BS EN ISO 6468-1997 Water quality - Determination of certain organochlorine insecticides polychlorinated biphenyls and chlorobenzenes - Gas chromatographic method after liquid-liqu.pdf

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1、BRITISH STANDARD BSENISO 6468:1997 BS 6068-2.57: 1997 Water quality Determination of certain organochlorine insecticides, polychlorinated biphenyls and chlorobenzenes Gas chromatographic method after liquid-liquid extraction The European Standard EN ISO6468:1996 has the status of a British Standard

2、ICS 13.060.01BSENISO6468:1997 This British Standard, having been prepared under the direction of the Health and Environment Sector Board, was published under the authority of the Standards Board and comes into effect on 15May1997 BSI 02-1999 The following BSI references relate to the work on this st

3、andard: Committee reference EH/3/2 Draft for comment 94/501672 DC ISBN 0 580 26676 1 Committees responsible for this British Standard The preparation of this British Standard was entrusted by Technical Committee EH/3, Water quality, to Subcommittee EH/3/2, Physical, chemical and biochemical methods,

4、 upon which the following bodies were represented: British Agrochemicals Association Ltd. British Ceramic Research British Gas plc British Soft Drinks Association Ltd. Chartered Institution of Water and Environmental Management Chemical Industries Association Convention of Scottish Local Authorities

5、 Environment Agency GAMBICA (BEAMA) Ltd. Industrial Water Society Laboratory of the Government Chemist Royal Society of Chemistry Soap and Detergent Industry Association Society of Chemical Industry Swimming Pool and Allied Trades Association Ltd. Water Companies Association Water Reseach Centre Wat

6、er Services Association of England and Wales Amendments issued since publication Amd. No. Date CommentsBSENISO6468:1997 BSI 02-1999 i Contents Page Committees responsible Inside front cover National foreword ii Foreword 2 Foreword ii Text of ISO 6468 1 List of references Inside back coverBSENISO6468

7、:1997 ii BSI 02-1999 National foreword This British Standard has been prepared by Subcommittee EH/3/2 and is the English language version of ENISO6468:1996 Water quality Determination of certain organochlorine insecticides, polychlorinated biphenyls and chlorobenzenes Gas chromatographic method afte

8、r liquid-liquid extraction published by the European Committee for Standardization (CEN). It is identical with ISO6468:1996, published by the International Organization for Standardization (ISO). BS EN ISO6468 is one of a series of standards on water quality, others of which have been, or will be, p

9、ublished as Sections of BS6068. This standard has therefore been given the secondary identifier BS6068-2.57. BS6068 comprises the following Parts, which are divided into Sections. Part 0: Introduction; Part 1: Glossary; Part 2: Physical, chemical and biochemical methods; Part 3: Radiological methods

10、; Part 4: Microbiological methods; Part 5: Biological methods; Part 6: Sampling; Part 7: Precision and accuracy. NOTEThe tests described in this British Standard should only be carried out by suitably qualified persons with an appropriate level of chemical expertise. Standard chemical procedures sho

11、uld be followed throughout. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Cross-referen

12、ces Publication referred to Corresponding British Standard EN 25667-1:1993 (ISO 5667-1:1980) BS 6068 Water quality Part 6 Sampling Section 6.1:1981 Guidance on the design of sampling programmes (also numbered BS EN 25667-1:1994) EN 25667-2:1993 (ISO 5667-2:1991) Section 6.2:1991 Guidance on sampling

13、 techniques (also numbered BS EN25667-2:1993) Summary of pages This document comprises a front cover, an inside front cover, pagesi andii, theEN title page, page 2, the ISO title page, pageii, pages1 to24, aninsidebackcover and a back cover. This standard has been updated (see copyright date) and ma

14、y have had amendments incorporated. This will be indicated in the amendment table on the inside front cover.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM ENISO6468 December1996 ICS13.060.10 Descriptors: See ISO document English version Water quality Determination of certain organochlorine insect

15、icides, polychlorinated biphenyls and chlorobenzenes Gas chromatographic method after liquid-liquid extraction (ISO6468:1996) Qualit de leau Dosage de certains insecticides organochlors des polychlorobiphnyles et des chlorobenznes Mthode par chromatographie en phase gazeuse aprs extraction liquide-l

16、iquide (ISO6468:1996) Wasserbeschaffenheit Bestimmung bestimmter Organochlorinsektizide, Polychlorbiphenyle und Chlorbenzole Gaschromatographisches Verfahren nach Flssig-Flssig-Extraktion (ISO6468:1996) This European Standard was approved by CEN on1996-11-08. CEN members are bound to comply with the

17、 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 obtained on application to the Central Secretariat or

18、 to any CEN member. The European Standards exist 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 Central Secretariat has the same status as the official versio

19、ns. CEN members are the national standards bodies of Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisati

20、on Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1996 Copyright reserved to CEN members Ref. No. ENISO6448:1996 EENISO6468:1996 BSI 02-1999 2 Foreword The text of the International Standard ISO6468:1996 has been prepared by Technical Committee ISO/TC147 “Wat

21、er quality” in collaboration with Technical Committee CEN/TC230 “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 June1997, and conflicting

22、 national standards shall be withdrawn at the latest by June1997. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ir

23、eland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of the International Standard ISO6468:1996 was approved by CEN as a European Standard without any modification. NOTENormative references to International Standards

24、are listed inAnnex ZA (normative). Contents Page Foreword 2 1 Scope 1 2 Normative references 1 3 Principle 1 4 Reagents and materials 1 5 Apparatus 3 6 Sampling and sample preparation 4 7 Procedure 4 8 Calibration 7 9 Identification and evaluation 9 10 Expression of results 10 11 Performance data 12

25、 12 Test report 12 Annex A (normative) Clean-up of the extract by means of pyrogenic copper for the elimination of sulfur 13 Annex B (informative) Examples of gas chromatographic conditions and the corresponding gas chromatographs 14 Annex C (informative) 18 Annex D (informative) 19 Page Annex E (in

26、formative) 20 Annex F (informative) 21 Annex G (informative)Clean-up on silica gel macrocolumn 22 Annex H (informative) 23 Annex ZA (normative) Normative references to international publications with their relevant European publications 24 Figure B.1 Capillary-column gas chromatogram of compounds li

27、sted in Table B.1 17 Figure B.2 Capillary-column gas chromatogram of compounds listed inTable B.2 17 Figure C.1 Microseparator 18 Figure D.1 Kuderna-Danish evaporation flask 19 Figure E.1 Drying and clean-up columns 20 Figure E.2 Reservoir (to fit top joint of column) 20 Figure F.1 Microcolumn for t

28、he silica gel clean-up 21 Table 1 Detection limits 2 Table 2 Explanation of the subscripts used in the symbols 7 Table 3 Characteristic data of the method using hexane as extraction solvent 11 Table B.1 Example of the sequence of elution, relative retention time and retention time, obtained with a n

29、on-polar capillary column 14 Table B.2 Example of the sequence of elution, relative retention time and retention time, obtained with a weakly polar capillary column 15 Table B.3 Gas chromatographic conditions 16 Table G.1 Sequence of elution of 27 halogenated hydrocarbons using the silica gel clean-

30、up with a macrocolumn 22 Table H.1 Typical mean recoveries, A i , according to8.3 23ENISO6468:1996 ii BSI 02-1999 Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standard

31、s is normally carried out through 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

32、part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International St

33、andard requires approval by at least75% of the member bodies casting a vote. International Standard ISO6468 was prepared by Technical Committee ISO/TC147, Water quality, Subcommittee SC2, Physical, chemical, biochemical methods. Annex A forms an integral part of this International Standard. Annex B

34、to Annex A are for information only.ENISO6468:1996 BSI 02-1999 1 WARNING AND SAFETY PRECAUTIONS This method makes use of flammable and toxic organic solvents. Observe the safety regulations in effect. The electron-capture detector (ECD) contains radionuclides. Adequate safety precautions and legal r

35、equirements must be observed. The halogenated hydrocarbons and chloropesticides, used for the preparation of the calibration standards are toxic. Therefore, the safety regulations pertaining must be strictly observed. 1 Scope This International Standard describes a method for determining certain org

36、anochlorine insecticides, polychlorinated biphenyls (PCBs) and chlorobenzenes (except the mono- and dichlorobenzenes) in drinking waters, ground waters, surface waters and waste waters. The method is applicable to samples containing up to0,05g/l of suspended solids. In the presence of organic matter

37、, suspended matter and colloids, interferences are more numerous and consequently the detection limits are higher. The method described in this International Standard only gives information on specific PCB compounds but no information on the level of total PCBs. According to the types of compounds t

38、o be detected and the source of the water, the detection limits given inTable 1 are applicable for the method described in this International Standard, with waters of low organic contents. Given the very low concentrations normally present in the waters, the problem of contamination is extremely imp

39、ortant. The lower the level measured, the more precautions have to be observed; below concentrations of10ng/l, special care is necessary. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At

40、the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on the International Standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO

41、 maintain registers of currently valid International Standards. ISO 5667-1:1980, Water quality Sampling Part1: Guidance on the design on sampling programmes. ISO 5667-2:1991, Water quality Sampling Part2: Guidance on sampling techniques. 3 Principle Liquid-liquid extraction of organochlorine insecti

42、cides, chlorobenzenes and PCBs by an extraction solvent. After the concentration of the components with low volatility and after any clean-up steps which may be necessary, the sample extracts are analysed by gas chromatography, using an electron-capture detector. Any substance capable of producing a

43、 response on the electron-capture detector, at a retention time indistinguishable from any compound of interest, will interfere. In practice, many potentially interfering substances will be removed during the extraction and clean-up procedures. NOTE 1In general, the use of two capillary columns of d

44、ifferent polarity is sufficient for the organochlorine compounds analysed according to this International Standard. The results so calculated should be considered as the maximum concentrations, possibly still influenced by coeluting substances. It is possible that there will be cases where a more de

45、finite identification is required. 4 Reagents and materials All reagents shall be sufficiently pure to not give rise to significant interfering peaks in the gas chromatograms of the blanks. The purity of reagents used in the procedure shall be checked by blank determinations (7.6). NOTE 2Commercial

46、“pesticide grade” solvents are available. The use of these products is recommended only after verifying their quality. The quality of a solvent is checked by evaporation of about200ml down to1ml and analysis of the concentrate to determine the compounds subsequently analysed. The solvent should be c

47、onsidered acceptable if it does not give any detectable interfering peaks in the chromatogram for the substance of interest. 4.1 Water purified, for example, using ion-exchange or carbon-column adsorption. 4.2 Extraction solvent Hexane, petroleum ether or heptane are suitable. NOTE 3Any other solven

48、ts meeting the requirements of8.3 (recovery rate 60%) may be used. 4.3 Sodium sulfate (Na 2 SO 4 ), anhydrous. Heat a portion of about250ml to300ml of sodium sulfate powder at500C 20C for4h 30min, cool to about200C in a muffle furnace and then to ambient temperature in a desiccator containing magnes

49、ium perchlorate or an equivalent alternative. 4.4 Decane (C 10 H 22 ) or dodecane (C 12 H 26 ), or any keeper which is not detected by the electron-capture detector.ENISO6468:1996 2 BSI 02-1999 Table 1 Detection limits Acronyms Chemical names (IUPAC) Detection limits Organochlorine insecticides: HCH 1, 2, 3, 4, 5, 6-hexachlorocyclohexane, five stereoisomers: alpha-HCH beta-HCH gamma-HCH delta-HCH epsilon-HCH Lindane o,p9-DDE p,p9-DDE o,p9-TDE p,p9-TDE o,p9-DDT p,p9-DDT Methoxychlor