EN 16181:2018
(Main)Soil, treated biowaste and sludge - Determination of polycyclic aromatic hydrocarbons (PAH) by gas chromatography (GC) and high performance liquid chromatography (HPLC)
Soil, treated biowaste and sludge - Determination of polycyclic aromatic hydrocarbons (PAH) by gas chromatography (GC) and high performance liquid chromatography (HPLC)
This European Standard specifies the quantitative determination of 16 polycyclic aromatic hydrocarbons (PAH) (see Table 2) in sludge, soil and treated biowaste using GC-MS and HPLC-UV-DAD/FLD covering a wide range of PAH contamination levels (see also Annex B).
When using fluorescence detection, acenaphthylene cannot be measured.
The limit of detection depends on the determinants, the equipment used, the quality of chemicals used for the extraction of the sample and the clean-up of the extract.
Typically, a lower limit of application of 0,01 mg/kg (expressed as dry matter) can be ensured for each individual PAH. This depends on instrument and sample.
Sludge, soil and treated biowaste can differ in properties and also in the expected contamination levels of PAHs and presence of interfering substances. These differences make it impossible to describe one general procedure. This European Standard contains decision tables based on the properties of the sample and the extraction and clean-up procedure to be used. Two general lines are followed, an agitation procedure (shaking) or use of soxhlet/pressurized liquid extraction.
NOTE Other PAH compounds can also be analysed with this method, provided suitability has been proven.
Boden, behandelter Bioabfall und Schlamm - Bestimmung von polycyclischen aromatischen Kohlenwasserstoffen (PAK) mittels Gaschromatographie (GC) und Hochleistungs-Flüssigkeitschromatographie (HPLC)
Diese Europäische Norm legt die quantitative Bestimmung von 16 polycyclischen aromatischen Kohlenwasserstoffen (PAK) (siehe Tabelle 2) in Schlamm und behandeltem Bioabfall unter Anwendung der GC MS und HPLC UV DAD/FLD fest, wobei ein breiter Bereich von PAK Kontaminationsniveaus (siehe auch Anhang B) abgedeckt wird.
Bei Anwendung der Fluoreszenzdetektion kann Acenaphthylen nicht gemessen werden.
Sols, biodéchets traités et boues - Dosage des hydrocarbures aromatiques polycycliques (HAP) par chromatographie en phase gazeuse et chromatographie liquide à haute performance
La présente Norme européenne spécifie le dosage de 16 hydrocarbures aromatiques polycycliques (HAP) (voir Tableau 2) dans les boues, les sols et les biodéchets traités, faisant appel à des méthodes CG-SM et HPLC-UV-DAD/FLD couvrant une large gamme de niveaux de contamination par les HAP (voir également l’Annexe B).
L’utilisation d’une méthode de détection fluorimétrique ne permet pas le mesurage de l’acénaphtylène.
(...)
La limite de détection dépend des composés à analyser, de l’équipement utilisé, de la qualité des réactifs chimiques utilisés pour l’extraction de l’échantillon et la purification de l’extrait.
En général, une limite inférieure d’application de 0,01 mg/kg (exprimée en matière sèche) peut être atteinte pour chacun des HAP. Cela dépend de l’instrument et de l’échantillon.
Les boues, les sols et les biodéchets traités peuvent présenter des propriétés, des niveaux de contamination par les HAP attendus et des substances interférentes différents. En raison de ces différences, il est impossible de décrire un mode opératoire général. La présente Norme européenne contient des tables de décision basées sur les propriétés de l'échantillon ainsi que sur le mode opératoire d'extraction et de purification à utiliser. Deux routes analytiques générales sont suivies : un mode opératoire par agitation ou l’utilisation d’une méthode d’extraction au Soxhlet/par liquide pressurisé.
NOTE D’autres composés HAP peuvent être également analysés avec cette méthode, à condition que l’aptitude à l’emploi soit prouvée.
Tla, obdelani biološki odpadki in blato - Določevanje policikličnih aromatskih ogljikovodikov (PAH) s plinsko kromatografijo (GC) in s tekočinsko kromatografijo visoke ločljivosti (HPLC)
Ta evropski standard določa kvantitativno določevanje 16 policikličnih aromatskih ogljikovodikov (PAH) (glej preglednico 2) v blatu, tleh ter obdelanih bioloških odpadkih z metodama GC-MS in HPLC-UV-DAD/FLD, ki zajemata široko območje ravni onesnaženja PAH (glej tudi dodatek B).
S fluorescenčnim zaznavanjem ni mogoče izmeriti acenaftilena.
(...)
Meja detekcije je odvisna od determinant, uporabljene opreme, kakovosti kemikalij, uporabljenih za ekstrakcijo vzorca in očiščenje izvlečka.
Običajno je mogoče za vsak posamezen policiklični aromatski ogljikovodik zagotoviti spodnjo mejo uporabe 0,01 mg/kg (izraženo kot suha snov). To je odvisno od instrumenta in vzorca.
Blato, tla in obdelani biološki odpadki se lahko razlikujejo glede lastnosti, predvidenih ravni onesnaženja s policikličnimi aromatskimi ogljikovodiki ter prisotnosti motečih snovi. Zaradi teh razlik ni možen opis enotnega splošnega postopka. Ta evropski standard vključuje tabele odločanja, ki temeljijo na lastnostih vzorca, ter postopek za ekstrakcijo in očiščenje, ki ga je treba uporabiti. Upoštevata se dve splošni smernici, in sicer stresanje ali tekočinska ekstrakcija po Soxhletu/pod tlakom.
OPOMBA: S to metodo je mogoče analizirati tudi druge snovi PAH pod pogojem, da je bila dokazana primernost.
General Information
Relations
Standards Content (Sample)
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
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Serbiaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey and United Kingdomä
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Rue de la Science 23,
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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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Frequently Asked Questions
EN 16181:2018 is a standard published by the European Committee for Standardization (CEN). Its full title is "Soil, treated biowaste and sludge - Determination of polycyclic aromatic hydrocarbons (PAH) by gas chromatography (GC) and high performance liquid chromatography (HPLC)". This standard covers: This European Standard specifies the quantitative determination of 16 polycyclic aromatic hydrocarbons (PAH) (see Table 2) in sludge, soil and treated biowaste using GC-MS and HPLC-UV-DAD/FLD covering a wide range of PAH contamination levels (see also Annex B). When using fluorescence detection, acenaphthylene cannot be measured. The limit of detection depends on the determinants, the equipment used, the quality of chemicals used for the extraction of the sample and the clean-up of the extract. Typically, a lower limit of application of 0,01 mg/kg (expressed as dry matter) can be ensured for each individual PAH. This depends on instrument and sample. Sludge, soil and treated biowaste can differ in properties and also in the expected contamination levels of PAHs and presence of interfering substances. These differences make it impossible to describe one general procedure. This European Standard contains decision tables based on the properties of the sample and the extraction and clean-up procedure to be used. Two general lines are followed, an agitation procedure (shaking) or use of soxhlet/pressurized liquid extraction. NOTE Other PAH compounds can also be analysed with this method, provided suitability has been proven.
This European Standard specifies the quantitative determination of 16 polycyclic aromatic hydrocarbons (PAH) (see Table 2) in sludge, soil and treated biowaste using GC-MS and HPLC-UV-DAD/FLD covering a wide range of PAH contamination levels (see also Annex B). When using fluorescence detection, acenaphthylene cannot be measured. The limit of detection depends on the determinants, the equipment used, the quality of chemicals used for the extraction of the sample and the clean-up of the extract. Typically, a lower limit of application of 0,01 mg/kg (expressed as dry matter) can be ensured for each individual PAH. This depends on instrument and sample. Sludge, soil and treated biowaste can differ in properties and also in the expected contamination levels of PAHs and presence of interfering substances. These differences make it impossible to describe one general procedure. This European Standard contains decision tables based on the properties of the sample and the extraction and clean-up procedure to be used. Two general lines are followed, an agitation procedure (shaking) or use of soxhlet/pressurized liquid extraction. NOTE Other PAH compounds can also be analysed with this method, provided suitability has been proven.
EN 16181:2018 is classified under the following ICS (International Classification for Standards) categories: 13.030.01 - Wastes in general; 13.080.10 - Chemical characteristics of soils. The ICS classification helps identify the subject area and facilitates finding related standards.
EN 16181:2018 has the following relationships with other standards: It is inter standard links to CEN/TS 16181:2013, EN 17503:2022. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.
EN 16181:2018 is associated with the following European legislation: EU Directives/Regulations: 86/278/EEC; Standardization Mandates: M/330. When a standard is cited in the Official Journal of the European Union, products manufactured in conformity with it benefit from a presumption of conformity with the essential requirements of the corresponding EU directive or regulation.
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The article discusses EN 16181:2018, a European Standard that specifies the quantitative determination of 16 polycyclic aromatic hydrocarbons (PAH) in sludge, soil, and treated biowaste. The article mentions that acenaphthylene cannot be measured when using fluorescence detection. The limit of detection depends on various factors such as equipment used, chemicals used for sample extraction, and clean-up of the extract. Typically, a lower limit of application of 0.01 mg/kg can be ensured for each individual PAH. The article also mentions that sludge, soil, and treated biowaste have different properties and expected contamination levels of PAHs, so a general procedure cannot be described. The article includes decision tables based on sample properties and extraction methods. Lastly, the article notes that other PAH compounds can also be analyzed with this method, as long as their suitability is proven.
기사 제목: EN 16181:2018 - 토양, 처리된 생물폐기물 및 슬러지 - 가스 크로마토그래피 (GC) 및 고성능 액체 크로마토그래피 (HPLC)를 이용한 다환방향탄화수소(PAH)의 결정 기사 내용: 이 유럽 표준은 GC-MS 및 HPLC-UV-DAD/FLD를 사용하여 슬러지, 토양 및 처리된 생물폐기물에서 16가지의 다환방향탄화수소(PAH) (표 2 참조)의 정량적 결정을 규정한다. 이 방법은 PAH 오염수준의 광범위한 범위에 대해 다루고 있으며, 형광 검출을 사용할 경우 acenaphthylene은 측정할 수 없다. 검출 한계는 결정 요인, 사용하는 장비, 견본 추출 및 추출물의 정화에 사용되는 화학물질의 품질에 따라 다를 수 있다. 일반적으로 각각의 PAH에 대해 0.01 mg/kg (건물을 기준으로 표현)의 낮은 적용 한계를 보장할 수 있다. 이는 기기 및 견본에 달려있다. 슬러지, 토양 및 처리된 생물폐기물은 특성 및 기대되는 PAH 오염수준과 간섭 물질의 존재로 인해 상이할 수 있다. 이러한 차이로 인해 일반적인 절차를 설명하는 것은 불가능하다. 이 유럽 표준에는 견본 특성 및 추출 및 정화 절차에 따른 의사 결정을 위한 표가 포함되어 있다. 마지막으로, 기사는 타당성이 입증된 경우 이 방법을 통해 다른 PAH 화합물도 분석할 수 있다고 언급한다.
記事タイトル：EN 16181:2018 - 土壌、処理されたバイオ廃棄物およびスラッジ - ガスクロマトグラフィー（GC）および高性能液体クロマトグラフィー（HPLC）による多環芳香族炭化水素（PAH）の決定 記事内容：この欧州規格は、GC-MSおよびHPLC-UV-DAD/FLDを使用して、スラッジ、土壌、および処理されたバイオ廃棄物中の16種類の多環芳香族炭化水素（PAH）の定量的な決定を規定しています（表2も参照）。蛍光検出を使用する場合はacenaphthyleneは測定できません。検出限界は、決定要因、使用する装置、サンプル抽出のための化学物質の品質、および抽出物のクリーンアップによって異なります。通常、各個別PAHにおいて0.01 mg/kg（乾物で表現）の適用下限が保証できますが、これは機器やサンプルに依存します。スラッジ、土壌、処理されたバイオ廃棄物は特性やPAHの予想される汚染レベル、および干渉物質の存在によって異なる場合がありますので、一般的な手順を説明することはできません。この欧州規格は、サンプルの特性と抽出方法に基づく意思決定表を含んでいます。最後に、この方法で他のPAH化合物も分析することができるが、適合性が証明されている必要があるという記事の注意事項も述べています。
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