BS EN ISO 18857-2-2011 Water quality Determination of selected alkylphenols Gas chromatographic-mass spectrometric determination of alkylphenols their ethoxylates and bisphenol A ir.pdf

1、BS EN ISO18857-2:2011ICS 13.060.50NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISHSTANDARDWaterqualityDeterminationofselectedalkylphenolsPart2:Gaschromatographic-massspectrometricdeterminationofalkylphenols,theirethoxylatesandbisphenolAinnon-filteredsamplesfollowingsolid

2、-phaseextractionandderivatisationCopyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-National forewordThis British Standard is the UK implementation of EN ISO 18857-2:2011. It is ide

3、ntical to ISO 18857-2:2009. It supersedes BS ISO 18857-2:2009, which is withdrawn.The UK participation in its preparation was entrusted by Technical Committee EH/3, Water quality to EH/3/2, Physical chemical and biochemical methods.A list of organizations represented on this subcommittee can be obta

4、ined on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunity from legal obligations.BS EN ISO 18857-2:2011This British Standardwas

5、published underthe authority of theStandards Policy andStrategy Committee on 30September 2009 BSI 2011Amendments/corrigenda issued since publicationDate Comments 31 December 2011 This corrigendum renumbers BS ISO 18857-2:2009 as BS EN ISO 18857-2:2011ISBN 978 0 580 74618 5Copyright European Committe

6、e for Standardization 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 18857-2 November 2011 ICS 13.060.50 English Version Water quality - Determination of selected alkylp

7、henols - Part 2: Gas chromatographic-mass spectrometric determination of alkylphenols, their ethoxylates and bisphenol A in non-filtered samples following solid-phase extraction and derivatisation (ISO 18857-2:2009) Qualit de leau - Dosage dalkylphnols slectionns - Partie 2: Dosage par chromatograph

8、ie en phase gazeuse-spectromtrie de masse dalkylphnols, de leurs thoxylates et du bisphnol A dans des chantillons non filtrs aprs extraction en phase solide et drivation (ISO 18857-2:2009) Wasserbeschaffenheit - Bestimmung von ausgewhlten Alkylphenolen - Teil 2: Gaschromatographische-massenspektrome

9、trische Bestimmung von Alkylphenolen, deren Ethoxylaten und Bisphenol A fr nichtfiltrierte Proben unter Verwendung der Festphasenextraktion und Derivatisierung (ISO 18857-2:2009) This European Standard was approved by CEN on 15 October 2011. CEN members are bound to comply with the CEN/CENELEC Inter

10、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

11、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

12、sions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, S

13、lovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2011 CEN All rights of exploitation in any form and by any means reserved worldwide for CE

14、N national Members. Ref. No. EN ISO 18857-2:2011: 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 18857-2:2009 has been prepared by Technical Committee

15、ISO/TC 147 “Water quality” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 18857-2:2011 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, e

16、ither by publication of an identical text or by endorsement, at the latest by May 2012, and conflicting national standards shall be withdrawn at the latest by May 2012. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CE

17、NELEC 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 Repu

18、blic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 18857-2:2009 has

19、 been approved by CEN as a EN ISO 18857-2:2011 without any modification. BS EN ISO 18857-2:2011 EN ISO 18857-2:2011 (E)Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-iiiContents

20、 PageForeword ivIntroduction.v1Scope12Normative references13Principle24Interferences25Reagents.36Apparatus.47Sampling and sample pretreatment 58Procedure.59Calibration and analysis of samples.810 Expression of results911 Test report10Annex A (informative) Example of a sorbent .11Annex B (informative

21、) Suitable capillary columns12Annex C (informative) Examples of chromatograms13Annex D (informative) Performance data.17Bibliography18BS EN ISO 18857-2:2011 EN ISO 18857-2:2011 (E)Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or

22、networking permitted without license from IHS-,-,-iv Foreword ISO (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. E

23、ach member body interested in a subject for which a tec hnical committee has beenestablished 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 closelywith the Internatio

24、nal Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordancewith the rules given in the ISO/IEC Directives, Part 2.The main task of technical committees is to prepare International Standards. Draft International Standards

25、adopted by the technical committees are circulated to the member bodies for voting. Public ation as an International Standard requires approval byat 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

26、patent rights. ISO shall not be held responsible for identifying an y or all such patent rights. ISO18857-2 was prepared by Technical Committee ISO/TC147, Water quality, Subcommittee SC 2, Physical,chemical and biochemical methods. ISO18857 consists of the following parts, under the general title Wa

27、ter quality Determination of selected alkylphenols: Part1:Method for non-filtered samples using liquid-liquid extraction and gas chromatography with massselective detection Part2: Gas chromatographic-mass spectrometric determination of alkylphenols, their ethoxylates and bisphenol A in non-filtered

28、samples following solid-phase extrac tion and derivatisation BS EN ISO 18857-2:2011 EN ISO 18857-2:2011 (E)Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-vIntroduction The user

29、should be aware that particular problems could require the specifications of additional marginal conditions.BS EN ISO 18857-2:2011 EN ISO 18857-2:2011 (E)Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted witho

30、ut license from IHS-,-,-BS EN ISO 18857-2:2011 EN ISO 18857-2:2011 (E)Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-INTERNATIONAL STANDA RD 1Water quality Determination of sele

31、cted alky lphenols Part 2: Gas chromatographic-mass spectrometric determination ofalkylphenols, their ethoxylates and bisphenol A in non-filteredsamples following solid-phase extraction and derivatisation WARNING Persons using this part of ISO 18857should be familiar with normal laboratory practice.

32、This part of ISO 18857 does not purport to address all of the safety problems, if any, associated withits use. It is the responsibility of the user to establish appropriate safetyand health practices and toensure compliance with any national regulatory conditions. IMPORTANT It is absolutely essentia

33、l that testsconducted in accordance with this part of ISO 18857be carried out by suitablyqualified staff.1 Scope This part of ISO18857 specifies a gas chromatographic-mass s pectrometric (GC-MS) determination of selected alkylphenols, their ethoxylates and bisphenolA in non-filtered samples of drink

34、ing, ground, surface, and waste watersfollowing solid-phase extractionand derivatisation. The lower limit of the working range depends on the matrix, on the specific compound to be analysed andon the sensitivityof the mass spectrometric detection unit. The method is applicable in a working range fro

35、m0,005 g/l to 0,2 g/l for 4-(1,1,3,3-tetramethylbutyl)phenol (OP), and its mono- (OP1 EO) and diethoxylate (OP2 EO), from 0,03 g/l to 0,2 g/l for 4-nonylphenol (mixture of isomers)(NP), and its mono- (NP1 EO) anddiethoxylate (NP 2 EO), and from 0,05 g/l to 0,2 g/l for bisphenol A (BPA). Depending on

36、 the matrix, the method is also applicable to waste water in a working range from 0,1 g/l to50g/l for OP, OP 1 EO, OP2 EO and BPA, and from 0,5g/l to 50 g/l for NP, NP 1 EO and NP 2 EO. The working ranges are based on experimental work carried out in ruggedness testing. Water samples containingsuspe

37、nded matter at concentrations ofmore than 500 mg/l and waste water samples are extracted bypassinga 100 ml sample through the cartridge. 2 NormativereferencesThe following referenced documents are indispensable for the application of this document. For datedreferences, only the edition cited applies

38、. For undated references, the latest edition of the referenceddocument (including anyamendments) applies.ISO 3696, Water for analytical laboratory use Specification and test methodsISO 5667-1, Water quality Sampling Part1: Guidance on the design of sampling programmes and sampling techniquesISO 5667

39、-3, Water quality Sampling Part3: Guidance on the preservation and handling of watersamples ISO 8466-1, Water quality Calibration and evaluation of analytical methods and estimation of performancecharacteristics Part1: Statistical evaluation of the linear calibration functionEN ISO 18857-2:2011 (E)B

40、S EN ISO 18857-2:2011 Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-2 3 Principle Extraction of the analytes listed in Table 1 from an acidified water sample by so lid-phase ex

41、traction, solvent elution, derivatisation and determination by GC-MS detection.Table 1 Analytes determinable by GC-MS following solid-phase extraction and derivatisationAnalyte Empirical formula Abbreviation CAS a No. 4-(1,1,3,3-Tetramethylbutyl)phenol C 14H 22O OP 140-66-9 4-(1,1,3,3-Tetramethylbut

42、yl)phenol monoethoxylate C 16H 26O 2 OP1 EO 4-(1,1,3,3-Tetramethylbutyl)phenol diethoxylate C 18H 30O 3 OP2 EO 4-Nonylphenol (mixture of isomers) C 15H 24O NP 84852-15-3b4-Nonylphenol monoethoxylate (mixture of isomers) C 17H 28O 2 NP1 EO 4-Nonylphenol diethoxylate (mixture of isomers) C 19H 32O 3 N

43、P2 EO Bisphenol A C 15H 16O 2 BPA 80-05-7 a CAS: Chemical Abstracts Service.b The commercially produced nonylphenols are predominantly 4-nonylphenol with a varied and undefined degree of branching in thealkyl groups. Thismixture of isomers falls under the CAS number 84852-15-3, but CAS numbers 104-4

44、0-5 (4-nonylphenol, straightchain) and 25154-52-3 (nonylphenol,straightchain) have also been incorrectly used to denote this isomermixture.4 Interferences 4.1Sampling and extractionSampling containers shall consist of materials that do not change the sa mple when in contact with it. Avoidcontact wit

45、h plastics and other organic materials during sampling, sample storage or extraction. Commercially available adsorbent materials are often of varying quality. Considerable batch-to-batchdifferences in quality and selectivity of this material are possible. The recovery of single substances can varywi

46、th the concentration. Therefore, check the recoveryregularly at different concentrations and whenever newbatches are used. Perform calibration and analysis with material from the same batch. 4.2Gas chromatography-mass spectrometrySubstances with retention times or which produce masses similar to the

47、 analytes to be determined caninterfere with the determination. These interferences may lead to incompletely resolved signals and to additional signals in the chromatographic patternof NP, NP1 EO and NP 2 EO. They may,depending on their magnitude, affectaccuracy and precision of the analytical resul

48、ts, since all three analytes are determined from the sum of a cluster of eight to ten chromatographic peaks (Table 3 and AnnexC). It is important that the interfering peaks are not included in the calculations. The presence of interfering compounds can, if necessary, be detected by recording full mass spectra (range of mass fragmentsto monitor m / z = 50 to m / z = 350). Matrix interferences can be caused by contaminants that are co-extracted from the sample. The extent of matrix interferences variesconsiderably, depending on the nature of the sample. In drinki