1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationSoil quality Gas chromatographic determination of volatile aromatic and halogenated hydrocarbons and selected ethers Static headspace methodBS EN ISO 22155:2013Copyright European
2、 Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN ISO 22155:2013National forewordThis British Standard is the UK implementation of EN ISO 22155:2013. It is identical to ISO 22155:2011. It supe
3、rsedes BS ISO 22155:2011 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee EH/4, Soil quality.A list of organizations represented on this committee can be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
4、 provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2013. Published by British Standards Limited 2013ISBN 978 0 580 79338 7 ICS 13.080.10 Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard
5、 was published under the authority of the Standards Policy and Strategy Committee on 30 April 2011.Amendments/corrigenda issued since publicationDate Text affected30 June 2013 This corrigendum renumbers BS ISO 22155:2011 as BS EN ISO 22155:2013BRITISH STANDARDCopyright European Committee for Standar
6、dization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 22155 February 2013 ICS 13.080.10 English Version Soil quality - Gas chromatographic determination of volatile ar
7、omatic and halogenated hydrocarbons and selected ethers - Static headspace method (ISO 22155:2011) Qualit du sol - Dosage des hydrocarbures aromatiques et halogns volatils et de certains thers par chromatographie en phase gazeuse - Mthode par espace de tte statique (ISO 22155:2011) Bodenbeschaffenhe
8、it - Gaschromatographische Bestimmung flchtiger aromatischer Kohlenwasserstoffe, Halogenkohlenwasserstoffe und ausgewhlter Ether - Statisches Dampfraum-Verfahren (ISO 22155:2011) This European Standard was approved by CEN on 5 February 2013. CEN members are bound to comply with the CEN/CENELEC Inter
9、nal 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 concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any
10、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 its own language and notified to the CEN-CENELEC Management Centre has the same status as the official ver
11、sions. 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,
12、 Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2013 CEN All rights of exploitation in any
13、form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 22155:2013: ECopyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-Foreword The text of ISO 22155:201
14、1 has been prepared by Technical Committee ISO/TC 190 “Soil quality” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 22155:2013 by Technical Committee CEN/TC 345 “Characterization of soils” the secretariat of which is held by NEN. This European Standard
15、shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by August 2013, and conflicting national standards shall be withdrawn at the latest by August 2013. Attention is drawn to the possibility that some of the elements of this do
16、cument may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any 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
17、: 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,
18、 Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 22155:2011 has been approved by CEN as EN ISO 22155:2013 without any modification. ii ISO 2013 All rights reservedBS EN ISO 22155:2013 EN ISO 22155:2013 (E)Copyright European Committee for Standardization Provide
19、d by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-iiiContents Page 1 Scope1 2 Normative references1 3 Principle .2 4 Reagents 2 5 Apparatus.5 6 Sampling, preservation and sample pretreatment.6 6.1 General .6 6.2 Sampling using vials pre
20、filled with methanol 6 6.3 Sampling using coring tube method.7 7 Procedure.7 7.1 Blank determination7 7.2 Extraction .7 7.3 Headspace analysis 7 7.4 Gas chromatographic analysis 8 8 Calculation .10 8.1 Calculation of the concentration of a volatile compound in the water sample 10 8.2 Calculation of
21、the concentration of a volatile compound in the soil sample11 9 Expression of results11 10 Precision 11 11 Test report11 Annex A (informative) Relative retention times with respect to ethylbenzene-D10 of volatile aromatic hydrocarbons and volatile halogenated hydrocarbons 12 Annex B (normative) Chec
22、k on internal standards .14 Annex C (informative) Validation (general) 15 Annex D (informative) Validation for the pathway soil/human.18 Bibliography21 BS EN ISO 22155:2013 ISO 22155:2011 (E)Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo repro
23、duction or networking permitted without license from IHS-,-,-iv Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-INTERNATIONAL STANDARD 1Soil quality Gas chromatographic determina
24、tion of volatile aromatic and halogenated hydrocarbons and selected ethers Static headspace method 1 Scope This International Standard specifies a static headspace method for quantitative gas chromatographic determination of volatile aromatic and halogenated hydrocarbons and selected aliphatic ether
25、s in soil. This International Standard is applicable to all types of soil. The limit of determination is dependent on the detection system 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 followi
26、ng limits of determination apply (expressed on the basis of dry matter): Typical limit of determination when using gas chromatography/flame ionization detection (GC/FID): volatile aromatic hydrocarbons: 0,2 mg/kg; aliphatic ethers as methyl tert-butyl ether (MTBE) and tert-amyl methyl ether (TAME):
27、0,5 mg/kg. Typical limit of determination when using gas chromatography/electron capture detection (GC/ECD): volatile halogenated hydrocarbons: 0,01 mg/kg to 0,2 mg/kg. Lower limits of determination can be achieved for some compounds by using mass spectrometry (MS) with selected ion detection (see A
28、nnex D). 2 Normative references The following referenced documents are 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 10381-1:2002,
29、 Soil quality Sampling Part 1: Guidance on the design of sampling programmes ISO 10381-2, Soil quality Sampling Part 2: Guidance on sampling techniques ISO 11465, Soil quality Determination of dry matter and water content on a mass basis Gravimetric method ISO 15680, Water quality Gas-chromatographi
30、c determination of a number of monocyclic aromatic hydrocarbons, naphthalene and several chlorinated compounds using purge-and-trap and theral desorption ISO 18512, Soil quality Guidance on long and short term storage of soil samples ISO 22155:201 (E)BS EN ISO 22155:2013 1Copyright European Committe
31、e for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-2 ISO 22892, Soil quality Guidelines for the identification of target compounds by gas chromatography and mass spectrometry 3 Principle Test samples are take
32、n from an untreated field-moist soil sample. To prevent losses of the volatiles, samples are taken in as undisturbed a way as possible in the field with a tube corer or by adding methanol immediately in the field. The test sample is extracted with methanol. An aliquot of the methanol extract is tran
33、sferred into a headspace vial with a defined amount of water and sealed. The temperature of the vials is stabilized in a thermostatic system to a temperature within the range 50 C to 80 C to achieve specified equilibrium conditions. Gas chromatographic analysis of the volatile compounds in gaseous p
34、hase in equilibrium with the water in the vials is carried out by using headspace injection and an appropriate capillary column. Volatile organic compounds are detected with appropriate detectors, such as a mass spectrometry detector (MS), flame ionization detector (FID), electron capture detector (
35、ECD), photo ionization detector (PID) or electrolytic conductivity detector (ELCD). Identification and quantification are made by comparison of retention times and peak heights (or peak areas), comparing to the internal standard added. When using non-specific detectors, such as FID and ECD, the conf
36、irmation 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 quantification can be done in a si
37、ngle run. 4 Reagents All 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 organic contaminants, showing negligible interferences in comparison with the smallest concen
38、tration to be determined. A sufficient amount of water from the same batch should be available to complete each batch of analyses, including all preparations. 4.2 Internal standard compounds 4.2.1 For the determination of volatile aromatic hydrocarbons, preferably two internal standards shall be sel
39、ected. They shall not interfere with compounds present in the methanol extract. Examples of suitable internal standards are: toluene-D8 (CAS-RN1)2037-26-5); ethylbenzene-D10 (CAS-RN 25837-05-2); 2-bromofluorobenzene (CAS-RN 1072-85-1). 4.2.2 For the determination of volatile halogenated hydrocarbons
40、, preferably two internal standards shall be selected. They shall not interfere with compounds present in the methanol extract. 1) CAS-RN: Chemical Abstracts System Registry Number BS EN ISO 22155:2013 ISO 22155:2011 (E)Copyright European Committee for Standardization Provided by IHS under license w
41、ith CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-3Examples of suitable internal standards are: 1,4-dichlorobutane (CAS-RN 110-56-5); ,-trifluorotoluene (CAS-RN 98-08-8); 2-bromofluorobenzene (CAS-RN 1072-85-1). 4.3 Volatile aromatic hydrocarbons Compound CAS-
42、RNBenzene 71-43-2Toluene 108-88-3Ethylbenzene 100-41-4o-Xylene 95-47-6m-Xylene 108-38-3p-Xylene 106-42-3Styrene 100-42-5Naphthalene 91-20-34.4 Volatile halogenated hydrocarbons Compound CAS-RNDichloromethane 75-09-2Trichloromethane 67-66-3Tetrachloromethane 56-23-51,1-Dichloroethane 75-34-31,2-Dichl
43、oroethane 107-06-21,1,1-Trichloroethane 79-01-61,1,2-Trichloroethane 79-00-51,2-Dichloropropane 78-87-51,2,3-Trichloropropane 98-18-4cis-1,3-Dichloropropene 10061-01-5trans-1,3-Dichloropropene 10061-02-6cis-1,2-Dichloroethene 156-59-2trans-1,2-Dichloroethene 156-60-53-Chloropropene 107-05-1Trichloro
44、ethene 79-01-6Tetrachloroethene 127-18-4Monochlorobenzene 108-90-71,2-Dichlorobenzene 95-50-1BS EN ISO 22155:2013 ISO 22155:2011 (E)Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-
45、,-4 4.5 Aliphatic ethers Compound CAS-RNMethyl tert-butyl ether (MTBE) 1634-04-4tert-Amyl methyl ether (TAME) 994-05-8NOTE This method can also be used for volatile organic compounds not included in this International Standard, provided it has been validated for each new compound. 4.6 Methanol (CAS-
46、RN 67-56-1), as a solvent for the extraction of soil samples and for the preparation of standard solutions. NOTE Other solvents which are readily soluble in water and do not interfere with the analytical process can be used as well, for example dimethylformamide (DMF) and dimethylsulfoxide (DMSO). 4
47、.7 Carrier gases for gas chromatography, helium, nitrogen or argon-methane ultrapure mixture. Other gases for gas chromatography shall be used in accordance with the instrument manufacturers instructions. 4.8 Standard solutions 4.8.1 Standard stock solutions for the volatile compounds in methanol Pr
48、epare the stock solutions by adding defined amounts (e.g. 100 l) of each standard compound (4.3, 4.4 and 4.5) with a microlitre syringe. Immerse the tip of the needle in the methanol solvent and weigh with an accuracy of 0,1 mg. NOTE 1 A convenient concentration (4 mg/ml) of the standard stock solution is obtained by weighing 100 mg of the standard substance and dissolving it in 25 ml of the solvent. The stock solution is stable for about 6 months when stored at 18 C. NOTE 2 For practical reasons, mixed standard stock solutions can also be prepared. 4.8.2
