1、BSI Standards PublicationBS ISO 15009:2012Soil quality Gas chromatographic determination of the content of volatile aromatic hydrocarbons, naphthalene and volatile halogenated hydrocarbons Purge-and-trap method with thermal desorptionBS EN ISO 15009:2013Copyright European Committee for Standardizati
2、on Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN ISO 15009:2013 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO 15009:2013. It is identical to ISO 15009:2012. It supersedes BS I
3、SO 15009:2012 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee EH/4, Soil quality.A list of organizations represented on this committee can be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 the necessary provisions
4、 of a contract. Users are responsible for its correct application. The British Standards Institution 2014. Published by BSI Standards Limited 2014ISBN 978 0 580 80026 9ICS 13.080.10Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published un
5、der the authority of the Standards Policy and Strategy Committee on 31 August 2012.Amendments/corrigenda issued since publicationDate Text affected31 January 2014 This corrigendum renumbers BS ISO 15009:2012 as BS EN ISO 15009:2013Copyright European Committee for Standardization Provided by IHS unde
6、r license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 15009 April 2013 ICS 13.080.10 English Version Soil quality - Gas chromatographic determination of the content of volatile aromatic hydrocarbo
7、ns, naphthalene and volatile halogenated hydrocarbons - Purge-and-trap method with thermal desorption (ISO 15009:2012) Qualit du sol - Dtermination par chromatographie en phase gazeuse des teneurs en hydrocarbures aromatiques volatils, en naphtalne et en hydrocarbures halogns volatils - Mthode par p
8、urge et pigeage avec dsorption thermique (ISO 15009:2012) Bodenbeschaffenheit - Gaschromatographische Bestimmung des Anteils an flchtigen aromatischen Kohlenwasserstoffen, Naphthalin und flchtigen Halogenkohlenwasserstoffen - Purge-und-Trap-Anreicherung mit thermischer Desorption (ISO 15009:2012)Thi
9、s European Standard was approved by CEN on 21 March 2013. 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 referenc
10、es 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 translation under the responsibility of a CEN me
11、mber 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, Finland, Former Yugoslav Republic of Macedonia, F
12、rance, 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 COMIT EUROPEN DE NORMALISATION EUROPISCHES
13、 KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2013 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 15009:2013: ECopyright European Committee for Standardization Provided by IHS under license with CENN
14、ot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN ISO 15009:2013 (E)EN ISO 15009:2013 (E)EN ISO 15009:2013 (E) 3 Foreword The text of ISO 15009:2012 has been prepared by Technical Committee ISO/TC 190 “Soil quality” of the International Organization for Standard
15、ization (ISO) and has been taken over as EN ISO 15009:2013 by Technical Committee CEN/TC 345 “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
16、the latest by October 2013, and conflicting national standards shall be withdrawn at the latest by October 2013. 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
17、or all such patent rights. 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 Republi
18、c 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. Endorsement notice The text of ISO 15009:2012 has been appro
19、ved by CEN as EN ISO 15009:2013 without any modification. Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS ISO 15009:2012ISO 15009:2012(E) ISO 2012 All rights reserved iiiConte
20、nts PageForeword iv1 Scope 12 Normative references . 13 Principle . 24 Reagents 24.1 Water, free of volatile aromatic and volatile halogenated hydrocarbons. 24.2 Internal standard compounds 24.3 Standard compounds . 34.4 Methanol (CAS RN 67-56-1) 44.5 Adsorbing agent 44.6 Cooling water for purge and
21、 trap 44.7 Inert carrier gas for the gas chromatograph 44.8 Nitrogen or helium as inert gas for the purge equipment 44.9 Standard solutions 45 Apparatus 56 Sampling, preservation and sample pretreatment . 76.1 General . 76.2 Sampling using vials prefilled with methanol . 76.3 Sampling using coring t
22、ube method 77 Procedure 77.1 Blank determination . 77.2 Extraction 87.3 Purge and trap 87.4 Gas chromatographic analysis 88 Calculation 109 Expression of results . 1110 Precision 1111 Test report . 11Annex A (informative) Relative retention time with respect to ethylbenzene-D10 of volatile aromatic
23、hydrocarbons and volatile halogenated hydrocarbons on the following columns: CP-Sil 5 CB and CP-Sil 13 CB .12Annex B (normative) Check on internal standards .13Annex C (informative) Validation 14Annex D (informative) Information on purge-and-trap instruments .17Bibliography .18BS ISO 15009:2012ISO 1
24、5009:2012(E) ISO 2012 All rights reserved iiiContents PageForeword iv1 Scope 12 Normative references . 13 Principle . 24 Reagents 24.1 Water, free of volatile aromatic and volatile halogenated hydrocarbons. 24.2 Internal standard compounds 24.3 Standard compounds . 34.4 Methanol (CAS RN 67-56-1) 44.
25、5 Adsorbing agent 44.6 Cooling water for purge and trap 44.7 Inert carrier gas for the gas chromatograph 44.8 Nitrogen or helium as inert gas for the purge equipment 44.9 Standard solutions 45 Apparatus 56 Sampling, preservation and sample pretreatment . 76.1 General . 76.2 Sampling using vials pref
26、illed with methanol . 76.3 Sampling using coring tube method 77 Procedure 77.1 Blank determination . 77.2 Extraction 87.3 Purge and trap 87.4 Gas chromatographic analysis 88 Calculation 109 Expression of results . 1110 Precision 1111 Test report . 11Annex A (informative) Relative retention time with
27、 respect to ethylbenzene-D10 of volatile aromatic hydrocarbons and volatile halogenated hydrocarbons on the following columns: CP-Sil 5 CB and CP-Sil 13 CB .12Annex B (normative) Check on internal standards .13Annex C (informative) Validation 14Annex D (informative) Information on purge-and-trap ins
28、truments .17Bibliography .18BS EN ISO 15009:2013ISO 15009:2012(E)Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-This page deliberately left blankCopyright European Committee for
29、 Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS ISO 15009:2012INTERNATIONAL STANDARD ISO 15009:2012(E)Soil quality Gas chromatographic determination of the content of volatile aromatic hydrocarbons, naphthal
30、ene and volatile halogenated hydrocarbons Purge-and-trap method with thermal desorption1 ScopeThis International Standard specifies a method for quantitative gas chromatographic determination of volatile hydrocarbons, naphthalene and volatile halogenated hydrocarbons in soil.This International Stand
31、ard 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 determination is dependent on the equipment used and the quality of the methanol grade used for the extraction of the soil sample.Under the condition
32、s specified in this International Standard, the following limits of determinations apply (expressed on a basis of dry matter):a) Typical limit of determination when using gas chromatography/flame ionization detection (GC/FID): volatile aromatic hydrocarbons: 0,1 mg/kg.b) Typical limit of determinati
33、on when using gas chromatography/electron capture detector (GC/ECD): volatile halogenated hydrocarbons: 0,01 mg/kgLower limits of determination for some compounds can be achieved by using mass spectrometry (MS) with selected ion detection.2 Normative referencesThe following referenced documents are
34、indispensable for the application 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.ISO 4799, Laboratory glassware CondensersISO 10381-1, Soil quality Sampling Part 1: Guida
35、nce 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 and industrial sites with regard to soil contaminationISO 11465, Soil quality Determin
36、ation of dry matter and water content on a mass basis Gravimetric method ISO 11465:1993/Cor 1:1994, Soil quality Determination of dry matter and water content on a mass basis Gravimetric method Technical Corrigendum 1ISO 15680, Water quality Gas-chromatographic determination of a number of monocycli
37、c aromatic hydrocarbons, naphthalene and several chlorinated compounds using purge-and-trap and thermal desorptionISO 18512, Soil quality Guidance on long and short term storage of soil samples ISO 2012 All rights reserved 1BS EN ISO 15009:2013Copyright European Committee for Standardization Provide
38、d by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS ISO 15009:2012ISO 15009:2012(E)ISO 22892, Soil quality Guidelines for the identification of target compounds by gas chromatography and mass spectrometry3 PrincipleTest samples are tak
39、en 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 methanol. After centrifugation, part of the methanol extract
40、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, whether or not via a cold trap, brought into a gas chromatograph.
41、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 detector (FID), electron capture detector (ECD), photo ionization det
42、ector (PID) or electrolytic conductivity detector (ELCD). Identification and quantification takes place by comparison of retention times and peak heights (or peak areas) towards an internal standard added with the corresponding variables of an external standard solution. The efficiency of the proced
43、ure 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 FIDs and ECDs, the confirmation of the identity of the detected c
44、ompounds 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 quantification can be done in a single run.NOTE 1 This International Standar
45、d follows the description of an off-line purge-and-trap method. The use of commercial available online instruments is allowed, provided that equivalent results are obtained during validation of this equipment. With such an instrument, purge and trap occurs on line with gas chromatography and detecti
46、on. Follow the manufacturers manual, especially regarding the items composing the apparatus which are listed in 5.1.1 to 5.1.9.NOTE 2 Other injection techniques, such as static headspace followed by thermal desorption (ISO 22155) or solid-phase micro-extraction (SPME), can be used, provided that the
47、ir applicability is proven.4 ReagentsAll reagents shall be of recognized analytical grade. Verify whether the reagents are applicable for this specific purpose and free of interfering compounds.4.1 Water, free of volatile aromatic and volatile halogenated hydrocarbonsUsually boiler water with a temp
48、erature 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 compounds from water. A sufficient amount of water from the same batch should be available to complete each batch of analyses, i
49、ncluding all preparations.4.2 Internal standard compounds4.2.1 For the determination of volatile aromatic hydrocarbons, preferably two internal standard compounds shall be selected that do not interfere with compounds present in the sample extract.Examples of suitable internal standards are toluene-D8 (CAS RN 2037-26-5),
