ARPN Journal of Engineering and Applied Sciences ‘www arpajounals. com ELECTROCHEMICAL ASSESSMENT OF CONCRETE TERNARY INHIBITORS USED IN RETARDING CORROSION OF STEEL. REINFORCEMENT Abdulrahmen, AS} and Mohammed Ismeil? 'Depastnent of Mechaiteal Engineering, Federal University of Teclnology, PMB 65, Mizna, Nigeia *Constuction Research Cente, Universit Telaologi Malaysia, $1310 UTM, Johor Balu, Joh, Malaysia E-Mail: sits alaru@ futon edu ng ABSTRACT Conosion of steel reinforcement in concrete is generally considered as an electrochemical process which reduces the service life of a structure exposed to chlonde ions attack. Therefore, laboratory experiments were performed in order to ascertain the effectiveness end sustainability of temary inhibitors (calcium aitite, ethanolamine and eco-friendly green Bambusa Arundinacea) in protecting stee] reinforcement in concrete fiom conosion attack due to chlonde. Concrete mix was designed to be 30MPa with 0.45 andl 0.65 WIC zatios. Inhibitors additions were 2% and 4% by weight of cement. The specimens were subjected to various duebility conosion test (using, electrochemical impedance spectroscopy (EIS)) for 360 days. The results showed that Bambusa arudknacea has exhibited lowest conosion rte, highest concrete resistance ‘and highest polarization resistance (Rp) values forthe period of expose, compared to calcium mitite and ethanolamine Bambusa arundinacea maybe considered a better substitute for nitrite and amine- based conosion inhibiting admixtures for durable concrete structues due to its viability, versatility and eco-friendliness. ‘Keywords: steel enforcement, concrete, consion, green Inibitoy, sustainability, EIS L INTRODUCTION Deterioration and collape of reinforced concrete structures is due fo comosion and muajor problem in the constriction industy especiely in the coastal region, which are charectenzed by high seliity. The cost of repaning or replacing deterinated structures has become @ anajor lsbity to govemment and the private sectors. The rimary cause ofthis deteioration is the conosion of steel reinforcement due to chlorides whose main sowce is the seawater and deicing salts (Abdulzahman etal, 2012, Ting nd Wo, 2011, Kaobkowski end Kozak, 2011; Inmil e¢ al, 20106). Im many counties with mepidly developing infastructures, economies in construction have led to poor quality concrete and low concrete cover to the steel resulting in comosion problems Also, the developed economies are not left out of this endemic problem, according to Invite al. QDL1), who reported that one cout of nine of existing concrete bridges in United States of ‘Amence is deficient as ¢ result of chlonde ions from Geicing salis on highway bridges exposed to feze-thaw fad diy-wet cycle witch translated to 31.7% of the nation’s 73, 800 structwally deficient bridges and this alone consuiues 31% of their GDP. Therefore, the major daunting challenge facing the civil engineerng commas isto execute pects tandem with nate ‘using the concept of sustainable development involving the wses of environmental benign aaterials produced at reasonable cost. In the context of concrete, which s the predominant building matenl, ts Imperative to identify conosion inhibitor which i= eco- fnendly to salvage the hfe span of concrete strctue exposed to hush envizonments, Several solutions to this problem have been roposed ane tested, albeit to date no idel solution has been found workeble (Abduliahman ef al, 20114; Boltry& ef al, 2011; Reamamam and Simonson, 2012), Thus, the yrinciple of the comosion inhibitor admixture is to prevent the chloride ions fiom reacting with the stel swface and also to inctease the time needed for the chlonde ions to penetrate through the concrete cover. Conosion inhibitors fue chemical substance which decreases the conosion rate when present im the comosion system at a suitable concentration without significantly changing the concentation of any other conosive agent (Ismail ef al, 20108) In recent studies (Abdulrahman ef al, 2011; Raje and Sethuraman, 2008, Uhlig, 2004) green inhibitors have proved more effective and envionmentaly benign than organic end inorgenic inhibitors in chemical and petrochemical industries. Consequently, more work in this fuea is necessary in order to ascertain the compatibility and suitebility of green inhibitor fo reinforced concrete 10 minimize the nisk posed by organic and inorganic inhibitors to envizonmental and sustainability. 2. EXPERIMENTAL PROCEDURE 2.1, Materials used Ordinary Portland Cement (OPC) was used in this eseaich. The chloride was admixed into the concrete fas magnesium chloride of analytical veagent grade. The concentrations of Magnesium chlonde sed was 1.5% and 45% by mass of cement and the conesponding chloride concentrations were 094% and 282% respectively Coarse aggregates of size 20 mm and 10 mm of quartzite origin wele used in the ratio of 1.78:1 to satisfy the overall grading requirement of coarse aggregate (Ismail et al, Sou), 750" ARPN Journal of Engine ering and Applied Sciences ‘www arpajounals. com Land quantied sand passing through ASTM sieve no. (457mm) conforming to zone II classification of Buitish standard was used as fine aggregete. The sand has « fineness modulus of 25. Tap water was used for the reparation of specimens. All the concrete mixes were designed for similar workability with shmup of 30-60 mm. ‘The water content was kept constant to 230 igi? forthe sized slump inal the mixes to have similar workability ‘The water-cement ratio (wl) used were 0.45 and 0.65, ‘The fiesh density of concrete was then obtained as per guidelines specified by Bntish method of mix selection G50e) tbe 2980 gin’. The design mux sas presented ‘companion paper (Abdulrahman ef al, 2012) 2.2. Corrosion rate measurement Comosion behaviows of embedded steel in concrete were monitored by electrochemical impedance spectroscopy (EIS) and linear polanzation resistence (LPR) using the Shikoku Research Institute Portable Rebar Conosion Meter (SRL-CMID, Measurements were done atthe conosion potential; the amplitude of the sine wave ‘extubation was 1OmV in fequency range of 10 Hz to 10 mHlz, 25 points sweep density per frequency decede were collected. Standard sikver chloride electode was ‘wed as reference seinlessstel dsc es centel and guard counter electode and 16 mam diameter mild steel was used ‘as working electode. EIS measwements were canied out after 360 days of expose to wet and ry eyeles. tally the specimens were cured in seawater for 28 days at @ lnborstory tempzratue of 28°C after 24h of casting Polarization resistance (Ry) (that is, charge tansier resistance) values obtained fiom Nyguis plot which was caleulaed fiom the chameter of the semi-cucle ‘extrapolated inthe low ftequency range between 10 KHz aad 10 mHz By essuning B as 26 mV, the conosion curent density (lq,) (# Alem!) was calculated using Stem-Geary equation in accordance with eatliey work of ‘Vishnudevan, Thangavel (2006) 2 loom = Where B is a constant which is a function of the anodic and cathodic Tafel slopes, b, and, Duy = Ryo + Raps + oS [Ryo '2 Z0UIE! Where © = angular fiequency ofthe applied signal, Cu= double layer capacitance From the above equation, the value of Z (@ ) at -verylow fiequencies becomes Ze = Ow) =Re Re = Gul 2ReD 2G + o!2 Rap! In this investigation B value of 26 mV was used for both active andl passive state of rebar, since the system was premixed with magnesium chloride except control sample (Vishnudevan, Thangavel, 2006) Comosion rate Gumpy) of the exposed rebar is ameaswed by wing following formule: 0.00822 X 0 % Feore Comosion rte (mum/yeas) =" xD Where ‘cere = conosion cuent density in Alem’, a = atomic weight of ion, thet is, 95845 g/mol, n= m0. of elections exchanged in comosion reecton, that is 2 for aon, D = deny of sel (185 glen’). The double layer capacitance was calculated fiom "> values using the formula: a Tie Fna XE Ce ‘Where Frnax ~ resistance For calculation of the conosion cunent density for EIS, the assumed model forthe steel/concrete interface is shown in Figue-I, Steelconcrete interface is represented by a simple equivalent electic cixcut. The equivalent cucut consists of concrete resistance Re in series with the interfece inpedance. The interface impedance consists of polanzation resistance Rp in parallel with a double layer capacitance Cu Frequency dependent impedance Z (w ) of the electical equivalent cixcuit shown in Figwe-1 is given by the following expression: frequency maximum, °» = polarization cal Re *e Figure-1. Equivalent electric circuit for stel/concrete interface And atweryhigh fequencies Zam ohidm Re ‘Therefore R, measured at high frequency can be subtracted fiom R, +R, measured at low fiequency to give a compensated value of R, fiee of ohmic interferences in high esistivity medium like concrete 751ARPN Journal of Engine ering and Applied Sciences ‘www arpajounals. com Ipedance bebaviowr of an electode may be expessed in Nyguist plot of 2°6) inagimmy component) as a function of 2" (3 (real component). The Nygust plot would slows a semicucle with ffequency incfeasing ina counterclockwise duection. At very high fiequeney, the imaginey component 2” C3} disappears, Teeving only the concrete resistance, R,. At very low fregueney, 2" (6) ogen dzepeas lewvng sun of R, P) ‘and Rp. Thus the radius ofthe semi cxcle is “7/2 3, RESULTS AND DISCUSSIONS 3.1, Corresion potential E.,,) of embedded steel Comosion potential” (Econ) monitonng and clectochemicel impedance spectroscopy (EIS) wes the techniques used for this stody. These techniques have ‘being extensively used in laboratory uwvestgations of the conosion behaviow of reinforeed concrete exposed to chlonie-confaining envionment (Ann ef al, 2006, De- Schutter and Luo, 2004 Kondhatova etal, 2003). EIS has the mejor advantage of providing the possibilty of establishing a physical infermetaion of the processes awolved, Figues 2-3 shows the typicel conosion potential (Econ) behaviour as a function of exposure tine in days, of weinforced concrete with wie rato of 0.45 subjected to wet and diy cycle. Stating potential was 10 mV vs. ‘AglBgCl electode. Starting at approximately sic months of exporue, potentials of reinforcing steel were nat indicative of comosion likelihood in the concrete mix according to ASTMC316.08. Generally, going by the potential results of all the Inhibitor, thei inhibitions were adequate for 0.45 wle ratios. But Bambusa armdinacea standout for excellent inhbaton for both mixes es can be seeing in Figures 2-3. However, with increasing peviods of exporure, the potential’ values tended to decrease (become "more Positive). This i due to the hytzation process of cement paste which conesponds to the compressive. stength ‘values recorded. This work demonstrates that edequate good protection is alady provided with 2% of inhibitor that is below the recommended amount (4%) (Pech-Canal sand Casto, 2002). Figure-2. Conosion potential asa function of exporwe time fora 0.45 wie with 1.5% MgCl; addition, Figure-3. Conosion potential asa function of exporwe time fora 0.45 wie with 4.5% MgCl addition 3.2 Corresion current Conosion cunent density (L,) represents instantaneous rate of conosion at the particular time of voltage measwement, and changes frequently over time for specimen according to Raafat ef al. 2011). laa values conesponding to reinforcement in the two mixes for this research axe resented in Figures 45 es a function of expose time, They are calculated fiom the polarization resistance values using a Stem-Geary constant of 26 mV Conosion cunent density is most widely treated as an, indication of the conosion performance of steel in concrete, Its values from 0.1 Alem? to 0.5 wAlem! were used as the bordevlines between passive and active conosion es was indicated in previous work by Kaolikowsli end Kuziek (2011). Starting with values m the order of 0.01 yA/em? conesponding 10 steel in passive condition according to earlier research by Pech-Canul and Castro (2002), there was tendency of Iq to increase beyond 0.2 wAlem? for MgCl, contaminated sample, 4% Ca (NO3): and 4% CyHINO inkdbited samples until 300 deys exporwe for (0.45 wie ratios as evident in Figue-4. While 2% for allARPN Journal of Engineering and Applied Sciences ‘www arpajounals. com tinee inhibitors, 4% Bambusa anodnacea and contol sample were stil within passive region for same expose penod. Also fiom Figure-5 only CyH;NO inhbstor and contol sample were within passive region (that is, below (0.2 wAlem’) forthe fast 300 days of exposue before the other inhibitors reduced to within the pesive region at 360 ays expose os a result of complete cement paste hhytietion. This behaviour is aat strmising and is in ‘gzeement with erlerveportby other authors (Jamal et al, 3003; Dhowbi et al, 2002; Tommeselli ef al, 2009, Pradhan, Bhattachayjee 009) Figure-4, Conosion cuent densities as factions of exposure time fora 0.45 wie with 1.5% MgCl, addition Figure-§, Conosion cuent densities as factions of exposure time fora 0.45 wie with 45% MgCl, addition 3. ec trochemical impedance spec troscopy (EIS) ‘measurements EIS is a powerful technique for obtaining detailed Imowiedge of conductive anode system and used to ‘monitor electrical propeities (material behaviow) of reinforced concrete in aggressive envionment, It provides infomation one number of parameters, such as the presence of surface films, interfacial reaction ancl mass- tuansfer phenomena (Jing, Wa, 2011). Impedance spectra (Gm Nyguist representation format) of EIS data obtained ‘before and after the additions of the three inhibitors at the different concentrations studied and used es conosion inhibitors after 12 months of exposme in the conosive redium (seawatei) for wet and dry cycles axe presented in Figues 6-9. Figure-6. Nyquist impedance plot of rbar embedded in concrete for 0.45wle with 1.5% MgCl; contamination of | 360 days exporue Figure-7. Nyquist impedance plot of rebar embedded in concrete for 0.45wle with 4.5% MgCl; contamination of | 360 days expose Vi Figure-8. Nyquist impedance plot of rebar embedded in concrete for 0.65wle with 1.5% MgCl; contamination of | 360 days exposure 753ARPN Journal of Engineering and Applied Sciences ‘www arpajounals. com owen tapedanee 2a Figure 9, Nyguist impedance plot of rebar embedded in, concrete for 0 65we with 45% MgCl, contamination of 360 days exposure The results of EIS data shows that the concrete resistance (R,) and polarization resistence (Ra) values were more higher for Ca(NOys, CaHyNO end Bambusa ‘rund nacea inhibitors admixtwe concrete es compared to the contol and chloride contaminated concrete. Re is considered to be high ifthe value is greater than 4 Ka. But Bambusa anowdmacea inhibitor was outstanding compared to two others inhibitors This might be due to its pore blocking effects which prevented the formation of chfferential aeration of cells that promote conosion on the steel suface as a result of oxygen level. Also the lower value of double layer capacitance Cy of Bambuse arundinacea could be associated with its edsomption mode ‘This confirmed its adsorbed molecules parelleled to metal surface, ancl decreased the number of surface active sites due to its hyeophobic characteristics, The nonlinear reactive put of the electode impedance contains double layer capacitance (Cy) and yeudlo capacitance in the fiequency measurement. In concrete, prendo capacitance arises due to the edsorption of OH, £*, Na? and Ca" ions on the reinforcement sunfaces. Vedalakshmi etal. (2009) suggested that if there is absence of double layer capacitance, then there will be no fiequency dependence. But data presented in Figures 6- T confirm that [ng is dependent on fiequency. Since the process may have lange tne constants, the reactive pat of the impedance specta cannot be eliminated completly. But at a lower fiequency of 10 mHz, both passive ancl active conditions of reinforcement were fulfilled, ensuing that the meeswed cument passes thuough the chage transfer resistance (R,) rither than Cy The douible layer capecitance reduces after adsorption of the inhibitors since the adsoibed film reduces the dielectric constant between the metal end the cement paste elecholyte From Figues 6 and 8, the Nyguist plots shows the same pattem of tends for the Bambusa arundinacea inhibitor efficiency 360 days exposue for inhibition of ‘MgCl, contaminated concrete containing 094% chlorides, even more then the contol suuples end other inhibitors. This might be attabuted to the hythophabic capacitive nature of the film (y-Fe;03) formed on the rebar sufece with a lage tine constant indicative of passive stel. The region of tel impedance and imaginary impedance which increase continously is Inown as Wasbuug impedance, which cause shielding or resistance effect for the metal conosion eccording to similar research by Alt al (GODT). The observed impedance of the inhibitors is as @ result ofthe slow diffusion of oxygen tuough the concrete mati and the dielectic film component of solid liydioride layer at the steelconeete interface. These processes canbe atibuted to the electrochemical reaction on the electiode (fl) suaface and the associated chaxge- transfer resince and double-layer capeitance which was azo observed in jevious woik by Tonelli eta (2009) On the other hand, in the contaminated concrete containing 282% chloride, the Nyquist plot yields a fovtenctuve indicating the break-down of delet fl due to chlorides which canbe observed in Figues 7 and 9. The addition of chlovide decreeses the charge transfer resisfnce which indicates the competion between the aggressive chlonde ions and the passating hydroxy ions Chloride ion might have reected with hyheted fnceleimaluninate” (GA) hytiate to fom chloroaluninate (CyA CaCl; 10H,0) which may contain 75.90% chloride ecconing to study by Indrt ef a (2011), Sine it has exceeded thestold chloride level, the Joective pesive layer would be destoyed as in the case Of chloride contaminated samples In genezel, the chloride thueshold is taken to be 015% of the soluble chloride by weight of cement. So, 094% and 282% chlonde has fat exceeded the commonly accepted conosion teshold in this work 1t is important fo note that the ee inhibitors exhibited almost the same beluviow dung all the test times and for ell the concentrations, The poleiztion resistance (Rj) of the steel surface reymesenting the resistance fo" cument flow across the =steelconerete interface ata conosion potential, is dependent on the formation of passive filu of ron hycroxidesloradesdwing the process of comosion and i expected fo decrease if ths yrotective flu is broken under certain conditions. Ry Which isthe rate detemnining resistence atthe reinforcing steel conosion, therefore a the R increases the conosion Inle decreeses and the ‘capecitiace of inferface also decreases, This is evident in this work as inhbited contaminated concrete shows low conosion ite. But Banca arundinacea exhibited lowest conosion ite, Ca and highest Ry values for the enfze period of exporure ‘The Inige acs observed fiom high fo low frequencies in Figues 69, indicates that the polarization resistance, Ry ‘becomes dominant due fo edsorpfion of inhibitors. Also the inhbiton efficiency derived fom the Ry values ofthe impedance” mearuement shows that Bambusa anind nacea is consistently higher compared t other two lnhbiton for 050i at 1 5% MgCl, contamination. Only ethanolamine inkbition efficiency was adequate for 754ARPN Journal of Engineering and Applied Sciences ‘www arpajounals. com O.4Swle at high 45% MgCl contamination. Inhibition ‘ficiency was derived fiom the below expession sccordng to Gruzet al. (2004). Rem IER) = ReGrta) 200, Where R, is the polarization resistence without Inhbitor end Ry(ih) is the polanzaton resistance with imbbitor. Mesiwhle the Ry values obtsined ffom Impedance mearwements enable ws to validate conosion inition properties of these tee inhibitors studied as @ function of tine 4. CONCLUSIONS In view of the outlined objectives earlier ‘mentioned in this research work and subsequent series of investigations condlucted as well as the results obtained, the following conclusions were drawn: + The electrode potentials of reinforcing steel were not indicative of early conosion likelihood in the concrete + The potential results of all the inhibitoas and their inhbitons were adequate for 0.45 we bios, but Bambusa arundmacea standout for excellent inition * Comosion cument density (lex) which represents instantaneous rate of conosion atthe puticular time of ‘voltage measurement, increases beyond O.2uA/emy for MgCl contaminated sample, 4% Ca(NOs) and 4% CHINO inhibited samples at age of 360. days expose for 0.45 wie ratios. While 2% forall thee inbbitors, 4% Bambusa arnvdnacea and contol sample vere stil within passive region for same expose period + The pore blocking effects of Bamibusa arundinacea prevented the fomation of diferentel aeration of cells that promote comosion on the steel suace as @ result of oxygen level due to it high concrete resistance. Also, the lower velue of double layer capecttnce Cy of Bambusa arménacea could be astociated with its adsorption mode. This confizmed sts adsorbed molecules pralleled to metal surface, end decreased the number of suface active sites due fo its hydrophobic chaectenstics. The double layer capacitance reduces after edsomption of the inhibitors sauce the adsoubed film reduces the dilectnc constant ‘between the metal and the cement paste electolye. + The addition of chlonde decreases the polezation resistance (Rj) which indicates the competition ‘between the ‘aggressive chlonde ions and. the passivating hydroxyl ons. Bambusa arudnacea ‘exhibited lowest conosion rate, lowest Cy and highest R, values for the entue period of exposure despite exceeding chloride threshold value + Nyguist plots shows the seme pattem of tends forthe Bambusa arundinacea ahibitor efficiency at 360 days exposue for mhbition of MgCl, contaminated concrete containing 0.94% chlorides, even more than the control samples end other inhibitors. This might be attabuted to the hyzhophobie capacitive nature of the film (7Fe;0)) formed on the rebar surface with a laage time constant indicative of passive steel, the region of real impedance and imaginary impedance which increase contimously cause shielding ox resistance effect for the metal conosion. The observed impedance of ths inkibitor is as a result of the slow dhffusion of oxygen through the concrete matnx and the dielectric film component of solid yeboxide layer atthe steel-concrete interface + It was obsewed thet comosion rte is iwesely loportional to concrete vesistance. 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