BS EN ISO 17353-2004 Water quality - Determination of selected organotin compounds - Gas chromatographic method《水质 选定有机锡化合物的测定 气相色谱分析法》.pdf

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1、BRITISH STANDARDBS EN ISO 17353:2005Incorporating Amendment No. 1 (to renumber BS ISO 17353:2004 to BS EN ISO 17353:2005)Water quality Determination of selected organotin compounds Gas chromatographic methodThe European Standard EN ISO 17353:2004 has the status of a British StandardICS 13.060.50 g49

2、g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN ISO 17353:2005This British Standard was published under the authority of the Standards Policy and

3、 Strategy Committee on 28 September 2004 BSI 17 March 2006ISBN 0 580 44509 7 National forewordThis British Standard is the official English language version of EN ISO 17353:2005. It is identical with ISO 17353:2004.The UK participation in its preparation was entrusted by Technical Committee EH/3, Wa

4、ter 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 its secretary.Additional informationThe responsible BSI committee would like to draw attention to th

5、e following. This international standard is applicable to waters containing a maximum of 2 g/l of suspended material. However, the application of this standard to samples containing amounts smaller than 2 g/l of suspended material can affect recovery during the alkylation and extraction stages. This

6、 is due to the adsorption of the suspended material onto the solid material. Once the performance of this standard has been verified, samples containing suspended material can be analysed.Cross-referencesThe British Standards which implement international publications referred to in this document ma

7、y 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 of British Standards Online.This publication does not purport to include all the necessary provisions of a contract. Users a

8、re 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; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, an

9、d keep UK interests informed; monitor related international and European developments and promulgate them in the UK.Summary of pagesThis document comprises a front cover, an inside front cover, the EN ISO title page, the EN ISO foreword page, the ISO title page, pages ii to v, a blank page, pages 1

10、to 31 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 Comments15964 March 2006 Renumbers BS ISO 17353:2004 as BS EN ISO 17353:2005EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 17

11、353August 2005ICS 13.060.50English VersionWater quality - Determination of selected organotin compounds -Gas chromatographic method (ISO 17353:2004)Qualit de leau - Dosage de composs organostanniquesslectionns - Mthode par chromatographie en phasegazeuse (ISO 17353:2004)Wasserbeschaffenheit - Bestim

12、mung von ausgewhltenOrganozinnverbindungen - Verfahren mittelsGaschromatographie (ISO 17353:2004)This European Standard was approved by CEN on 18 July 2005.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the st

13、atus 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 European Standard exists in three official versions (English, French, German). A v

14、ersion 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 national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Eston

15、ia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE

16、 FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2005 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 17353:2005: EForeword The text of ISO 17353:2004 has been prepared by Technical Committee ISO/TC 147 “Water qu

17、ality“ of the International Organization for Standardization (ISO) and has been taken over as EN ISO 17353:2005 by 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

18、of an identical text or by endorsement, at the latest by February 2006, and conflicting national standards shall be withdrawn at the latest by February 2006. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this

19、 European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Endorsem

20、ent notice The text of ISO 17353:2004 has been approved by CEN as EN ISO 17353:2005 without any modifications. EN ISO 17353:2005Reference numberISO 17353:2004(E)OSI 4002INTERNATIONAL STANDARD ISO17353First edition2004-09-15Water quality Determination of selected organotin compounds Gas chromatograph

21、ic method Qualit de leau Dosage de composs organostanniques slectionns Mthode par chromatographie en phase gazeuse EN ISO 17353:2005IS:35371 O4002(E) DPlcsid Fremia ihTs PDF file may ctnoian emdebt dedyfepcaes. In ccaocnadrw eith Aebods licensilop gnic,y this file mairp eb ynted iv roweb detu slahl

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24、 memdob rebeis. In tlnu ehikletneve y ttah lborp aem leratit gno it is f,dnuo plsaee inform ttneC ehlar Secrteiraat ta the serddaig sleb nevwo. ISO 4002 All irthgs erse.devr lnUeto sswrehise specified, on trap fo this lbupictaion maeb y cudorperro de tuilizi den yna form ro na ybm ynae,s lecetrinoc

25、ro mecinahcal, inclidung tohpcoiypodna gn micrfoilm, wittuoh repmissii non writign from ietI rehSa Ot tsserdda eh ebolw or ISOs memreb i ydobn the cnuotrfo y ttseuqer ehe.r ISO cirypothg fofice saCe tsopale 65 xeneG 1121-HC 02 avleT. 4 + 10 947 22 1 11 xaF0 947 22 14 + 9 74 E-mail coirypthgiso.o grW

26、e bwww.is.o groPulbisdehi n Switlrez dnaii I SO 4002 Allr ithgsr esedevriiIS:35371 O4002(E) I SO 4002 All irthgs ersedevr iiiContents Page Foreword iv Introduction v 1 Scope 1 2 Normative references . 1 3 Terms and definitions. 2 4 Principle . 2 5 Interferences 2 6 Reagents 2 7 Apparatus. 7 8 Proced

27、ure. 8 9 Identification 11 10 Calibration 13 11 Calculation. 16 12 Precision 18 13 Test report 18 Annex A (informative) Gas chromatographic conditions. 19 Annex B (informative) Precision data. 29 Bibliography . 31 iiiiEN ISO 17353:2005ISO 17353:2004(E) iv ISO 2004 All rights reservedForeword ISO (th

28、e 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 interested in a subject for which a technical committ

29、ee 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 Commission (IEC) on all matters of electrotechn

30、ical 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 Standards. Draft International Standards adopted by the technical committees are circulated to the member

31、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 this document may be the subject of patent rights. ISO shall not be held responsible for identifying

32、any or all such patent rights. ISO 17353 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical, chemical and biochemical methods. iiivEN ISO 17353:2005IS:35371 O4002(E) I SO 4002 All irthgs ersedevr vIntroduction It should be noted whether and to what extent part

33、icular problems will require the specification of additional boundary conditions. This International Standard describes a gas-chromatographic/organotin specific determination of organotin compounds after derivatization with sodium tetraethyl borate and liquid/liquid extraction. The user should be aw

34、are that particular problems could require the specification of additional marginal conditions. vEN ISO 17353:2005blankINTENRATIONAL TSANDADR IS:35371 O4002(E)I SO 4002 All irthgs ersedevr 1Water quality Determination of selected organotin compounds Gas chromatographic method WARNING Persons using t

35、his 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 practices and to ensure

36、compliance with any national regulatory conditions. IMPORTANT It is absolutely essential that tests conducted according to this International Standard be carried out by suitably trained staff. 1 Scope This International Standard specifies a method for the identification and quantification of organot

37、in compounds and/ or cations as mentioned in Table 1 in drinking water, surface water and wastewater containing not more than 2 g/l of suspended material. The working range is 10 ng/l to 1 000 ng/l. The respective anions are not determined. This method can also be applicable to other compounds such

38、as R methyl, n 1 to 2 and R phenyl, n 1 to 2. This International Standard is also applicable to marine water. Table 1 Organotin compounds and cations determined using this International Standard RnSn(4-n)R n Name Acronym BuSn3Butyl 1 Monobutyltin cation MBT Bu2Sn2Butyl 2 Dibutyltin cation DBT Bu3SnB

39、utyl 3 Tributyltin cation TBT Bu4Sn Butyl 4 Tetrabutyltin TTBT OcSn3Octyl 1 Monooctyltin cation MOT Oc2Sn2Octyl 2 Dioctyltin cation DOT Ph3SnPhenyl 3 Triphenyltin cation TPhT Cy3SnCyclohexyl 3 Tricyclohexyltin cation TCyT 2 Normative references The following referenced documents are indispensable fo

40、r the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 3696:1987, Water for analytical laboratory use Specification and test methods 1EN ISO 17353:2005ISO

41、5667-1, Water quality Sampling Part 1: Guidance on the design on 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 Terms and definitions For the purpos

42、es of this International Standard, the following terms and definitions apply. 3.1 organotin compound OTC substance with at least one Sn-C bond NOTE The number of Sn-C bonds is a measure of the degree of substitution. 3.2 organotin cation OC part of the organotin compound that contains all Sn-C bonds

43、 (and which is formally loaded) NOTE In this International Standard, the abbreviation OC is also used for the non-dissociated tetrasubstituted organotin. OC therefore comprises the cations MBT, DBT, TBT, TTBT, MOT, DOT, TCyT, and TPhT. 4 Principle Organotin compounds in water are alkylated with sodi

44、um tetraethylborate and extracted with hexane. The extract can be cleaned with silica. After concentration, the tetrasubstituted OTC are separated by capillary gas chromatography and detected with a suitable system such as MS (mass spectrometry), FPD (flame photometric detection), AED (atomic emissi

45、on detection). The concentration is determined by calibration for the total procedure using an internal standard mixture. 5 Interferences The reagents sometimes contain impurities of organotin compounds. It is absolutely essential to verify the blanks (see A.4.6). 6 Reagents Use reagents of highest

46、purity. 6.1 Water, free of substances causing interference with this method and complying with ISO 3696:1987, Grade 1. 6.2 Nitric acid, U(HNO3) 1,4 g/ml. 6.3 Acetic acid, CH3COOH, glacial. 6.4 Sodium hydroxide solution, c(NaOH) 1 mol/l. 6.5 Sodium acetate, CH3COONa, anhydrous. 2EN ISO 17353:20056.6

47、Sodium sulfate, Na2SO4, anhydrous. 6.7 Silica, grain size 0,2 mm to 0,063 mm (200 mesh to 63 mesh). 6.8 Tetrahydrofurane, C4H8O, free of peroxides and water. 6.9 Acetone, (propanone) (CH3)2CO. 6.10 Methanol, CH3OH. 6.11 Hexane, C6H14. 6.12 Sodium tetraethylborate, NaB(C2H5)4. 6.13 Monobutyltin trich

48、loride, MBTCl, C4H9SnCl3. 6.14 Dibutyltin dichloride, DBTCl, (C4H9)2SnCl2. 6.15 Tributyltin chloride, TBTCl, (C4H9)3SnCl. 6.16 Tetrabutyltin, TTBT, (C4H9)4Sn. 6.17 Monooctyltin trichloride, MOTCl, C8H17SnCl3. 6.18 Dioctyltin dichloride, DOTCl, (C8H17)2SnCl2. 6.19 Triphenyltin chloride, TPhTCl, (C6H5

49、)3SnCl. 6.20 Tricyclohexyltin chloride, TCyTCl, (C6H11)3SnCl. 6.21 Monoheptyltin trichloride, MHTCl, C7H15SnCl3; (internal standard). 6.22 Diheptyltin dichloride, DHTCl, (C7H15)2SnCl2; (internal standard). 6.23 Tripropyltin chloride, TPTCl, (C3H7)3SnCl; (internal standard). 6.24 Tetrapropyltin, TTPT, (C3H7)4Sn; (internal standard). 6.25 Multicomponent solutions and prepared reagents. Since stability of multicomponent standard solutions is a matter of concern, it is recommended to p