ASTM G59-1997(2003) Standard Test Method for Conducting Potentiodynamic Polarization Resistance Measurements《动电势极化电阻测量的标准试验方法》.pdf

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1、Designation: G 59 97 (Reapproved 2003)Standard Test Method forConducting Potentiodynamic Polarization ResistanceMeasurements1This standard is issued under the fixed designation G 59; the number immediately following the designation indicates the year of originaladoption or, in the case of revision,

2、the year of last revision. A number in parentheses indicates the year of last reapproval. A superscriptepsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method describes an experimental procedurefor polarization resistance measurements which can be

3、 used forthe calibration of equipment and verification of experimentaltechnique. The test method can provide reproducible corrosionpotentials and potentiodynamic polarization resistance mea-surements.1.2 This test method does not purport to address all of thesafety concerns, if any, associated with

4、its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:G 3 Practice for Conventions Applicable to ElectrochemicalMeasurements

5、 in Corrosion Testing2G 5 Test Method for Making Potentiostatic and Potentiody-namic Anodic Polarization Measurements2G 102 Practice for Calculation of Corrosion Rates andRelated Information from Electrochemical Measurements22.2 Adjunct:Samples of the Standard AISI Type 430 Stainless Steel (UNSS4300

6、0)33. Significance and Use3.1 This test method can be utilized to verify the perfor-mance of polarization resistance measurement equipment in-cluding reference electrodes, electrochemical cells, poten-tiostats, scan generators, measuring and recording devices. Thetest method is also useful for train

7、ing operators in samplepreparation and experimental techniques for polarization resis-tance measurements.3.2 Polarization resistance can be related to the rate ofgeneral corrosion for metals at or near their corrosion potential,Ecorr. Polarization resistance measurements are an accurate andrapid way

8、 to measure the general corrosion rate. Real timecorrosion monitoring is a common application. The techniquecan also be used as a way to rank alloys, inhibitors, and so forthin order of resistance to general corrosion.3.3 In this test method, a small potential scan, DE(t), definedwith respect to the

9、 corrosion potential (DE=EEcorr), isapplied to a metal sample. The resultant currents are recorded.The polarization resistance, RP, of a corroding electrode isdefined from Eq 1 as the slope of a potential versus currentdensity plot at i =0(1-4):4Rp5SDE iDi50, dE/dt0(1)The current density is given by

10、 i. The corrosion currentdensity, icorr, is related to the polarization resistance by theStern-Geary coefficient, B. (3),icorr5 106BRp(2)The dimension of Rpis ohm-cm2, icorris muA/cm2, and B isin V. The Stern-Geary coefficient is related to the anodic, ba,and cathodic, bc, Tafel slopes as per Eq 3.B

11、 5babc2.303ba1 bc!(3)The units of the Tafel slopes are V. The corrosion rate, CR,in mm per year can be determined from Eq 4 in which EW isthe equivalent weight of the corroding species in grams and ris the density of the corroding material in g/cm3.CR 5 3.27 3 103icorrEWr(4)Refer to Practice G 102 f

12、or derivations of the above equa-tions and methods for estimating Tafel slopes.3.4 The test method may not be appropriate to measurepolarization resistance on all materials or in all environments.See 8.2 for a discussion of method biases arising from solutionresistance and electrode capacitance.4. A

13、pparatus4.1 The apparatus is described in Test Method G 5. Itincludesa1Lround bottom flask modified to permit the1This practice is under the jurisdiction of ASTM Committee G01 on Corrosionof Metals, and is the direct responsibility of Subcommittee G 01.11 on Electro-chemical Measurements in Corrosio

14、n Testing.Current edition approved Dec. 10, 1997. Published February 1998. Originallyapproved in 1978. Last previous edition approved in 1991 as G 59 91.2Annual Book of ASTM Standards, Vol 03.02.3Available from ASTM Headquarters. Order PCN 12-700050-00.4The boldface numbers in parentheses refer to t

15、he list of references at the end ofthis standard.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.addition of inert gas, thermometer, and electrodes. This stan-dard cell or an equivalent cell can be used. An equivalent cellmust be con

16、structed of inert materials and be able to reproducethe standard curve in Test Method G 5.4.2 A potentiostat capable of varying potential at a constantscan rate and measuring the current is needed.4.3 A method of recording the varying potential and result-ing current is needed.5. Test of Electrical

17、Equipment5.1 Before the polarization resistance measurement is made,the instrument system (potentiostat, X-Y recorder or dataacquisition system) must be tested to ensure proper function-ing. For this purpose, connect the potentiostat to a testelectrical circuit (5). While more complex dummy cells ar

18、esometimes needed in electrochemical studies, the simple resis-tor shown in Fig. 1 is adequate for the present application.5.2 Use R = 10.0 V. Set the applied potential on thepotentiostat to E = 30.0 mV and apply the potential. Thecurrent should be 3.0 mA by Ohms Law, I = E/R.NOTE 1When polarization

19、 resistance values are measured for systemswith different corrosion currents, the value of R should be chosen to coverthe current range of the actual polarization resistance measurement.Expected corrosion currents in the microampere range requireR=1to10kV.5.3 Record the potentiodynamic polarization

20、curve at a scanrate of 0.6 V/h from DE = 30 mV to DE = +30 mV and backto DE = 30 mV. The plot should be linear, go through theorigin, and have a slope 10 V. The curves recorded for theforward and reverse scans should be identical.5.4 If the observed results are different than expected, theelectroche

21、mical equipment may require calibration or servicingin accordance with the manufacturers guidelines.6. Experimental Procedure6.1 The 1.0 N H2SO4test solution should be prepared fromAmerican Chemical Society reagent grade acid and distilledwater as described in Test Method G 5. The standard test cell

22、requires 900 mL of test solution. The temperature must bemaintained at 30C within 1.6.2 The test cell is purged at 150 cm3/min with an oxygen-free gas such as hydrogen, nitrogen, or argon. The purge isstarted at least 30 min before specimen immersion. The purgecontinues throughout the test.6.3 The w

23、orking electrode should be prepared as detailed inTest Method G 5. The experiment must commence within 1 hof preparing the electrode. Preparation includes sequential wetpolishing with 240 grit and 600 grit SiC paper. Determine thesurface area of the specimen to the nearest 0.01 cm2andsubtract for th

24、e area under the gasket (typically 0.20 to 0.25cm2).6.4 Immediately prior to immersion the specimen is de-greased with a solvent such as acetone and rinsed with distilledwater. The time delay between rinsing and immersion shouldbe minimal.NOTE 2Samples of the standard AISI Type 430 stainless steel (

25、UNSS45000) used in this test method are available to those wishing to evaluatetheir equipment and test procedure from Metal Samples, P.O. Box 8,Mumford, AL 36268.6.5 Transfer the test specimen to the test cell and positionthe Luggin probe tip 2 to 3 mm from the test electrode surface.The tip diamete

26、r must be no greater than 1 mm.6.6 Record the corrosion potential Ecorrafter 5 and 55-minimmersion.6.7 Apply a potential 30 mV more negative that the re-corded 55 min corrosion potential (See Note 3).NOTE 3Practice G 3 provides a definition of sign convention forpotential and current.6.8 One minute

27、after application of the 30 mV potential,begin the anodic potential scan at a sweep rate of 0.6 V/h(within 5 %). Record the potential and current continuously.Terminate the sweep at a potential 30 mV more positive thanthe 55 min corrosion potential.6.9 Plot the polarization curve as a linear potenti

28、al-currentdensity plot as shown in Practice G 3. Determine the polariza-tion resistance, Rp, as the tangent of the curve at i=0.7. Report7.1 Report the following information:7.1.1 The 5 and 55 min corrosion potentials and the polar-ization resistance value,7.1.2 Duplicate runs may be averaged, and7.

29、1.3 Note any deviation from the procedure or test condi-tions established in this test method.8. Precision and Bias8.1 PrecisionPrecision in this test method refers to thecloseness of agreement between randomly selected measuredvalues. There are two aspects of precision, repeatability andreproducibi

30、lity. Repeatability refers to the closeness of agree-ment between measurements by the same laboratory on iden-tical Type 430 stainless steel specimens repeated with as closeas possible adherence to the same procedure. Reproducibilityrefers to the closeness of agreement between different labora-torie

31、s using identical Type 430 stainless steel specimens andFIG. 1 Arrangement for Testing of Electrical Equipment (Potentiostat, X-Y Recorder)G 59 97 (2003)2the procedure specified. An interlaboratory test program with13 laboratories participating and two, three or four replicatemeasurements was carrie

32、d out to establish the precision. Themeasured values included (Table 1) the corrosion potentialmeasured after 5 and 55 min and the polarization resistance. Aresearch report has been filed with the results of this program.8.1.1 Repeatability The lack of repeatability is measuredby the repeatability s

33、tandard deviation sr. The 95 % confidenceinterval was calculated as 6 2.8 sr. The values obtained areshown in Table 2.The 95 % confidence interval refers to theinterval around the average that 95 % of the values should befound.8.1.2 Reproducibility The lack of reproducibility is mea-sured by the rep

34、roducibility standard deviation, sR. The 95 %confidence interval was calculated as 6 2.8 sR. The valuesobtained are shown in Table 3.8.2 BiasThe polarization resistance as measured by theTest Method G 59 has two sources of bias. The potentiody-namic method includes a double layer capacitance chargin

35、geffect that may cause the polarization resistance to be under-estimated. There is also a solution resistance effect that maycause the polarization resistance to be overestimated. This biaswill depend on the placement of the reference electrode andelectrolyte conductivity. Refer to Practice G 102 fo

36、r furtherdiscussion on the effects of double layer capacitance andsolution resistance on polarization resistance measurements.9. Keywords9.1 anodic polarization; auxiliary electrode; cathodic polar-ization; corrosion; corrosion potential; corrosion rate; currentdensity; electrochemical cell; electro

37、chemical potential; Lug-gin probe; mixed potential; open-circuit potential; overvoltage;polarization resistance; potentiodynamic; reference electrode;solution resistance; Stern-Geary coefficient; Tafel slope; work-ing electrodeREFERENCES(1) Stern, M., and Roth, R. M., Journal of the Electrochemical

38、Society,Vol104, 1957, p. 390.(2) Stern, M., Corrosion, Vol 14, 1958, p. 440 t.(3) Mansfeld, F., “The Polarization Resistance Technique for MeasuringCorrosion Currents”, Corrosion Science and Technology, PlenumPress, New York, NY, Vol VI, 1976, p.163.(4) Mansfeld, F., “Evaluation of Polarization Resi

39、stance Round RobinTesting Conducted by ASTM G01.11”, Paper No. 106, CORROSION/76, NACE, Houston, TX, March 22-26, 1976.(5) Gileadi, E., Kirowa-Eisner, E., and Penciner, J. Interfacial Electro-chemistry, an Experimental Approach, Chapter III.1, Addison-WesleyPublishing Co., Reading, MA 1975.TABLE 1 I

40、nterlaboratory Test Program Polarization Data forStainless Steel Type 430 in 1.0 N H2SO4at 30CLaboratory Ecorr5min Ecorr55min Rp(mV) (mV) (ohm-cm2)1 0.519 0.506 6.470.519 0.505 5.882 0.542 0.521 5.950.540 0.519 5.043 0.524 0.513 6.930.520 0.508 6.404 0.555 0.545 7.700.565 0.545 7.705 0.539 0.524 7.5

41、80.530 0.510 6.186 0.519 0.510 7.600.522 0.512 7.160.521 0.509 6.657 0.522 0.510 9.060.520 0.511 7.070.523 0.510 5.858 0.520 0.508 7.110.520 0.508 7.520.521 0.510 6.949 0.529 0.513 7.110.530 0.513 7.220.529 0.514 7.190.529 0.515 7.1910 0.514 0.505 5.170.516 0.506 6.9011 0.543 0.529 5.070.538 0.524 4

42、.6412 0.520 0.505 5.630.519 0.507 6.1613 0.531 0.519 5.080.529 0.517 5.380.529 0.517 5.90TABLE 2 Repeatability StatisticsAverage Sr95 % ConfidenceIntervalEcorr5 min, mV versus SCE 0.5287 0.00260 6 0.0073 VEcorr55 min, mV versus SCE 0.5151 0.00273 6 0.0076 VRp, ohm-cm26.46 0.713 62.00 ohm-cm2TABLE 3

43、Reproducibility StatisticsAverage SR95 % ConfidenceIntervalEcorr5 min, mV versus SCE 0.5287 0.0127 6 0.0356 mVEcorr55 min, mV versus SCE 0.5151 0.0111 6 0.0311 mVRpohm-cm26.46 1.01 62.83 ohm-cm2G 59 97 (2003)3ASTM International takes no position respecting the validity of any patent rights asserted

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46、reful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM Internatio

47、nal, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).G 59 97 (2003)4