EN ISO 27108-2013 en Water quality - Determination of selected plant treatment agents and biocide products - Method using solid-phase microextraction (SPME) followed by gas chromat.pdf

1、BS ISO27108:2010ICS 13.060.50NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDWater quality Determinationof selected planttreatment agents andbiocide products Method using solid-phase microextraction(SPME) followed by gaschromatography-massspectrometry (GC-MS)BS

2、EN ISO 27108:2013BS EN ISO 27108:2013ISBN 978 0 580 80224 9Amendments/corrigenda issued since publicationDate Comments31 December 2013 This corrigendum renumbers BS ISO 27108:2010 as BS EN ISO 27108:2013This British Standard was published under the authority of the Standards Policy and Strategy Comm

3、ittee on 31 May 2010. The British Standards Institution 2013. Published by BSI Standards Limited 2013National forewordThis British Standard is the UK implementation of EN ISO 27108:2013. It is identical to ISO 27108:2010. It supersedes BS ISO 27108:2010 which is withdrawn.The UK participation in its

4、 preparation was entrusted to Technical Committee EH/3, Water quality.A list of organizations represented on this committee can be obtained on request to its secretary.The publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct applic

5、ation.Compliance with a British Standard cannot confer immunity from legal obligations.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 27108 August 2013 ICS 13.060.50 English Version Water quality - Determination of selected plant treatment agents and biocide products - Method using solid-p

6、hase microextraction (SPME) followed by gas chromatography-mass spectrometry (GC-MS) (ISO 27108:2010) Qualit de leau - Dtermination dagents de traitement et de produits dusine slectionns - Mthode utilisant une micro-extraction en phase solide (MEPS) suivie dune chromatographie en phase gazeuse-spect

7、romtrie de masse (CG-SM) (ISO 27108:2010) Wasserbeschaffenheit - Bestimmung ausgewhlter Pflanzenschutzmittel und Biozidprodukte - Verfahren mittels Festphasenmikroextraktion (SPME) gefolgt von der Gaschromatographie und Massenspektrometrie (GC-MS) (ISO 27108:2010) This European Standard was approved

8、 by CEN on 12 April 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 references concerning such national stan

9、dards 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 its own language and n

10、otified 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, Germany, Greece, Hungary,

11、 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 KOMITEE FR NORMUNG CEN-CENELEC

12、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 27108:2013: EEN ISO 27108:2013 (E)3ForewordThe text of ISO 27108:2010 has been prepared by Technical Committee ISO/TC 147

13、 “Water quality” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 27108:2013 by Technical Committee CEN/TC 230 “Water analysis” the secretariat of which is held by DIN.This European Standard shall be given the status of a national standard, either by publ

14、ication of an identical text or by endorsement, at the latest by February 2014, and conflicting national standards shall be withdrawn at the latest by February 2014.Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELE

15、C 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: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic,

16、 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.Endorsemen

17、t noticeThe text of ISO 27108:2010 has been approved by CEN as EN ISO 27108:2013 without any modification.iiBS EN ISO 27108:2013EN ISO 27108:2013BS ISO 27108:2010ISO 27108:2010(E) ISO 2010 All rights reserved iiiContents Page Foreword iv Introduction.v 1 Scope1 2 Normative references1 3 Principle1 4

18、 Interferences 2 5 Reagents.4 6 Apparatus.5 7 Sampling and sample pretreatment 6 8 Procedure.6 9 Calibration8 10 Calculation .11 11 Expression of results11 12 Test report11 Annex A (informative) Examples of gas chromatograms for compounds listed in Table 1 .12 Annex B (informative) Mass spectra of c

19、ompounds of Table 1 (full-scan, EI, 70 eV)21 Annex C (informative) Precision data .35 Annex D (informative) General information about SPME .36 Bibliography37 BS ISO 27108:2010ISO 27108:2010(E) ISO 2010 All rights reserved iiiContents Page Foreword ivIntroduction.v1 Scope2 Normative references3 Princ

20、iple14 Interferences 25 Reagents.46 Apparatus.57 Sampling and sample pretreatment 8 Procedure.69 Calibration810 Calculation .11 Expression of results12 Test report11A Examples of gas chromatograms for compounds listed in Table 1 .12B Mass spectra of compounds of Table 1 (full-scan, EI, 70 eV)21C Pre

21、cision data .35Annex D (informative) General information about SPME .36Bibliography37 BS EN ISO 27108:2013ISO 27108:2010iiiI ( ) I 2010 All rights res rved iiiivIntr . e ref . t .i r .i tra of of ble 1 (full-scan, I, )i r isi .(inf tive) l .BS ISO 27108:2010ISO 27108:2010(E) ISO 2010 All rights rese

22、rved vIntroduction In recent years, ground water contamination as well as surface water contamination by pesticides has become a matter of public concern. Identification and quantification of pesticides at trace level concentrations often require both high sensitive chromatographic equipment and eff

23、ective enrichment steps. In the analysis of aqueous samples, sample preparation techniques including solid-phase extraction (SPE) are frequently the most time-consuming steps and in many cases can be effectively replaced by solid-phase microextraction (SPME). When using this International Standard,

24、it may be necessary in some cases to determine whether and to what extent particular problems could require the specification of additional marginal conditions. BS EN ISO 27108:2013ISO 27108:2010ivBS ISO 27108:2010ISO 27108:2010(E) iv ISO 2010 All rights reservedForeword ISO (the International Organ

25、ization 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 committee has beenestablishe

26、d 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 electrotechnical standardization.

27、International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Pub

28、lication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. 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

29、 rights. ISO 27108 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical, chemical and biochemical methods. BS ISO 27108:2010INTERNATIONAL STANDARD ISO 27108:2010(E) ISO 2010 All rights reserved 1Water quality Determination of selected plant treatment agents and

30、biocide products Method using solid-phase microextraction (SPME) followed by gas chromatography-mass spectrometry (GC-MS) WARNING Persons using this International Standard should be familiar with normal laboratory practice. This International Standard does not purport to address all of the safety pr

31、oblems, 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 International Standard be c

32、arried out by suitably trained staff. 1 Scope This International Standard specifies a method for the determination of the dissolved amount of selected plant treatment agents and biocide products in drinking water, ground water and surface water by solid-phase microextraction (SPME) followed by gas c

33、hromatography-mass spectrometry (GC-MS). The limit of determination depends on the matrix, on the specific compound to be analysed and on the sensitivity of the mass spectrometer. For most plant treatment agents and biocides to which this International Standard applies, it is at least 0,05 g/l. Vali

34、dation data related to a concentration range between 0,05 g/l and 0,3 g/l have been demonstrated in an interlaboratory trial. This method may be applicable to other compounds not explicitly covered by this International Standard or to other types of water. However, it is necessary to verify the appl

35、icability of this method for these special cases. NOTE Determinations by this International Standard are performed on small sample amounts (e.g. sample volumes between 8 ml and 16 ml). 2 Normative references The following referenced documents are indispensable for the application of this document. F

36、or dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 3696, Water for analytical laboratory use Specification and test methods ISO 5667-1, Water quality Sampling Part 1: Guidance on the desig

37、n of sampling programmes and sampling techniques ISO 5667-3, Water quality Sampling Part 3: Guidance on the preservation and handling of water samples 3 Principle Substances under investigation are extracted from the water sample by solid-phase microextraction (SPME) according to their equilibrium o

38、f distribution. The extraction is performed by a chemically modified fused-silica BS EN ISO 27108:2013ISO 27108:2010BS ISO 27108:2010ISO 27108:2010(E) 2 ISO 2010 All rights reservedfibre, the surface of which is coated with a suitable adsorbent polymer. During extraction, the fibre is immersed in th

39、e liquid sample. After completion of the extraction procedure, the fibre is drawn back into the needle, removed from the sample vial, and introduced directly into the GC injector. The analytes are transferred to the GC column by thermal desorption. The analytes are separated, identified and quantifi

40、ed by means of capillary gas chromatography with mass spectrometric detection (GC-MS) using electron impact (EI) ionisation mode. Table 1 Plant treatment agents and biocide products determined by this method Molar mass Reference No. in example chromatograms of Figure Name Molecular formula CAS regis

41、try No. g/mol A.1 A.2 A.3 Dichlobenil C7H3Cl2N 1194-65-6 172,0 1 1 1 Desethylatrazine C6H10ClN56190-65-4 187,6 2 2 3 Desethylterbutylazine C7H12ClN530125-63-4 201,7 3 3 2 Simazine C7H12ClN5122-34-9 201,7 4 4 7 Atrazine C8H14ClN51912-24-9 215,7 6 5 5 Lindane C6H6Cl658-89-9 290,8 7 6 8 Terbutylazine C

42、9H16ClN55915-41-3 229,7 8 7 6 Metribuzine C8H14N4OS 21087-64-9 214,3 9 8 14 Parathion-methyl C8H10NO5PS 298-00-0 263,2 10 9 11 Heptachlor C10H5Cl776-44-8 373,3 11 10 9 Terbutryn C10H19N5S 886-50-0 241,4 12 11 12 Aldrin C12H8Cl6309-00-2 364,9 13 12 10 Metolachlor C15H22ClNO251218-45-2 283,8 14 13 13

43、Parathion-ethyl C10H14NO5PS 56-38-2 291,3 15 14 15 exo-Heptachlorepoxide C10H5Cl7O 1024-57-3 389,3 16 16 16 Pendimethalin C13H19N3O440487-42-1 281,3 17 15 17 endo-Heptachlorepoxide C10H5Cl7O 28044-83-9 389,3 18 17 18 Triclosan C12H7Cl3O23380-34-5 289,5 19 18 19 Dieldrin C12H8Cl6O 60-57-1 380,9 20 19

44、 20 Carfentrazone-ethyl C15H14Cl2F3N3O3128639-02-1 412,2 21 20 21 Diflufenican C19H11F5N2O283164-33-4 394,3 22 21 22 Mefenpyr-diethyl C16H18Cl2N2O4135590-91-9 373,2 23 22 23 4 Interferences 4.1 Interferences during sampling To avoid interference, collect samples as specified in Clause 7, observing t

45、he instructions specified in ISO 5667-1 and ISO 5667-3. BS EN ISO 27108:2013ISO 27108:2010BS ISO 27108:2010ISO 27108:2010(E) ISO 2010 All rights reserved 34.2 Interferences during extraction procedure Commercially available SPME fibres differ frequently in quality. Variations in the selectivity of t

46、he materials also frequently occur from batch to batch, thus possibly causing significant deviations in extraction yield. This does not basically impair their suitability, apart from a resulting higher detection limit of individual substances. Inadequately conditioned fibres frequently result in low

47、er extraction yields and poorly reproducible results; therefore precondition new fibres according to Clause 8. Also condition used fibres by performing the whole SPME process using at least two sampling vials containing only water (5.1) prior to starting with the first sample of a new sample sequenc

48、e. Sensitivity of fibres gradually decreases throughout a sequence of samples. Therefore regular measurements of the reference solution within the sample sequence (see 9.1) are recommended. The fibre is still usable if the method shows required sensitivity for substances under investigation. Adding

49、sodium chloride to the sample results in a clear improvement of the extraction yield for most substances listed in Table 1. The addition of common salt (near saturation) is therefore recommended. Some substances listed in Table 1 show a reverse effect, which in most cases is weaker. Salt additions of 20 % of the saturation concentration (e.g. about 0,5 g of NaCl in an 8 ml water sample) cause a deterioration in reproducibility. It is important to keep to exactly the same salt additions for all samples of a calibrat