1、BRITISH STANDARDBS EN ISO 15181-5:2008 BS 3900-K5:2008Paints and varnishes Determination of release rate of biocides from antifouling paints Part 5: Calculation of the tolylfluanid and dichlofluanid release rate by determination of the concentration of dimethyltolylsulfamide (DMST) and dimethylpheny
2、lsulfamide (DMSA) in the extractICS 87.040g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN ISO 15181-5:2008This British Standard was published
3、under the authority of the Standards Policy and Strategy Committee on 29 August 2008 BSI 2008ISBN 978 0 580 54641 9National forewordThis British Standard is the UK implementation of EN ISO 15181-5:2008.The UK participation in its preparation was entrusted to Technical Committee STI/10, Test methods
4、for paints.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application.Compliance with a British Standard cannot confer imm
5、unity from legal obligations.Amendments/corrigenda issued since publicationDate CommentsEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 15181-5May 2008ICS 87.040English VersionPaints and varnishes - Determination of release rate of biocidesfrom antifouling paints - Part 5: Calculation of the t
6、olylfluanid 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 antisalissures -Partie
7、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-Beschichtungen
8、- 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 with the CEN
9、/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
10、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.C
11、EN 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, Swe
12、den, 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 Members.Ref
13、. No. EN ISO 15181-5:2008: EForeword This 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 held by DIN. This European Standard shall be give
14、n 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 possibility that some of the elements of this document ma
15、y 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 bound to implement this European Standard: Austria
16、, 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 the United Kingdom. Endorsement
17、notice The text of ISO 15181-5:2008 has been approved by CEN as a EN ISO 15181-5:2008 without any modification. BS EN ISO 15181-5:2008iiiContents Page 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 Tes
18、t samples . 3 8 Preparation of calibration standards 4 9 Recovery and conversion check standards 5 10 Procedure 6 11 Calculation and expression of results 7 12 Validation of the method 11 13 Test report . 11 Annex A (normative) Supplementary information 13 Annex B (informative) Additional informatio
19、n on tolylfluanid, DMST, dichlofluanid and DMSA. 14 Bibliography . 17 BS EN ISO 15181-5:2008blankvIntroduction 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
20、 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, s
21、uch 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 environmental biocide release rates for antifouling products and are not s
22、uitable 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 t
23、he 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 biocides under in-service conditions. Published results demonstrate t
24、hat 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. A similar relationship is expected to be found for other biocid
25、es. 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 process of generating environmental-risk assessments, producing
26、 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
27、-life conditions to be obtained. This can be accomplished through the application of appropriate correction factors2. BS EN ISO 15181-5:2008blank1Paints and varnishes Determination of release rate of biocides from antifouling paints Part 5: Calculation of the tolylfluanid and dichlofluanid release r
28、ate by determination of the concentration of dimethyltolylsulfamide (DMST) and dimethylphenylsulfamide (DMSA) in the extract 1 Scope This part of ISO 15181 specifies the apparatus and analytical method for determining the amount of tolylfluanid and dichlofluanid that has been released from an antifo
29、uling 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 dimethyltolylsulfamide (DMST) and dimethylphenylsulfamide (DMSA), respectively. This part of ISO 15181 specifies a met
30、hod 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 release rate of tolylfluanid and dichlofluanid under the specified laboratory conditions. This part of ISO 1518
31、1 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 analysis of separate sub-samples of an artificial seawater extract generated in accordance with ISO 15181-1. When
32、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 will require the use of an analytical method with a lower limit of quantitation for tolylfluanid, dichlofl
33、uanid, 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 application of this document. For dated references, only the edition cited applies. For undated references, the lates
34、t 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 bioc
35、ides ASTM D 6442-06, Standard Test Method for Determination of Copper Release Rate from Antifouling Coatings in Substitute Ocean Water BS EN ISO 15181-5:20082 3 Principle The amount of tolylfluanid released from a test cylinder into artificial seawater by the method given in ISO 15181-1 is determine
36、d by promoting the degradation of the tolylfluanid in the leachate under controlled conditions and subsequently quantifying the concentration of the degradation product, dimethyltolylsulfamide (DMST), by a high-performance liquid chromatography (HPLC) method or by an alternative analytical method, p
37、rovided 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 conditions is then calculated as tolylfluanid. The amount of dichlofluanid released from a test cylinder into artificial seawater by th
38、e 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 degradation product, dimethylphenylsulfamide (DMSA), by a similar HPLC method or by an alternative analytical method, provided that it de
39、monstrates 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 conditions is then calculated as dichlofluanid. Additional information on tolylfluanid, dichlofluanid, DMST and DMSA is given in Annex B. 4 Sup
40、plementary information The items of supplementary information required to be able to use the general extraction procedure, described in ISO 15181-1, for dichlofluanid and tolylfluanid are given in Annex A. 5 Apparatus 5.1 High-performance liquid chromatograph (HPLC), or other suitable instrument, wh
41、ich 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 determined by the general procedure given in Annex 2 of ASTM D 6442-06 (Determination of the LOQ for Copper in Substitute Ocean Water
42、for the Analytical Method), suitably modified for tolylfluanid, dichlofluanid, or both (as appropriate). If HPLC is used, the system shall, where possible, include the 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 o
43、f 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 reverse-phase column with an internal diameter of 2,0 mm and a length of 150 mm, packed with a microparticulate octadecylsilane (C-18, end-
44、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.
45、5 Column oven, providing a constant column temperature of 40 C. 5.1.6 Electronic data-processing system, capable of controlling the HPLC system, acquiring data and enabling automated integration of peak areas. 5.2 Glass vials, volume 30 ml, screw-topped. 5.3 Dispensers, automatic or repeating, for r
46、eagents. 5.4 Pipettes, with disposable tips. BS EN ISO 15181-5:200835.5 Volumetric flasks, volume 25 ml and 100 ml. 5.6 Microlitre syringe, capable of accurately dispensing volumes of between 1 l and 100 l. 5.7 Syringe, glass or disposable, capable of dispensing 2 ml. 6 Reagents and materials Suppli
47、ers material safety data sheets should be consulted for details 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 rec
48、ognized analytical grade. 6.1 Cleaning reagents. Use one of the 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 Tolylfluanid, analytical standard with a certified m
49、ass fraction of tolylfluanid of at least 99,0 %, for use in determining the tolylfuanid release rate. See also Clause 9. 6.3 Dichlofluanid, analytical standard with a certified mass fraction of at least 99,0 %, for use in determining the dichlofluanid release rate. See also Clause 9. 6.4 Dimethyltolylsulfamide (DMST), analytical standard with a certified mass fraction of at least 99,0 %, for use in preparing the calibration standard for determination of the tolylfluanid release rate. See also Clause 8. 6.5 Dimethylphenylsulfamide (DMSA),
