SIST-TS CEN/TS 16181:2013
(Main)Sludge, treated biowaste and soil - Determination of polycyclic aromatic hydrocarbons (PAH) by gas chromatography (GC) and high performance liquid chromatography (HPLC)
Sludge, treated biowaste and soil - Determination of polycyclic aromatic hydrocarbons (PAH) by gas chromatography (GC) and high performance liquid chromatography (HPLC)
This Technical Specification 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) may be ensured for each individual PAH. This depends on instrument and sample. Sludge, soil and treated biowaste may 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 Technical Specification 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/pressurised liquid extraction.
Schlamm, behandelter Bioabfall und Boden - Bestimmung von polycyclischen aromatischen Kohlenwasserstoffen (PAK) mittels Gaschromatographie (GC) und Hochleistungs-Flüssigkeitschromatographie (HPLC)
Diese Technische Spezifikation 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.
Die Nachweisgrenze hängt von den zu bestimmenden Substanzen, den verwendeten Geräten, der Qualität der für die Extraktion verwendeten Chemikalien und der Reinigung des Extrakts ab.
Üblicherweise kann für jeden einzelnen PAK eine untere Anwendbarkeitsgrenze von 0,01 mg/kg (angegeben als Trockenmasse) sichergestellt werden. Diese ist geräte und probenabhängig.
Schlamm und behandelter Bioabfall können sich in ihren Eigenschaften sowie in den erwarteten Kontaminationsniveaus von PAK und bei der Anwesenheit von störenden Substanzen unterscheiden. Aufgrund dieser Unterschiede ist es unmöglich, ein allgemeines Verfahren zu erarbeiten. Die vorliegende Technische Spezifikation enthält Entscheidungstabellen, die auf den Probeneigenschaften und den anzuwendenden Extraktions und Reinigungsverfahren basieren. Es werden zwei allgemeine Extraktionsverfahren angewendet – das Schüttelverfahren oder die Soxhlet /Hochdruck Flüssigextraktion.
ANMERKUNG Mit diesem Verfahren können auch weitere PAK Verbindungen analysiert werden, sofern die Eignung des Verfahrens nachgewiesen ist.
Boue, biodéchet traité et sol - Dosage des hydrocarbures aromatiques polycycliques (HAP) par chromatographie en phase gazeuse et chromatographie liquide à haute performance
La présente Spécification technique spécifie le dosage de 16 hydrocarbures aromatiques polycycliques (HAP) (voir Tableau 2) dans les boues, les sols et les bio-déchets traités, faisant appel à des méthodes CG-SM et CLHP-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 bio-déchets 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 Spécification technique 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/liquide sous pression.
NOTE D’autres composés HAP peuvent être également analysés avec cette méthode, à condition que l’aptitude à l’emploi soit prouvée.
Blato, obdelani biološki odpadki in tla - Določevanje policikličnih aromatskih ogljikovodikov (PAO) s plinsko kromatografijo (GC) in s tekočinsko kromatografijo visoke ločljivosti (HPLC)
Ta tehnična specifikacija določa kvantitativno določevanje 16 policikličnih aromatskih ogljikovodikov (PAH) (glej preglednico 2) v blatu, tleh in obdelanih bioloških odpadkih z 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 in prisotnosti motečih snovi. Zaradi teh razlik ni možen opis enega splošnega postopka. Ta tehnična specifikacija vključuje preglednice odločanja, ki temeljijo na lastnostih vzorca, in 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.
General Information
Relations
Standards Content (Sample)
SIST-TS CEN/TS 16181
SLOVENSKA
TEHNIČNA
december 2013
SPECIFIKACIJA
Blato, obdelani biološki odpadki in tla – Določevanje policikličnih
aromatskih ogljikovodikov (PAO) s plinsko kromatografijo (GC) in s
tekočinsko kromatografijo visoke ločljivosti (HPLC)
Sludge, treated biowaste and soil – Determination of polycyclic aromatic
hydrocarbons (PAH) by gas chromatography (GC) and high performance liquid
chromatography (HPLC)
Boue, biodéchet traité et sol – Dosage des hydrocarbures aromatiques
polycycliques (HAP) par chromatographie en phase gazeuse et chromatographie
liquide à haute performance
Schlamm, behandelter Bioabfall und Boden – Bestimmung von polycyclischen
aromatischen Kohlenwasserstoffen (PAK) mittels Gaschromatographie (GC) und
Hochleistungs-Flüssigkeitschromatographie (HPLC)
Referenčna oznaka
ICS 13.030.20; 13.080.10 SIST-TS CEN TS 16181:2013 ((sl),en)
Nadaljevanje na straneh II do IV in od 1 do 42
© 2013-12. Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST-TS CEN/TS 16181 : 2013
NACIONALNI UVOD
Tehnična specifikacija SIST-TS CEN/TS 16181 ((sl),en), Blato, obdelani biološki odpadki in tla –
Določevanje policikličnih aromatskih ogljikovodikov (PAO) s plinsko kromatografijo (GC) in s
tekočinsko kromatografijo visoke ločljivosti (HPLC), 2013, ima status slovenske tehnične specifikacije
in je istovetna z evropsko tehnično specifikacijo CEN/TS 16181, Sludge, treated biowaste and soil –
Determination of polycyclic aromatic hydrocarbons (PAH) by gas chromatography (GC) and high
performance liquid chromatography (HPLC), 2013.
NACIONALNI PREDGOVOR
Evropsko tehnično specifikacijo CEN/TS 16181:2013 je pripravil tehnični odbor Evropskega komiteja
za standardizacijo CEN/TC 400 Horizontalni standardi na področju blata, obdelanih bioloških
odpadkov in tal, katerega sekretariat vodi DIN.
CEN je pripravil ta dokument na podlagi mandata M/330 Evropske komisije in Evropskega združenja
za prosto trgovino, ki narekuje pripravo standardov za vzorčenje in analizne metode za higienske in
biološke kakor tudi za anorganske in organske parametre, ki bi bili primerni za blata, obdelane
biološke odpadke in tla, kolikor je to tehnično izvedljivo.
Odločitev za privzem te tehnične specifikacije je dne 25. septembra 2013 sprejel tehnični odbor
SIST/TC KAT Kakovost tal.
ZVEZE S STANDARDI
S privzemom te evropske tehnične specifikacije veljajo za omenjeni namen referenčnih standardov vsi
standardi, navedeni v izvirniku, razen tistih, ki so že sprejeti v nacionalno standardizacijo:
SIST EN 15934 (en) Blato, obdelani biološki odpadki, tla in odpadki – Izračun suhe snovi z
določevanjem suhega ostanka ali vsebnosti vode
SIST EN 16179 (en) Blato, obdelani biološki odpadki in tla – Navodilo za pripravo vzorcev
SIST EN ISO 5667-15 (en) Kakovost vode – Vzorčenje – 15. del: Navodilo za konzerviranje in
ravnanje z blatom in vzorci sedimenta (ISO 5667-15)
SIST EN ISO 16720 (en) Kakovost tal – Priprava vzorcev za analizo z liofilizacijo (ISO 16720)
SIST EN ISO 22892 (en) Kakovost tal – Smernice za identifikacijo ciljnih spojin s plinsko
kromatografijo in masno spektrometrijo (ISO 22892)
SIST ISO 8466-1 (en) Kakovost vode – Umerjanje in vrednotenje analitskih metod in določitev
delovnih karakteristik – 1. del: Statistično vrednotenje linearne umerjalne
funkcije
IZRAZI IN DEFINICIJE
V tem dokumentu se uporabljajo naslednji izrazi in definicije:
3.1
kritični par
par kongenerjev, ki bodo ločeni po vnaprej določeni stopnji (npr. R = 0,5), s čimer se zagotovi, da
kromatografsko ločevanje izpolnjuje minimalna merila kakovosti
[VIR: EN 15308:2008, 3.6]
OPOMBA 1: Glej sliko 1.
II
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SIST-TS CEN/TS 16181 : 2013
Legenda:
∆t razlika v retenzijskem času dveh vrhov a in b v sekundah (s)
Ya širina vrha na bazni liniji vrha a v sekundah (s)
Yb širina vrha na bazni liniji vrha b v sekundah (s)
Slika 1: Primer kromatograma za kritični par
Naslednji definiciji sta opisani v SIST EN 16167, Blato, obdelani biološki odpadki in tla – Določevanje
polikloriranih bifenilov (PCB) s plinsko kromatografijo z masno selektivno detekcijo (GC/MS) in s
plinsko kromatografijo z detekcijo z zajetjem elektronov (GC/ECD):
3.2
kongener
element iste vrste, razreda ali skupine kemikalij, na primer vsak od 209 predstavnikov PCB
OPOMBA: Številke kongenerjev po IUPAC so za lažjo identifikacijo in ne predstavljajo zaporedja kromatografskih eluatov.
[VIR: EN 15308:2008, 3.2]
3.3
poliklorirani bifenil
PCB
bifenil, substituiran z enim do desetimi atomi klora
[VIR: EN 15308:2008, 3.1]
OSNOVA ZA IZDAJO TEHNIČNE SPECIFIKACIJE
– privzem tehnične specifikacije CEN/TS 16181:2013
III
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SIST-TS CEN/TS 16181 : 2013
OPOMBE
– Povsod, kjer se v besedilu tehnične specifikacije uporablja izraz “evropska tehnična
specifikacija”, v SIST-TS CEN/TS 16181:2013 to pomeni “slovenska tehnična specifikacija”.
– Nacionalni uvod in nacionalni predgovor nista sestavni del te tehnične specifikacije.
– Ta nacionalni dokument je istoveten s CEN/TS 16181:2013 in je objavljen z dovoljenjem
CEN
Management Centre
Avenue Marnix 17
B-1000 Brussels
This national document is identical with CEN/TS 16181:2013 and is published with the permission of
CEN
Management Centre
Avenue Marnix 17
B-1000 Brussels
IV
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TECHNICAL SPECIFICATION
CEN/TS 16181
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
October 2013
ICS 13.030.20
English Version
Sludge, treated biowaste and soil - Determination of polycyclic
aromatic hydrocarbons (PAH) by gas chromatography (GC) and
high performance liquid chromatography (HPLC)
Boues, bio-déchets traités et sols - Dosage des Schlamm, behandelter Bioabfall und Boden - Bestimmung
hydrocarbures aromatiques polycycliques (HAP) par von polycyclischen aromatischen Kohlenwasserstoffen
chromatographie en phase gazeuse et chromatographie (PAK) mittels Gaschromatographie (GC) und
liquide à haute performance Hochleistungs-Flüssigkeitschromatographie (HPLC)
This Technical Specification (CEN/TS) was approved by CEN on 16 July 2012 for provisional application.
The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to submit their
comments, particularly on the question whether the CEN/TS can be converted into a European Standard.
CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS available
promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the CEN/TS)
until the final decision about the possible conversion of the CEN/TS into an EN is reached.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United
Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2013 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 16181:2013: E
worldwide for CEN national Members.
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CEN/TS 16181:2013 (E)
Contents Page
Foreword .4
Introduction.5
1 Scope .6
2 Normative references . 7
3 Terms and definitions . 7
4 Principle .8
5 Interferences .8
5.1 Interference with sampling and extraction . 8
5.2 Interference with GC-MS . 9
5.3 Interferences with the HPLC . 9
6 Safety remarks . 9
7 Reagents . 10
7.1 General . 10
7.2 Reagents for extraction. 10
7.3 Reagents for clean-up . 10
7.3.1 Clean-up using aluminium oxide . 10
7.3.2 Clean-up using silica gel 60 for column chromatography . 10
7.3.3 Clean-up using gel permeation chromatography (GPC) . 11
7.3.4 Clean-up using liquid-liquid partition/DMF/cyclohexane . 11
7.4 Reagents for chromatographic analysis . 11
7.4.1 GC-Analysis . 11
7.4.2 HPLC-analysis . 11
7.5 Standards . 11
7.5.1 Reference substances, internal standards . 11
7.5.2 Injection standard . 12
7.6 Preparation of standard solutions . 12
7.6.1 General . 12
7.6.2 Standard solutions for HPLC-Analysis . 13
7.6.3 Standard solutions for GC-MS analysis . 13
7.6.4 Calibration standard solutions . 13
7.7 Preparation of internal standard solutions . 14
7.8 Preparation of injection standard solution . 14
8 Apparatus . 14
8.1 Extraction and clean-up procedures . 14
8.2 Gas chromatograph . 15
8.2.1 General . 15
8.3 High-performance liquid chromatograph . 15
9 Sample storage and preservation . 15
9.1 Sample storage . 15
9.2 Sample pretreatment . 16
10 Procedure . 16
10.1 Blank test . 16
10.2 Extraction . 16
10.2.1 General . 16
10.2.2 Extraction procedure 1: acetone/petroleum ether and agitation . 17
10.2.3 Extraction procedure 2: Soxhlet extraction (dry samples) . 18
10.2.4 Extraction procedure 3: acetone/petroleum ether/sodium chloride and agitation . 18
10.3 Concentration or dilution . 19
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CEN/TS 16181:2013 (E)
10.3.1 General .1 9
10.3.2 For HPLC analysis .1 9
10.4 Clean-up of the extract .1 9
10.4.1 General .1 9
10.4.2 Clean-up A – Aluminium oxide .2 0
10.4.3 Clean-up B – Silica gel .2 0
10.4.4 Clean-up C – Gel permeation chromatography (styrene divinylbenzene resin) . 21
10.4.5 Clean-up D – DMF/cyclohexane partitioning for aliphatic hydrocarbons removal . 21
10.5 Addition of the injection standard . 21
10.6 Gas chromatographic analysis (GC) .2 1
10.6.1 Gas chromatographic analysis with mass spectrometric detection . 21
10.6.2 Calibration of the method using an internal standard .2 2
10.6.3 Measurement .2 4
10.6.4 Identification .2 4
10.6.5 Check on method performance .2 4
10.6.6 Calculation .2 5
10.7 High-performance liquid chromatographic analysis (HPLC). 25
10.7.1 General .2 5
10.7.2 Chromatographic separation .2 5
10.7.3 Detection .2 6
10.7.4 Calibration .2 7
10.7.5 Measurement of samples .2 7
10.7.6 Calculation .2 7
11 Performance characteristics .2 8
12 Precision .2 8
13 Test report .2 8
Annex A (informative) Repeatability and reproducibility data .2 9
A.1 Materials used in the interlaboratory comparison study . 29
A.2 Interlaboratory comparison results .3 0
Annex B (informative) Examples of instrumental conditions and chromatograms. 32
B.1 Measurement of PAH with GC-MS . 32
B.2 Measurement of PAH with HPLC fluorescence .3 8
Bibliography .4 2
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CEN/TS 16181:2013 (E)
Foreword
This document (CEN/TS 16181:2013) has been prepared by Technical Committee CEN/TC 400 “Project
Committee - Horizontal standards in the fields of sludge, biowaste and soil”, the secretariat of which is held by
DIN.
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.
The preparation of this document by CEN is based on a mandate by the European Commission (Mandate
M/330), which assigned the development of standards on sampling and analytical methods for hygienic and
biological parameters as well as inorganic and organic determinants, aiming to make these standards
applicable to sludge, treated biowaste and soil as far as this is technically feasible.
According to the CEN-CENELEC Internal Regulations, the national standards organisations of the following
countries are bound to announce this Technical Specification: Austria, Belgium, Bulgaria, Croatia, Cyprus,
Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany,
Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,
Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.
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CEN/TS 16181:2013 (E)
Introduction
Polycyclic aromatic hydrocarbons (PAH) are ubiquitous because they are released in appreciable quantities
every year into the environment through the combustion of organic matters such as coal, fuel oils, petrol,
wood, refuse and plant materials. Since some of these PAH compounds are carcinogenic or mutagenic, their
presence in the environment (air, water, soil, sediment and waste) is regularly monitored and controlled. At
present determination of PAH is carried out in these matrices in most of the routine laboratories following the
preceding steps for sampling, pretreatment, extraction, clean-up by measurement of specific PAH by means
of gas chromatography in combination with mass spectrometric detection (GC-MS) or by high performance
liquid chromatography (HPLC) in combination with UV-DAD- or fluorescence-detection (HPLC-UV-DAD/FLD).
Both the GC-MS and the HPLC methods are included in this horizontal standard.
It is to be underlined that the target contamination level of PAH can lie in the range of about 0,01 mg/kg per
individual PAH (agricultural soil and sediment) to about 200 mg/kg and higher (e.g. contaminated soil at
coking plant sites or waste). The use of internal and injection standards is described in order to have an
internal check on execution of the extraction and clean-up procedure. The method is as far as possible in
agreement with the method described for PCBs (see EN 16167).
This document is the result of a desk study "Horizontal Technical Specification for determination of PAH in
sludge, soil and biowaste" in the project "Horizontal" and aims at evaluating the latest developments in
assessing PAH in sludge, soil, treated biowaste and neighbouring fields. After an evaluation study, in which
the ruggedness of the method was studied, a European-wide validation of the draft standard has taken place.
The results of the desk studies as well as the evaluation and validation studies have been subject to
discussions with all parties concerned in CEN.
This Technical Specification is applicable and validated for several types of matrices as indicated in Table 1
(see also Annex A for the results of the validation).
Table 1 — Matrices for which this Technical Specification is applicable and validated
Matrix Materials used for validation
Sludge Municipal sludge
Biowaste Fresh compost
WARNING — Persons using this Technical Specification should be familiar with usual laboratory
practice. This Technical Specification does not purport to address all of the safety problems, if any,
associated with its use. It is the responsibility of the user to establish appropriate safety and health
practices and to ensure compliance with any national regulatory conditions.
IMPORTANT — It is absolutely essential that tests conducted according to this Technical
Specification be carried out by suitably trained staff.
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CEN/TS 16181:2013 (E)
1 Scope
This Technical Specification 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.
Table 2 — Polycyclic aromatic hydrocarbons
which can be analysed using this Technical Specification
a
Target analyte
CAS-RN
Naphthalene 91-20-3
Acenaphthene 83-32-9
Acenaphthylene 208-96-8
Fluorene 86-73-7
Anthracene 120-12-7
Phenanthrene 85-01-8
Fluoranthene 206-44-0
Pyrene 129-00-0
Benz(a)anthracene 56-55-3
Chrysene 218-01-9
Benzo(b)fluoranthene 205-99-2
Benzo(k)fluoranthene 207-08-9
Benzo(a)pyrene 50-32-8
Indeno(1,2,3-cd)pyrene 193-39-5
Dibenz(a,h)anthracene 53-70-3
Benzo(ghi)perylene 191-24-2
a
CAS-RN Chemical Abstracts Service Registry Number.
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) may be ensured for each
individual PAH. This depends on instrument and sample.
Sludge, soil and treated biowaste may 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 Technical Specification 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/pressurised liquid extraction.
NOTE Other PAH compounds can also be analysed with this method, provided suitability has been proven.
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CEN/TS 16181:2013 (E)
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated references,
the latest edition of the referenced document (including any amendments) applies.
EN 15934, Sludge, treated biowaste, soil and waste — Calculation of dry matter fraction after determination of
dry residue or water content
EN 16179, Sludge, treated biowaste and soil — Guidance for sample pretreatment
EN ISO 5667-15, Water quality — Sampling — Part 15: Guidance on the preservation and handling of sludge
and sediment samples (ISO 5667-15)
EN ISO 16720, Soil quality — Pretreatment of samples by freeze-drying for subsequent analysis (ISO 16720)
EN ISO 22892, Soil quality — Guidelines for the identification of target compounds by gas chromatography
and mass spectrometry (ISO 22892)
ISO 8466-1, Water quality — Calibration and evaluation of analytical methods and estimation of performance
characteristics — Part 1: Statistical evaluation of the linear calibration function
ISO 18512, Soil quality — Guidance on long and short term storage of soil samples
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
critical pair
pair of congeners that will be separated to a predefined degree (e.g. R = 0,5) to ensure chromatographic
separation meets minimum quality criteria
[SOURCE: EN 15308:2008, 3.6]
Note 1 to entry: See Figure 1.
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CEN/TS 16181:2013 (E)
Key
∆t difference in retention times of the two peaks a and b in seconds (s)
Y peak width at the base of peak a in seconds (s)
a
Y peak width at the base of peak b in seconds (s)
b
Figure 1 — Example of a chromatogram of a critical pair
4 Principle
After pretreatment to reduce the moisture content and to increase the homogeneity (see 9.2), the test sample
is extracted with a solvent.
The extract is concentrated and interfering compounds are removed by a clean-up method suitable for the
specific matrix. The eluate is concentrated. For HPLC analysis, the concentrated eluate is taken up in an
appropriate less volatile water miscible polar solvent and the non-polar eluate residue is removed.
The extract is analysed by GC-MS using a capillary column with a stationary phase of low polarity or by
HPLC-UV-DAD/FLD with an appropriate reversed phase column.
PAH are identified and quantified with GC-MS by comparison of relative retention times and relative peak
heights (or peak areas) with respect to internal standards added, and with HPLC by using the corresponding
variables of the external standard solutions. The efficiency of the procedure depends on the composition of
the matrix that is investigated.
5 Interferences
5.1 Interference with sampling and extraction
Use sampling containers of materials (preferably of steel, aluminium or glass) that do not change the sample
during the contact time. Avoid plastics and other organic materials during sampling, sample storage or
extraction. Keep the samples from direct sunlight and prolonged exposure to light.
During storage of the samples, losses of PAH may occur due to adsorption on the walls of the containers. The
extent of the losses depends on the storage time.
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CEN/TS 16181:2013 (E)
5.2 Interference with GC-MS
Substances that co-elute with the target PAH may interfere with the determination. These interferences may
lead to incomplete resolved signals and may, depending on their magnitude, affect accuracy
...
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