BS EN ISO 11369-1997 Water quality - Determination of selected plant treatment agents - Method using high performance liquid chromatography with UV detection after solid-liquid ext.pdf

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、 13.060.30BSENISO11369:1997 This British Standard, having been prepared under the direction of the Health and Environment Sector Board, waspublished under the authority of the Standards Board and comes intoeffect on 15 December 1997 BSI 05-1999 ISBN 0 580 28841 2 Amendments issued since publication

3、Amd. No. Date CommentsBSENISO11369:1997 BSI 05-1999 i Contents Page National foreword ii Foreword 2 Foreword iii Text of ISO 11369 1BSENISO11369:1997 ii BSI 05-1999 National foreword This British Standard is the English language version of ENISO11369:1997. Itis identical with ISO11369:1997. The UK p

4、articipation in its preparation was entrusted by Technical Committee EH/3, Water quality, to SubcommitteeEH/3/2, Physical, chemical and biochemical methods, which has the responsibility to: aid enquirers to understand the text; present to the responsible international/European committee any enquirie

5、s 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 secretary. BS EN ISO 11369 is one of

6、 a series of standards on water quality, others of which have been, or will be, published as Sections of BS6068. This standard has therefore been given the secondary identifier BS6068-2.61. The various Sections of BS6068 are comprised within Parts1 to7, which, together with Part0, are listed below.

7、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 this British Standard should only be car

8、ried 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. It has been reported to ISO in a prop

9、osal to amend the text of the international standard. Clause9.4. The end of the definition for the term ? i,nfdshould read: “. the concentration level n, calculated with equation (1) in9.2, in micrograms per litre;” Further information The term Calibration with External Standard (Clause9.3) is more

10、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 publications. The British Standards which i

11、mplement 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.BSENISO11369:1997 BSI 05-1999 iii A British Standard

12、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. Summary of pages This document comprises a front cover, an i

13、nside front cover, pages i to iv, theENISO title page, page 2, the ISO title page, pages ii to iv, pages 1 to 16 and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on theinside front cover.iv b

14、lankEUROPEAN 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 performance liquid chromatography with UV detection after solid-liquid extractio

15、n (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 (ISO11369:1997) This European Standard was approved by CEN on1997-07-13. CEN members are bound to

16、 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 obtained on application to the Centra

17、l 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 language and notified to the Central Secretariat has the same status as the

18、 official versions. CEN members are the national standards bodies of Austria, Belgium, CzechRepublic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and UnitedKingdom. CEN European Committee for Standardizatio

19、n 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 CENnational Members. Ref. No. EN ISO 11369:1997 EENISO11369:1997 BSI 05-1999 2 Foreword The

20、 text of the International Standard ISO11369:1997 has been prepared by TechnicalCommittee ISO/TC147 “Water 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,

21、either by publication of an identical text or by endorsement, at the latest by February1998, and conflicting national standards shall be withdrawn at the latest by February1998. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bou

22、nd to implement this European Standard: Austria, Belgium, CzechRepublic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the UnitedKingdom. Endorsement notice The text of the International Standard ISO11369

23、:1997 was approved by CEN as a European Standard without any modification.ENISO11369:1997 ii BSI 05-1999 Contents Page Foreword iii 1 Scope 1 2 Interferences 2 3 Normatives references 2 4 Principle 2 5 Reagents 2 6 Apparatus 3 7 Sampling and samples 4 8 Procedure 4 9 Calibration 9 10 Evaluation 11 1

24、1 Expression of results 12 12 Test report 12 13 Precision data 12 Annex A (informative) Recovery rates 13 Annex B (informative) Results of interlaboratory trial 14 Figure 1 Chromatograms of a low-concentration standard of plant treatment agents, separated with acetronitrile buffer gradient 6 Figure

25、2 Chromatograms of a high-concentration standard of plant treatment agents, separated with methanol/water gradient 7 Table 1 Plant treatment agents to which this International Standard applies 1 Table 2 Definition of subscripts 9 Table B.1 Results from an interlaboratory trial.: Standard solution in

26、 methanol 15 Table B.2 Results from an interlaboratory trial. Matrix: Spiked drinking water 15 Table B.3 Results from an interlaboratory trial. Matrix: Ground water 16 Table B.4 Results from an interlaboratory trial. Matrix: Spiked ground water 16 Descriptors: Water, quality, water pollution, water

27、tests, chemical analysis, determination of content, phytopharmaceuticals, high performance liquid chromatography.ENISO11369:1997 BSI 05-1999 iii Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of p

28、reparing International Standards 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,

29、in liaison with ISO, also take 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. Pub

30、lication as an International Standard requires approval by at least75% of the member bodies casting a vote. International Standard ISO11369 was prepared by Technical Committee ISO/TC147, Water quality, Subcommittee SC2, Physical, chemical and biochemical methods. Annex A and Annex B of this Internat

31、ional Standard are for information only.iv blankENISO11369:1997 BSI 05-1999 1 1 Scope This International Standard describes a method for the determination of organic plant treatment agents in drinking and ground water using high performance liquid chromatography (HPLC) with UV detection after solid-

32、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 (metabolites) in drinking water with a validated reporting limit of about0,14g/l. Limited additional data indicate

33、that it can be extended to0,054g/l (seeTable 1 for examples). The method may be extended to include additional substances and ground water, provided the method is validated for each individual case. The selection of the plant treatment agents and main degradation products inTable 1 has been made acc

34、ording 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 Standard applies Name Molecular formula Molar mass CAS No. a Substance family b Atrazine C 8 H 14 CIN 5 215,7 00191

35、2-24-9 T Chlorotoluron C 10 H 13 CIN 2 O 212,7 015545-48-9 H Cyanazine d C 9 H 13 CIN 6 240,7 021725-46-2 T Desethylatrazine c C 6 H 9 CIN 5 186,6 006190-65-4 T Diuron C 9 H 10 CI 2 N 2 O 233,1 000330-54-1 H Hexazinone d C 12 H 20 N 4 O 2 252,3 051235-04-2 T Isoproturon C 12 H 18 N 2 O 206,3 034123-

36、59-6 H Linuron C 9 H 10 CI 2 N 2 O 2 249,1 000330-55-2 H Metazachlor C 14 H 16 CIN 2 O 3 277,8 067129-08-2 A Methabenzthiazuron C 10 H 11 N 3 OS 221,3 018691-97-9 H Metobromuron d C 9 H 11 BrN 2 O 2 259,1 003060-89-7 H Metolachlor C 15 H 22 CINO 2 283,8 051218-45-2 A Metoxuron d C 10 H 13 CIN 2 O 2

37、228,7 19937-59-8 H Monolinuron C 9 H 11 CIN 2 O 2 214,6 1746-81-2 H Sebutylazine d C 9 H 15 CIN 5 228,7 00728-69-3 T Simazine C 7 H 12 CIN 5 201,7 000122-34-9 T Terbutylazine C 9 H 16 CIN 5 229,7 005915-41-3 T a CAS No.: Chemical abstracts number b Substance family: T: Triazine; H: Phenylurea herbic

38、ide; A: substituted anilide c : Main degradation product of atrazine d : Not included in the performance dataENISO11369:1997 2 BSI 05-1999 2 Interferences 2.1 Interferences with the enrichment The commercially available RP (reversed phase)-C18 materials, are often of varying quality. Considerable ba

39、tch-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 calibration and analysis are perform

40、ed 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 case the water sample is filtered thro

41、ugh 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 determination. This shall especially be taken in

42、to 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 editions indicated were valid. All s

43、tandards 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 currently valid International Standards. I

44、SO 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 handling of samples. ISO 8466-1:1990, Water

45、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 analysis 1) . 4 Principle The plant treatmen

46、t 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, identified and quantified by high performance liquid chromatography (HPLC) using UV detection. 5 Reagents 5.1 General requirements Water, solv

47、ents and reagents shall be of sufficient purity (e.g. residue grade or HPLC grade) as far as available and shall not contain any measurable UV absorbing substances interfering with the compounds of interest. 5.2 Nitrogen, high purity, for drying solvents and, if need be, for concentration by evapora

48、tion of the eluates. 5.3 Helium, high purity, for degassing HPLC solvents (see also6.13) 5.4 Mineral acid, e.g. phosphoric acid, c(H 3 PO 4 )=1mol/I. 5.5 Sodium hydroxide solution c(NaOH)=1mol/I. 5.6 RP-C18 sorbent, for the solid-phase extraction. For quality and selectivity of the material see2.1.

49、NOTEOther solid-phase adsorbents may be used, if the performance is comparable to this material and if it has been proved suitable according to2.1. 1) To be published.ENISO11369:1997 BSI 05-1999 3 5.7 Solvents, e.g. methanol (CH 3 OH), acetonitrile (CH 3 CN), acetone (C 3 H 6 O). WARNING These solvents, especially acetonitrile, are toxic agents. Caution shall be exercised when handling. 5.8 Reference standards (seeTable 1), of high purity or certified material. 5.9 Solutions of the indiv