EN ISO 13129-2012 en Paints and varnishes - Electrochemical measurement of the protection provided to steel by paint coatings - Current interrupter (CI) technique relaxation voltam.pdf

1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN ISO 13129:2012Paints and varnishes Electrochemical measurement of the protection provided to steel by paint coatings Current interrupter (CI) technique, relaxation voltamme

2、try (RV) technique and DC transient (DCT) measurementsBS EN ISO 13129:2012 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO 13129:2012.The UK participation in its preparation was entrusted to Technical Committee STI/10, Test methods for paints.A list of organ

3、izations 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. The British Standards Institution 2013. Published by BSI Standards Limited 20

4、13 ISBN 978 0 580 67120 3 ICS 87.040 Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 28 February 2013. Amendments issued since publicationDate Text affectedEUROP

5、EAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 13129 December 2012 ICS 87.040 English Version Paints and varnishes - Electrochemical measurement of the protection provided to steel by paint coatings - Current interrupter (CI) technique, relaxation voltammetry (RV) technique and DC transient (DC

6、T) measurements (ISO 13129:2012) Peintures et vernis - Mesurage lectrochimique de la protection apporte lacier par des revtements de peinture - Technique du courant interrompu (CI), voltamtrie de relaxation (VR) ou mesurages de courants continus transitoires (CCT) (ISO 13129:2012) Beschichtungsstoff

7、e - Elektrochemische Messung der Schutzwirkung von Beschichtungen auf Stahl - Stromunterbrechnugsverfahren (CI), Relaxationsvoltametrie (RV) oder Gleichstromtransientenmessung (DCT) (ISO 13129:2012) This European Standard was approved by CEN on 1 September 2012. CEN members are bound to comply with

8、the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Managem

9、ent 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 translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same statu

10、s as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,

11、 Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2012 CEN All rights of

12、 exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 13129:2012: EBS EN ISO 13129:2012BS EN ISO 13129:2012 EN ISO 13129:2012 (E) 3 Foreword This document (EN ISO 13129:2012) has been prepared by Technical Committee ISO/TC 35 “Paints andvarnishes“ in

13、 collaboration with Technical Committee CEN/TC 139 “Paints and varnishes” the secretariat ofwhich is held by DIN. This European Standard shall be given the status of a national standard, either by publication of an identicaltext or by endorsement, at the latest by June 2013, and conflicting national

14、 standards shall be withdrawn atthe latest by June 2013. Attention is drawn to the possibility that some of the elements of this document may be the subject of patentrights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. According to the CEN/CENELEC I

15、nternal Regulations, the national standards organisations of the followingcountries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, CzechRepublic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece,Hungary, Iceland, I

16、reland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 13129:2012 has been approved by CEN as a EN ISO 13129:2012 without any modification. I

17、SO 2012Paints and varnishes Electrochemical measurement of the protection provided to steel by paint coatings Current interrupter (CI) technique, relaxation voltammetry (RV) technique and DC transient (DCT) measurementsPeintures et vernis Mesurage lectrochimique de la protection apporte lacier par d

18、es revtements de peinture Technique du courant interrompu (CI), voltamtrie de relaxation (VR) et mesurages de courants continus transitoires (CCT)INTERNATIONAL STANDARDISO 13129First edition 2012-10-01Reference number ISO 13129:2012(E)BS EN ISO 13129:2012BS EN ISO 13129:2012 ISO 13129:2012(E) ISO 20

19、12 All rights reserved iiiContents PageForeword iv Introduction v 1 Scope 1 2 Normative references . 1 3 Terms and definitions . 1 4 Apparatus 24.1 Faraday cage 24.2 Cell for sample, including electrode holder . 24.3 Galvanostat . 34.4 Potentiostat . 34.5 Electrodes . 34.6 Electrolyte . 45 Specimens

20、 . 45.1 Preconditioning of specimens . 45.2 Environmental control . 45.3 Evaluation of specimens exposed to weathering in the laboratory and in the field . 45.4 Number of specimens and repeatability of results 56 Experimental procedure 56.1 General . 56.2 Current interrupter technique 56.3 Relaxatio

21、n voltammetry . 66.4 DC transient measurements . 7 7 Expression of results . 8 8 Precision 8 9 Test report . 8 Annex A (normative) Description of the dummy cell 10 Annex B (informative) Further considerations concerning measurements on coatings 12 Annex C (informative) Examples of results .14 Biblio

22、graphy .15BS EN ISO 13129:2012ISO 13129:2012(E)ForewordISO (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 mem

23、ber 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 El

24、ectrotechnical 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 adopt

25、ed 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

26、 rights. ISO shall not be held responsible for identifying any or all such patent rights.ISO 13129 was prepared by Technical Committee ISO/TC 35, Paints and varnishes, Subcommittee SC 9, General test methods for paints and varnishes.iv ISO 2012 All rights reservedBS EN ISO 13129:2012ISO 13129:2012(E

27、)IntroductionQuantitative assessment of protection performance of organic coatings has been required in industry, for example for evaluating the durability of organic coatings or judging the life of protective coatings. Electrochemical methods can be used for these purposes. The current interrupter

28、(CI) technique, relaxation voltammetry (RV) and DC transient (DCT) measurements are simple techniques giving effective data which are comparable with electrochemical impedance spectroscopy (EIS) in principle.An advantage is that the principle is simple and time for one measurement is short. ISO 2012

29、 All rights reserved vBS EN ISO 13129:2012BS EN ISO 13129:2012Paints and varnishes Electrochemical measurement of the protection provided to steel by paint coatings Current interrupter (CI) technique, relaxation voltammetry (RV) technique and DC transient (DCT) measurements1 ScopeThis International

30、Standard specifies the procedure for evaluation of the experimental set-up of electrochemical measurements on high-impedance coated samples using methods that are based on the current interrupter (CI) technique, relaxation voltammetry (RV) or DC transient (DCT) measurements.It provides specific defi

31、nitions and guidance on optimizing the collection of CI, RV and DCT data from high-impedance systems. High impedance in the context of intact coatings refers to systems with an impedance greater than 109/cm2. This does not preclude measurements on systems with lower impedance. This International Sta

32、ndard deals in particular with: instrumental set-up: requirements and shortcomings; data validation: checking the measurement range and the accuracy of the data; performing CI, RV, DCT measurements: specimen considerations and instrumental parameters; the experimental results: different methods of p

33、resenting CI, RV and DCT data.Following the recommendations should ensure the acquisition of CI, RV and DCT data that can be used to study the performance of the specimen. This International Standard does not give guidelines for the interpretation of the data.2 Normative referencesThe following refe

34、renced 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 16773-1, Paints and varnishes Electrochemical impedance spectros

35、copy (EIS) on high-impedance coated specimens Part 1: Terms and definitions3 Terms and definitionsFor the purposes of this document, the terms and definitions given in ISO 16773-1 and the following apply.3.1excitationapplication of a voltage, Uexc, or current, Iexc, to force the system into a new st

36、ate3.2current interrupter methodCI methodelectrochemical technique which allows the relaxation potential of an electrochemical system to be recorded as a function of time just after the excitation current is interrupted and the potential decay curve obtained to be analysedINTERNATIONAL STANDARD ISO

37、13129:2012(E) ISO 2012 All rights reserved 1BS EN ISO 13129:2012ISO 13129:2012(E)3.3relaxation voltammetryRVelectrochemical technique in which a potential is applied for a given excitation time and then the current is interrupted and just the potential is monitored as a function of time3.4DC transie

38、nt measurementDCT measurementelectrochemical technique in which a coated sample is charged such that the potential is shifted and then the sample is isolated and the potential is monitored against time while the potential returns to the open-circuit potential3.5potential/time decay curvecurve of pot

39、ential, U(t), plotted over time, while potential is changing after a defined excitation is removed3.6sampling ratenumber of data points per time interval3.7time constantproduct of resistor and capacitor values used in equivalent circuits, which has the dimensions of time4 Apparatus4.1 Faraday cageTh

40、e Faraday cage shall be constructed of metal sheet which reduces electromagnetic interference to the electrochemical cell (or circuit), and shall be connected to the instrument earth.4.2 Cell for sample, including electrode holderNOTE 1 Various types of measurement cell exist which are suitable for

41、use with this International Standard. Most commonly used are two-electrode and three-electrode arrangements for measurements in an aqueous electrolyte.The cell should be constructed of materials that will not corrode, otherwise deteriorate or contaminate the solution (e.g. PMMA, PTFE or glass). A ma

42、terial compatibility test should be carried out.The cell shall be leak-proof to ensure that the geometrical surface of the specimen does not change with time.The cell should preferably be designed to allow the following items to be inserted into the electrolyte chamber: the working electrode, the re

43、ference electrode, the counter-electrode.Sometimes a thermometer (for temperature control) and gas inlet/outlet tubes to modify the oxygen content of the electrolyte are used. When using an inert gas, a gas scrubber should be used.An example of an electrochemical cell is shown in Figure 1.2 ISO 2012

44、 All rights reservedBS EN ISO 13129:2012ISO 13129:2012(E)Key1 reference electrode2 counter-electrode3 electrolyte4 O-ring5 coating6 working electrodeFigure 1 Example of an electrochemical cellThe components shown in Figure 1 are described in ISO 16773-2.NOTE 2 This drawing does not imply that other

45、designs are unsuitable.4.3 GalvanostatUse a galvanostat which applies a current with a rectangular pulse waveform and has a fall time no less than 10 times faster than that of the time constant of the sample.4.4 PotentiostatThe potentiostat controls the potential of the working electrode with respec

46、t to the reference electrode. The potentiostat input impedance shall be high and the response time shall be fast.4.5 Electrodes4.5.1 Working electrodeUse as the working electrode a conductive substrate covered by the coating to be investigated. The exposed area should be accurately known, constant w

47、ith time, and adequate for the investigation. A large area makes the measurement more sensitive for single defects (pores) and gives better signal-to-noise ratio.4.5.2 Reference electrodeA low-impedance and low-noise reference electrode is recommended (a Luggin probe is not required). The potential

48、of the reference electrode should be checked periodically to verify the accuracy of the electrode and its stability with time. ISO 2012 All rights reserved 3BS EN ISO 13129:2012ISO 13129:2012(E)4.5.3 Counter-electrodeUse an inert conductor such as platinum with preferably a large surface area orient

49、ed parallel to the working electrode in order to ensure a homogeneous current distribution.4.6 ElectrolyteThe resistance of the solution should be low in comparison to the impedance of the system being investigated. Different types of electrolyte may be used. Non-aggressive electrolytes can be employed to characterize the properties of the system without introducing corrosion. An aggressive solution may be selected to characterize the corrosion resistance of the system. The electrolyte should be chosen with the end use o