EN ISO 15009-2016 en Soil quality - Gas chromatographic determination of the content of volatile aromatic hydrocarbons naphthalene and volatile halogenated hydrocarbons - Purge-and.pdf

1、BSI Standards PublicationBS EN ISO 15009:2016Soil quality Gaschromatographicdetermination of thecontent of volatile aromatichydrocarbons, naphthaleneand volatile halogenatedhydrocarbons Purge-and-trap method with thermaldesorptionBS EN ISO 15009:2016 BRITISH STANDARDNational forewordThis British Sta

2、ndard is the UK implementation of EN ISO 15009:2016. It supersedes BS EN ISO 15009:2013 which iswithdrawn.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.

3、This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2016.Published by BSI Standards Limited 2016ISBN 978 0 580 87551 9 ICS 13.080.10 Compliance with a British Standard cannot con

4、fer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 March 2016.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 15009 March 2

5、016 ICS 13.080.10 Supersedes EN ISO 15009:2013English Version Soil quality - Gas chromatographic determination of the content of volatile aromatic hydrocarbons, naphthalene and volatile halogenated hydrocarbons - Purge-and-trap method with thermal desorption (ISO 15009:2016) Qualit du sol - Dtermina

6、tion par chromatographie en phase gazeuse des teneurs en hydrocarbures aromatiques volatils, en naphtalne et en hydrocarbures halogns volatils - Mthode par purge et pigeage avec dsorption thermique (ISO 15009:2016) Bodenbeschaffenheit - Gaschromatographische Bestimmung des Anteils an flchtigen aroma

7、tischen Kohlenwasserstoffen, Naphthalin und flchtigen Halogenkohlenwasserstoffen - Purge-und-Trap-Anreicherung mit thermischer Desorption (ISO 15009:2016) This European Standard was approved by CEN on 23 January 2016. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which st

8、ipulate 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 Europea

9、n 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 t

10、he 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, Roman

11、ia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2016 CEN All rights of exploitation in any form and by

12、any means reserved worldwide for CEN national Members. Ref. No. EN ISO 15009:2016 EBS EN ISO 15009:2016EN ISO 15009:2016 (E) 3 European foreword This document (EN ISO 15009:2016) has been prepared by Technical Committee ISO/TC 190 “Soil quality” in collaboration with Technical Committee CEN/TC 345 “

13、Characterization of soils” 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 identical text or by endorsement, at the latest by September 2016, and conflicting national standards shall be withdrawn at the lat

14、est by September 2016. 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 supersedes EN ISO 15009:2013. According to the CE

15、N-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, France, Germany, Greece, Hunga

16、ry, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 15009:2016 has been approved by CEN as EN ISO 15009:2016 without any mo

17、dification. ISO 15009:2016(E)Foreword iv1 Scope . 12 Normative references 13 Principle 24 Reagents 24.1 Water, free of volatile aromatic and volatile halogenated hydrocarbons . 24.2 Internal standards 24.3 Standard compounds . 34.3.1 Volatile aromatic hydrocarbons 34.3.2 Volatile halogenated hydroca

18、rbons . 34.4 Methanol . 44.5 Adsorbing agent . 44.6 Cooling water for purge and trap 44.7 Inert gas for the gas chromatograph 54.8 Nitrogen or helium as inert gas for the purge equipment . 54.9 Standard solutions . 54.9.1 Standard stock solutions for volatile aromatic and halogenated compounds in me

19、thanol, 4 g/l . 54.9.2 Internal standard solutions in methanol, 4 g/l 54.9.3 Calibration solutions 54.10 Methanol containing internal standards 65 Apparatus . 66 Sampling, preservation and sample pretreatment 76.1 General . 76.2 Sampling using vials pre-filled with methanol 86.3 Sampling using corin

20、g tube method . 87 Procedure. 87.1 Blank determination 87.2 Extraction 97.3 Purge and trap . 97.4 Gas chromatographic analysis . 97.4.1 Gas chromatographic conditions . 97.4.2 Calibration 107.4.3 Measurement . 118 Calculation .128.1 Calculation of the concentration of a volatile compound in the wate

21、r sample 128.2 Calculation of the concentration of a volatile compound in the soil sample 129 Expression of results .1310 Precision 1311 Test report 13Annex A (informative) Relative retention time with respect to ethylbenzene-D10 of volatile aromatic hydrocarbons and volatile halogenated hydrocarbon

22、s on following columns: CP-Sil 5 CB and CP-Sil 13 CB 14Annex B (normative) Check on internal standards 16Annex C (informative) Validation 17Annex D (informative) Information on purge and trap instruments.20 ISO 2016 All rights reserved iiiContents PageBS EN ISO 15009:2016 ISO 15009:2016(E)ForewordIS

23、O (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical co

24、mmittee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electro

25、technical standardization.The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was draf

26、ted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rig

27、hts. Details of any patent rights identified during the development of the document will be in the Introduction and/or on the ISO list of patent declarations received (see www.iso.org/patents).Any trade name used in this document is information given for the convenience of users and does not constit

28、ute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationThe commi

29、ttee responsible for this document is ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical methods and soil characteristics.This third edition cancels and replaces the second edition (ISO 15009:2012), which has been technically revised.iv ISO 2016 All rights reservedBS EN ISO 15009:2016 INTERNATION

30、AL STANDARD ISO 15009:2016(E)Soil quality Gas chromatographic determination of the content of volatile aromatic hydrocarbons, naphthalene and volatile halogenated hydrocarbons Purge-and-trap method with thermal desorption1 ScopeThis International Standard specifies a method for quantitative gas-chro

31、matographic determination of volatile aromatic hydrocarbons, naphthalene and volatile halogenated hydrocarbons in soil.This International Standard is applicable to all types of soil.NOTE In the case of unsaturated peaty soils, absorption of the extraction solution may occur.The lower limit of quanti

32、fication is dependent on the equipment used and the quality of the methanol grade used for the extraction of the soil sample.Under the conditions specified in this International Standard the following limits of quantification apply (expressed on basis of dry matter):Typical limit of quantification w

33、hen using GC-FID: Volatile aromatic hydrocarbons: 0,1 mg/kgTypical limit of quantification when using GC-ECD: Volatile halogenated hydrocarbons: 0,01 mg/kgLower limits of quantification for some compounds can be achieved by using mass spectrometry (MS) with selected ion detection.2 Normative referen

34、cesThe 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.ISO 4

35、799, Laboratory glassware CondensersISO 10381-1, Soil quality Sampling Part 1: Guidance on the design of sampling programmesISO 10381-2, Soil quality Sampling Part 2: Guidance on sampling techniquesISO 10381-5, Soil quality Sampling Part 5: Guidance on the procedure for the investigation of urban an

36、d industrial sites with regard to soil contaminationISO 11465, Soil quality Determination of dry matter and water content on a mass basis Gravimetric methodISO 15680, Water quality Gas-chromatographic determination of a number of monocyclic aromatic hydrocarbons, naphthalene and several chlorinated

37、compounds using purge-and-trap and thermal desorptionISO 18512, Soil quality Guidance on long and short term storage of soil samples ISO 2016 All rights reserved 1BS EN ISO 15009:2016 ISO 15009:2016(E)ISO 22892, Soil quality Gui delines for the identification of target compounds by gas chromatograph

38、y and mass spectrometry3 PrincipleTest samples are taken from an untreated field moist soil sample. To prevent losses of the volatiles, samples are taken as undisturbed as possible in the field with a tube corer or by adding methanol immediately in the field.The test sample is extracted with methano

39、l. After centrifugation, if necessary, part of the methanol extract is brought into a purge vessel filled with water. The volatile compounds are purged with nitrogen or helium and adsorbed on a suitable adsorbing agent. The adsorbed compounds are desorbed thermally and by means of a carrier gas flow

40、, whether or not via a cold trap, brought into a gas chromatograph. The various compounds are separated by using a capillary column with an immobile phase of low polarity. Volatile organic compounds are detected with appropriate detectors such as: mass spectrometric detector (MS), flame ionization d

41、etector (FID), electron capture detector (ECD), photo ionization detector (PID) or electrolytic conductivity detector (ELCD). Identification and quantification takes place by comparison of retention times and peak heights (or peak areas) towards internal standard added with the corresponding variabl

42、es of an external standard solution. The efficiency of the procedure depends on the composition of the soil that is investigated. The described procedure does not take into account incomplete extraction caused by structure and composition of the soil sample.When using non-specific detectors such as

43、FID and ECD, the confirmation of the identity of the detected compounds and their concentrations should be done by repeating the gas chromatographic analysis using a column of different polarity. When using gas chromatography-mass spectrometry (GC-MS), the identity confirmation and the quantificatio

44、n can be done in a single run.NOTE This International Standard follows the description of an off-line purge and trap method. The use of commercially available online instruments is allowed provided that equivalent results are obtained during validation of this equipment. With such an instrument purg

45、e and trap occurs on line with gas chromatography and detection. Follow the manual of the manufacturer especially regarding the items 5.2.1 to 5.2.9.4 ReagentsAll reagents shall be of recognized analytical grade. Verify whether the reagents are applicable for this specific purpose and free of interf

46、ering compounds.4.1 Water, free of volatile aromatic and volatile halogenated hydrocarbonsUsually boiler water with a temperature of at least 80 C and 1 day old can be applied. Purging with an inert gas, e.g. a flow of 10 ml/min of nitrogen for 30 min, is another means of removing interfering compou

47、nds from water. A sufficient amount of water from the same batch should be available to complete each batch of analyses, including all preparations.4.2 Internal standards4.2.1 For the determination of volatile aromatic hydrocarbons preferably two internal standards shall be selected from Table 1. Th

48、ey shall not interfere with compounds present in the sample extract.2 ISO 2016 All rights reservedBS EN ISO 15009:2016 ISO 15009:2016(E)Table 1 Examples of suitable internal standards for the determination of volatile aromatic hydrocarbonsCompound name CAS-RNaEC-NbToluene-D8 2037265 2180095Ethylbenz

49、ene-D10 25837052 24729282-Bromofluorobenzene 1072851 2140183aChemical Abstracts Service Registry NumberbEC-Number4.2.2 For the determination of volatile halogenated hydrocarbons preferably two internal standards shall be selected from Table 2. They shall not interfere with compounds present in the sample extract.Table 2 Examples of suitable internal standards for the determination of volatile halogenated hydrocarbonsCompound name CAS-RNaEC-Nb1,4-Dichlorobutane 110565 2037781,-Trifluorotoluene 9808