1、October 2007DEUTSCHE NORM English price group 10No 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!$IuH“1388237www
2、.din.deDDIN EN ISO 15181-2Paints and varnishes Determination of release rate of biocides from antifouling paints Part 2: Determination of copper-ion concentration in the extract andcalculation of the release rate (ISO 15181-2:2007)English version of DIN EN ISO 15181-2:2007-10Beschichtungsstoffe Best
3、immung der Auswaschrate von Bioziden aus Antifouling-Beschichtungen Teil 2: Bestimmung der Kupferionen-Konzentration im Extrakt und Berechnung derAuswaschrate (ISO 15181-2:2007)Englische Fassung DIN EN ISO 15181-2:2007-10SupersedesDIN EN ISO 15181-2:2004-09www.beuth.deDocument comprises 18 pagesDIN
4、EN ISO 15181-2:2007-10 2 National foreword This standard falls in the domain of Technical Committee CEN/TC 139 “Paints and varnishes” (Secretariat: DIN, Germany). It is identical with International Standard ISO 15181-2 which was prepared by ISO/TC 35/SC 9 “General test methods for paints and varnish
5、es” (Secretariat: BSI, United Kingdom). The responsible German body involved in its preparation was the Normenausschuss Beschichtungsstoffe und Beschichtungen (Coatings and Coating Materials Standards Committee), Technical Committee NA 002-00-07 AA Allgemeine Prfverfahren fr Beschichtungsstoffe und
6、Beschichtungen. DIN EN ISO 15181 consists of the following parts, under the general title Paints and varnishes Determination of release rate of biocides from antifouling paints: Part 1: General method for extraction of biocides Part 2: Determination of copper-ion concentration in the extract and cal
7、culation of the release rate Part 3: Calculation of the zinc ethylene-bis(dithiocarbamate) (zineb) release rate by determination of the concentration of ethylenethiourea in the extract Part 4: Determination of pyridine-triphenylborane (PTPB) concentration in the extract and calculation of the releas
8、e (at draft stage) Part 5: Calculation of the tolylfluanid and dichlofluanid release rate by determination of the concentration of dimethyltolylsulfamide (DMST) and dimethylphenylsulfamide (DMSA) in the extract (at draft stage) The DIN Standards corresponding to the International Standards referred
9、to in the EN are as follows: ISO 3696 DIN ISO 3696 ISO 15181-1 DIN EN ISO 15181-1 Amendments This standard differs from DIN EN ISO 15181-2:2004-09 as follows: a) Subclauses 5.1, 5.8.4, 6.3, 6.4 and clause 7, Annex A and Annex B have been editorially revised. Previous editions DIN EN ISO 15181-2: 200
10、4-09 DIN EN ISO 15181-2:2007-10 3 National Annex NA (informative) Bibliography DIN EN ISO 15181-1, Paints and varnishes Determination of release rate of biocides from antifouling paints Part 1: General method for extraction of biocides DIN ISO 3696, Water for analytical laboratory use Specification
11、and test methods DIN EN ISO 15181-2:2007-10 4 This page is intentionally blank EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 15181-2June 2007ICS 87.040 Supersedes EN ISO 15181-2:2004 English VersionPaints and varnishes - Determination of release rate of biocidesfrom antifouling paints - Part
12、 2: Determination of copper-ionconcentration in the extract and calculation of the release rate(ISO 15181-2:2007)Peintures et vernis - Dtermination du taux de lixiviationdes biocides contenus dans les peintures antisalissures -Partie 2: Dtermination de la concentration ionique ducuivre dans lextrait
13、 et calcul du taux de lixiviationBeschichtungsstoffe - Bestimmung der Auswaschrate vonBioziden aus Antifouling-Beschichtungen - Teil 2:Bestimmung der Kupferionen-Konzentration im Extrakt undBerechnung der Auswaschrate (ISO 15181-2:2007)This European Standard was approved by CEN on 16 May 2007.CEN me
14、mbers are bound to comply 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 applicati
15、on to the CEN 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 translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the
16、 same status as theofficial 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,R
17、omania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2007 CEN All rights of exploitation in any form and by any means reserved
18、worldwide for CEN national Members.Ref. No. EN ISO 15181-2:2007: E(ISO 15181-2:2007)EN ISO 15181-2:2007 (E) 2 Contents Page Foreword3 Introduction .4 1 Scope 5 2 Normative references 5 3 Principle5 4 Supplementary information required for the copper extraction procedure 6 5 Apparatus .6 6 Reagents a
19、nd materials 6 7 Test samples 6 8 Procedure .7 9 Calculation and expression of results.8 10 Precision.11 11 Test report 11 Annex A (normative) Supplementary information required for the copper extraction procedure .13 Bibliography 14 Foreword This document (EN ISO 15181-2:2007) has been prepared by
20、Technical Committee ISO/TC 35 “Paints and varnishes” in collaboration with Technical 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 endorse
21、ment, at the latest by December 2007, and conflicting national standards shall be withdrawn at the latest by December 2007. This document supersedes EN ISO 15181-2:2004. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to im
22、plement 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, Switzerla
23、nd and United Kingdom. Endorsement notice The text of ISO 15181-2:2007 has been approved by CEN as EN ISO 15181-2:2007 without any modifications. EN ISO 15181-2:2007 (E) 3 Introduction By using standard conditions of temperature, salinity and pH at low biocide concentrations in the surrounding artif
24、icial seawater, 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
25、 ships hulls into the environment will, however, depend on many factors, such as ship operating schedules, length of service, berthing conditions, paint condition, as well as the temperature, salinity, pH, pollutants and biological community in a particular area. The results of this test do not refl
26、ect environmental 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 o
27、rganotin release 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
28、rates of biocides under in-service conditions. Published results demonstrate that the results of this test method are generally higher than direct in situ measurements of copper and organotin release rates from in-service ship hulls by a factor of about 10 or more for several commercial antifouling
29、coatings1, 2. 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 ar
30、e used in the 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 accur
31、ate estimate of 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. EN ISO 15181-2:2007 (E) 4 1 Scope This part of ISO 15181 specifies the apparatus and analytical method fo
32、r determining the amount of copper (based) biocide that has been released from an antifouling paint into artificial seawater in accordance with the procedure given in ISO 15181-1. It determines the copper-ion concentration and gives the final calculation for the release rate of copper under the spec
33、ified laboratory conditions. This part of ISO 15181 is designed to generally allow the concurrent determination of copper ions and other biocides that might be released by a given antifouling paint through the analysis of separate sub-samples of an artificial seawater extract generated in accordance
34、 with the procedure given in ISO 15181-1, and analysed in accordance with the procedures given in other parts of this International Standard. When used in conjunction with ISO 15181-1, the practical limits on the quantitative measurement of release rates by this method are from 1,8 gcm2d1to 500 gcm2
35、d1. The quantitative measurement of release rates below this range will require the use of an analytical method with a lower limit of quantitation for copper in artificial seawater than the limit specified in 5.1. 2 Normative references The following referenced documents are indispensable for the ap
36、plication 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 varnis
37、hes Determination 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 3 Principle The concentration of the copper ions r
38、eleased into artificial seawater in accordance with the procedure given in ISO 15181-1 is determined by the use of an atomic absorption spectrometer or by an alternative analytical method, provided that it demonstrates a limit of quantitation for copper in artificial seawater of 10 g/l or less. The
39、release rate of the biocide is then calculated as copper metal. EN ISO 15181-2:2007 (E) 5 4 Supplementary information required for the copper extraction procedure The items of supplementary information required to be able to use the general extraction procedure, described in ISO 15181-1, for copper-
40、based biocides are given in Annex A. 5 Apparatus 5.1 Atomic absorption spectrometer, preferably with autosampler, or other suitable instrument, which has a limit of quantitation for copper in artificial seawater of 10 g/l or less. The limit of quantitation shall be determined by the procedure given
41、in Annex 2 (Determination of the LOQ for Copper in Substitute Ocean Water for the Analytical Method) of ASTM D 6442-06. 5.2 Mechanical shaker, with appropriate holders. 5.3 Dispensers, automatic or repeating, for reagents. 5.4 Pipettes, of appropriate volume, with disposable tips. 5.5 Volumetric fla
42、sks, of appropriate volume. 5.6 Sample tubes, of appropriate capacity, with screw closures, made of an inert material. NOTE Polypropylene, polycarbonate and borosilicate glass have been found to be suitable. 6 Reagents and materials Suppliers material safety data sheets should be consulted for detai
43、ls of any hazards associated with the reagents listed below, and the risks associated with their use should be assessed. Appropriate protective clothing and equipment should be utilized. Unless otherwise specified, use only reagents of recognized analytical grade. 6.1 Cleaning reagents. Use one of t
44、he following reagents for cleaning all the equipment: 6.1.1 Hydrochloric acid, concentrated aqueous solution, 37 % by mass. 6.1.2 Hydrochloric acid, aqueous solution, 10 % by volume. 6.2 Nitric acid, concentrated ( approximately 1,42 g/ml). 6.3 Artificial seawater, as defined in ISO 15181-1. 6.4 Wat
45、er, conforming to the requirements of grade 2 of ISO 3696. 7 Test samples Use extracts taken from the release rate measuring containers as described in ISO 15181-1. EN ISO 15181-2:2007 (E) 6 8 Procedure 8.1 General Carry out all determinations on the extract using the following method. An alternativ
46、e method of analysis is allowed providing it has a limit of quantitation for copper ions in artificial seawater of 10 g/l or less, determined by the procedure given in Annex 2 (Determination of the LOQ for Copper in Substitute Ocean Water for the Analytical Method) of ASTM D 6442-06, a recovery of (
47、100 10) % for artificial seawater recovery check standards containing copper ions at concentrations of 50 g/l and 200 g/l, and a recovery of (100 15) % for an artificial seawater recovery check standard containing copper ions at a concentration of 10 g/l. Clean all non-disposable or re-used apparatu
48、s by immersion in concentrated hydrochloric acid (6.1.1) for at least 30 min, or dilute acid (6.1.2) for at least 6 h, to remove all traces of biocide. Rinse thoroughly with grade 2 water (6.4). NOTE Some biocides have a strong tendency to adsorb on certain glass or plastic surfaces, which necessita
49、tes the above precautions. Operate the spectrometer or other apparatus in accordance with the manufacturers instructions. 8.2 Sample treatment Immediately acidify the test samples by the addition of 0,10 ml of concentrated nitric acid (6.2) per 100 ml of test sample, agitate for at least 10 min, and then filter through a 0,45 m filter. The solution may then be stored at a temperature between 2 C to 6 C for up to 14 days before analysis. Solutions shall be allowed to come to equilibrium at room temperature befor
