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1、BRITISH STANDARD BS EN ISO 11369:1997 BS 6068-2.61: 1997 Water quality Determination of selected plant treatment agents Method using high performance liquid chromatography with UV detection after solid-liquid extraction The European Standard EN ISO 11369:1997 has the status of a British Standard ICS
2、 13.060.30 Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:12 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 11369:1997 This British Standard, having been prepared under the direction of the Health and Environment Sector Board, was published under the authority of the Standards Bo
3、ard and comes into effect on 15 December 1997 BSI 05-1999 ISBN 0 580 28841 2 Amendments issued since publication Amd. No.DateComments Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:12 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 11369:1997 BSI 05-1999i Contents Page National fo
4、rewordii Foreword2 Forewordiii Text of ISO 113691 Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:12 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 11369:1997 ii BSI 05-1999 National foreword This British Standard is the English language version of EN ISO 11369:1997. It is identic
5、al with ISO 11369:1997. 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: aid enquirers to understand the text; present to the responsible internationa
6、l/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. A list of organizations represented on this subcommittee can be obtained on request to its sec
7、retary. BS EN ISO 11369 is one of a series of standards on water quality, others of which have been, or will be, published as Sections of BS 6068. This standard has therefore been given the secondary identifier BS 6068-2.61. The various Sections of BS 6068 are comprised within Parts 1 to 7, which, t
8、ogether with Part 0, are listed below. Part 0: Introduction; Part 1: Glossary; Part 2: Physical, chemical and biochemical methods; Part 3: Radiological methods; Part 4: Microbiological methods; Part 5: Biological methods; Part 6: Sampling; Part 7: Precision and accuracy. NOTEThe tests described in t
9、his British Standard should only be carried out by suitably qualified persons with an appropriate level of chemical expertise. Standard chemical procedures should be followed throughout. Textual error The textual error set out below was discovered when adopting the text of the international standard
10、. It has been reported to ISO in a proposal to amend the text of the international standard. Clause 9.4. The end of the definition for the term ?i,nfd should read: “. the concentration level n, calculated with equation (1) in 9.2, in micrograms per litre;” Further information The term Calibration wi
11、th External Standard (Clause 9.3) is more commonly referred to as Internal Standard Calibration. Cross-references Attention is drawn to the fact that CEN and CENELEC Standards normally include an annex which lists normative references to international publications with their corresponding European p
12、ublications. The British Standards which implement these international or European publications may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. Licensed C
13、opy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:12 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 11369:1997 BSI 05-1999iii 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. Co
14、mpliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i to iv, the EN ISO title page, page 2, the ISO title page, pages ii to iv, pages 1 to 16 and a back cover. This standard h
15、as been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:12 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iv blank Licensed Copy: sheffieldun sheff
16、ieldun, na, Sat Nov 18 01:48:12 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 11369 August 1997 ICS 13.060.30 Descriptors: See ISO document English version Water quality Determination of selected plant treatment agents Method using high performan
17、ce liquid chromatography with UV detection after solid-liquid extraction (ISO 11369:1997) Qualit de leau Dosage de certains agents de traitement des plantes Mthode par chromatographie en phase liquide haute performance (CLHP) avec dtection UV aprs extraction solide-liquide (ISO 11369:1997) This Euro
18、pean Standard was approved by CEN on 1997-07-13. 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 concer
19、ning such national standards may be obtained on application to the Central Secretariat or 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 la
20、nguage and notified to the Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden
21、, Switzerland and United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1997 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Mem
22、bers. Ref. No. EN ISO 11369:1997 E Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:12 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 11369:1997 BSI 05-1999 2 Foreword The text of the International Standard ISO 11369:1997 has been prepared by Technical Committee ISO/TC 147 “Water qual
23、ity” 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 endorsement, at the latest by February 1998, and conflicting
24、national standards shall be withdrawn at the latest by February 1998. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany,
25、 Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of the International Standard ISO 11369:1997 was approved by CEN as a European Standard without any modification. Licensed Copy: sheffieldun she
26、ffieldun, na, Sat Nov 18 01:48:12 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:12 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 11369:1997 ii BSI 05-1999 Contents Page Forewordiii 1Scope1 2Interferences2 3Normatives references2 4Principl
27、e2 5Reagents2 6Apparatus3 7Sampling and samples4 8Procedure4 9Calibration9 10Evaluation11 11Expression of results12 12Test report12 13Precision data12 Annex A (informative) Recovery rates13 Annex B (informative) Results of interlaboratory trial14 Figure 1 Chromatograms of a low-concentration standar
28、d of plant treatment agents, separated with acetronitrile buffer gradient6 Figure 2 Chromatograms of a high-concentration standard of plant treatment agents, separated with methanol/water gradient7 Table 1 Plant treatment agents to which this International Standard applies1 Table 2 Definition of sub
29、scripts9 Table B.1 Results from an interlaboratory trial.: Standard solution in methanol15 Table B.2 Results from an interlaboratory trial. Matrix: Spiked drinking water15 Table B.3 Results from an interlaboratory trial. Matrix: Ground water16 Table B.4 Results from an interlaboratory trial. Matrix:
30、 Spiked ground water16 Descriptors: Water, quality, water pollution, water tests, chemical analysis, determination of content, phytopharmaceuticals, high performance liquid chromatography. Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:12 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN I
31、SO 11369:1997 BSI 05-1999iii 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. Each member body interest
32、ed 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 collaborates closely with the International Electrotechnical Co
33、mmission (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 Standard requires approval by at least 75 % of the member bodies casting a vote. Intern
34、ational Standard ISO 11369 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical, chemical and biochemical methods. Annex A and Annex B of this International Standard are for information only. Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:12 GMT+00
35、:00 2006, Uncontrolled Copy, (c) BSI iv blank Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:12 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 11369:1997 BSI 05-19991 1 Scope This International Standard describes a method for the determination of organic plant treatment agents in dr
36、inking and ground water using high performance liquid chromatography (HPLC) with UV detection after solid-liquid extraction. The method described in this International Standard is applicable to the determination of selected plant treatment agents and some of their main degradation products (metaboli
37、tes) in drinking water with a validated reporting limit of about 0,1 4g/l. Limited additional data indicate that it can be extended to 0,05 4g/l (see Table 1 for examples). The method may be extended to include additional substances and ground water, provided the method is validated for each individ
38、ual case. The selection of the plant treatment agents and main degradation products in Table 1 has been made according to the knowledge at the time of the interlaboratory trial (1992). Data for some other substances are given in Annex A. Table 1 Plant treatment agents to which this International Sta
39、ndard applies NameMolecular formulaMolar massCAS No.aSubstance familyb AtrazineC8H14CIN5215,7001912-24-9T ChlorotoluronC10H13CIN2O212,7015545-48-9H CyanazinedC9H13CIN6240,7021725-46-2T DesethylatrazinecC6H9CIN5186,6006190-65-4T DiuronC9H10CI2N2O233,1000330-54-1H HexazinonedC12H20N4O2252,3051235-04-2
40、T IsoproturonC12H18N2O206,3034123-59-6H LinuronC9H10CI2N2O2249,1000330-55-2H MetazachlorC14H16CIN2O3277,8067129-08-2A MethabenzthiazuronC10H11N3OS221,3018691-97-9H MetobromurondC9H11BrN2O2259,1003060-89-7H MetolachlorC15H22CINO2283,8051218-45-2A MetoxurondC10H13CIN2O2228,719937-59-8H MonolinuronC9H1
41、1CIN2O2214,61746-81-2H SebutylazinedC9H15CIN5228,700728-69-3T SimazineC7H12CIN5201,7000122-34-9T TerbutylazineC9H16CIN5229,7005915-41-3T a CAS No.: Chemical abstracts number b Substance family: T: Triazine; H: Phenylurea herbicide; A: substituted anilide c : Main degradation product of atrazine d :
42、Not included in the performance data Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:12 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 11369:1997 2 BSI 05-1999 2 Interferences 2.1 Interferences with the enrichment The commercially available RP (reversed phase)-C18 materials, are ofte
43、n of varying quality. Considerable batch-to-batch differences regarding quality and selectivity of this material even from one manufacturer are possible. The recovery may vary with the concentration. Co-extractants eluted from the sorbent material can affect the blank and the recovery. Therefore the
44、 calibration and analysis are performed on exactly the same batch of sorbent. Also any UV-absorbing material occurring in the water which passes through the procedure and has a retention time similar to the standard will interfere. Suspended matter in the water sample may clog the packing. In this c
45、ase the water sample is filtered through a glass fibre filter prior to the enrichment. 2.2 Interferences with the HPLC measurement Substances which absorb at the wavelengths of detection and have retention times similar to those of the compounds to be investigated will interfere with the determinati
46、on. This shall especially be taken into account when examining samples other than ground- and drinking water. 3 Normative references The following standards contain provisions which, through reference to this text, constitute provisions of this International Standard. At the time of publication, the
47、 editions indicated were valid. All standards are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate the possiblity of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain registers of curre
48、ntly valid International Standards. ISO 5667-1:1980, Water quality Sampling Part 1: Guidance on the design of sampling programmes. ISO 5667-2:1991, Water quality Sampling Part 2: Guidance on sampling techniques. ISO 5667-3:1994, Water quality Sampling Part 3: Guidance on the preservation and handlin
49、g of samples. ISO 8466-1:1990, Water quality Calibration and evaluation of analytical methods and estimation of performance characteristics Part 1: Statistical evaluation of the linear calibration function. ISO/TR 13530:, Water quality General guidance to analytical quality control for water analysis1). 4 Principle The plant treatment substances in the water sample are extracted by solid-liquid extraction on RP-C18 material (RP = reversed phase), eluted with a solvent and then separated, i