Designation: G 59 - 97 (Reapproved 2003) “Tis sundae isd uate tse desgation G5 the mane ineitely following the designate the year evga ‘lopince ia Ws ese ef ys th orf lst so nur pcre he ear of st cpa A supe Standard Test Method for Conducting Potentiodynamic Polarization Resistance Measurements* ‘poo (aes eo change sce hs vs epg 1. Scope 1.1 This cest method describes an experimental procedure for polarization resistance measurements which can be used for the calibration of equipment and verification of experimental technique. The test method can provide reproducible corrosion potentials and potentiodynamie polarization resistance mea surements, 1.2. This test method does noi purport to axddvess all of the safety concerns, if any, associated with its use, It is the responsibility of the user of this standard 10 establish appro- priate safety and health practices and determine the applica: bility of regulatory limitations prior t0 use. 2. Referenced Documents 2.1 ASTM Standacas: G3 Practice for Conventions Applicable to Electrochemical ‘Measurements in Corrosion Testing? G5 Test Method for Making Potentiostatic and Potentiody- namic Anodic Polarization Measurements? G02 Practice for Calculation of Corrosion Rates and Related Information from Electrochemical Measurements? 22 Adjunct: ‘Samples of the Standard AISI Type 430 Stainless Steel (UNS ‘s43000)° 3, Significance and Use 31 This test method can be utilized to verify the perfor. ‘mance of polarization resistimce measurement equipment in- cluding reference electrodes, electrochemical cells, poten tiostats, scan generators, measuring and recording deviees. The test method is also useful for training operators in sample preparation and experimental techniques for polarization resis lance measurements. 3.2 Polarization resistance can be related (0 the rate of «general corrosion for metals at or near their corrosion potential, Polarization resistance measurements are an accurate and Ecour "Tis pratce is wir he arin of ASTM Commitee GO on Con of Maul and he Gacet responsi of Subsomnaitee G LI ex Ecce ‘Cnen! elt sproel Pec, 1607: Pebied Febwary 1698. Ovigilly approved in 1973 List revs eli agyrned in 1981 as @ 59 ~ 91 Sere Bos of ASTM Standards, Nou (S. rapid sway to measure the general corrosion rate. Real time corosion monitoring is common application. The technique cam also be used as a way to rank alloys, inhibitors, and so forth in onder of resistance to general corrosion. 33 Is I potential sean, AEI¢), defined with rexpect to the comosion potential (XE = E~ E.,.) is applied to a metal sample. ‘The resultant currents ste reconled The polarization resistance, Kj, of a comnding electrode is defined from Eq 1 as the slope of a potential versus eurrent emity plot at = 0 (hed) ase) TT) we o is test mex as ‘The current density is given by j. The corrosion current density, fg, 58 telated to the polarization resistance by the ‘Stem-Geary coofficient, B. (3), ge = 1 ° The dimension of ,, is ohm-em?, i, 8 muAlem?, and Bis in V. The Sterm-Geury’ coefficient is related 10 the anodic, b, and cathodic, b,, Tafel slopes as per Eq 4 by, The units of the Tafel slopes are V. The corrosion rate, CR, in mm per yeur can be determined from Eq 4 in which EW is the equivalent weight of the conoding species in grams and p is the density of the corroding material in gvem’. R= 327% 10 e 7 Refer to Practice © 102 for derivations of the above eu tions and methods for estimating Tafel slopes. 34 The test method may not he appropriate to measure polarization resistance on all materials or in ull environments, See 8.2 for a discussion of method biases arising from solution resistance und electrode capueitance. 4, Apparatus 4.1 The apparatus is described in Test Method GS. 11 jades TL round bottom flusk modified wo permit the lace murs in eros feo te Lito efeonces ats eataddition of inest gos. dhermometer, and electrodes. This stan dard cell or an equivalent cell can be used. Am equivalent cell ‘must be constructed of inert materials and be able to reproduee the standard curve in Test Method G 5. 4.2 A potentiostat enable of varying potential al a constant scan rate and measuring the curenl is needed, 4.3 Aamiethod of recording the varying potential und result. Jing euirent is needed. 5, Test of Hlectrical Equipment 5.1 Before the polarization resistance measurement 8m the instrument system (potentiostal, N-Y recorder or data acquisition system) must be tested 9 ensure proper function= ing. For this purpose. connect the potentiesiat 1 a test electrical circuit (§). While more complex dummy cells are sometimes needed in electrochemical studies, the simple ro tor shown i Fig, [is adequate for the present application, 52 Use R = 100 Set the applied potential on the potentiostat to E =~ 30.0 mV and apply the potential. The ‘current should be 30 mA by Olun’s Law, f= B/R. ‘Nore 1-When polarization resists vlues ans mearared for systems with differnt corrosion currents dhe valu of R shouldbe chosen to cover the eument range of the actiel polarization revstnce. measurement [Expssted corion currents inthe msroumpere rane race R= 14010 ka 53 Record the potentiodyoamic polarization curve atu scan rate of 0.6 Vib from AE =—30 mV to AE = 430 mV und back to AE = -30 mv. The plot should be linear, go through the origin, and have a slope 10 Q. The curves recorded for the forward and reverse seans should be identical Sa IP the observed results are different than expected. the electrochemical equipment may require calibration or servicing, in aceonlance with the manufacturer's guidelines, 6. Experimental Procedure 6.1 "The 1,0 N H.SO, test solution should be prepared from ‘American Chemis! Society reagent grade acid and distilled ‘water as described in Test Method G 5. The standard test cell requires 900 mL of test solution, The temperature must be ‘maintained at 30°C within 1°, 6.2 The test cell is purged at 150 ear"/min with an oxygen- free gas such as hydrogen, nitmigen, or argon. The purge is sMarted at least 30 min before specimen immersion, The purge ‘continues throughout the test. 6.3 The working electrode should be prepared as detailed in| Test Method G 5. The experiment must commence within Tl, of preparing the electwode, Preparation includes sequential wet polishing with 240 grit and 600 grit SiC puper. Determine the surface area of the specimen ( the nearest 0.01 ea? and subtract for the area under the gasket (iypically 0.20 to 0.25 64 Immediately prior to immersion the specimen ix de- _greaved with a solvent suc as acetone and rinsed with ‘water. The time delay between rinsing and immersi be enna Nome 2 Sumples ofthe tundard AISU Type 430 stainless steel (ONS S430) wae in thistest method ae ashe to ene wishing to eae heir equipment and test procedure from Mstal Samples. PO. Box 8, Monin AL R18. 6.5 Transfer the test specimen 19 the test cell and position the Luggin probe tip 2 to 3 mm from the test electrode surface, ‘The tip diameter must be no greuier than 1 man, 16.6 Record the corrosion potential... after Sand SS-min 6.7 Apply a potential 30 mV mone negative that the re= corded 55 min corrosion potential (See Note 3). Nore 3. Price G3 provides 2 defaion of sign convention for poke and caren 6.8 One minute afler application of the -30 mV potential, begin the anodic potential scan at a sweep rate of 0.6 Vit (within 3%), Record the potential und current continuously ‘Terminate the sweep ata porential 30 mV more positive than the 55 min corasion potenti 16. Plot the polarization curve as a linear potential-current density plot as shown in Practice G 3, Determine the polar tion resistance, Ra the tangent of the curve at #=0. Report 7.1 Report the following informal TAA The 5 and 55 min corres n potentials and the polar ization resistance value, 7.1.2 Duplicate runs may be averaged, and 7.1.3 Note any deviation from the procedure or test condi- tions established in this test methexl 8, Precision and Bias 8.1 Precision—Precision in this (est method refers wo the closeness of agreement between randomly selected measured values, There ure wvo aspects of precision, repeutability and reproducibility. Repeatability refers t the closeness of agree: ‘ment between measurements by the same laboratory on iden= tical Type 430 stainless steel specimens repeated with as close as possible adherence lo the same procedure, Reproducibility refers (o the closeness of agreement between different laburs- tories using identical Type 430 stainless steel specimens and Tourer Reference Eecrode| Ny ouspet Working Flecrote R Contes Feros MonitorRecorder FIG. 1 Arrangement for Testing of Electrical Equipment (Potentistst, XY Recorder) Potentiostated. An interlaboratory test program with 13 laboratories participating and two. three or four replicate meusurements was carried out 1 establish the precision. The measured values included (Table 1) the comosion potential ‘meusured after 5 and $5 min and the polarization resistance, A. research report has been filed with the results of this program, BLT Repeauabilin— The lack of repeatability iy measured, by the repeatability standard deviation s,. The 95 % confidence interval was calculated as + 2.8 s,. The values obiained are shown in Table 2.The 95 % confidence interval refers 1 the alerval around the average that 95 “% of the values should be found, ‘TABLE 1 interlaboratory Test Program Polarization Data for ‘Stsinlose Stool Typo 430 in 1.0 N H,SO, at 20°C TABLE 2 Repostabilty Sttictice eves 5) CherSninmi'versus So=_ Tpenar _ecnaaD ESrssmnmvverss Soe | “OEts1 oars oman ae 78 1.2. Reproducibility — The luck of reproducibility is mes sured by the reproducibility standard deviation, s,. ‘The 95 ‘confidence interval was calculated as -£ 2.8 sy. The values obtained are shown in Tuble 3. TABLE 9 Reproductbilty Statsties Diy Scion Ea om o omen) foeape Sq Cencenes 1 ang 08 am Sexy S min, mVversus SCE 08287 OTT 0386 mv ahs cae sf Eqs S83 0 oie 2 38 ae 2 a520 co505 040 4 22 wose 2 82 Bias—The polarization resistance as measered by the : as ose 12 ‘eat Methoa G58 han two sours of bias The penta 28 oe a namic method includes a ceuble layer expitance charging 5 aig 780 ‘effect that may cause the polarization resistance to be under- 22 ne estimated, There ab a solution reac efeet tat tay 7 2S = ise the poleivaton resistonce to be overeat Tis in a0 or will depend on the placement of the reference electrode and : 28 = seco fy. Retr to Proce G 102 fr fat 38 ao Giseusion on the effects of double layer eapavitance and : 23) sa solution resistance on polarization resistance mneasurements, 25 2 33 a 9. Keywords . 3s ae sat anodic plaeaton uni eles; cto polar . 3h is ization; corrosion; corrosion polenta; corosion rae; current density: eleciecherial eel, electrochemical potential: Las 38 a : 2 38 SS gin probe; mined potentil oper pent overolge s set fe polarization resistance; potentiodynamic; reference electrode; 22 = Solution esstnce; Stem-Geary cbelien: Tafel slope: work 3 Eo ing eecwode REFERENCES (1 Stem, Mad Rev, RM. Journal of de Eleochemice! Sacer. Vl 10d, 1953, p. 300, {@) Stem, M, Comocion, Vol 4, 1958, p. 440 6 (G) Mansfeld. F. “The Polarization Resstance Technique for Measuring Conosion Caronts", Corroninn Scencr and Frehiniagy, Plena reve, New York, NY, Nol VI 1976, p68 ( Mansfeld, F, “Exalation of Polarization Resisance Row Robin ‘Tentng Condncsl by ASTM GO1.11", Paper No 106, CORROSION! 76, NACE, Houston, TX, Macch 22-26, 1976, (5) Gilead. E Kirn Eisner, and Povcice, J. faerfocial Het chemists. an Experimental Approach. Chapter HLT, Addison Wesley Publishing Co, Reading, MA 1975,