1、BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06Soil, treated biowaste and sludge - Determination of polycyclic aromatic hydrocarbons (PAH) by gas chromatography (GC) and high performance liquid chromatography (HPLC)BS EN 16181:2018EUROPEAN STANDARD NORME EUROPENNE E
2、UROPISCHE NORM EN 16181 June 2018 ICS 13.030.01; 13.080.10 Supersedes CEN/TS 16181:2013English Version Soil, treated biowaste and sludge - Determination of polycyclic aromatic hydrocarbons (PAH) by gas chromatography (GC) and high performance liquid chromatography (HPLC) Sols, biodchets traits et bo
3、ues - Dosage des hydrocarbures aromatiques polycycliques (HAP) par chromatographie en phase gazeuse et chromatographie liquide haute performance Boden, behandelter Bioabfall und Schlamm - Bestimmung von polycyclischen aromatischen Kohlenwasserstoffen (PAK) mittels Gaschromatographie (GC) und Hochlei
4、stungs-Flssigkeitschromatographie (HPLC) This European Standard was approved by CEN on 4 April 2018. 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
5、-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 trans
6、lation 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, Finlan
7、d, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDAR
8、DIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels 2018 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16181:2018 ENational forewordThis Brit
9、ish Standard is the UK implementation of EN 16181:2018.The UK participation in its preparation was entrusted to Technical Committee EH/4, Soil quality.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all th
10、e necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2018 Published by BSI Standards Limited 2018ISBN 978 0 580 99391 6ICS 13.030.01; 13.080.10Compliance with a British Standard cannot confer immunity from legal obligations. This
11、British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 June 2018.Amendments/corrigenda issued since publicationDate Text affectedBRITISH STANDARDBS EN 16181:2018EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16181 June 2018 ICS 13.030.01; 13.080
12、.10 Supersedes CEN/TS 16181:2013English Version Soil, treated biowaste and sludge - Determination of polycyclic aromatic hydrocarbons (PAH) by gas chromatography (GC) and high performance liquid chromatography (HPLC) Sols, biodchets traits et boues - Dosage des hydrocarbures aromatiques polycyclique
13、s (HAP) par chromatographie en phase gazeuse et chromatographie liquide haute performance Boden, behandelter Bioabfall und Schlamm - Bestimmung von polycyclischen aromatischen Kohlenwasserstoffen (PAK) mittels Gaschromatographie (GC) und Hochleistungs-Flssigkeitschromatographie (HPLC) This European
14、Standard was approved by CEN on 4 April 2018. 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 concernin
15、g 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 it
16、s 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, Former Yugoslav Republic of Macedonia, France, Germa
17、ny, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOM
18、ITEE FR NORMUNG CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels 2018 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16181:2018 EBS EN 16181:2018EN 16181:2018 (E) 2 Contents Page European foreword 4 Introductio
19、n 5 1 Scope 6 2 Normative references 7 3 Terms and definitions . 7 4 Principle . 8 5 Interferences 9 5.1 Interference with sampling and extraction. 9 5.2 Interference with GC-MS 9 5.3 Interferences with the HPLC . 9 6 Safety remarks . 10 7 Reagents . 10 8 Apparatus 15 9 Sample storage and preservati
20、on . 17 9.1 Sample storage . 17 9.2 Sample pretreatment 17 10 Procedure 18 10.1 Blank test . 18 10.2 Extraction 18 10.2.1 General 18 10.2.2 Extraction procedure 1: acetone/hexane-like solvent and agitation 19 10.2.3 Extraction procedure 2: Soxhlet extraction (dry samples) . 19 10.2.4 Extraction proc
21、edure 3: acetone/petroleum ether/sodium chloride and agitation . 20 10.3 Concentration or dilution 20 10.3.1 General 20 10.3.2 For HPLC analysis . 21 10.4 Clean-up of the extract 21 10.4.1 General 21 10.4.2 Clean-up A Aluminium oxide . 22 10.4.3 Clean-up B Silica gel 22 10.4.4 Clean-up C Gel permeat
22、ion chromatography (styrene divinylbenzene resin) 22 10.4.5 Clean-up D DMF/cyclohexane partitioning for aliphatic hydrocarbons removal 23 10.5 Addition of the injection standard 23 10.6 Gas chromatographic analysis (GC) . 23 10.6.1 Gas chromatographic analysis with mass spectrometric detection . 23
23、10.6.2 Calibration of the method using an internal standard 24 10.6.3 Measurement 25 10.6.4 Identification 25 10.6.5 Check on method performance 25 10.6.6 Calculation . 26 10.7 High-performance liquid chromatographic analysis (HPLC) . 27 10.7.1 General 27 10.7.2 Chromatographic separation 27 BS EN 1
24、6181:2018EN 16181:2018 (E) 3 10.7.3 Detection 27 10.7.4 Calibration. 28 10.7.5 Measurement of samples . 29 10.7.6 Calculation 29 11 Performance characteristics 29 12 Precision 30 13 Test report 30 Annex A (informative) Repeatability and reproducibility data 31 A.1 Materials used in the interlaborato
25、ry 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 BS EN 16181:2018EN 16181:2018 (E) 4 European for
26、eword This document (EN 16181:2018) has been prepared by Technical Committee CEN/TC 444 “Test methods for environmental characterization of solid matrices”, the secretariat of which is held by NEN. This European Standard shall be given the status of a national standard, either by publication of an i
27、dentical text or by endorsement, at the latest by December 2018, and conflicting national standards shall be withdrawn at the latest by December 2018. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN not be held responsible for
28、 identifying any or all such patent rights. This document supersedes CEN/TS 16181:2013. 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 Commi
29、ssion (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 fea
30、sible. 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, Former Yugoslav Republic of Macedonia, Fran
31、ce, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 16181:2018EN 16181:2018 (E) 5 Introduction Polycyclic aromatic hyd
32、rocarbons (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 prese
33、nce 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 s
34、pecific 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 standar
35、d. 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 “Horizont
36、al European Standard 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 stud
37、ied, 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 European Standard is applicable and validated for several types of matrices
38、 as indicated in Table 1 (see also Annex A for the results of the validation). Table 1 Matrices for which this European Standard is applicable and validated Matrix Materials used for validation Sludge Municipal sludge Biowaste Fresh compost Soil Sandy soil WARNING Persons using this European Standar
39、d should be familiar with usual laboratory practice. This European Standard 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 re
40、gulatory conditions. IMPORTANT It is absolutely essential that tests conducted according to this European Standard be carried out by suitably trained staff. BS EN 16181:2018EN 16181:2018 (E) 6 1 Scope This European Standard specifies the quantitative determination of 16 polycyclic aromatic hydrocarb
41、ons (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 usin
42、g this European Standard Target analyte CAS-RNaNaphthalene 91203 Acenaphthene 83329 Acenaphthylene 208968 Fluorene 86737 Anthracene 120127 Phenanthrene 85018 Fluoranthene 206440 Pyrene 129000 Benzaanthracene 56553 Chrysene 218019 Benzobfluoranthene 205992 Benzokfluoranthene 207089 Benzoapyrene 50328
43、 Indeno1,2,3-cdpyrene 193395 Dibenza,hanthracene 53703 Benzoghiperylene 191242 aCAS-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. T
44、ypically, 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 s
45、ubstances. 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 so
46、xhlet/pressurized liquid extraction. NOTE Other PAH compounds can also be analysed with this method, provided suitability has been proven. BS EN 16181:2018EN 16181:2018 (E) 7 2 Normative references The following documents are referred to in the text in such a way that some or all of their content co
47、nstitutes requirements 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 15934, Sludge, treated biowaste, soil and waste Calculation of dry matter fraction after determi
48、nation 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 sample
49、s 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
