DIN EN ISO 18857-2-2012 Water quality - Determination of selected alkylphenols - Part 2 Gas chromatographic-mass spectrometric determination of alkylphenols their ethoxylates and b.pdf

1、January 2012 Translation by DIN-Sprachendienst.English price group 13No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).IC

2、S 13.060.50!$y-“1861057www.din.deDDIN EN ISO 18857-2Water quality Determination of selected alkylphenols Part 2: Gas chromatographic-mass spectrometric determination ofalkylphenols, their ethoxylates and bisphenol A in non-filtered samplesfollowing solid-phase extraction and derivatisation (ISO 1885

3、7-2:2009)English translation of DIN EN ISO 18857-2:2012-01Wasserbeschaffenheit Bestimmung von ausgewhlten Alkylphenolen Teil 2: Gaschromatographisch-massenspektrometrische Bestimmung von Alkylphenolen,deren Ethoxylaten und Bisphenol A fr nichtfiltrierte Proben unter Verwendung derFestphasenextraktio

4、n und Derivatisierung (ISO 18857-2:2009)Englische bersetzung von DIN EN ISO 18857-2:2012-01Qualit de leau Dosage dalkylphnols slectionns Partie 2: Dosage par chromatographie en phase gazeuse-spectromtrie de massedalkylphnols, de leurs thoxylates et du bisphnol A dans des chantillons non filtrsaprs e

5、xtraction en phase solide et drivation (ISO 18857-2:2009)Traduction anglaise de DIN EN ISO 18857-2:2012-01www.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be considered authoritative.2601.12 DIN EN ISO 18857-2:2012-01 2 A comma is used as the decimal marker. N

6、ational foreword This standard has been prepared by Technical Committee ISO/TC 147 “Water quality” in collaboration with Technical Committee CEN/TC 230 “Water analysis” (Secretariat: DIN, Germany). The responsible German body involved in its preparation was the Normenausschuss Wasserwesen (Water Pra

7、ctice Standards Committee), Working Committees NA 119-01-03-02-02 AK Phenole mit GC and NA 119-01-03 AA Wasseruntersuchung. ISO 18857 consists of the following parts, under the general title Water quality Determination of selected alkylphenols: Part 1: Method for non-filtered samples using liquid-li

8、quid extraction and gas chromatography with mass selective detection Part 2: Gas chromatographic-mass spectrometric determination of alkylphenols, their ethoxylates and bisphenol A in non-filtered samples following solid-phase extraction and derivatisation This standard is part of the series Deutsch

9、e Einheitsverfahren zur Wasser-, Abwasser- und Schlammunter-suchung Gemeinsam erfassbare Stoffgruppen (Gruppe F) (German standard methods for the examination of water, waste water and sludge Substance group analysis (group F) and describes method F 32. Designation of method F 32 “Determination of se

10、lected alkylphenols Part 2: Gas chromatographic-mass spectrometric determination of alkylphenols, their ethoxylates and bisphenol A in non-filtered samples following solid-phase extraction and derivatisation”: Method DIN EN ISO 18857-2 F 32 This standard has been published to implement the Water Fra

11、mework Directive (WFD), Directive 2000/60/EC of the European Parliament and of the Council of 23 October 2000 establishing a framework for Community action in the field of water policy.*)The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 1

12、042 DIN EN ISO 1042 ISO 3696 DIN ISO 3696 ISO 5667-1 DIN EN ISO 5667-1 ISO 5667-3 DIN EN ISO 5667-3 ISO 8466-1 DIN 38402-51 Expert assistance and specialized laboratories will be required to perform the analysis described in this standard. Existing safety regulations are to be taken into account. De

13、pending on the objective of the analysis, a check shall be made on a case-by-case basis as to whether and to what extent additional conditions will have to be specified. Standard methods published as DIN Standards are obtainable from Beuth Verlag GmbH, either individually or grouped in volumes. The

14、standard methods included in the loose-leaf publication entitled Deutsche *) Registered in the DITR database of DIN Software GmbH, obtainable from Beuth Verlag GmbH, 10772 Berlin. German standard methods for the examination of water, waste water and sludge DIN EN ISO 18857-2:2012-01 3 Einheitsverfah

15、ren zur Wasser-, Abwasser- und Schlammuntersuchung will continue to be published jointly by Wiley-VCH Verlag and Beuth Verlag GmbH. All standard methods relevant to the Abwasserverordnung (Waste Water Regulation) (AbwV*) included in the new Regulation on Section 57, paragraph 1, number 1, of the Ges

16、etz zur Ordnung des Wasserhaushaltes (German Water Management Act*) concerning Anforderungen an das Einleiten von Abwasser in Gewsser together with the Abwasserverordnung and the Gesetz zur Ordnung des Wasserhaushalts have been published by Beuth-Verlag GmbH as a loose-leaf collection Analysenverfah

17、ren in der Abwasserverordnung Rechtsvorschriften und Normen (Supplements). Standards or draft standards bearing the group title “German standard methods for the examination of water, waste water and sludge” are classified under the following categories (main titles): General information (group A) (D

18、IN 38402) Sensory analysis (group B) (DIN 38403) Physical and physicochemical parameters (group C) (DIN 38404) Anions (group D) (DIN 38405) Cations (group E) (DIN 38406) Substance group analysis (group F) (DIN 38407) Gaseous constituents (group G) (DIN 38408) Parameters characterizing effects and su

19、bstances (group H) (DIN 38409) Biological-ecological methods of analysis (group M) (DIN 38410) Microbiological methods (group K) (DIN 38411) Test methods using water organisms (group L) (DIN 38412) Individual constituents (group P) (DIN 38413) Sludge and sediments (group S) (DIN 38414) Bio-assays wi

20、th microorganisms (group T) (DIN 38415) In addition to the methods described in the DIN 38402 to DIN 38415 series of standards, there are a number of European and International Standards available as DIN EN, DIN EN ISO and DIN ISO Standards, which also form part of the collection of German standard

21、methods. Information on Parts of these series of standards that have already been published can be obtained from the offices of the Normenausschuss Wasserwesen, telephone +49 30 2601-2448, or from Beuth Verlag GmbH, Burggrafenstr. 6, 10787 Berlin. *) Registered in the DITR database of DIN Software G

22、mbH, obtainable from: Beuth Verlag GmbH, 10772 Berlin. DIN EN ISO 18857-2:2012-01 4 National Annex NA (informative) Bibliography DIN 38402-51, German standard methods for the examination of water, waste water and sludge General information (group A) Calibration of a nalytical m ethods,e valuation o

23、f a nalytical r esults a nd li near c alibration functions used to determine the performance characteristics of analytical methods (A 51) DIN EN ISO 1042, Laboratory glassware One-mark volumetric flasks DIN EN ISO 5667-1, Water quality Sampling Part 1: Guidance on the design of sampling programmes a

24、nd sampling techniques DIN EN ISO 5667-3, Water quality Sampling Part 3: Guidance on the preservation and handling of water samples DIN ISO 3696, Water for analytical laboratory use Specification and test methods EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 18857-2 November 2011 ICS 13.0

25、60.50 English Version Water quality - Determination of selected alkylphenols - 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

26、 - Dosage dalkylphnols slectionns - Partie 2: Dosage par chromatographie 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 aus

27、gewhlten Alkylphenolen - Teil 2: Gaschromatographisch-massenspektrometrische 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 Oct

28、ober 2011. 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 standards may be ob

29、tained 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 notified to the

30、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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembour

31、g, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, 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 o

32、f exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 18857-2:2011: EContents EN ISO 18857-2:2011 (E) DIN EN ISO 18857-2:2012-01 2 Page Foreword 3 Introduction .4 1 Scope 5 2 Normative references 5 3 Principle 6 4 Interferences 6 5 Reagents .7 6 App

33、aratus .8 7 Sampling and sample pretreatment .9 8 Procedure .9 9 Calibration and analysis of samples. 12 10 Expression of results . 13 11 Test report . 14 Annex A (informative) Example of a sorbent . 15 Annex B (informative) Suitable capillary columns 16 Annex C (informative) Examples of chromatogra

34、ms 17 Annex D (informative) Performance data . 21 Bibliography . 22 Foreword The text of ISO 18857-2:2009 has been prepared by Technical Committee 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 Commit

35、tee 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 endorsement, at the latest by May 2012, and conflicting national standards shall be withdrawn at the late

36、st 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 CENELEC shall not be held responsible for identifying any or all such patent rights. According to the CEN/CENELEC Internal Regulations, the national standa

37、rds organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Po

38、land, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 18857-2:2009 has been approved by CEN as a EN ISO 18857-2:2011 without any modification. EN ISO 18857-2:2011 (E) DIN EN ISO 18857-2:2012-01 3 Introduction The user shoul

39、d be aware that particular problems could require the specifications of additional marginal conditions. EN ISO 18857-2:2011 (E) DIN EN ISO 18857-2:2012-01 4 WARNING Persons using this part of ISO 18857 should be familiar with normal laboratory practice. This part of ISO 18857 does not purport to add

40、ress all of the safety problems, 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 in accordance with t

41、his part of ISO 18857 be carried out by suitably qualified staff. 1 Scope This part of ISO 18857 specifies a gas chromatographic-mass spectrometric (GC-MS) determination of selected alkylphenols, their ethoxylates and bisphenol A in non-filtered samples of drinking, ground, surface, and waste waters

42、 following solid-phase extraction and derivatisation. The lower limit of the working range depends on the matrix, on the specific compound to be analysed and on the sensitivity of the mass spectrometric detection unit. The method is applicable in a working range from 0,005 g/l to 0,2 g/l for 4-(1,1,

43、3,3-tetramethylbutyl)phenol (OP), and its mono- (OP1EO) and diethoxylate (OP2EO), from 0,03 g/l to 0,2 g/l for 4-nonylphenol (mixture of isomers) (NP), and its mono- (NP1EO) and diethoxylate (NP2EO), and from 0,05 g/l to 0,2 g/l for bisphenol A (BPA). Depending on the matrix, the method is also appl

44、icable to waste water in a working range from 0,1 g/l to 50 g/l for OP, OP1EO, OP2EO and BPA, and from 0,5 g/l to 50 g/l for NP, NP1EO and NP2EO. The working ranges are based on experimental work carried out in ruggedness testing. Water samples containing suspended matter at concentrations of more t

45、han 500 mg/l and waste water samples are extracted by passing a 100 ml sample through the cartridge. 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 lat

46、est 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 design of sampling programmes and sampling techniques ISO 5667-3, Water quality Sampling

47、Part 3: Guidance on the preservation and handling of water samples ISO 8466-1, Water quality Calibration and evaluation of analytical methods and estimation of performance characteristics Part 1: Statistical evaluation of the linear calibration function EN ISO 18857-2:2011 (E) DIN EN ISO 18857-2:201

48、2-01 5 3 Principle Extraction of the analytes listed in Table 1 from an acidified water sample by solid-phase extraction, solvent elution, derivatisation and determination by GC-MS detection. Table 1 Analytes determinable by GC-MS following solid-phase extraction and derivatisation Analyte Empirical formula Abbreviation CASaNo. 4-(1,1,3,3-Tetramethylbutyl)phenol C14H22O OP 140-66-9 4-(1,1,3,3-Tetramethylbutyl)phenol monoethoxylate C16H26O2OP1EO 4-(1,1