SIST EN ISO 15181-4:2009

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Beschichtungsstoffe - Bestimmung der Auswaschrate von Bioziden aus Antifouling-Beschichtungen - Teil 4: Bestimmung der Konzentration von Pyridintriphenylboran (PTPB) im Extrakt und Berechnung der Auswaschrate (ISO 15181-4:2008)Peintures et vernis - Détermination du taux de lixiviation des biocides contenus dans les peintures antisalissures - Partie 4: Détermination de la concentration de pyridine-triphénylborane (PTPB) dans l'extrait et calcul du taux de lixiviation (ISO 15181-4:2008)Paints and varnishes - Determination of release rate of biocides from antifouling paints - Part 4: Determination of pyridine-triphenylborane (PTPB) concentration in the extract and calculation of the release rate (ISO 15181-4:2008)87.040Barve in lakiPaints and varnishesICS:Ta slovenski standard je istoveten z:EN ISO 15181-4:2008SIST EN ISO 15181-4:2009en,fr,de01-januar-2009SIST EN ISO 15181-4:2009SLOVENSKI
STANDARD
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN ISO 15181-4August 2008ICS 87.040 English VersionPaints and varnishes - Determination of release rate of biocidesfrom antifouling paints - Part 4: Determination of pyridine-triphenylborane (PTPB) concentration in the extract andcalculation of the release rate (ISO 15181-4:2008)Peintures et vernis - Détermination du taux de lixiviationdes biocides contenus dans les peintures antisalissures -Partie 4: Détermination de la concentration de pyridine-triphénylborane (PTPB) dans l'extrait et calcul du taux delixiviation (ISO 15181-4:2008)Beschichtungsstoffe - Bestimmung der Auswaschrate vonBioziden aus Antifouling-Beschichtungen - Teil 4:Bestimmung der Konzentration von Pyridintriphenylboran(PTPB) im Extrakt und Berechnung der Auswaschrate (ISO15181-4:2008)This European Standard was approved by CEN on 26 July 2008.CEN members 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 application 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 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,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2008 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 15181-4:2008: ESIST EN ISO 15181-4:2009

Reference numberISO 15181-4:2008(E)© ISO 2008
INTERNATIONAL STANDARD ISO15181-4First edition2008-08-01Paints and varnishes — Determination of release rate of biocides from antifouling paints — Part 4: Determination of pyridine-triphenylborane (PTPB) concentration in the extract and calculation of the release rate Peintures et vernis — Détermination du taux de lixiviation des biocides contenus dans les peintures antisalissures — Partie 4: Détermination de la concentration de pyridine-triphénylborane (PTPB) dans l'extrait et calcul du taux de lixiviation
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ii © ISO 2008 – All rights reserved
ISO 15181-4:2008(E) © ISO 2008 – All rights reserved iiiContents Page Foreword.iv Introduction.v 1 Scope.1 2 Normative references.1 3 Principle.2 4 Supplementary information.2 5 Apparatus.2 6 Reagents and materials.3 7 Test samples.3 8 Procedure.3 9 Calculation and expression of results.5 10 Validation of the method.8 11 Test report.8 Annex A (normative)
Supplementary information.10 Annex B (informative)
Additional information on PTPB.11 Bibliography.12
ISO 15181-4:2008(E) iv © ISO 2008 – All rights reserved Foreword ISO (the 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 committee 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 electrotechnical 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 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 any or all such patent rights. ISO 15181-4 was prepared by Technical Committee ISO/TC 35, Paints and varnishes, Subcommittee SC 9, General test methods for paints and varnishes. 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 calculation 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 release rate ⎯ Part 5: Calculation of the tolylfluanid and dichlofluanid release rate by determination of the concentration of dimethyltolylsulfamide (DMST) and dimethylphenylsulfamide (DMSA) in the extract The following part is under preparation: ⎯ Part 6: Determination of tralopyril release rate by quantification of its degradation product in the extract
ISO 15181-4:2008(E) © ISO 2008 – All rights reserved vIntroduction By 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 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 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 reflect 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 organotin release rates obtained either by direct or indirect measurements of the copper and organotin release rate from ships’ hulls and from measurements made on panels exposed in harbours, all available data indicate that the results of this generic test method significantly overestimate the release rate 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 coatings [1, 2]. A similar relationship is expected to be found for other biocides. Realistic estimates of the biocide release rate from a ship’s 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 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 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 factors [2].
INTERNATIONAL STANDARD ISO 15181-4:2008(E) © ISO 2008 – All rights reserved 1Paints and varnishes — Determination of release rate of biocides from antifouling paints — Part 4: Determination of pyridine-triphenylborane (PTPB) concentration in the extract and calculation of the release rate 1 Scope This part of ISO 15181 specifies the apparatus and analytical method for determining the amount of pyridine-triphenylborane (PTPB) that has been released from an antifouling paint into artificial seawater in accordance with the procedure given in ISO 15181-1. It determines the PTPB concentration in the artificial seawater extract and gives the final calculation for the release rate of PTPB under the specified laboratory conditions. This part of ISO 15181 is designed to allow the concurrent determination of PTPB and other biocides 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 the procedure given in ISO 15181-1. 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 µg⋅cm−2⋅d−1 to 500 µg⋅cm−2⋅d−1. The quantitative measurement of release rates below this range will require the concentration step described in the last paragraph in 8.2 or the use of an analytical method with a limit of quantitation for PTPB in artificial seawater which is lower than the limit specified in Clause 3 and in 5.1. 2 Normative references The following referenced documents are indispensable 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 methods ISO 15181-1:2007, Paints and varnishes — 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 SIST EN ISO 15181-4:2009

ISO 15181-4:2008(E) 2 © ISO 2008 – All rights reserved 3 Principle The quantity of PTPB biocide released into artificial seawater by the method given in ISO 15181-1 is determined by the use of a high-performance liquid chromatograph (HPLC) with UV detection at 220 nm after pre-concentration by solid-phase extraction (SPE), or by an alternative analytical method provided that it demonstrates a limit of quantitation for PTPB in artificial seawater of 10 µg/l or less. The release rate of the biocide under the specified laboratory conditions is then calculated as PTPB. The use of the HPLC method in conjunction with the additional sample concentration step described in the last paragraph in 8.2 can allow a limit of quantitation for PTPB in artificial seawater of 0,5 µg/l to be achieved. NOTE Additional information on PTPB is given in Annex B. Additional background information on the analytical method has been published by Takahashi, et al. [3]. 4 Supplementary information The items of supplementary information required to be able to use the general extraction procedure, described in ISO 15181-1, for PTPB are given in Annex A. 5 Apparatus 5.1 High-performance liquid chromatograph (HPLC), or other equivalent instrument, which has a limit of quantitation for PTPB in artificial seawater of 10 µg/l or less. The limit of quantitation shall be 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, suitably modified for PTPB. 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 and a flow-rate of 1,0 ml/min. 5.1.2 Ultraviolet detector, capable of monitoring at 220 nm. 5.1.3 Autosampler, capable of making 10 µl injections. 5.1.4 Chromatography column: A reverse-phase column with an internal diameter of 4,6 mm and a length of 250 mm, packed with a microparticulate octadecylsilane (C-18, end-capped) stationary phase (mean particle size 5,0 µm) or equivalent. 5.1.5 Column oven, capable of maintaining a constant column temperature of 30 °C. 5.1.6 Electronic data-processing system, capable of controlling the HPLC system, acquiring data and automatically integrating peak areas. 5.2 Pipettes, with disposable tips. 5.3 Volumetric flasks, made of glass. 5.4 Solid-phase extraction (SPE) cartridges, packed with 360 mg of C-18 sorbent, and sequentially conditioned prior to use with 10 ml of a solvent blend of acetonitrile and pyridine in a ratio of 99:1 parts by volume, then 10 ml of water, an
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