EN ISO 16773-3-2009 0625 Paints and varnishes - Electrochemical impedance spectroscopy (EIS) on high-impedance coated specimens - Part 3 Processing and analysis of data from dummy .pdf

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1、BS EN ISO16773-3:2009ICS 87.040NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDPaints and varnishes Electrochemicalimpedancespectroscopy (EIS) onhigh-impedance coatedspecimensPart 3: Processing and analysis of datafrom dummy cells (ISO 16773-3:2009)Copyright Eur

2、opean Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 November 2009. BSI 2009ISBN 978 0

3、580 59287 4Amendments/corrigenda issued since publicationDate CommentsBS EN ISO 16773-3:2009National forewordThis British Standard is the UK implementation of EN ISO16773-3:2009. The UK participation in its preparation was entrusted to TechnicalCommittee STI/10, Test methods for paints.A list of org

4、anizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunityfrom legal obligatio

5、ns.Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 16773-3May 2009ICS 87.040English VersionPaints and varnishes - Electroche

6、mical impedance spectroscopy(EIS) on high-impedance coated specimens - Part 3: Processingand analysis of data from dummy cells (ISO 16773-3:2009)Peintures et vernis - Spectroscopie dimpdancelectrochimique (SIE) sur des prouvettes revtues dehaute impdance - Partie 3: Traitement et analyse desdonnes o

7、btenues partir de cellules test (ISO 16773-3:2009)Beschichtungsstoffe - ElektrochemischeImpedanzspektroskopie (EIS) von beschichteten Probenmit hoher Impedanz - Teil 3: Verarbeitung und Analyse vonDaten von Testschaltkreisen (ISO 16773-3:2009)This European Standard was approved by CEN on 30 April 20

8、09.CEN members are 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

9、application to the 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 Centr

10、e has the same status 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, P

11、ortugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: Avenue Marnix 17, B-1000 Brussels 2009 CEN All rights of exploitation in any form and by any means r

12、eservedworldwide for CEN national Members.Ref. No. EN ISO 16773-3:2009: ECopyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN ISO 16773-3:2009EN ISO 16773-3:2009 (E) 3 Foreword

13、This document (EN ISO 16773-3:2009) 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,

14、either by publication of an identical text or by endorsement, at the latest by November 2009, and conflicting national standards shall be withdrawn at the latest by November 2009. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CE

15、N 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 this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Re

16、public, 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 the United Kingdom. Endorsement notice The text of ISO 16773-3:2009 h

17、as been approved by CEN as a EN ISO 16773-3:2009 without any modification. Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN ISO 16773-3:2009ISO 16773-3:2009(E) ISO 2009 All

18、rights reserved iiiContents Page Foreword iv 1 Scope 1 2 Description of the dummy cells .1 2.1 General1 2.2 Components of the dummy cells .1 2.3 Accuracy requirements for the components 2 2.4 Circuit description .2 3 Procedure .3 4 Data analysis3 5 Presentation of the results .3 6 Acceptance criteri

19、a for the measurement system .5 7 Repeatability and reproducibility.6 Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN ISO 16773-3:2009ISO 16773-3:2009(E) iv ISO 2009 All ri

20、ghts reservedForeword ISO (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 interested in a subject

21、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 Electrotechnical Commission (IEC) o

22、n 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 adopted by the technical committees

23、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 rights. ISO shall not be held

24、 responsible for identifying any or all such patent rights. ISO 16773-3 was prepared by Technical Committee ISO/TC 35, Paints and varnishes, Subcommittee SC 9, General test methods for paints and varnishes. ISO 16773 consists of the following parts, under the general title Paints and varnishes Elect

25、rochemical impedance spectroscopy (EIS) on high-impedance coated 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 specimens Copyright European Committee for Standardization Provi

26、ded by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN ISO 16773-3:2009INTERNATIONAL STANDARD ISO 16773-3:2009(E) ISO 2009 All rights reserved 1Paints and varnishes Electrochemical impedance spectroscopy (EIS) on high-impedance coate

27、d specimens Part 3: Processing and analysis of data from dummy cells 1 Scope This part of ISO 16773 specifies a procedure for the evaluation of the experimental set-up used for carrying out EIS on high-impedance coated samples. For this purpose, dummy cells are used to simulate high-impedance coated

28、 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 in the test protocol, including making measurements, curve fitting and data presentation. 2 Description of the dummy cells 2.1 General A set of four

29、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 Table 1. NOTE In Clause 7, th

30、e 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 consisting of an equivalent circuit of type B with unknown component values. 2.2 Components of the dummy cells Each

31、 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 (equivalent circuits) are often used in work on high-impedance coated specimens. NOTE Because of the very high o

32、verall 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 resistance is around 100 to 500 . As a consequence, the electrolyte resistance is not significant in this kind of EIS

33、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 input capacitance of the measurement equipment. Dummy cells 2 to 4 should check the capability of the evaluation

34、 software and the impedance measurement equipment to distinguish between only slightly different resistor/capacitor combinations. Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-

35、BS EN ISO 16773-3:2009ISO 16773-3:2009(E) 2 ISO 2009 All rights reservedFigure 1 Equivalent circuits of the dummy cells Table 1 Values of the components of the dummy cells Dummy cell Circuit R1 109 R2 109 C1 109F C2 109F 1 A 50 0,15 2 B 1 10 0,15 0,47 3 B 1 0,2 0,1 20 4 B 0,1 0,1 10 10 2.3 Accuracy

36、requirements for the components The accuracy required for resistors below 109 is 2 % and 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 description Usually, the measurement of high-impedance co

37、atings requires only a two-electrode set-up, but electrochemical workstations offer the 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 connecto

38、rs being connected internally in pairs. To avoid contamination (e.g. by fingerprints) of the printed-circuit board, each dummy cell is protected by acrylic plates mounted on top of and underneath the cell. Key 1, 2 connector pairs Figure 2 Photograph of a dummy cell used in the interlaboratory test

39、Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN ISO 16773-3:2009ISO 16773-3:2009(E) ISO 2009 All rights reserved 33 Procedure Perform all measurements in a Faraday cage in

40、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. Perform the measurements in accord

41、ance with the manufacturers recommendations in the potentiostatic mode at a DC value of zero volts, using an amplitude of 20 mV. A frequency range between 104Hz and 102Hz is sufficient for measurements with dummy cells 2 to 4. For dummy cell 1, a frequency range of 100 Hz to 5 103Hz is recommended.

42、About 30 min to 40 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 analysis Using suitable software, e.g. that supplied by the manufacturer of the electro

43、chemical 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 Unfortunately, the curve-fitting error given for

44、 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 the quality of the measured data, especially

45、 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 results Present the measured data as Bode plots for comparison purposes. The Bode plots in Figure 3 show how the dummy-cell measurements should look. These diag

46、rams were calculated using simulation software and can be used to compare with results from dummy-cell measurements. Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN ISO 167

47、73-3:2009ISO 16773-3:2009(E) 4 ISO 2009 All rights reserveda) Cell 1 b) Cell 2 c) Cell 3 Figure 3 (continued) Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN ISO 16773-3:20

48、09ISO 16773-3:2009(E) ISO 2009 All rights reserved 5d) Cell 4 e) Cell 5 (values of components unknown) Key X logf (f in Hz) Y1log|Z| (Z in ) Y2| (degrees) 1 phase angle 2 impedance Z Figure 3 Bode plots of the simulated impedance spectra of the dummy cells and the unknown cell Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN ISO 16773-3:2009ISO