1、BRITISH STANDARDBS EN ISO 15181-4:2008 BS 3900-K4: 2008Paints 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 rateICS 87.040g49g50g3g38g50g51g60g44g49g
2、42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN ISO 15181-4:2008This British Standard was published under the authority of the Standards Policy and Strategy Committee on
3、 30 September 2008 BSI 2008ISBN 978 0 580 54640 2National forewordThis British Standard is the UK implementation of EN ISO 15181-4:2008. The UK participation in its preparation was entrusted to Technical Committee STI/10, Test methods for paints.A list of organizations represented on this committee
4、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 immunity from legal obligations.Amendments/corrigenda issued since p
5、ublicationDate CommentsEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 15181-4August 2008ICS 87.040English VersionPaints and varnishes - Determination of release rate of biocidesfrom antifouling paints - Part 4: Determination of pyridine-triphenylborane (PTPB) concentration in the extract andc
6、alculation of the release rate (ISO 15181-4:2008)Peintures et vernis - Dtermination du taux de lixiviationdes biocides contenus dans les peintures antisalissures -Partie 4: Dtermination de la concentration de pyridine-triphnylborane (PTPB) dans lextrait et calcul du taux delixiviation (ISO 15181-4:2
7、008)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 ar
8、e 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 th
9、e 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 st
10、atus 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,
11、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 2008 CEN All rights of exploitation in any form and by any means reservedworldwid
12、e for CEN national Members.Ref. No. EN ISO 15181-4:2008: EForeword This document (EN ISO 15181-4:2008) 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 E
13、uropean Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by February 2009, and conflicting national standards shall be withdrawn at the latest by February 2009. Attention is drawn to the possibility that some of th
14、e 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 bound to implement t
15、his 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, Switzerland and th
16、e United Kingdom. Endorsement notice The text of ISO 15181-4:2008 has been approved by CEN as a EN ISO 15181-4:2008 without any modification. BS EN ISO 15181-4:2008iiiContents Page ivIntroduction . 1 Scope 1 2 Normative references 1 3 Principle2 4 Supplementary information2 5 Apparatus .2 6 Reagents
17、 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 PTPB11 Bibliography 12 BS EN ISO 15181-4:2008iv Foreword ISO (th
18、e 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 committ
19、ee 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 electrotechn
20、ical 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
21、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
22、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 b
23、iocides 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 concentra
24、tion 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 (DM
25、ST) 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 BS EN ISO 15181-4:2008vIntroduction By using standard conditions of temperature, salinity and pH
26、 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 act
27、ual 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
28、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 f
29、or 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 ge
30、neric 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
31、 of about 10 or more for several commercial antifouling 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 take
32、n 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 environm
33、ental 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 factors2. BS EN ISO 15181-4:2008blank1Paints and varnishes
34、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 pyrid
35、ine-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 s
36、pecified 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 accord
37、ance 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 gcm2d1to 500 gcm2d1. The quantitative measurement of release rates below this range will require the concentratio
38、n 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 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 BS EN ISO 15181-4:20082 3 Principle The quantity of PTPB b
41、iocide 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 demonstr
42、ates a limit of quantitation for PTPB in artificial seawater of 10 g/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 paragrap
43、h in 8.2 can allow a limit of quantitation for PTPB in artificial seawater of 0,5 g/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
44、 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 seaw
45、ater of 10 g/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
46、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 l injections. 5.1.4 Chromatography column: A reverse-phase
47、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 m) or equivalent. 5.1.5 Column oven, capable of maintaining a constant column temperature of 30 C. 5.1.6 Electronic data-proce
48、ssing 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
49、 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, and finally 10 ml of artificial seawater. 5.5 Solid-phase extraction system, or equivalent system suitable for use with the extraction cartridges. 5.6 Rotary vacuum evaporator, with heating bath. BS EN ISO 15181-4:200836 Reagents and materials Suppliers material safety data sheets should be consulted for details of any hazards associated with the reagents listed below, and the risks associated with their
