1、BSI Standards PublicationBS EN ISO 18635:2016W a t e r q u a l i t y D e t e r m i n a t i o nof short-chain polychlorinatedalkanes (SCCPs) in sediment,sewage sludge and suspended(particulate) matter Methodusing gas chromatography-mass spectrometry (GC-MS)and electron capture negativeionization (ECN
2、I)BS EN ISO 18635:2016 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO18635:2016. The UK participation in its preparation was entrusted to TechnicalCommittee EH/3/2, Physical chemical and biochemical methods.A list of organizations represented on this commit
3、tee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2016.Published by BSI Standards Limited 2016ISBN 978 0 580 82369 5ICS 13.060.50Co
4、mpliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 30 April 2016.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dEUROPEAN STANDARD NORME EUROP
5、ENNE EUROPISCHE NORM EN ISO 18635 April 2016 ICS 13.060.50 English Version Water quality - Determination of short-chain polychlorinated alkanes (SCCPs) in sediment, sewage sludge and suspended (particulate) matter - Method using gas chromatography-mass spectrometry (GC-MS) and electron capture negat
6、ive ionization (ECNI) (ISO 18635:2016) Qualit de leau - Dtermination des alcanes polychlors chane courte dans les sdiments et matires en supsension (particules) - Mthode par chromatographie en phase gazeuse-spectromtrie de masse (CPG-SM) et ionisation chimique ngative (ICN) (ISO 18635:2016) Wasserbe
7、schaffenheit - Bestimmung kurzkettiger polychlorierter Alkane (SCCP) in Sediment, Klrschlamm und Schwebstoffen - Gaschromatographisch-massenspektrometrisches Verfahren (GC-MS) unter Anwendung negativer chemischer Ionisation und Elektroneneinfang (ECNI) (ISO 18635:2016) This European Standard was app
8、roved by CEN on 20 February 2016. 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 natio
9、nal 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 its own langua
10、ge 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, Germany, Greece,
11、Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey andUnited Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-C
12、ENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2016 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 18635:2016 EBS EN ISO 18635:2016EN ISO 18635:2016 (E) 3 European foreword This document (EN ISO 18635:2016) has be
13、en prepared by Technical Committee ISO/TC 147 “Water quality” in collaboration with 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 publication of an identical text or by endor
14、sement, at the latest by October 2016, and conflicting national standards shall be withdrawn at the latest by October 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 ident
15、ifying 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, Denmark, Estonia, Finland, Former Yugos
16、lav 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. Endorsement notice The text of ISO 18635:2016 has
17、 been approved by CEN as EN ISO 18635:2016 without any modification. BS EN ISO 18635:2016ISO 18635:2016(E)Foreword ivIntroduction v1 Scope . 12 Normative references 13 Principle 14 Interferences 25 Reagents . 36 Apparatus . 67 Sampling and sample pretreatment 78 Procedure. 78.1 Extraction 78.2 Extra
18、ct clean-up . 78.3 Measurement and integration of the chromatogram. 88.4 Calibration 88.4.1 General 88.4.2 Basic calibration . 98.4.3 Identification and quantification with mass fragment combinations 108.4.4 Calculation of the results . 108.4.5 Quality checks for internal standardization 119 Express
19、ion of results .1110 Test report 11Annex A (normative) Programme for pressurized liquid extraction 12Annex B (informative) Explanation of the calibration of the sum of SCCPs with multiple linear regression .13Annex C (informative) Examples of typical GC-MS conditions 18Annex D (normative) Alternativ
20、e clean-up with column chromatography .22Annex E (informative) Alternative clean-up with gel chromatography 24Annex F (informative) Typical chromatograms of standard solutions 1 g/ml .25Annex G (informative) Presentation of goodness of fit of the calibration 26Annex H (informative) Example for recov
21、eries of quality assurance solutions .27Annex I (informative) Chromatograms of real samples.29Annex J (informative) Performance data 31Annex K (informative) Quality control check solutions 32Bibliography .33 ISO 2016 All rights reserved iiiContents PageBS EN ISO 18635:2016ISO 18635:2016(E)ForewordIS
22、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
23、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
24、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
25、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
26、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
27、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
28、ttee responsible for this document is ISO/TC 147, Water quality, Subcommittee SC 2, Physical, chemical and biochemical methods.iv ISO 2016 All rights reservedBS EN ISO 18635:2016ISO 18635:2016(E)IntroductionThe user should be aware that particular problems might require the specifications of additio
29、nal marginal conditions. ISO 2016 All rights reserved vBS EN ISO 18635:2016BS EN ISO 18635:2016Water quality Determination of short-chain polychlorinated alkanes (SCCPs) in sediment, sewage sludge and suspended (particulate) matter Method using gas chromatography-mass spectrometry (GC-MS) and electr
30、on capture negative ionization (ECNI)WARNING Persons using this document should be familiar with normal laboratory practice. This document 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
31、 health practices and to ensure compliance with any national regulatory conditions.IMPORTANT It is absolutely essential that tests conducted in accordance with this document be carried out by suitably qualified staff.1 ScopeThis International Standard specifies a method for the quantitative determin
32、ation of the sum of short-chain polychlorinated n-alkanes also known as short-chain polychlorinated paraffins (SCCPs) in the carbon bond range, n-C10to n-C13, inclusive in mixtures with chlorine mass fractions (“contents“) between 50 % and 67 %, including approximately 6 000 of approximately 8 000 c
33、ongeners.This method is applicable to the determination of the sum of SCCPs in sediment and suspended (particulate) matter, sewage sludge, and soil using gas chromatography-mass spectrometry with electron capture negative ionization (GC-ECNI-MS).Depending on matrix and the detection capabilities of
34、the GC-ECNI-MS, the method can be applied to samples containing, e.g. 0,03 g/g to 3 g/g sum of SCCPs.2 Normative referencesThe 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
35、 applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 5667-12, Water quality Sampling Part 12: Guidance on sampling of bottom sedimentsISO 5667-13, Water quality Sampling Part 13: Guidance on sampling of sludgesISO 5667-17, Water quali
36、ty Sampling Part 17: Guidance on sampling of bulk suspended solidsISO 8466-1, Water quality Calibration and evaluation of analytical methods and estimation of performance characteristics Part 1: Statistical evaluation of the linear calibration functionISO 12010, Water quality Determination of short-
37、chain polychlorinated alkanes (SCCPs) in water Method using gas chromatography-mass spectrometry (GC-MS) and negative-ion chemical ionization (NCI)ISO/TS 13530, Water quality Guidance on analytical quality control for chemical and physicochemical water analysis3 PrincipleDetermination of the sum of
38、SCCPs in the carbon bond range, n-C10to n-C13, inclusive in technical and environmental transposed mixtures with chlorine mass fractions (“contents“) between 50 % and 67 % INTERNATIONAL STANDARD ISO 18635:2016(E) ISO 2016 All rights reserved 1BS EN ISO 18635:2016ISO 18635:2016(E)(e.g. approximately
39、3 to 10 chlorine atoms per molecule) and independent of the C-number distribution pattern of the congeners. No recognition of the chlorine content is necessary.The samples are fortified with an internal standard and extracted using pressurized liquid extraction with an organic solvent. The sample ex
40、traction procedure is followed by a clean-up procedure by column chromatography and gel permeation chromatography to eliminate interfering compounds. Gas chromatography (GC) is undertaken using a short capillary column within a short retention time range. The detection of selected mass fragments is
41、carried out using mass spectrometry (MS) in selected ion-monitoring mode using electron capture negative ionization mode (ECNI). The mass fragments and the compositions of the calibration solutions used in this International Standard are essential for the analysis of the sum of SCCPs.The selected io
42、n chromatogram is integrated over the full retention time range of the SCCPs. The quantification of the sum of SCCPs is carried out after establishing a calibration by a multiple linear regression measuring solutions of different SCCP mixtures fortified with an internal standard.The analysed sum of
43、SCCPs includes the variety of SCCPs with their differing chlorine content and C-number distribution patterns as found in technical mixtures, as well as compositions in the environment. The calibration requires at least three differently composed standard mixtures.These standard mixtures mimic differ
44、ent mixtures found in the environment. Only the multiple linear regression quantification with these specific mixtures enables the quantification of the variety of observed mixtures of SCCP in the environment and in technical compositions described in the scope and in Reference 6. It is not possible
45、 to use only one standard mixture for that complex task.4 InterferencesNon-specific matrix interferences, as well as interferences from other environmental situations, are dealt with using the given clean-up procedure. A further reduction of matrix effects can be achieved by reducing the mass spectr
46、ometric resolution to, e.g., 0,4 amu, which is often possible with a quadrupole mass spectrometer. The exact masses are 374,9588; 410,9169; and 422,9355 (see Reference 6).Applying the entire procedure, a selection of chlorinated pollutants has been tested and found not to cause interferences below t
47、he concentrations given in Table 1.Table 1 Highest concentration level which causes no interferences higher than the limit of quantification of 0,03 g/gPotential interfering compounds Highest concentration level which causes no interferences higher than the limit of quantification of 0,03 g/gAroclor
48、 1262a0,25 g/gAroclor 1242a2 g/gAroclor 1221a2 g/gCampheclor (toxaphene) 0,35 g/gHalowax 1014a2 g/gHalowax 1051a0,08 g/gMCCP (medium-chain chlorinated n-alkanes) 42 % 2 g/gMCCP (medium-chain chlorinated n-alkanes) 52 % 1,2 g/gMCCP (medium-chain chlorinated n-alkanes) 57 % 2 g/gaAroclor 1262, Aroclor
49、 1242, Aroclor 1221, Halowax 1014, and Halowax 1051 are products commercially available. This information is given for the convenience of users of this document and does not constitute an endorsement by ISO of these products.2 ISO 2016 All rights reservedBS EN ISO 18635:2016ISO 18635:2016(E)5 Reagents Use solvents and reagents of sufficient purity, i.e. with negligibly low concentrations of SCCPs, e.g. lower than the limit of detection of the method.Check blanks regularly over the entire procedure t
