Development of an electrochemically integrated SR-GIXRD flow cell to study FeCO3 formation kinetics

Burkle, D.; Motte, Rehan De; Taleb, Wassim; Kleppe, Annette P.; Comyn, Tim P.; Vargas, Silvia; Neville, Anne

doi:10.1063/1.4965971

Cited by 16 publications

(16 citation statements)

References 18 publications

(23 reference statements)

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“…The following sections provide information relating to the experimental approach and the test conditions evaluated using the SR-XRD flow cell. The flow cell design is described in detail in our previous publication [15] , which also discusses the setup, operation and full capabilities of the system. However, a brief summary of the setup and operation is provided here for completeness.…”

Section: Methodsmentioning

confidence: 99%

“…However, one key challenge in studying FeCO3 precipitation is following the growth kinetics and relating this to the corrosion rate of the steel substrate either in a quantitative or qualitative manner. Therefore, in this work, we demonstrate the capabilities of in situ Synchrotron Radiation-X-Ray Diffraction (SR-XRD) to study the film growth processes with a custom designed flow cell which is described in our previous publication [15] .…”

Section: Feco3 Nucleation and Growth Is Governed By The Saturation Ramentioning

confidence: 99%

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In situ SR-XRD study of FeCO3 precipitation kinetics onto carbon steel in CO2-containing environments: The influence of brine pH

Burkle

Motte

Taleb

et al. 2017

Electrochimica Acta

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The growth of iron carbonate (FeCO3) on the internal walls of carbon steel pipelines used for oil and gas transportation can reduce internal corrosion significantly. Solution pH can be considered as one of the most influential factors with regards to the kinetics, morphology and protection afforded by FeCO3 films. This paper presents results from a recently developed in situ Synchrotron Radiation-X-ray Diffraction (SR-XRD) flow cell integrated with electrochemistry for corrosion measurements. The cell was used to follow the nucleation and growth kinetics of corrosion products on X65 carbon steel surfaces in a carbon dioxide (CO2)saturated 3.5 wt.% NaCl brine at 80 º C and a flow rate of 0.1 m/s over a range of solution pH values (6.3, 6.8 and 7). In all conditions, FeCO3 was identified as the only crystalline phase to form. Electrochemical results coupled with post-test surface analysis indicate that at higher pH, larger portions of the surface become covered faster with thinner, more protective films consisting of smaller, denser and more compact crystals. The comparison between XRD main peak area intensities and FeCO3 surface coverage, mass and volume indicates a qualitative relationship between these parameters at each pH, providing valuable information on the kinetics of film growth.

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Section: Methodsmentioning

confidence: 99%

Section: Feco3 Nucleation and Growth Is Governed By The Saturation Ramentioning

confidence: 99%

In situ SR-XRD study of FeCO3 precipitation kinetics onto carbon steel in CO2-containing environments: The influence of brine pH

Burkle

Motte

Taleb

et al. 2017

Electrochimica Acta

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“…These angle ranges were found satisfactory as four main Bragg angles representative of the FeCO 3 crystals are in this range. In-situ synchrotron XRD characterisation shown in Supplementary information was carried out as described by Burkle et al 38 Scanning electron microscopy was carried out on the CS samples using a Carl Zeiss EVO MA15 to assess coverage and topography of the FeCO 3 corrosion products. All micrographs were collected at an accelerating voltage of 20 kV and at a working distance between 8 and 10 mm.…”

Section: Electrochemical Testsmentioning

confidence: 99%

Siderite micro-modification for enhanced corrosion protection

et al. 2017

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Production of oil and gas results in the creation of carbon dioxide (CO2) which when wet is extremely corrosive owing to the speciation of carbonic acid. Severe production losses and safety incidents occur when carbon steel (CS) is used as a pipeline material if corrosion is not properly managed. Currently corrosion inhibitor (CI) chemicals are used to ensure that the material degradation rates are properly controlled; this imposes operational constraints, costs of deployment and environmental issues. In specific conditions, a naturally growing corrosion product known as siderite or iron carbonate (FeCO3) precipitates onto the internal pipe wall providing protection from electrochemical degradation. Many parameters influence the thermodynamics of FeCO3 precipitation which is generally favoured at high values of temperatures, pressure and pH. In this paper, a new approach for corrosion management is presented; micro-modifying the corrosion product. This novel mitigation approach relies on enhancing the crystallisation of FeCO3 and improving its density, protectiveness and mechanical properties. The addition of a silicon-rich nanofiller is shown to augment the growth of FeCO3 at lower pH and temperature without affecting the bulk pH. The hybrid FeCO3 exhibits superior general and localised corrosion properties. The findings herein indicate that it is possible to locally alter the environment in the vicinity of the corroding steel in order to grow a dense and therefore protective FeCO3 film via the incorporation of hybrid organic-inorganic silsesquioxane moieties. The durability and mechanical integrity of the film is also significantly improved.

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“…Dugstad [ 4] suggested that a 'high degree' of super saturation is necessary in the bulk solution to obtain appreciable levels of FeCO3 formation on the steel sur face. However, more recent studies have indicated that enough sur face deposition to provide suppression of carbon steel corrosion rates can occur in systems with a bulk saturation below [2,[5][6][7].…”

Section: Understanding the Degree Of Pr Otection Afforded By The Layementioning

confidence: 99%

“…According to the bulk equilibrium calculations based on the CO2-H2O system at 80 o C[15], the CO3 2ion concentration can be calculated to be 7.70 10 -5 mol dm -3 for pH 6.8 and 7.70 10 -6 mol dm -3 for pH 6.3. The value of Ksp was determined to be 1.58 10 -5 mol 2 dm -6 using the model proposed by Sun and Nesic which is a function of temperature as well as ionic strength as shown in Equation(6).…”

mentioning

confidence: 99%

Iron carbonate formation kinetics onto corroding and pre-filmed carbon steel surfaces in carbon dioxide corrosion environments

Barker

Shaaili

Motte

et al. 2019

Applied Surface Science

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This work investigates the Corrosion Layer Accumulation Rate (CLAR) of iron carbonate (FeCO3 onto X65 carbon steel in carbon dioxide containing environments using the direct method of corrosion layer mass gain measur ement. Glass cell experiments wer e per formed at 80 o C and pH 6.3 or 6.8 over a range of bulk FeCO3 saturation ratios using both actively corroding carbon steel and steel pre-filmed with FeCO3 The CLARs obtained from experiments using actively corroding samples displayed strong agreement with the most recently developed precipitation model by Sun and Nesic at high supersaturation for pH 6.3 and 6.8, but a disparity at low supersaturation for the solution at pH 6.8. The observed discrepancy was attributed to the significant difference in surface saturation ratio between the two conditions when the steel is actively corroding. CLARs determined for pre-FeCO3 filmed carbon steel show that the kinetics of FeC O3 formation reduce significantly once the film establishes a protective barr ier at lower values of supersaturation. The results highlight the contrast between surface layer accumulation kinetics in the early stages of growth and those encountered in the long-term after the development of a protective film.

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Development of an electrochemically integrated SR-GIXRD flow cell to study FeCO3 formation kinetics

Cited by 16 publications

References 18 publications

In situ SR-XRD study of FeCO3 precipitation kinetics onto carbon steel in CO2-containing environments: The influence of brine pH

In situ SR-XRD study of FeCO3 precipitation kinetics onto carbon steel in CO2-containing environments: The influence of brine pH

Siderite micro-modification for enhanced corrosion protection

Iron carbonate formation kinetics onto corroding and pre-filmed carbon steel surfaces in carbon dioxide corrosion environments

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