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Effect of Calcium on the Formation and Protectiveness of Iron Carbonate

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Effect of Calcium on the Formation and Protectiveness of Iron Carbonate CORROSION SCIENCE SECTION Effect of Calcium on the Formation and Protectiveness of Iron Carbonate Layer in CO2 Corrosion Saba Navabzadeh Esmaeely,‡,* Yoon-Seok Choi,* David Young,* and Srdjan Nešic´* ABSTRACT INTRODUCTION 2+ The effect of calcium (Ca ) on the carbon dioxide (CO2) corro- The carbon capture and storage (CCS) process con- sion of mild steel was investigated in simulated saline aquifer tains three stages: environments (1 wt% sodium chloride [NaCl], 80°C, pH 6.6) —carbon dioxide (CO ) capture at its generation 2+ 2 with different concentrations of Ca (10, 100, 1,000, and source (coal or gas-fi red power plant, refi nery, 10,000 ppm). Electrochemical methods (open-circuit potential syngas unit, cement works, or some other in- [OCP]) and linear polarization resistance [LPR] measurements) dustrial process) were used to evaluate the corrosion behavior. Surface analy- sis techniques (scanning electron microscopy [SEM], energy- —transportation to the geologic storage site (usu- dispersive x-ray spectroscopy [EDS], and x-ray diffraction ally by pipeline transmission) 1 [XRD]) were used to characterize the morphology and identity —injection into geologic host reservoirs the corrosion products. The results showed that with low con- Among the known options in CCS, injection and 2+ centrations of Ca (10 ppm and 100 ppm), the corrosion rate storage of CO2 in deep saline aquifers has the potential decreased with time as a result of the formation of protective to cause casing corrosion because of the direct con- iron carbonate (FeCO ) and/or mixed carbonate (Fe Ca CO ) 3 x y 3 tact between injected CO2 and the saline aquifer with (x + y = 1). However, the presence of high concentrations of highly concentrated aqueous salts such as sodium Ca2+ (1,000 ppm and 10,000 ppm) resulted in the change of chloride (NaCl) and calcium chloride (CaCl2). Aqueous corrosion product from protective FeCO3 to non-protective cal- CO2 is known as a corrosive agent. Studies have been cium carbonate (CaCO3), and an increasing corrosion rate with time. Results of surface analysis revealed a different steel performed on CO2 corrosion at high pressures. All surface morphology with pitting observed in the presence of studies showed that the initial “bare steel” corrosion 2+ 10,000 ppm Ca . rate at high partial pressure CO2 (~70 bars) is very 2-3 high. For high pressure CO2 the concentration of 2+ 2+ + KEY WORDS: Ca , CaCO3, carbon capture and storage, Fe , hydrogen ions ([H ]) is rather high, as a result of the FeCO3, localized corrosion excessive amount of carbonic acid (H2CO3) and, hence, its dissociation. Also, the presence of H2CO3 can pro- vide another pathway for the cathodic reaction:2 + – He+ 1/2H2 (1) Submitted for publication: February 5, 2013. Revised and ac- cepted: May 2, 2013. Preprint available online: May 31, 2013, – – doi: http://dx.doi.org/10.5006/0942 . HC23O2++e1 /2 HH23CO (2) ‡ Corresponding author. E-mail: [email protected]. * Institute for Corrosion and Multiphase Technology, Department of Chemical and Biomolecular Engineering, Ohio University, Ohio, In stagnant conditions, the system may reach favor- 45701. able conditions for formation of FeCO3, when the cor- ISSN 0010-9312 (print), 1938-159X (online) 912 13/000165/$5.00+$0.50/0 © 2013, NACE International CORROSION—SEPTEMBER 2013 CORROSION SCIENCE SECTION rosion rate starts to decrease.3 Even though the bulk TABLE 1 pH remains very low (~pH 3) at a very high pressure Test Matrix 2+ of CO2, there is a high concentration of Fe near the Parameters Conditions surface because of the high corrosion rate. This would Total Pressure 0.1 MPa create favorable conditions for iron carbonate (FeCO3) pCO2 0.05 MPa precipitation. Temperature 80°C The role of FeCO3 formation during the corrosion Solution 1 wt% NaCl process has been studied over the past few decades.4-8 pH 6.6 Nešic´ suggested that FeCO is protective when it is Flow condition Stagnant 3 Steel G10180 dense and adhesive at the steel surface, because such a layer retards the transportation of corrosive spe- cies toward the steel surface and blocks portions of TABLE 2 the steel surface making them unavailable for corro- Test Conditions sion.9 The corrosion product layer properties in terms Test Condition No. Initial Concentrations of Fe2+ and Ca2+ of both structure and composition have been studied 2+ in recent years.10-13 Different parameters affect the 1 10 ppm Fe 2+ 2+ 2 10 ppm Fe + 10 ppm Ca formation of FeCO3 and its diffusion-limiting proper- 2+ 2+ 9,14 3 10 ppm Fe + 100 ppm Ca ties. The chemical and mechanical properties of the 4 10 ppm Fe2+ + 1,000 ppm Ca2+ layer formed on the surface are a function of many 5 10 ppm Fe2+ + 10,000 ppm Ca2+ factors, such as temperature, supersaturation, and chemical composition of the layer.14-16 Ingham, et al., 29 reported an enhancement in protectiveness of the cor- in CaCl2-containing electrolytes. Gao, et al., reported rosion product layer when a small concentration of pitting in conjunction with the formation of FexCayCO3 2+ 17 magnesium (Mg ) was present. and Fex(Mg,Ca)yCO3 (x + y = 1) on the steel surface. A – Calcium carbonate (CaCO3) is isostructural with broader review of the literature indicates that Cl ions 2+ FeCO3. Therefore, Ca readily incorporates into the are often associated with pitting; however, the role of 18 2+ FeCO3 structure and vice versa. Therefore, the overall water chemistry, and in particularly Ca ions, properties of FeCO3, both morphologically and chemi- is generally not clear. In many instances, some of cally, in the presence of Ca2+, are subject to change. the key parameters are not measured or reported; for It has been established already that the morphol- example, the pH of the aqueous solution is often “un- ogy of FeCO3 plays a significant role in the corrosion known” making any discussion of the results uncon- 19-20 process. While many studies have addressed the vincing. In CO2 corrosion of mild steel, only higher pH different parametric effects on the formation and pro- is associated with the formation of protective FeCO3 8-9,14,16,19-21 2+ tectiveness of FeCO3, the role of brine chem- layers; therefore, any influence of Ca concentration istry, particularly in terms of the effect of individual must be analyzed in the context of the overall water ions on corrosion product layer formation, was not chemistry effects. 17 studied in great detail. For example, one of the im- Although CO2 is stored in liquid or supercritical 2+ 2+ portant species in brines is Ca , which can be present phase at high pressure, the effect of Ca on FeCO3 22 at high concentrations (up to 30,000 ppm). However, formation is not known even if at low CO2 partial pres- effects of Ca2+ on corrosion mechanisms have not sures. Therefore, the work reported, conducted at low been well documented. CO2 partial pressures, can be considered as a prelimi- Little has been reported on the effect of Ca2+ on nary study on the effect of Ca2+ in saline aquifers on corrosion in the literature, with findings often appear- corrosion of casing steel related to the injection of CO2 ing contradictory. Zhao, et al.,23-24 claimed that corro- for its geologic storage. sion rate decreased in the “short term” in the presence of Ca2+ and Mg2+, but there was no special difference EXPERIMENTAL PROCEDURES in “long-term exposure.” Ding, et al., reported the corrosion rate increased with an increase in the Ca2+ Experiments were conducted in a 2-L glass cell concentration.25 Jiang, et al., reported pitting associ- using a three-electrode setup. In each experiment, – (1) ated with CaCl2. They claimed that while Cl caused three flat specimens made from AISI 1018 mild steel pitting, the presence of Ca2+ postponed the initiation (UNS G10180)(2) with an exposed area of 5.4 cm2 were of the pitting.26 Ren, et al.,27 as well as Zhu, et al.,28 used for electrochemical measurement and for surface reported pitting with reference to the presence of Cl– analysis. Prior to insertion, the specimens were wet- polished with silicon carbide (SiC) paper, down to (1) American Iron and Steel Institute, 25 Masachusetts Ave., NW Ste. 600 grit, and rinsed with isopropyl alcohol (C3H8O) in 800, Washington, DC 20001. an ultrasonic bath and dried. (2) UNS numbers are listed in Metals and Alloys in the Unified Num- bering System, published by the Society of Automotive Engineers Tables 1 and 2 show the test matrix and test (SAE International) and cosponsored by ASTM International. conditions, respectively. The glass cell was filled with CORROSION—Vol. 69, No. 9 913 CORROSION SCIENCE SECTION (a) (b) FIGURE 1. Variations of (a) corrosion rate and (b) OCP for mild steel exposed to a simulated brine with different initial 2+ 2+ concentrations of Ca at 80°C and pCO2 of 0.05 MPa with 10 ppm Fe . 2 L of 1 wt% NaCl electrolyte (prepared with deionized face and preventing the underlying steel from under- water). The solution was stirred with a magnetic stir- going further oxidative dissolution.9,31 2+ rer and the temperature was set to 80°C; CO2 gas was For the low initial Ca concentration conditions purged continuously through the solution. The solu- (0, 10, and 100 ppm), the formation of a protective tion pH was adjusted to 6.6 by addition of a deoxygen- FeCO3 layer apparently occurred without signifi cant ated 1.0 M sodium hydroxide (NaOH) solution. After interference by Ca2+ ions. However, the corrosion be- the pH stabilized, the magnetic stir bar was stopped havior of mild steel with higher initial Ca2+ concentra- and samples were inserted into the glass cell.
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