Green Corrosion inhibition of mild steel by Asafoetida extract extract in 3.5% NaCl

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ScienceDirect Materials Today: Proceedings 14 (2019) 590–601

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ICRAMC2018

Green Corrosion inhibition of mild steel by Asafoetida extract extract in 3.5% NaCl S.Devikala*, P.Kamaraj, M.Arthanareeswari, S Pavithra SRM Institute of Science and Technology, Kattankulathur, Kancheepuram.603203

Abstract Corrosion is the deterioration of a metal by chemical or electrochemical reaction with its environment. It is impossible to eliminate corrosion completely. So prevention would be more practical than elimination. There are several methods to effectively control and minimize corrosion. The small quantity of corrosion inhibitors can effectively decrease the corrosion process. Mild steel is a material of used in industries due to easy availability and fabrication of machineries. Corrosion can damage the materials which are used to construct automobiles, pipeline systems, bridges and buildings, petroleum refineries, etc. Plant extracts have been recently studied as corrosion inhibitors for different metals in various environments. In the present work, an aqueous extract of asafoetida have been used as a corrosion inhibitor in controlling corrosion of mild steel. The formation of protective layer on the surface of metal are to be confirmed by FTIR, XRD and SEM. The corrosion inhibition of mild steel have been be studied by potentiodynamic polarization and electrochemical impedance spectroscopic techniques. © 2019 Elsevier Ltd. All rights reserved. Selection and/or Peer-review under responsibility of 2nd International Conference On Recent Advances In Material Chemistry. Keywords: Corrosion inhibition; mild steel; Asafoetida extract; 3.5%NaCl;

1. Introduction Mild steel is apparently one of the most versatile metallic materials that is widely used in construction, manufacturing, marine and diverse areas of other industrial and engineering purposes. However, the versatility of mild steel and hence its engineering performance is continually being threatened as it is subject to corrosive environmental degradation in service. One of the means to mitigate this destructive phenomenon which can be disastrous and with economic and technological consequences is the use of chemical inhibitors[10,11]. These are chemical compounds that are adsorbed on the metal surfaces to minimize, control and/or prevent corrosion destructive processes and reactions. The use of chemical inhibitors to decrease the rate of corrosion processes is quite varied. In the oil extraction and processing industries, inhibitors have always been considered to be the first line of defense against corrosion. A great number of scientific studies have been devoted to the subject of corrosion inhibitors[12]. Controlled syntheses of metal oxide nanoparticles are essential for the several applications and 2214-7853 © 2019 Elsevier Ltd. All rights reserved. Selection and/or Peer-review under responsibility of 2nd International Conference On Recent Advances In Material Chemistry.

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solution phase methods provide a large degree of control over the synthesis products.SnO2 is an important material due to its properties such as high degree of transparency in the visible spectrum, strong physical and chemical interactions with adsorbed species, low operating temperature and strong thermal stability in air (up to 500o C). It is an n-type semiconductor with a band gap of 3.6 to 3.8 eV [13,14] . However, most of what is known has grown from trial and error experiments, both in the laboratories and in the field. Rules, equations, and theories to guide inhibitor development or use are very limited. By definition, a corrosion inhibitor is a chemical substance that, when added in small concentration to an environment, effectively decreases the corrosion rate. In simple terms corrosion is disintegration of any substance like a metal and the process is termed as corrosion. Natural substances like water, oxygen are the major sources for corrosion to occur, though other substances on the earth and its atmosphere can also cause corrosion[15]. Corrosion of metals and alloy structures cause dreadful impacts which in turn lead to economic crisis. In present days, some inhibitors that have been used with success in typical corrosive environments to protect the metallic elements of industrial systems. Commercial inhibitors are available under various trade names and labels that usually provide little or no information about their chemical composition. It is sometimes very difficult to distinguish between products from different sources because they may contain the same basic anticorrosion agent. Commercial formulations generally consist of one or more inhibitor compounds with other additives such as surfactants, film enhancers, de-emulsifiers, oxygen scavengers, and so forth. The inhibitor solvent package used can be critical in respect of the solubility/dispersibility characteristics and hence the application and performance of the products[16]. Many works were conducted to examine extracts from naturally occurring substances. So in this work we have taken natural product as our corrosion inhibitor. Some references are coated here in which natural products are used as corrosion inhibitor. Corrosion inhibition of carbon steel in low chloride media by an aqueous extract of Hibiscus rosa - sinensis Linn has been evaluated by mass – loss method and electrochemical studies[17]; corrosion inhibition by beet root extract in well water[18]; electrochemical studies confirm the formation of a protective film on the metal surface by spirulina solution, this offers 90% corrosion inhibition efficiency[19] ;corrosion resistance of metals inartificial saliva in the absence and also in the presence of spirulina[20]; corrosion behavior of aluminium in various media has been used to control corrosion of aluminium. To prevent the corrosion of aluminium in acid medium, inhibitors such as Chlomolaena Odorata L.1[21], Ananas Sativum[22], Ipomoea Invulcrata[23] have been used. There are several reviews on the use of plant extracts as corrosion inhibitors[24].Recently aqueous extract of Cocos nucifera - Coconut Palm – Petiole[25], Fennel (Foeniculum Vulgare) Essential[26], Pericarp of the Fruit of Garcinia Mangostana[27], Natural[28] and Ethanol extract of Vernonia Amygdalina[29] and Ipomoea involcrata[30] have been used as corrosion inhibitors. Langmuir adsorption isotherm proved the effects of Alovera on corrosion of Zinc in HCl solution[31], in the presence of fruit peel in hydrochloric acid on carbon steel[32], and it also proved that Murraya Koenigii acts as corrosion inhibitor on mild steel in hydrochloric acid and sulphuric acid solutions[33]. Investigation on natural inhibitors is particularly interesting because they are non –expensive, ecologically friendly, acceptable and possess no threat to the environment. Asafoetida is an ingredient of a plant mixture reported to have antidiabetic properties in rats[34]. Asafoetida has a broad range of uses in traditional medicine as an antimicrobial, antiepileptic, used for treating chronic bronchitis and whooping cough[35,36]. The present work is undertaken: i. To evaluate the inhibition efficiency (IE) of an aqueous extract of asafotida (ASF) in controlling the corrosion of carbon steel in sea water, in the absence and presence of Zn2+ ii. To investigate the influence of immersion period on the IE of the system. iii. To analyze the protective film formed on the carbon steel by FTIR spectra, Polarization study and Atomic Force Microscope techniques. An environment reduces the corrosion rate of a metal exposed to that environment. These are also known as site blocking elements or blocking species or an adsorption site blocker, due to their adsorptive properties. Due to excellent antimicrobial, Anti-bacterial, Antibiotic property of Asafoetida (as a solvent) is used as an inhibitor for mild steel corrosion. Asafoetida is used as a flavoring agent in food and as a traditional medicine for many diseases in many parts of the world. Asafoetida (ferula asafoetida) is an oleo-gum-resin obtained from the stems of ferula plants belonging to the family umbelliferae. Out of more than 170 species, sixty spices of ferula are widely distributed in central Asia, Europe and North Africa[37].F.asafoetida is the important species of ferula and is more native to Afghanistan and Iran and grows about 2 m in height and is in two types bitter and sweet[38]. Asafoetida is called hing or hingu in india[39]. The collection of resin and slicing of the root are repeated until excudation ceases[40].

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Asafoetida has a strong,tenacious and sulfurous odour. Asafoetida is traditionally used for the treatment of different diseases, such as whooping cough, asthma, ulcer, epilepsy, stomachache, flatulence, bronchitis, antispasmodic, weak digestion and influenza.[41-44]. Recent pharmacological and biological studies have also shown several activities, such as antioxidant,[45,46] antimicrobial,[47-51] antiviral,[43] antifungal,[52-55] cancer chemopreventive,[56] anti-diabetic,[57] anticarcinogenesis,[58-59] antispasmodic and hypotensive,[60] relaxant effect,[61,62] neuroprotective,[63,64] and molluscicidal[65] from this asafoetida. In general, asafoetida consists around 68% of carbohydrates, 16% of moisture, 4% protein, 1% of fat, 7% of minerals and 4% of fibre. It consist of three main fractions, including resin (40-64%), gum (25%) and essential oil (10-17%).The resin fraction contains ferulic acid and its esters, coumarins, sesquiterpene coumarins and other terpenoids. The gum includes glucose, galactose, 1-arabinose, glucuronic acid, polysaccharides and glycoproteins, and the volatile fraction contains sulfurcontaining compounds, monoterpenes and other volatile terpenoids.sulfur compounds in F.asafoetida resin show various biogical activities and can be valuable in medicine. 2.Experimental 2.1 Preparation of Asafoetida extract 10g of asafetida was boiled with double distilled water for 10mintues and then suspended impurities were removed by filteration and made up to 100 ml. The extract was used as corrosion inhibitor. 50ml of well water was taken in beaker with 50ml of simulated concrete pore solution(SCPS) solution. Preparation of SCPS (1g of calcium hydroxide made upto to 500ml and the mild steel specimen was immersed(Blank ) and left undisturbed for one day . Varying concentrations of asafoetida extract (2ml , 4ml,6ml, 8ml and 10ml) in well water was prepared and kept for 24hours.

Figure1 Mild steel plates immersed in varied concentration of garlic extract Table 1 Parameters of well water Parameter

Value

pH Conductivity

8.6 2620 μ mho/cm

TDS Chloride

1835mg/l 450

Sulphate Total hardness

110 96

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2.2 Preparation of mild steel specimens Mild steel specimens of dimensions 3cm x 2 x 1.5 cm were washed with 10 % dilute sulphuric acid and then with acetone and were allowed to dry at room temperature and used for linear polarization and impedance studies. Table 2 shows the characterization of steel plate. Table 2 Elemental composition of mild steel plate Element

Minimum

Maximum

Carbon Manganese Sulphur Phosphorous

----0.30% ---------

0.10% 0.50% 0.05% 0.04%

Actual value 0.064% 0.38% 0.035% 0.027%

2.3 Characterisation Techniques The XRD patterns were recorded using Philips X’Pert pro diffractometer. The FTIR spectrums were recorded using Shimadzu FTIR spectrophotometer. The SEM images were recorded using Hitachi Scanning Electron Microscope SU1510.The Scanning electron microscope is a technique mainly used for surface study of materials. 2.4 Polarization and Electrochemical Impedance Studies The experiments were performed in a classical three-electrode electrochemical cell (Fig.3). Mild steel specimen of 1 cm2 area was used as the working electrode. A platinum electrode and saturated calomel electrode were used as counter electrode and reference electrode respectively. The saturated calomel electrode was connected via Luggin capillary, the tip of which was held very close to the surface of the working electrode to minimize the IR drop. Open circuit potential (OCP) measurements were recorded for 30 minutes, the time necessary to reach quasi stationary state for open circuit potential, followed by polarization measurements at a scan rate of 1mV/s for Tafel plots. Biologic Electrochemical analyzer (model SP 300) with EC Lab software was used for data acquisition and analysis. For polarization and impedance studies the period of immersion maintained was 30 minutes. Polarization technique was carried out from a cathodic potential of -250 mV to an anodic potential of +250 mV with respect to OCP at a scan rate of 1 mV/s. The electrochemical parameters including corrosion potential (Ecorr), corrosion current density (Icorr) and corrosion rate were calculated from Tafel plots. In EIS technique a small amplitude AC signal of 10 mV and a frequency spectrum from 105 to 10-2 Hz was impressed at the OCP and the impedance data were analysed using Nyquist plots. The impedance data were fit into appropriate equivalent electrical circuit using EC lab software. The parameters obtained from the best fit equivalent circuit were analysed. 3.Results and Discussion The XRD pattern of asafoetida extract showed a characteristic peak at 20°(Fig. 2). This peak confirms that the extract used is asafoetida. With increase in the concentration of the extract, there is increase in crystallinity. There is a regular molecular arrangement. This is confirmed by XRD results (Fig. 3-4).

Figure 2 XRD pattern of pure dried ASF

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Figure 3 XRD spectrum of the film formed on the metal surface after immersed in the well water containing 2ml of ASF.

Figure 4 XRD spectrum of the film formed on the metal surface after immersed in the well water containing 10ml of ASF. Earlier researchers have confirmed that FTIR spectrometer is a powerful instrument that can be used to determine the type of bonding for organic inhibitors adsorbed on the metal surface. FTIR spectra have been used to analyze the protective film formed on metal surface. FTIR spectrum of pure dried Asofoetida ASF is given in figure 5. The FTIR spectrum of the film formed on the metal surface after immersion in the well water for 1 day containing 2ml and 10ml of ASF is shown in Fig-6 and Fig-7.The OH stretching frequency has increased from3118 cm-1 to 3243 cm-1,C=O stretching frequency has shifted from 1632 cm-1 to 1636cm-1,ring O stretching frequency has increased from 1012cm-1 to 1028 cm-1. The band due to conjugated double bonds shifts from 3737 cm-1 to 3696 cm-1.

Figure 5 FTIR spectrum of pure dried ASF

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Figure 6 FTIR spectrum of the film formed on the metal surface after immersed in the well water containing 2ml of ASF.

Figure 7 FTIR spectrum of the film formed on the metal surface after immersed in the well water containing 10ml of ASF. The Fig. 8 shows the SEM image of mild steel plate before immersion in solution without corrosion inhibitor ,where it can been seen that the steel exposed to the solution without inhibitor forms a porous layer full of micro cracks. And as a result the Chemicals can easily penetrate though these cracks and can corrode the plate. However, in presence of inhibitor Fig.9, the surface is remarkably improved with respect to its smoothness, less porous and micro cracks, indicating the reduction in corrosion rate. This improvement in surface morphology is due to the formation of a protective layer by Asafoetida on the metal surface. Hence these studies shows that Asafoetida has a strong tendency to adhere to the steel surface and can be regarded as good inhibitor for mild steel plate used in acidic medium.

Fig.8 represents the SEM images of mild steel, immersed in the well water containing 2ml of ASF.

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Fig.9 represents the SEM images of mild steel, immersed in the well water containing 10ml of ASF. It is observed from the Table 3 that as the concentration of asafoetida extract increases, the corrosion inhibition efficiency also increases. The active component of asafoetida extract, namely umbelliferone coordinated with Fe2+ on the metal surface and forms a protective film consisting of Fe2+- umbelliferone complex. Thus the anodic reaction of metal dissolution is prevented (Fig.10). Ew e vs. log (||) 0ml lp.mpr

2ml lp.mpr

4ml lp.mpr

6ml lp.mpr

8ml lp.mpr

10ml lp.mpr #

-0.1 -0.15 -0.2

Ew e /V

-0.25 -0.3 -0.35 -0.4 -0.45 -0.5 -0.55 -6

-4 lo g ( |/m A|)

Figure 10 Tafel plots of blank and and varying concentrations of ASF extract Table 3 Inhibition efficiency obtained from Polarization studies for blank and and varying concentrations of ASF extract

System studied

Ecorr (mV)

0ml 2ml 4ml 6ml 8ml 10ml

-554.61 -135.98 -142.91 -133.04 -149.25 -156.89

Icorr (µA/cm2) 1.340 0.998 0.807 0.760 0.726 0.387

Corrosion rate (mpy) 0.4088 0.3045 0.2236 0.1750 0.1182 0.0425

Inhibition efficiency % 26 45 57 71 90

From the Table 4, it is found that Rct(Charge transfer resistance) values increases as the Cdl(Double layer capacitance) value decreases. Therefore corrosion rate decreases. This infers formation of protective layer on the surface(Fig.11 and 12).

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Table 4 Electrochemical parameters obtained from Impedance studies for blank and and varying concentrations of ASF extract

System studied

Rct (Ohm cm2)

0ml 2ml 4ml 6ml 8ml 10ml

5010 6074 11120 12863 13200 16050

Cdl (µF) x10-6 48.93 30.18 27.64 20.15 17.58 10.74

-Im(Z) vs. Re(Z) 0ml peis.mpr

2ml peis.mpr

4ml peis.mpr

6ml peis.mpr

8ml peis.mpr

10ml peis.mpr #

7,000

6,000

-Im (Z )/O h m

5,000

4,000

3,000

2,000

1,000

0

-1,000 5,000

10,000

15,000

Re (Z)/Ohm

Figure 11 Nyquist plots of 0ml /blank and varying concentrations of ASF extract 0ml peis.mpr : log (|Z|) vs. log (freq) 2ml peis.mpr : Phase(Z) vs. log (freq) 6ml peis.mpr : log (|Z|) vs. log (freq) 8ml peis.mpr : Phase(Z) vs. log (freq)

0ml peis.mpr : Phase(Z) vs. log (freq) 4ml peis.mpr : log (|Z|) vs. log (freq) 6ml peis.mpr : Phase(Z) vs. log (freq) 10ml peis.mpr : log (|Z|) vs. log (freq)

2ml peis.mpr : log (|Z|) vs. log (freq) 4ml peis.mpr : Phase(Z) vs. log (freq) 8ml peis.mpr : log (|Z|) vs. log (freq) 10ml peis.mpr : Phase(Z) vs. log (freq) #

4.2 30 4 20

3.8

10

3.4

0

3.2

-10

3

Ph as e( Z )/d e g

lo g ( |Z |/O h m )

3.6

-20

2.8 -30 2.6 -40 2.4 0

2

4

lo g ( f r e q /Hz )

Figure 12 Bode plots of blank and varying concentrations of ASF extract

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Conclusion The prospect of using Umbelliferone(asafoetida) extract as a corrosion inhibitor has been evaluated. Umbelliferone was proved to be an excellent Green inhibitor with its highest inhibition efficiency of 90% . From the Electrochemical and Impedance studies it was proved that decrease in the corrosion rate by umbelliferone extract was due to the formation of a protective external film which contained compounds present in asafoetida extract. Hence it is concluded that, Asafoetida is a non toxic, environmental friendly inhibitor. It controls mild steel corrosion effectively. 10 ml of inhibitor offers 90% inhibition efficiency. Polarization study shows that asafoetida extract acts as mixed type inhibitor and protective film is formed on the metal surface. FTIR confirms that the protective film consists of Fe2+ - Umbelliferone complex. References [1] J. Buchweishaija, “Phytochemicals as green corrosion inhibitors in various corrosive media a review,” Chemistry Department, College of Natural and Applied Sciences, University of Dares Salaam. [2] Kuznetsov, Y.I. (2004) Physicochemical Aspects of Metal Corrosion Inhibition in Aqueous Solutions. Russian ChemicalReviews, 73, 75-87. [3] Bendahou, M.A., Benadellah, M.B.E. and Hammouti, B.B. (2006)A Study of Rosemary Oil as a Green Corrosion Inhibitorfor Steel in 2 M H3PO4. Pigment and Resin Technology, 35, 95-100. [4] Bouklah, M., Hammouti, B., Benhadda, T. and Benkadour, M. (2005) Thiophene Derivatives as Effective Inhibitors for the Corrosion of Steel in 0.5 M H2SO4. Journal of Applied Electrochemistry, [5] Valek, L., Martinez, S., Mater. Lett, (2007) Copper corrosion inhibition by Azadirachta indica leaves extract in 0.5 M sulphuric acid 148–151. [6] P.Bothi Raja and M.G. Sethuraman. Materials Letters 62, 113 (2008). Natural products as corrosion inhibitor for metals in corrosive media [7] P.B. Raja and M.G. Sethuraman, Mater. Lett. 62(2008) 2977. Inhibitive effect of black pepper extract on the sulphuric acid corrosion of mild steel [8] G. Gunasekaran and L.R. Chauhan, Electrochim.Acta. 49 (2004) 4387. Characterization and electrochemical studies of Nafion/nano-TiO2 film modified electrodes [9] A.M. Abdel-Gaber, B.A. Abd El-Nabey, I.M.Sidahmed, A.M. El-Zayady and M. Saadawy, Corros. Effect of Temperature on Inhibitive Action of Damsissa Extract on the Corrosion of Steel in Acidic Media, CORROSION. 2006;62(4):293-299. [10] GD Davis, JAFraunhofer.Materials Performance, 2003, 2, 56 – 60 [11] JAFraunhofer,Inhibiting Corrosion with Tobacco,Advanced Materials and Processes, 2000, 158, 33 [12] JAFraunhofer. Tobacco Extract Composition and Methods, U.S. Patent 1995, 43, 941 [13] Vennila Raj, Kamaraj Palanisamy, Arthanareeswari M and Devikala S, Biological Activities Of Tin Oxide Nanoparticles Synthesized Using Plant Extract, World Journal Of Pharmacy And Pharmaceutical Sciences, 3, (9) pp. 382-388, 2014. [14] R.Vennila, P.Kamaraj, M. Arthanareeswari, B.Sivakumar, Green Synthesis of Silver Nanoparticles from Cleistanthus Collinus Leaf Extract and Their Biological Effects International Journal of Chemistry, Vol.34, Issue.1 1103-1107 (2013) [15]. CA Loto,J. Mater. EnvronSci, 2011, 2 4, 335-344. Inhibition Effect of Tea (Camellia Sinensis) Extract on the Corrosion of Mild Steel in Dilute Sulphuric Acid [16] CA Loto, RT Loto, APIPopoola, Int. Jof Physic. Sci. 2011, 6,15,3689-3696

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