DIN EN ISO 13129-2013 Paints and varnishes - Electrochemical measurement of the protection provided to steel by paint coatings - Current interrupter (CI) technique relaxation voltau.pdf

1、April 2013 Translation by DIN-Sprachendienst.English price group 13No part of this translation 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

2、87.040!%#ke“2007266www.din.deDDIN EN ISO 13129Paints and varnishes Electrochemical measurement of the protection provided to steel bypaint coatings Current interrupter (CI) technique, relaxation voltammetry (RV) techniqueand DC transient (DCT) measurements (ISO 13129:2012);English version EN ISO 131

3、29:2012,English translation of DIN EN ISO 13129:2013-04Beschichtungsstoffe Elektrochemische Messung der Schutzwirkung von Beschichtungen auf Stahl Stromunterbrechungsverfahren (CI), Relaxationsvoltametrie (RV) undGleichstromtransientenmessung (DCT) (ISO 13129:2012);Englische Fassung EN ISO 13129:201

4、2,Englische bersetzung von DIN EN ISO 13129:2013-04Peintures et vernis Mesurage lectrochimique de la protection apporte lacier par des revtements depeinture Technique du courant interrompu (CI), voltamtrie de relaxation (VR) et mesurages decourants continus transitoires (CCT) (ISO 13129:2012);Versio

5、n anglaise EN ISO 13129:2012,Traduction anglaise de DIN EN ISO 13129:2013-04www.beuth.deDocument comprises 21 pagesIn case of doubt, the German-language original shall be considered authoritative.04.13DIN EN ISO 13129:2013-04 2 A comma is used as the decimal marker. National foreword This document (

6、EN ISO 13129:2012) has been prepared by Technical Committee ISO/TC 35 “Paints and varnishes”, Subcommittee SC 9 “General test methods for paints and varnishes” (Secretariat: BSI, United Kingdom) in collaboration with Technical Committee CEN/TC 139 “Paints and varnishes” (Secretariat: DIN, Germany).

7、The responsible German body involved in its preparation was the Normenausschuss Beschichtungsstoffe und Beschichtungen (Coatings and Coating Materials Standards Committee), Working Committee NA 002-00-07 AA Allgemeine Prfverfahren fr Beschichtungsstoffe und Beschichtungen. The DIN Standards correspo

8、nding to the International Standards referred to in this document are as follows: ISO 2808 DIN EN ISO 2808 ISO 6270-1 DIN EN ISO 6270-1 ISO 9227 DIN EN ISO 9227 ISO 16773-1 DIN EN ISO 16773-1 ISO 16773-2 DIN EN ISO 16773-2 National Annex NA (informative) Bibliography DIN EN ISO 2808, Paints and varn

9、ishes Determination of film thickness DIN EN ISO 6270-1, Paints and varnishes Determination of resistance to humidity Part 1: Continuous condensation DIN EN ISO 9227, Corrosion tests in artificial atmospheres Salt spray tests DIN EN ISO 16773-1, Paints and varnishes Electrochemical impedance spectro

10、scopy (EIS) on high-impedance coated specimens Part 1: Terms and definitions DIN EN ISO 16773-2, Paints and varnishes Electrochemical impedance spectroscopy (EIS) on high-impedance coated specimens Part 2: Collection of data EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 13129 December 201

11、2 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 (DCT) measurements (ISO 13129:2012) Peintures et vernis - Mesurage lectro

12、chimique 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) Beschichtungsstoffe - Elektrochemische Messung der Schutzwirkung von Beschichtungen auf

13、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 the CEN/CENELEC Internal Regulations which stipulate the conditions fo

14、r 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 Management Centre or to any CEN member. This European Standard exists in thre

15、e 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 status as the official versions. CEN members are the national standards bod

16、ies 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, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, S

17、pain, 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 exploitation in any form and by any means reserved worldwide for CEN

18、national Members. Ref. No. EN ISO 13129:2012: EContents PageForeword .Introduction 1 Scope 2 Normative references .3 Terms and definitions .4 Apparatus 4.1 Faraday cage 4.2 Cell for sample, including electrode holder .4.3 Galvanostat .4.4 Potentiostat .4.5 Electrodes .4.6 Electrolyte .5 Specimens .5

19、.1 Preconditioning of specimens .5.2 Environmental control .5.3 Evaluation of specimens exposed to weathering in the laboratory and in the field .5.4 Number of specimens and repeatability of results 6 Experimental procedure 6.1 General .6.2 Current interrupter technique 6.3 Relaxation voltammetry .6

20、.4 DC transient measurements .7 Expression of results .8 Precision 9 Test report .Annex A (normative) Description of the dummy cell 13Annex B (informative) Further considerations concerning measurements on coatings 15Annex C (informative) Examples of results .17Bibliography .18DIN EN ISO 13129:2013-

21、04 EN ISO 13129:2012 (E) 2345556667778888899991011121212Foreword This document (EN ISO 13129:2012) 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 Europ

22、ean Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by June 2013, and conflicting national standards shall be withdrawn at the latest by June 2013. Attention is drawn to the possibility that some of the elements o

23、f 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 organisations of the following countries are bound to implement this European

24、 Standard: 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, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Sloveni

25、a, 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. DIN EN ISO 13129:2013-04 EN ISO 13129:2012 (E) 3 IntroductionQuantitative assessment of protection performance of orga

26、nic 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 (CI) technique, relaxation voltammetry (RV) and DC transient (DCT) mea

27、surements 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.DIN EN ISO 13129:2013-04 EN ISO 13129:2012 (E) 41 ScopeThis International Stand

28、ard 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 definitio

29、ns 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 Standard

30、 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 presen

31、ting 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 reference

32、d 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 spectroscopy

33、(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 state3.

34、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 analysedDIN EN ISO 13129:2013-04 EN ISO

35、13129:2012 (E) 5 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 transient measurementDCT measurementelectrochemical technique in which

36、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 potential, U(t), plotted over time, while potential is changing aft

37、er 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 cageThe Faraday cage shall be constructed of metal sheet which reduces

38、 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 use with this International Standard. Most commonly used are two

39、-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 material compatibility test should be carried out.The cell shall b

40、e 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 reference electrode, the counter-electrode.Sometimes a thermometer

41、 (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.DIN EN ISO 13129:2013-04 EN ISO 13129:2012 (E) 6Key1 reference electrode2

42、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 designs are unsuitable.4.3 GalvanostatUse a galvanostat which applies a current wit

43、h 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 respect to the reference electrode. The potentiostat input impedance shall be high and th

44、e 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 with time, and adequate for the investigation. A large area makes the measurement mo

45、re 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 of the reference electrode should be checked periodically to verify the accuracy of

46、 the electrode and its stability with time.DIN EN ISO 13129:2013-04 EN ISO 13129:2012 (E) 7 4.5.3 Counter-electrodeUse an inert conductor such as platinum with preferably a large surface area oriented parallel to the working electrode in order to ensure a homogeneous current distribution.4.6 Electro

47、lyteThe 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

48、 may be selected to characterize the corrosion resistance of the system. The electrolyte should be chosen with the end use of the coating in mind.5 Specimens5.1 Preconditioning of specimensProper preparation and preconditioning of coated specimens is critical for successful and reliable experimental data.5.2 Environmental controlThe coating should be applied and cured in accordance with the manufacturers recommendations unless otherwise agreed upon between the interested parties. The film thickness should be as uniform as possible. The exact film thickness should be measured and reported