BS EN ISO 16773-2-2016 Electrochemical impedance spectroscopy (EIS) on coated and uncoated metallic specimens Collection of data《涂覆和未涂覆金属试样的电化学阻抗频谱 (EIS) 数据收集》.pdf

1、BSI Standards PublicationBS EN ISO 16773-2:2016Electrochemical impedancespectroscopy (EIS) on coatedand uncoated metallicspecimensPart 2: Collection of dataBS EN ISO 16773-2:2016 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO16773-2:2016. It supersedes BS E

2、N ISO 16773-2:2007 which iswithdrawn. The UK participation in its preparation was entrusted to TechnicalCommittee STI/10, Test methods for paints.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the nece

3、ssaryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2016.Published by BSI Standards Limited 2016ISBN 978 0 580 85634 1ICS 87.040Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was pub

4、lished under the authority of theStandards Policy and Strategy Committee on 30 April 2016.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 16773-2 April 2016 ICS 87.040 Supersedes EN ISO 16773-2:2007English Version Ele

5、ctrochemical impedance spectroscopy (EIS) on coated and uncoated metallic specimens - Part 2: Collection of data (ISO 16773-2:2016) Spectroscopie dimpdance lectrochimique (SIE) sur des prouvettes mtalliques revtues et non revtues -Partie 2: Recueil des donnes (ISO 16773-2:2016) Elektrochemische Impe

6、danzspektroskopie (EIS) an beschichteten und unbeschichteten metallischen Proben - Teil 2: Datenerfassung (ISO 16773-2:2016) This European Standard was approved by CEN on 11 March 2016. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for givin

7、g 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 three offic

8、ial 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 bodies of

9、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, Spain, S

10、weden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2016 CEN All rights of exploitation in any form and by any means reserved worldwide for

11、 CEN national Members. Ref. No. EN ISO 16773-2:2016 EBS EN ISO 16773-2:2016EN ISO 16773-2:2016 (E) 3 European foreword This document (EN ISO 16773-2:2016) has been prepared by Technical Committee ISO/TC 35 “Paints and varnishes” in collaboration with Technical Committee CEN/TC 139 “Paints and varnis

12、hes” the secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by October 2016, and conflicting national standards shall be withdrawn at the latest by October 2016. Att

13、ention is drawn to the possibility that some of the 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. This document supersedes EN ISO 16773-2:2007. According to the CEN-CENELEC Internal Regul

14、ations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, It

15、aly, 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 16773-2:2016 has been approved by CEN as EN ISO 16773-2:2016 without any modification. BS EN IS

16、O 16773-2:2016ISO 16773-2:2016(E)Foreword iv1 Scope . 12 Normative references 13 Terms and definitions . 14 Principle 15 Electrochemical cell 25.1 General . 25.2 Electrodes 35.3 Exposed area . 35.4 Electrolyte . 36 Procedure. 46.1 Grounding 46.2 Shielding . 46.3 Cell cable ground contacts 46.4 Local

17、 conditions . 46.5 Measurement equipment characteristics 56.6 Confidence test 56.6.1 General 56.6.2 Use of interlaboratory test cells for confidence test . 66.6.3 Error estimate and accuracy 66.7 Specimens . 66.7.1 Preconditioning of specimens 66.7.2 Environmental control 66.8 Evaluation of laborato

18、ry and field coating specimens 66.9 Number of specimens and repeatability of results 77 Instrumental parameters 77.1 General . 77.2 Conditioning potential and conditioning time 87.3 Frequency spectrum 87.4 Data point spacing and points per decade 87.5 D.C. potential control . 87.6 Amplitude of pertu

19、rbation 97.7 Current range settings 97.8 Data averaging settings 98 Data presentation 98.1 General . 98.2 Bode plot 98.3 Nyquist plot. 109 Exchange file format 1110 Test report 11Annex A (informative) Determination of maximum measurable impedance with the open-lead test .13Annex B (normative) Data e

20、xchange file format .15Annex C (informative) Considerations about the precise determination of the exposed area .19Bibliography .24 ISO 2016 All rights reserved iiiContents PageBS EN ISO 16773-2:2016ISO 16773-2:2016(E)ForewordISO (the International Organization for Standardization) is a worldwide fe

21、deration 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 com

22、mittee. 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.The procedures used to develop this document a

23、nd those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Pa

24、rt 2 (see www.iso.org/directives).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. Details of any patent rights identified during the development of t

25、he document will be in the Introduction and/or on the ISO list of patent declarations received (see www.iso.org/patents).Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific ter

26、ms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 35, Paints and varnishes, S

27、ubcommittee SC 9, General test methods for paints and varnishes.This second edition cancels and replaces the first edition (ISO 16773-2:2007), which has been technically revised. The main changes are the following:a) the introductory element of the title, Paints and varnishes, has been omitted, beca

28、use the scopeis broadened to include metals and alloys and the main element of the title has been changed to:Electrochemical impedance spectroscopy (EIS) on coated and uncoated metallic specimens;b) a reference to ISO/TR 16208 has been added;c) considerations about the precise determination of the e

29、xposed area have been added as aninformative annex;d) a test report has been added.ISO 16773 consists of the following parts, under the general title Electrochemical impedance spectroscopy (EIS) on coated and uncoated metallic specimens: Part 1: Terms and definitions Part 2: Collection of data Part

30、3: Processing and analysis of data from dummy cells Part 4: Examples of spectra of polymer-coated and uncoated specimensiv ISO 2016 All rights reservedBS EN ISO 16773-2:2016INTERNATIONAL STANDARD ISO 16773-2:2016(E)Electrochemical impedance spectroscopy (EIS) on coated and uncoated metallic specimen

31、s Part 2: Collection of data1 ScopeThis part of ISO 16773 gives guidelines for optimizing the collection of EIS data with focus on high-impedance systems. High impedance in the context of intact coatings refers to systems with an impedance greater than 109cm2. This does not preclude measurements on

32、systems with lower impedance. For uncoated samples extra information can be found in ISO/TR 16208.This part of ISO 16773 deals with the following: instrumental set-up: requirements and pit-falls; data validation: checking the measurement range and the accuracy of the data; performing an EIS measurem

33、ent: specimen considerations and instrumental parameters; the experimental results: different methods of presenting EIS data.These guidelines are intended to ensure the acquisition of EIS data that can be used to study the performance of the specimen. This part of ISO 16773 does not give guidelines

34、for the interpretation of the data.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the refere

35、nced document (including any amendments) applies.ISO 16773-1, Electrochemical impedance spectroscopy (EIS) on coated and uncoated metallic specimens Part 1: Terms and definitions3 Terms and definitionsFor the purposes of this document, the terms and definitions given in ISO 16773-1 apply.4 Principle

36、A so-called “confidence” test is described in order to check the suitability of the entire set-up and recommendations are given as to how to perform EIS experiments. For convenience, only potentiostatically controlled EIS measurements are described, although it is also possible to make EIS measureme

37、nts under galvanostatic control.A potentiostat is connected either to a dummy cell or to an electrochemical cell (with working, counter- and reference electrodes). A single-sinusoidal- or multi-sinusoidal-waveform potential, either in conjunction with a d.c. offset or not, is applied by the potentio

38、stat to the dummy cell or to the electrochemical cell, and the resulting a.c. current is measured. Both potential and a.c. current data are collected and analysed for amplitude and phase shift. This can be done in a variety of ways, depending ISO 2016 All rights reserved 1BS EN ISO 16773-2:2016ISO 1

39、6773-2:2016(E)on the type of equipment used. All data are presented and compared graphically or computed for equivalent circuits. In the case of the dummy cell, the values of these equivalent components are compared to the actual cell components connected to the potentiostat and evaluated for cohere

40、nce.5 Electrochemical cell5.1 GeneralNOTE 1 Various types of measurement cell exist which are suitable for use with this part of ISO 16773. Most commonly used are two-electrode and three-electrode arrangements for measurements in an aqueous electrolyte.The cell shall be constructed of materials that

41、 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 be leak-proof to ensure that the geometrical surface of the specimen does not change with time. Use an electrically insulating gasket ma

42、terial (O-ring, etc.) for the seal, i.e. with a through-thickness resistance much greater than that of the coating.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, a

43、 thermometer (for temperature control) and gas inlet/outlet tubes to modify the oxygen content of the electrolyte. When using an inert gas, a gas scrubber should be used.An example of an electrochemical cell is shown in Figure 1.1234Key1 reference electrode2 counter electrode3 electrolyte4 O-ring5 c

44、oating6 working electrodeFigure 1 Example of an electrochemical cellNOTE 2 Other designs can be suitable.For uncoated metallic specimens, IR drop should be considered.2 ISO 2016 All rights reservedBS EN ISO 16773-2:2016ISO 16773-2:2016(E)The components shown in Figure 1 are described in 5.2 to 5.4.5

45、.2 ElectrodesTo perform EIS in aqueous solution, the more conventional set-up is composed of a three-electrode arrangement: a working electrode, a reference electrode and a counter-electrode.Working electrode: A conductive substrate covered by the coating to be investigated. A large surface area is

46、preferred to better take into account any defects and to decrease the impedance of the system to give a better signal-to-noise ratio.Counter electrode: Inert material such as platinum with a large surface area oriented parallel to the working electrode in order to ensure a homogeneous current distri

47、bution.Reference electrode: A low-impedance and low-noise reference electrode is recommended, according to suppliers user manual when testing organic coatings, a salt bridge (e.g. Luggin capillary) is not required. The potential of the reference electrode should be checked periodically to control th

48、e accuracy of the electrode and its stability with time. At very high frequencies, the presence of the reference electrode can induce some spurious effects.NOTE 1 To improve the quality of the high-frequency signal, a platinum wire with a capacitor may be placed in parallel with the reference electr

49、ode. The capacitor ensures that the d.c. potential is coming from the reference electrode and a.c. potential from the platinum wire.NOTE 2 For specific applications, it can be acceptable to use a pseudo-reference electrode consisting of an inert material such as a high-nickel alloy or a chloridized silver wire. Pseudo-reference electrodes are useful for measurements in the field, where a reference electrode can be easily broken.5.3 Exposed areaThe exposed area should be known, constant with time, and should be adequate for the investigation.