DIN EN ISO 15181-6-2014 Paints and varnishes - Determination of release rate of biocides from antifouling paints - Part 6 Determination of tralopyril release rate by quantitation o.pdf

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1、September 2014 Translation by DIN-Sprachendienst.English price group 11No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).

2、ICS 87.040!%:F“2233592www.din.deDDIN EN ISO 15181-6Paints and varnishes Determination of release rate of biocides from antifouling paints Part 6: Determination of tralopyril release rate by quantitation of itsdegradation product in the extract (ISO 15181-6:2012);English version EN ISO 15181-6:2014,E

3、nglish translation of DIN EN ISO 15181-6:2014-09Beschichtungsstoffe Bestimmung der Auswaschrate von Bioziden aus Antifouling-Beschichtungen Teil 6: Bestimmung der Auswaschrate von Tralopyril durch Quantifizierung seinerAbbauprodukte im Extrakt (ISO 15181-6:2012);Englische Fassung EN ISO 15181-6:2014

4、,Englische bersetzung von DIN EN ISO 15181-6:2014-09Peintures et vernis Dtermination du taux de lixiviation des biocides contenus dans les peinturesantisalissures Partie 6: Calcul du taux de lixiviation du tralopyril par dtermination de la concentration deson produit de dgradation dans lextrait (ISO

5、 15181-6:2012);Version anglaise EN ISO 15181-6:2014,Traduction anglaise de DIN EN ISO 15181-6:2014-09www.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be considered authoritative.2008.14 DIN EN ISO 15181-6:2014-09 2 A comma is used as the decimal marker. Nation

6、al foreword This document (EN ISO 15181-6:2014) has been prepared by Technical Committee ISO/TC 35 “Paints and varnishes”, Subcommittee SC 9 “General test methods for paints and varnishes” (Secretariat: BSI, United Kingdom) in collaboration with Technical Committee CEN/TC 139 “Paints and varnishes”

7、(Secretariat: DIN, Germany). The responsible German body involved in its preparation was the Normenausschuss Beschichtungsstoffe und Beschichtungen (DIN Standards Committee Coatings and Coating Materials), Working Committee NA 002-00-07 AA Allgemeine Prfverfahren fr Beschichtungsstoffe und Beschicht

8、ungen. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 3696 DIN ISO 3696 ISO 15181-1 DIN EN ISO 15181-1 DIN EN ISO 15181 consists of the following parts, under the general title Paints and varnishes Determination of release rate of bioc

9、ides from antifouling paints: Part 1: General method for extraction of biocides Part 2: Determination of copper-ion concentration in the extract and calculation of the release rate Part 3: Calculation of the zinc ethylene-bis(dithiocarbamate) (zineb) release rate by determination of the concentratio

10、n of ethylenethiourea in the extract Part 4: Determination of pyridinetriphenylborane (PTPB) concentration in the extract and calculation of the release rate Part 5: Calculation of the tolylfluanid and dichlofluanid release rate by determination of the concentration of dimethyltolylsulfamide (DMST)

11、and dimethylphenylsulfamide (DMSA) in the extract Part 6: Determination of tralopyril release rate by quantitation of its degradation product in the extract National Annex NA (informative) Bibliography DIN ISO 3696, Water for analytical laboratory use Specification and test methods DIN EN ISO 15181-

12、1, Paints and varnishes Determination of release rate of biocides from antifouling paints Part 1: General method for extraction of biocides EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 15181-6 June 2014 ICS 87.040 English Version Paints and varnishes - Determination of release rate of bi

13、ocides from antifouling paints - Part 6: Determination of tralopyril release rate by quantitation of its degradation product in the extract (ISO 15181-6:2012) Peintures et vernis - Dtermination du taux de lixiviation desbiocides contenus dans les peintures antisalissures -dtermination de la concentr

14、ation de son produit Beschichtungsstoffe - Bestimmung der Auswaschrate von Bioziden aus Antifouling-Beschichtungen - Teil 6: Bestimmung der Auswaschrate von Tralopyril durch Quantifizierung seiner Abbauprodukte im Extrakt This European Standard was approved by CEN on 8 May 2014. CEN members are boun

15、d 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 concerning such national standards may be obtained on application to the CE

16、N-CENELEC Management Centre or to any CEN member. This European Standard exists 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 CEN-CENELEC Management Centre h

17、as the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, L

18、uxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Br

19、ussels 2014 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 15181-6:2014 EPartie 6: Calcul du taux de lixiviation du tralopyril par (ISO 15181-6:2012) (ISO 15181-6:2012)de dgradation dans lextrait Contents DIN EN ISO 15181-6:20

20、14-09 EN ISO 15181-6:2014 (E) 2 Page Foreword 3 Introduction .4 1 Scope 5 2 Normative references 5 3 Principle 5 4 Supplementary information 6 5 Apparatus .6 6 Reagents and materials 6 7 Test samples 7 8 Preparation of calibration standards .7 8.1 General 7 8.2 Stock solution A .7 8.3 Stock solution

21、 B .7 8.4 Preparation of calibration standards from stock solutions 7 9 Recovery and conversion check standards .8 9.1 General 8 9.2 Stock solution C .8 9.3 Stock solution D .8 9.4 Preparation of recovery and conversion check standards .8 10 Procedure .9 10.1 General 9 10.2 Sample treatment .9 10.3

22、Preparation of chromatography eluent .9 10.4 Instrument calibration .9 10.5 Conversion and recovery determination .10 10.6 Sample determination .10 11 Calculation and expression of results .10 11.1 Calculation of the tralopyril concentration .10 11.2 Release rate for each test cylinder 11 11.3 Mean

23、release rate for each set of three cylinders 12 11.4 Cumulative tralopyril release 12 11.5 Mean tralopyril release rate 12 11.6 Pseudo-steady-state mean tralopyril release rate 13 12 Validation of the method .13 13 Test report 13 Annex A (normative) Supplementary information .15 Annex B (informative

24、) Additional information on tralopyril and BCCPCA 16 Bibliography 18 Foreword The text of ISO 15181-6:2012 has been prepared by Technical Committee ISO/TC 35 “Paints and varnishes” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 15181-6:2014 by Technical

25、 Committee CEN/TC 139 “Paints and varnishes” 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 December 2014, and conflicting national standards shall be wit

26、hdrawn at the latest by December 2014. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. According to the CEN-CENELEC Internal Regulatio

27、ns, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy,

28、 Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 15181-6:2012 has been approved by CEN as EN ISO 15181-6:2014 without any modification. DIN EN ISO 1

29、5181-6:2014-09 EN ISO 15181-6:2014 (E) 3 IntroductionBy using standard conditions of temperature, salinity and pH at low biocide concentrations in the surrounding artificial seawater, a repeatable value of the release rate under the specified laboratory conditions can be determined using the method

30、given in this part of ISO 15181, which can be used for quality assurance and material selection purposes. The actual release rate of biocides from antifouling paints on ships hulls into the environment depends, however, on many factors, such as ship operating schedules, length of service, berthing c

31、onditions, paint condition, as well as temperature, salinity, pH, pollutants, and biological community.The results of this test do not reflect environmental biocide release rates for antifouling products and are not suitable for direct use in the process of generating environmental risk assessments,

32、 producing environmental loading estimates or for establishing release rate limits for regulatory purposes. In comparison with copper and organotin release rate measurements obtained either by direct or indirect measurements of the copper release rate from ships hulls and from measurements made on p

33、anels exposed in harbours, all available data indicate that the results of this generic test method significantly overestimate the release rate of biocide under in-service conditions. Published results demonstrate that the results of this test method are generally higher than direct in-situ measurem

34、ents of copper and organotin release rate from the hulls of harboured ships by a factor of about 10 or more for several commercial antifouling coatings.12A similar relationship is expected to be found for other biocides. Realistic estimates of the biocide release from a ships hull under in-service c

35、onditions can only be obtained from this test method if this difference is taken into account.Where the results of this test method are used in the process of generating environmental risk assessments, producing environmental loading estimates or for regulatory purposes, it is most strongly recommen

36、ded that the relationship between laboratory release rates and actual environment inputs be taken into account to allow a more accurate estimate of the biocide release rate from antifouling coatings under real-life conditions to be obtained. This can be accomplished through the application of approp

37、riate correction factors.2DIN EN ISO 15181-6:2014-09 EN ISO 15181-6:2014 (E) 4 1 ScopeThis part of ISO 15181 specifies a method for determining the amount of tralopyril that has been released from an antifouling paint into artificial seawater in accordance with the procedure given in ISO 15181-1.Tra

38、lopyril is unstable in water and degrades hydrolytically to form 3-bromo-5-(4-chlorophenyl)-4-cyano-1H-pyrrole-2-carboxylic acid (BCCPCA). This part of ISO 15181 specifies a method for accelerating the conversion of the released tralopyril into this degradation product by heat treatment and quantify

39、ing the concentration of the BCCPCA degradation product in the artificial seawater extract, and gives the final calculation for the release rate of tralopyril under the specified laboratory conditions.This part of ISO 15181 is designed to allow the concurrent determination of tralopyril and other bi

40、ocides that can be released by a given antifouling paint (for example, zineb) through the analysis of separate sub-samples of an artificial seawater extract generated in accordance with ISO 15181-1.When used in conjunction with ISO 15181-1, the practical limits for quantifying release rates by this

41、method are from 0,36 g cm2d1to 270 g cm2d1. The quantitation of release rates lower than this range requires the use of an analytical method with a limit of quantitation for tralopyril in artificial seawater of less than 2 g/l.2 Normative referencesThe following referenced documents are indispensabl

42、e for 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, Water for analytical laboratory use Specification and test methodsISO 15181-1:2007, Paints

43、and varnishes Determination of release rate of biocides from antifouling paints Part 1: General method for extraction of biocidesASTM D6442-06, Standard test method for determination of copper release rate from antifouling coatings in substitute ocean water3 PrincipleThe quantity of tralopyril relea

44、sed into artificial seawater by the method given in ISO 15181-1 is determined by accelerating the hydrolytic degradation of the tralopyril in the leachate by heat treatment under controlled conditions and subsequently quantifying the concentration of the degradation product, 3-bromo-5-(4-chloropheny

45、l)-4-cyano-1H-pyrrole-2-carboxylic acid (BCCPCA) by high-performance liquid chromatography (HPLC) or by an alternative method, provided that it demonstrates a limit of quantitation for tralopyril in artificial seawater of 2 g/l or less. The release rate of the biocide under the specified laboratory

46、conditions is then calculated as tralopyril.NOTE Additional information on tralopyril and BCCPCA is given in Annex B.DIN EN ISO 15181-6:2014-09 EN ISO 15181-6:2014 (E) 5 4 Supplementary informationThe items of supplementary information required to be able to use the general extraction procedure, des

47、cribed in ISO 15181-1, for tralopyril are given in Annex A.5 Apparatus5.1 High-performance liquid chromatograph (HPLC), or other suitable instrument, which demonstrates a limit of quantitation for tralopyril in artificial seawater by the analytical method of 2 g/l or less. The limit of quantitation

48、shall be determined by the general procedure given in ASTM D6442-06, Annex 2 (determination of the LOQ for copper in substitute ocean water for the analytical method), suitably modified for tralopyril. If HPLC is used, the system shall, where possible, include the components specified in 5.1.1 to 5.1.6.5.1.1 Isocratic pump, capable of achieving a pressure of 150 bar (15 MPa) and a flow-rate of 1,5 ml/min.5.1.2 Ultraviolet detector, capable of monitoring at 280 nm.5.1.3 Autosampler, capable of making