EN ISO 16773-3-2016 en Electrochemical impedance spectroscopy (EIS) on coated and uncoated metallic specimens - Part 3 Processing and analysis of data from dummy cells《电化学阻抗谱(EIS)涂.pdf

1、BSI Standards PublicationBS EN ISO 16773-3:2016Electrochemical impedancespectroscopy (EIS) on coatedand uncoated metallicspecimensPart 3: Processing and analysis of data fromdummy cellsBS EN ISO 16773-3:2016 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO167

2、73-3:2016. It supersedes BS EN ISO 16773-3:2009 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 pur

3、port to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2016.Published by BSI Standards Limited 2016ISBN 978 0 580 79681 4ICS 87.040Compliance with a British Standard cannot confer immunity fromlegal obligations.T

4、his British Standard was published 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 16773-3 April 2016 ICS 87.040 Supersedes EN ISO 167

5、73-3:2009English Version Electrochemical impedance spectroscopy (EIS) on coated and uncoated metallic specimens - Part 3: Processing and analysis of data from dummy cells (ISO 16773-3:2016) Spectroscopie dimpdance lectrochimique (SIE) sur des prouvettes mtalliques revtues et non revtues -Partie 3: T

6、raitement et analyse des donnes obtenues partir de cellules test (ISO 16773-3:2016) Elektrochemische Impedanzspektroskopie (EIS) an beschichteten und unbeschichteten metallischen Proben - Teil 3: Verarbeitung und Analyse von Daten von Testschaltkreisen (ISO 16773-3:2016) This European Standard was a

7、pproved by CEN on 11 March 2016. CEN members are bound to comply with 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 nation

8、al standards may be obtained on application to the CEN-CENELEC 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 translation under the responsibility of a CEN member into its own languag

9、e and notified to the CEN-CENELEC Management Centre has the same status 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, H

10、ungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey andUnited Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CE

11、NELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2016 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 16773-3:2016 EBS EN ISO 16773-3:2016EN ISO 16773-3:2016 (E) 3 European foreword This document (EN ISO 16773-3:2016)

12、 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 given the status of a national standard, either by publication of an identic

13、al text or by endorsement, at the latest by October 2016, and conflicting national standards shall be withdrawn at the latest by October 2016. Attention 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 re

14、sponsible for identifying any or all such patent rights. This document supersedes EN ISO 16773-3:2009. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia

15、, 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, Sweden, Switzerland, Turkey and the

16、United Kingdom. Endorsement notice The text of ISO 16773-3:2016 has been approved by CEN as EN ISO 16773-3:2016 without any modification. BS EN ISO 16773-3:2016ISO 16773-3:2016(E)Foreword iv1 Scope . 12 Description of the dummy cells 12.1 General . 12.2 Components of the dummy cells . 12.3 Accuracy

17、requirements for the components . 22.4 Circuit description . 23 Procedure. 34 Data analysis . 35 Presentation of the results . 36 Acceptance criteria for the measurement system . 57 Test report . 58 Repeatability and reproducibility 6Bibliography .11 ISO 2016 All rights reserved iiiContents PageBS E

18、N ISO 16773-3:2016ISO 16773-3:2016(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 member body i

19、nterested 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 Electrotechn

20、ical Commission (IEC) on all matters of electrotechnical standardization.The procedures used to develop this document and 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 do

21、cuments should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 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 respons

22、ible for identifying any or all such patent rights. Details of any patent rights identified during the development of the 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 fo

23、r the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms 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

24、: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 35, Paints and varnishes, Subcommittee SC 9, General test methods for paints and varnishes.This second edition cancels and replaces the first edition (ISO 16773-3:2009), which has been technically revised. Th

25、e main changes are the following:a) the introductory element of the title, Paints and varnishes, has been omitted, because 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 meta

26、llic specimens;b) a reference to ISO/TR 16208 for dummy cells with low impedance values (10 to 1 000 ) hasbeen added;c) a reference to ASTM G106 for the precision data of low impedance measurements has been added;d) a test report has been added.ISO 16773 consists of the following parts, under the ge

27、neral title Electrochemical impedance spectroscopy (EIS) on coated and uncoated metallic specimens: Part 1: Terms and definitions Part 2: Collection of data Part 3: Processing and analysis of data from dummy cells Part 4: Examples of spectra of polymer-coated and uncoated specimensiv ISO 2016 All ri

28、ghts reservedBS EN ISO 16773-3:2016INTERNATIONAL STANDARD ISO 16773-3:2016(E)Electrochemical impedance spectroscopy (EIS) on coated and uncoated metallic specimens Part 3: Processing and analysis of data from dummy cells1 ScopeThis part of ISO 16773 specifies a procedure for the evaluation of the ex

29、perimental set-up used for carrying out EIS on high-impedance coated samples. For this purpose, dummy cells are used to simulate high-impedance coated samples. On the basis of the equivalent circuits described, this part of ISO 16773 gives guidelines for the use of dummy cells to increase confidence

30、 in the test protocol, including making measurements, curve fitting and data presentation.NOTE Due to the nature of the measurements, investigations of high-impedance coated samples are more susceptible to artefacts coming from electromagnetic interferences. Therefore, this part of ISO 16773 conside

31、rs the aspects for measuring high-impedance samples by using appropriate dummy cells in a Faraday cage. However, most manufacturers offer complementary dummy cells in the low and medium impedance range. This allows checking the setup in the respective low impedance range.2 Description of the dummy c

32、ells2.1 GeneralA set of four equivalent circuits (dummy cells) is used to check the overall experimental arrangement. The dummy cells are mounted separately. Two types of equivalent circuit, A and B, are used, as shown in Figure 1. The specific electrical components of these four cells are given in

33、Table 1. Dummy cells with low impedance values (10 to 1 000 ) are described in ISO/TR 16208.NOTE In Clause 8, the results of an interlaboratory test are used to evaluate the precision of this method. During the interlaboratory test, the participating laboratories also measured a fifth dummy cell con

34、sisting of an equivalent circuit of type B with unknown component values.2.2 Components of the dummy cellsEach dummy cell consists of a combination of resistors and capacitors which are soldered directly onto a printed-circuit board (see Figures 1 and 2). Such networks of resistors and capacitors (e

35、quivalent circuits) are often used in work on high-impedance coated specimens.NOTE Because of the very high overall resistance of circuits A and B, the resistor simulating the electrolyte can be neglected. Typically, the values of resistances R1and R2are above 100 M whereas the electrolyte resistanc

36、e is around 100 to 500 . As a consequence, the electrolyte resistance is not significant in this kind of EIS application.The values of the components of the four dummy cells are chosen in accordance with the following considerations. Dummy cell 1 should check the input resistance as well as the inpu

37、t capacitance of the measurement equipment. Dummy cells 2 to 4 should check the capability of the evaluation software and the impedance measurement equipment to distinguish between only slightly different resistor/capacitor combinations. ISO 2016 All rights reserved 1BS EN ISO 16773-3:2016ISO 16773-

38、3:2016(E)Figure 1 Equivalent circuits of the dummy cellsTable 1 Values of the components of the dummy cellsDummy cell CircuitR1GR2GC1nFC2nF1 A 50 0,15 2 B 1 10 0,15 0,473 B 1 0,2 0,1 204 B 0,1 0,1 10 102.3 Accuracy requirements for the componentsThe accuracy required for resistors below 109 is 2 % a

39、nd for resistors above 109 it is 5 %. The accuracy required for the capacitors is 5 %. Such resistors and capacitors are available commercially.2.4 Circuit descriptionUsually, the measurement of high-impedance coatings requires only a two-electrode set-up, but electrochemical workstations offer the

40、possibility of connecting up three or four electrodes. To simplify the connection of the dummy cells to electrochemical workstations, each cell should have four connectors (as indicated in Figure 2), the connectors being connected internally in pairs. To avoid contamination (e.g. by fingerprints) of

41、 the printed-circuit board, each dummy cell is protected by acrylic plates mounted on top of and underneath the cell.Key1, 2 connector pairsFigure 2 Photograph of a dummy cell used in the interlaboratory test2 ISO 2016 All rights reservedBS EN ISO 16773-3:2016ISO 16773-3:2016(E)3 ProcedurePerform al

42、l measurements in a Faraday cage in order to minimize electromagnetic interference.NOTE The four dummy cells allow the suitability of a shielding technique (i.e. a Faraday cage) to be determined, as well as helping to find the location in the laboratory where electromagnetic noise levels are lowest.

43、Perform the measurements in accordance with the manufacturers recommendations in the potentiostatic mode at a DC value of zero volts, using an amplitude of 20 mV (peak-to-zero).A frequency range between 104Hz and 102Hz is sufficient for measurements with dummy cells 2 to 4. For dummy cell 1, a frequ

44、ency range of 1 000 Hz to 5 103Hz is recommended. About 30 min to40 min are required for a single measurement (for dummy cell 1, about 1 h).If the results of the measurements are not satisfactory when using an amplitude of 20 mV, increase the amplitude.4 Data analysisUsing suitable software, e.g. th

45、at supplied by the manufacturer of the electrochemical workstation, analyse the results obtained from the dummy cell with equivalent circuit A (see Table 1). Record the result of curve fitting, the theoretical values of the circuit components and the excitation potential which was applied.NOTE 1 Unf

46、ortunately, the curve-fitting error given for the data analysed differs from manufacturer to manufacturer, so direct comparison is not possible.Prepare a Bode plot with the measured and simulated data.NOTE 2 Although the curve-fitting errors are not comparable, the Bode plot gives an indication of t

47、he quality of the measured data, especially at low frequencies.Repeat the analysis with the results from cells 2 to 4 using equivalent circuit B (see Table 1).5 Presentation of the resultsPresent the measured data as Bode plots for comparison purposes.The Bode plots in Figure 3 show how the dummy-ce

48、ll measurements should look. These diagrams were calculated using simulation software and can be used to compare with results from dummy-cell measurements.12Y Y1211109876907560453015a) Cell 1 ISO 2016 All rights reserved 3BS EN ISO 16773-3:2016ISO 16773-3:2016(E)Y1Y2126090678910b) Cell 212Y2Y1907560

49、789c) Cell 3Y129021Y4578d) Cell 44 ISO 2016 All rights reservedBS EN ISO 16773-3:2016ISO 16773-3:2016(E)12YY1247891090e) Cell 5 (values of components unknown)KeyX logf (f in Hz)Y1log|Z| (Z in )Y2| (degrees)1 phase angle 2 impedance ZFigure 3 Bode plots of the simulated impedance spectra of the dummy cells and the unknown cell6 Acceptance criteria for the measurement systemThe EIS system shall be capable of measuring and extracting the values of the resistors and capacitors in the dummy cells. Deviations of th