1、September 2008DEUTSCHE NORM English price group 12No part of this standard 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).ICS 87.040!$QtY“1468154w
2、ww.din.deDDIN EN ISO 15181-5Paints and varnishes Determination of release rate of biocides from antifouling paints Part 5: Calculation of the tolylfluanid and dichlofluanid release rate bydetermination of the concentration of dimethyltolylsulfamide (DMST)and dimethylphenylsulfamide (DMSA) in the ext
3、ract (ISO 15181-5:2008)English version of DIN EN ISO 15181-5:2008-09Beschichtungsstoffe Bestimmung der Auswaschrate von Bioziden aus Antifouling-Beschichtungen Teil 5: Berechung der Auswaschrate von Tolylfluanid und Dichlofluanid durch Bestimmungder Konzentration von Dimethyltolylsulfamid (DMST) und
4、 Dimethylphenylsulfamid (DMSA)im Extrakt (ISO 15181-5:2008)Englische Fassung DIN EN ISO 15181-5:2008-09www.beuth.deDocument comprises 23 pagesDIN EN ISO 15181-5:2008-09 2 National foreword This standard falls in the domain of Technical Committee CEN/TC 139 “Paints and varnishes” (Secretariat: DIN, G
5、ermany). It is identical with International Standard ISO 15181-5 which was prepared by ISO/TC 35/SC 9 “General test methods for paints and varnishes” (Secretariat: BSI, United Kingdom). The responsible German body involved in its preparation was the Normenausschuss Beschichtungsstoffe und Beschichtu
6、ngen (Coatings and Coating Materials Standards Committee), Technical Committee NA 002-00-07 AA Allgemeine Prfverfahren fr Beschichtungsstoffe und Beschichtungen. DIN EN ISO 15181 consists of the following parts, under the general title Paints and varnishes Determination of release rate of biocides f
7、rom 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 concentration of e
8、thylenethiourea in the extract Part 4: Determination of pyridine-triphenylborane (PTPB) concentration in the extract and calculation of the release Part 5: Calculation of the tolylfluanid and dichlofluanid release rate by determination of the concentration of dimethyltolylsulfamide (DMST) and dimeth
9、ylphenylsulfamide (DMSA) in the extract The following part is under preparation: Part 6: Determination of tralopyril release rate by quantification of its degradation product 3-bromo-5-(4-chlorophenyl)-4-cyano-1H-pyrrole-2-carboxylic acid (BCCPCA) in the extract The DIN Standards corresponding to th
10、e International Standards referred to in the EN are as follows: ISO 3696 DIN ISO 3696 ISO 15181-1 DIN EN ISO 15181-1 National Annex NA (informative) Bibliography DIN ISO 3696, Water for analytical laboratory use Specification and test methods DIN EN ISO 15181-1, Paints and varnishes Determination of
11、 release rate of biocides from antifouling paints Part 1: General method for extraction of biocides EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 15181-5May 2008ICS 87.040English VersionPaints and varnishes - Determination of release rate of biocidesfrom antifouling paints - Part 5: Calculat
12、ion of the tolylfluanid anddichlofluanid release rate by determination of the concentrationof dimethyltolylsulfamide (DMST) and dimethylphenylsulfamide(DMSA) in the extract (ISO 15181-5:2008)Peintures et vernis - Dtermination du taux de lixiviationdes biocides contenus dans les peintures antisalissu
13、res -Partie 5: Calcul du taux de lixiviation du tolylfluanide et dudichlofluanide par dtermination de la concentration dudimthyl-tolylsulfamide (DMST) et du dimthyl-phnylsulfamide (DMSA) dans lextrait (ISO 15181-5:2008)Beschichtungsstoffe - Bestimmung der Auswaschrate vonBioziden aus Antifouling-Bes
14、chichtungen - Teil 5:Berechung der Auswaschrate von Tolylfluanid undDichlofluanid durch Bestimmung der Konzentration vonDimethyltolylsulfamid (DMST) und Dimethylphenylsulfamid(DMSA) im Extract (ISO 15181-5:2008)This European Standard was approved by CEN on 8 May 2008.CEN members are bound to comply
15、with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the CEN Management C
16、entre or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficia
17、l versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia
18、, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2008 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national
19、 Members.Ref. No. EN ISO 15181-5:2008: E2 DIN EN ISO 15181-5:2008-09EN ISO 15181-5:2008 (E)Contents Page Foreword3 Introduction .4 1 Scope 5 2 Normative references 5 3 Principle6 4 Supplementary information 6 5 Apparatus .6 6 Reagents and materials 7 7 Test samples 7 8 Preparation of calibration sta
20、ndards.8 9 Recovery and conversion check standards .9 10 Procedure 10 11 Calculation and expression of results 11 12 Validation of the method 15 13 Test report . 15 Annex A (normative) Supplementary information 17 Annex B (informative) Additional information on tolylfluanid, DMST, dichlofluanid and
21、DMSA. 18 Bibliography. 21 Foreword 3 EN ISO 15181-5:2008 (E)DIN EN ISO 15181-5:2008-09This document (EN ISO 15181-5:2008) has been prepared by Technical Committee ISO/TC 35 “Paints and varnishes“ in collaboration with Technical Committee CEN/TC 139 “Paints and varnishes” the secretariat of which is
22、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 November 2008, and conflicting national standards shall be withdrawn at the latest by November 2008. Attention is drawn to the possibil
23、ity 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 Regulations, the national standards organizations of the following countries are b
24、ound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden,
25、 Switzerland and the United Kingdom. Endorsement notice The text of ISO 15181-5:2008 has been approved by CEN as a EN ISO 15181-5:2008 without any modification. Introduction By using standard conditions of temperature, salinity and pH at low biocide concentrations in the surrounding artificial seawa
26、ter, a repeatable value of the release rate under the specified laboratory conditions can be determined using the method 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 hull
27、s into the environment will, however, depend on many factors, such as ship operating schedules, length of service, berthing conditions, paint condition, as well as temperature, salinity, pH, pollutants and biological community in a particular area. The results of this test do not reflect environment
28、al biocide release rates for antifouling products and are not suitable for direct use in the process of generating environmental-risk assessments, producing environmental-loading estimates or for establishing release rate limits for regulatory purposes. In comparison with copper and organotin releas
29、e rates obtained either by direct or indirect measurements of the copper release rate from ships hulls and from measurements made on panels exposed in harbours, all available data indicate that the results obtained using this generic test method significantly overestimate the release rates of biocid
30、es under in-service conditions. Published results demonstrate that the results of this test method are generally higher by a factor of about 10 or more for several commercial antifouling coatings than direct in situ measurements of copper and organotin release rates from in-service ship hulls 1, 2.
31、A similar relationship is expected to be found for other biocides. Realistic estimates of the biocide release rate from a ships hull under in-service conditions 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
32、process of generating environmental-risk assessments, producing environmental-loading estimates or for regulatory purposes, it is most strongly recommended that the relationship between laboratory release rates and actual environmental inputs be taken into account to allow a more accurate estimate o
33、f the biocide release rate from antifouling coatings under real-life conditions to be obtained. This can be accomplished through the application of appropriate correction factors2. 4 DIN EN ISO 15181-5:2008-09EN ISO 15181-5:2008 (E)1 Scope This part of ISO 15181 specifies the apparatus and analytica
34、l method for determining the amount of tolylfluanid and dichlofluanid that has been released from an antifouling paint into artificial seawater in accordance with the procedure given in ISO 15181-1. Tolylfluanid and dichlofluanid are unstable in the marine environment and degrade to form dimethyltol
35、ylsulfamide (DMST) and dimethylphenylsulfamide (DMSA), respectively. This part of ISO 15181 specifies a method for converting the released species into these degradation products, quantifying their concentration in the treated artificial seawater samples, and gives the final calculation for the rele
36、ase rate of tolylfluanid and dichlofluanid under the specified laboratory conditions. This part of ISO 15181 is designed to allow the concurrent determination of tolylfluanid, dichlofluanid and other biocides that can be released by a given antifouling paint (for example, copper) through the analysi
37、s 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 method are from 1,3 gcm2d1to 500 gcm2d1. The quantitation of release rates lower than this range
38、 will require the use of an analytical method with a lower limit of quantitation for tolylfluanid, dichlofluanid, or both (as appropriate) in artificial seawater than that specified in Clause 3 and in 5.1. 2 Normative references The following referenced documents are indispensable for the applicatio
39、n 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 methods ISO 15181-1:2007, Paints and varnishes Dete
40、rmination of release rate of biocides from antifouling paints Part 1: General method for extraction of biocides ASTM D 6442-06, Standard Test Method for Determination of Copper Release Rate from Antifouling Coatings in Substitute Ocean Water 5 EN ISO 15181-5:2008 (E)DIN EN ISO 15181-5:2008-093 Princ
41、iple The amount of tolylfluanid released from a test cylinder into artificial seawater by the method given in ISO 15181-1 is determined by promoting the degradation of the tolylfluanid in the leachate under controlled conditions and subsequently quantifying the concentration of the degradation produ
42、ct, dimethyltolylsulfamide (DMST), by a high-performance liquid chromatography (HPLC) method or by an alternative analytical method, provided that it has a limit of quantitation for tolylfluanid in artificial seawater of 7 g/l or less. The release rate of the biocide under the specified laboratory c
43、onditions is then calculated as tolylfluanid. The amount of dichlofluanid released from a test cylinder into artificial seawater by the method given in ISO 15181-1 is determined by promoting the controlled degradation of the dichlofluanid in the leachate, and quantifying the concentration of the deg
44、radation product, dimethylphenylsulfamide (DMSA), by a similar HPLC method or by an alternative analytical method, provided that it demonstrates a limit of quantitation for dichlofluanid in artificial seawater of 7 g/l or less. The release rate of the biocide under the specified laboratory condition
45、s is then calculated as dichlofluanid. Additional information on tolylfluanid, dichlofluanid, DMST and DMSA is given in Annex B. 4 Supplementary information The items of supplementary information required to be able to use the general extraction procedure, described in ISO 15181-1, for dichlofluanid
46、 and tolylfluanid are given in Annex A. 5 Apparatus 5.1 High-performance liquid chromatograph (HPLC), or other suitable instrument, which has a limit of quantitation for tolylfluanid, dichlofluanid, or both (as appropriate) in artificial seawater of 7 g/l or less. The limit of quantitation shall be
47、determined by the general procedure given in Annex 2 of ASTM D 6442-06 (Determination of the LOQ for Copper in Substitute Ocean Water for the Analytical Method), suitably modified for tolylfluanid, dichlofluanid, or both (as appropriate). If HPLC is used, the system shall, where possible, include th
48、e components specified in 5.1.1 to 5.1.6. 5.1.1 Gradient-programmed pump, capable of achieving a pressure of 150 bar and a flow-rate of 0,5 ml/min. 5.1.2 Ultraviolet detector, capable of monitoring at 195 nm. 5.1.3 Autosampler, capable of making 200 l injections. 5.1.4 Chromatography column: a rever
49、se-phase column with an internal diameter of 2,0 mm and a length of 150 mm, packed with a microparticulate octadecylsilane (C-18, end-capped) stationary phase (mean particle size 5,0 m) or equivalent, and equipped with a reverse-phase pre-column with an internal diameter of 4,6 mm and a length of 30 mm, packed with a microparticulate octadecylsilane (C-18, end-capped) stationary phase (mean particle size 5,0 m) or equivalent. 5.1.5 Column oven, providing a constant column temperature of 40 C. 5.1.6 Electronic data-proc
