EN ISO 18857-1-2006 en Water quality - Determination of selected alkylphenols - Part 1 Method for non-filtered samples using liquid-liquid extraction and gas chromatography with ma.pdf

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1、BRITISH STANDARDBS EN ISO 18857-1:2006Including Amendment No. 1 (to renumber BS ISO 18857-1:2005 as BS EN ISO 18857-1:2006)Water quality Determination of selected alkylphenols Part 1: Method for non-filtered samples using liquid-liquid extraction and gas chromatography with mass selective detectionT

2、his European Standard EN ISO 18857-1:2006 has the status of a British Standard.ICS 13.060.50g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN IS

3、O 18857-1:2006This British Standard was published under the authority of the Standards Policy and Strategy Committee on 1 February 2005 BSI 2006ISBN 0 580 45393 6National forewordThis British Standard was published by BSI. It is the UK implementation of EN ISO 18857-1:2006. It is identical with ISO

4、18857-1:2005.The UK participation in its preparation was entrusted by Technical Committee EH/3, Water quality, to Subcommittee EH/3/2, Physical, chemical and biochemical methods, which has the responsibility to: A list of organizations represented on this subcommittee can be obtained on request to i

5、ts secretary.Cross-referencesThe British Standards which implement international publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or

6、 of British Standards Online.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 does not of itself confer immunity from legal obligations. aid enquirers to understand the text;

7、 present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK.Summary of pagesThis document comprises a front cover,

8、an inside front cover, the ISO title page, pages ii to iv, pages 1 to 18, an inside back cover and a back cover.The BSI copyright notice displayed in this document indicates when the document was last issued.Amendments issued since publicationAmd. No. Date Comments16672 31 October 2006 Renumbers BS

9、ISO 18857-1:2005 as BS EN ISO 18857-1:2006EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 18857-1August 2006ICS 13.060.50English VersionWater quality - Determination of selected alkylphenols - Part 1:Method for non-filtered samples using liquid-liquid extraction andgas chromatography with mass

10、 selective detection (ISO 18857-1:2005)Qualit de leau - Dosage dalkylphnols slectionns -Partie 1: Mthode pour chantillons non filtrs parextraction en phase liquide-liquide et chromatographie enphase gazeuse avec dtection slective de masse (ISO18857-1:2005)Qualit de leau - Dosage dalkylphnols slectio

11、nns -Partie 1 : Mthode pur chantillons non filtrs partextraction en phase liquide-liquide et chromatographie enphase gazeuse avec dtection slective de masse (ISO18857-1:2005)This European Standard was approved by CEN on 3 August 2006.CEN members are bound to comply with the CEN/CENELEC Internal Regu

12、lations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Central Secretariat or to any CEN member.This Euro

13、pean Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the officialversions.CEN members are the nationa

14、l standards bodies of Austria, Belgium, Cyprus, Czech Republic, 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 United Kingdom.

15、EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2006 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 18857-1:2006: EForeword

16、 The text of ISO 18857-1:2005 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 18857-1:2006 by Technical Committee CEN/TC 230 “Water analysis“, the secretariat of which is held by DIN. Th

17、is 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 February 2007, and conflicting national standards shall be withdrawn at the latest by February 2007. According to the CEN/CENELEC Internal Regulations

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

19、Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Endorsement notice The text of ISO 18857-1:2005 has been approved by CEN as EN ISO 18857-1:2006 without any modifications. EN ISO 18857-1:2006Reference numberISO 18857-1:2005(E)OSI 5002INTERNATIONAL STANDAR

20、D ISO18857-1First edition2005-01-15Water quality Determination of selected alkylphenols Part 1: Method for non-filtered samples using liquid-liquid extraction and gas chromatography with mass selective detection Qualit de leau Dosage dalkylphnols slectionns Partie 1: Mthode pour chantillons non filt

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26、dehi n Switlrez dnaii ISO 5002 Allr ithgsr esedevrI SO 5002 All irthgs ersedevr iiiContents Page Foreword iv 1 Scope 1 2 Normative references . 1 3 Principle . 1 4 Interferences 2 5 Reagents 2 6 Apparatus. 3 7 Sampling and sample pretreatment 4 8 Procedure. 4 9 Calibration 6 10 Calculation. 10 11 Ex

27、pression of results 11 12 Test report 11 Annex A (informative) Suitable capillary columns 12 Annex B (informative) Examples of chromatograms 13 Annex C (informative) Recovery tests 4-nonylphenol (mixture of isomers) 15 Annex D (informative) Example of a separator 16 Annex E (informative) Method perf

28、ormance data 17 Bibliography . 18 EN ISO 18857-1:2006iv I SO 5002 All irthgs ersedevrForeword 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 thr

29、ough ISO technical committees. Each member body interested in a subject for which a technical committee 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 collabo

30、rates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. 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 Stand

31、ards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication 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

32、this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 18857-1 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical, chemical and biochemical methods. ISO 18857 consists of the foll

33、owing parts, under the general title Water quality Determination of selected alkylphenols: Part 1: Method for non-filtered samples using liquid-liquid extraction and gas chromatography with mass selective detection Part 2: Method for filtered samples using solid phase extraction and gas chromatograp

34、hy with mass selective detection EN ISO 18857-1:2006INTENRATIONAL TSANDADR IS-75881 O1:(5002E)I SO 5002 All irthgs ersedevr 1Water quality Determination of selected alkylphenols Part 1: Method for non-filtered samples using liquid-liquid extraction and gas chromatography with mass selective detectio

35、n 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 problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health

36、 practices and to ensure compliance with any national regulatory conditions. IMPORTANT It is absolutely essential that tests conducted in accordance with this part of ISO 18857 be carried out by suitably qualified staff. 1 Scope This part of ISO 18857 specifies a method for the determination of 4-no

37、nylphenol (mixture of isomers) and 4-(1,1,3,3-tetramethylbutyl)phenol in non-filtered samples of drinking water, ground water and surface water. The method is applicable in a concentration range from 0,005 g/l to 0,2 g/l for 4-(1,1,3,3-tetramethylbutyl)phenol and from 0,02 g/l to 0,2 g/l for 4-nonyl

38、phenol (mixture of isomers). Depending on the matrix, the method is also applicable to waste water containing the analyzed compounds in the concentration range from 0,1 g/l to 50 g/l. Higher concentrations can be measured after appropriate dilution of the sample. 2 Normative references The following

39、 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 reference document (including any amendments) applies. ISO 3696:1987, Water for analytical laboratory use Specificatio

40、n and test methods ISO 5667-1, Water quality Sampling Part 1: Guidance on the design of sampling programmes ISO 5667-2, Water quality Sampling Part 2: Guidance on sampling techniques ISO 5667-3, Water quality Sampling Part 3: Guidance on the preservation and handling of water samples 3 Principle The

41、 compounds 4-(1,1,3,3-tetramethylbutyl)phenol and 4-nonylphenol (mixture of isomers) are extracted from the acidified water sample with toluene. The extract is cleaned, if necessary, with silica and the alkylphenols are separated by gas chromatography using capillary columns. The alkylphenols are id

42、entified by mass spectrometry and quantified using an internal standard over the total procedure. The response factor using 4-(1,1,3,3-tetramethylbutyl)phenol and a technical mixture of isomers of 4-nonylphenol is determined daily. EN ISO 18857-1:20062 I SO 5002 All irthgs ersedevr4 Interferences Th

43、e extent and the importance of interferences are sample-dependent. There are many sources of sample contamination, including contamination of reagents during storage, contamination of equipment reused in the sequential extraction of samples and standards and carryover contamination from the septum s

44、eal on a sample bottle or vial and GC septa. Organic polymers can form alkyl phenols thus leading to elevated values. Avoid direct contact with plastics material as these can contain alkylphenols that can contaminate the sample. 5 Reagents Use reagents with negligibly low concentrations of target al

45、kyl phenols compared with the concentration to be determined and verify by blank determinations. 5.1 Water, grade 1, as specified in ISO 3696:1987. 5.2 Acid, e.g. hydrochloric acid, c(HCl) = 37 %, or sulfuric acid, c(H2SO4) = 1 mol/l. 5.3 Silica, medium pore size 6 nm (60 ), grain-size 0,063 mm to 0

46、,2 mm (230 mesh to 70 mesh). Purify about 100 g of silica in a quartz beaker (6.5) by heating to 550 C 20 C in a muffle furnace (6.6) for at least 10 h. Let the silica cool to about 100 C and transfer it to a wide-necked glass bottle. Let it cool to room temperature in a desiccator. Add water (5.1)

47、to the silica to produce a concentration of about 3 % mass fraction. Homogenize on a shaking device for 2 h. Store tightly sealed. 5.4 Hexane, C6H14. 5.5 Toluene, C7H8. Other extracting solvents may be used if equivalent recoveries can be achieved (see Annex C). 5.6 Sodium sulfate, Na2SO4, anhydrous

48、, powdered. 5.7 Acetone, C3H6O. 5.8 4-n-nonylphenol(ring-13C6) solution, C9H19-13C6H4-OH, 1 ng/l, used as an internal standard. Weigh 10 mg of 4-n-nonylphenol(ring-13C6) in a 100 ml measuring flask and bring to volume with acetone (5.7). Dilute this solution with acetone (5.7) in the ratio 1:100. Al

49、ternative internal standards (e.g. 4-n-nonylphenol) that meet the internal standard requirements are acceptable. An internal standard should have the following characteristics: It should be stable and should not interfere with the analyte. It should be as similar in structure to the analyte as possible, to ensure that it will show the same properties relative to, for example, adsorption on glass surfaces, extraction, concentration as the analyte. It should not be presen