]anthracene (CAS-RN 53-70-3) Dibenz[a,h]anthracene -d14 (CAS-RN 13250-98-1) Benzo[ghi]perylene (CAS-RN 191-24-2) Benzo[ghi]perylene-d12 (CAS-RN 93951-66-7) a Not part of 16 target analytes, but applicable for resolution check for the separation with benzo[a]pyrene for GC measurements. NOTE 1 13C12-labelled PAH standards can also be used as internal standards. NOTE 2 Certified solutions of PAH, and single solid PAH substances with certified purity are available from a limited number of suppliers. When highly contaminated samples are analysed, an aliquot of the extract is often used for a further clean-up. For HPLC, a extraction recovery control shall be made by addition, using a surrogate which is not interfering with the target analytes. A suitable native PAH not mentioned in the scope, e.g. 6-methylchrysene, is added to the sample before extraction. The recovery range for this control should be between 70 % and 110 %. SIST EN 16181:2018

–15 °C, diluted standard solutions at (5 ± 3) °C. Stock solutions are stable for about one year when protected from sunlight and evaporation. The stability of the standard solution shall be checked regularly by comparison with an independent, preferably certified, standard solution. 7.5.1 Standard solutions for HPLC-Analysis 7.5.1.1 Single substance stock solutions Prepare solutions of the single substances (see Table 3) in acetonitrile (7.3.2.2) to achieve a mass concentration of 10 µg/ml. These solutions are used for confirmation and identification of single PAHs in the chromatogram. 7.5.1.2 Multiple substance stock solution Prepare solutions of the reference substances (see Table 3) in acetonitrile (7.3.2.2) to achieve a mass concentration of the respective individual substance of 10 µg/ml. 7.5.1.3 Calibration solutions Prepare at least five calibration solutions by appropriate dilution of the stock solution (7.5.1.1 or 7.5.1.2), using acetonitrile (7.3.2.2) or methanol (7.3.2.2) as solvent. The choice of solvent depends on the composition of the mobile phase. Transfer 50 µl of the stock solution into a graduated 5 ml flask and fill up to the mark with acetonitrile. One µl of this reference solution contains 100 pg of the respective individual substances. Check the stability of the reference solutions regularly. Check the mass concentration of the PAH in the stock solution by comparison with an independent, preferably certified, standard solution. 7.5.2 Standard solutions for GC-MS analysis 7.5.2.1 Single substance stock solution Prepare solutions of the single substances of native and deuterated PAH (see Table 3) in toluene (7.1.3) or cyclohexane (7.2.3.3) to achieve a mass concentration of 10 µg/ml. These solutions are used for confirmation and identification of single PAHs in the chromatogram. 7.5.2.2 Multiple substance stock solution of native PAH Dilute the solution of the reference substances, i.e. native PAH (see Table 3) in toluene (7.1.3) or cyclohexane (7.2.3.3), to achieve a mass concentration of the respective individual substance, i.e. 10 µg/ml. SIST EN 16181:2018

(EN ISO 16720) Na2SO4 No drying Sludge xa xb
Biowaste (compost, mixed waste) x x x Soil (e.g. sand, clay) x x x a Loss of volatile PAH is possible. b Na2SO4 can be used for the preservation of hygroscopic dried sludge. SIST EN 16181:2018
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