J.

Atoms and Molecules / 3(2); 2013 / 509519 Research Article

Iloamaeke IM et al

Journal of Atoms and Molecules

An International Online Journal
ISSN 2277 1247

A COMPARATIVE STUDY OF VITEX DONIANA AND PTEROCARPUS SOYAUXI AS CORROSION INHIBITORS OF MILD STEEL IN HCL MEDIUM I. M. Iloamaeke, T. U. Onuegbu, U. C. Umeobika, and Onyema C. T. Department of Pure and Industrial Chemistry, Nnamdi Azikiwe University Awka, Anambra State, Nigeria. Received on: 02-02-2013 ABSTRACT: Corrosion inhibition of mild steel using Vitex doniana (VD) and Pterocarpus soyauxi (PS) leaves extract were studied using thermometric and gasometric methods at 30oC and 60oC. The inhibition efficiency was found to increase as the concentration of extracts increase from 0.1g/l to 0.5g/l with Pterocarpus soyauxi having the highest inhibition efficiency of 70.67% from Thermometric and 69.28% from gasometric method, while Vitex doniana has 68.49% from thermometric and 68.28% from gasometric all at 30oC. Adsorption of Vitex doniana leaves extract on the surface of the mild steel obeyed Langmuir and Tempkin adsorption isotherm while that of Pterocarpus soyauxi leaves extract on the surface of the mild steel followed Tempkin and freudlich isotherm. From the values obtained from the degree of surface coverage, Ea, H and G was calculated and all indicated physical adsorption. KEY WORDS: corrosion, inhibition, mild steel, Vitex doniana and Pterocarpus soyauxi INTRODUCTION: Corrosion is the chemical or electrochemical reaction between a metal and its environment that produces deterioration of the material and its properties. (Eml. Meligi, 2010). It is a problem that started gradually and ending up destroying the material or the object in which the metal and its alloy is made of resulting to economic waste. Acid solution is always used in industries for acid cleaning, prickling, descaling, and oil well acidizing therefore, this require the use of corrosion inhibitor in order to retard corrosion attack on the metallic objects. Recently, corrosion control using plant extract has become an interesting research because it can be easily extracted, environmentally friendly, easily affordable, www.jamonline.in 509 Revised on: 20-03-2013 Accepted on: 16042013

* Corresponding author I. M. Iloamaeke, Email: ifeomailoamaeke@yahoo.com

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J. Atoms and Molecules / 3(2); 2013 / 509519 and renewable. These plants extract contained O, N and S which are the active centre for adsorption process on the metal surface (Peter et al., 2009; Umoren et al., 2007; 2008a, 2008b; Arora et al 2007). The mechanism of this process is that O, N, and S have lone pair and electron which facilitate electron transfer from inhibitor to the metal surface thereby forming a compact barrier reducing corrodent attack. When an H atom attached to C in the ring is replaced by a substituent group (-NH2, -NO2, -CHO or COOH), its improves inhibition (Amathar Ram and Bharahi Bai, 2011). The electro density in the metal at a point of attachment changes resulting in the retardation of the cathodic or anodic reaction. Some of the plants extract that have been used as corrosion inhibitors are solanum melongena l. leaf (Ihebrodike et al., 2010), Azwarin (Sing Ambrish and Quraishi, 2012), Tecoma stans (Saratha, 2011), Azadricahta indica (Okafor et al., 2010), gum extrudate from pachylobus edulis (Umoren et al., 2008a), Kalmegh (Ambrish Singh et al., 2010), Curry leaf (Beenakumari, 2010), Emblica officinalis (Sarath, 2010), black pepper extract (Dahmani et al.,2010), Cocos nicifera l. coir dust (Eduok et al., 2012). As contribution to the current research on environmentally friendly, green corrosion inhibitors, this study investigated the inhibition effect of Vitex doniana (VD) and Pterocarpus soyauxi (PS) on the corrosion of mild steel in HCl corrodent using thermometric and gasometric methods at 30oC and 60oC. MATERIALS & METHODS: Preparation of Pterocarpus soyauxi and Vitex doniana leaves extract: 1424g of Ptercarpus soyauxi leaves (PS) and 1500g of Vitex doniana leaves (VD) was air dried in a shade for 8-12 days and ground into powder. 350g of the powder was taken in All rights reserved 2011

Iloamaeke IM et al 1000ml round bottom flask and enough quantity of ethanol was added as a solvent for extraction. The round bottom flask was covered with a stopper and left for 48hrs. Then the resulting paste was refluxed for 5hrs and filtered. The solvent was removed by concentrating the filtrate to about 20%. From this 0.1-0.5g/l concentration was made. Specimen preparation: Mild steel of thickness 1.4mm was obtained locally and was mechanically cut into coupons of 320.14cm. A small hole was drilled at one end of the coupons for easy hooking. The coupons were degreased in absolute ethanol, dried in acetone and stored in a desiccator. Test solution preparation: All the chemicals used were of Analytical grade. Solution was prepared by using double distilled water, and different concentrations of 1.0M 2.5M HCl were prepared. Thermometric Method: The procedure for determining this has been described by (Ebenso, 2003a, 2003b; Umoren, 2006a). The mild steel of 2x 3 x 0.14cm was used here. Volume of the test solution was at 100ml reagent. From the rise in temperature of the system per minutes, the reaction number (RN) was calculated using this: RN (0C min-1) =

(1)

Where Tm is the maximum temperature attained by the system, Tt is the initial temperature and t is the time (mins). Inhibition efficiency I(%) of the inhibitors can as well be calculated using: I% =

100

(2)

Where RN is the reaction number in the absence of inhibitors while the RN is the reaction number in the presence of inhibitors.

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J. Atoms and Molecules / 3(2); 2013 / 509519 Gasometric Method: Mild steel of 2 x 3 x 0.144cm was used here and this experiment was carried out at 30oC and 60oC.The procedure for this experiment has been documented in literature (Umoren et al., 2006a, 2008b). From the volume of hydrogen evolved per minute inhibition efficiency (I %) and degree of surface coverage () were calculated using equation 3 &4 I% = 1 =

Iloamaeke IM et al Where HR is the rate of hydrogen evolution, Vt and Vi are the volume of hydrogen evolved at time Tt and Ti respectively. RESULTS & DISCUSSION: Thermometric method Table1: shows the reaction number and inhibition efficiency (1%) of the mild steel in the presence of the ethanol extract of VD and PS. It could be deduced from the result that reaction number decreases from o -1 o -1 0.03827 Cmins to 0.02058 Cmins as the inhibition efficiency increases from 41.23% to 68.49% while PS decreases from o -1 o -1 0.0345 Cmins to 0.0191 Cmins as the inhibition efficiency increases from 45.38% 70.67% with an increase in the concentration of the ethanol extract of VD and PS. This explained that ethanol extract of VD and PS had adsorbed on the surface of the mild steel thereby inhibiting further corrosion attack.

100

(3) (4)

Where V1Ht and V0Ht are the volume of H2 gas evolve at time t for inhibited and uninhibited solution respectively. Rate of hydrogen evolution was computed using equation 5 (Obot et al., 2011) =

(5)

Table 1: Reaction number, inhibition efficiency (I%) and degree of surface coverage of mild steel in different concentration of ethanol extract of leaves VD and PS Concentration of VD inhibitor in (g/l) 0.1 0.2 0.3 0.4 0.5 Concentration of PS inhibitor in (g/l) 0.1 0.5 68.15 0.0221 0.4692 0.2 45.38 70.67 0.0207 0.6600 0.3 46.92 0.0355 0.0191 0.6815 0.4 66.00 0.0345 0.4538 0.7067 Inhibition Efficiency (%) 41.23 43.71 63.55 67.18 68.49 Reaction number (oC Mins-1) 0.03827 0.02393 0.02048 0.4371 0.6718 Degree of surface coverage () 0.03659 0.02133 0.4123 0.6355 0.6849

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J. Atoms and Molecules / 3(2); 2013 / 509519 Gasometric Method: Fig.1, 2, 3 and 4 showed the variation in volume of H2 evolved with time at 300C and 600C with different concentrations of the VD and PS extract. It could be observed from the plot that volume of H2 evolved increased with time. The rate of hydrogen evolved decrease as the concentrations of VD and PS extract increase compare with the blank. This result correlated with thermometric method result

Iloamaeke IM et al that VD and PS extract are good inhibitors for corrosion of mild steel. Table 2 shows different concentrations of the VD and PS extract and inhibition efficiency. It could be deduced from the table that inhibition efficiency increase as the concentrations of the both extract increase with decrease in temperature inferring physical adsorption of the VD and PS extract on the surface of the mild steel.

7 Volume of hydrogen evolved (cm3) 6 5 4 3 2 1 0 0 5 10 Time (mins) 15 20 blank 0.1g/l 0.2g/l 0.3g/l 0.4g/l 0.5g/l

Fig.1: Volume of hydrogen evolved with time for corrosion of mild steel in 2.5M HCl in the presence and absence of Vitex doniana at 30oC

volume of hydrogen evolume (cm3)

7 6 5 4 3 2 1 0 0 5 10 time (mins) 15 20
30OC

blank at 30oC 0.1g/l 0.2g/l 0.3g/l 0.4g/l 0.5g/l

Fig.2: Volume of hydrogen evolved with time for corrosion of mild steel in 2.5M HCl in the presence and absence of pterocarpus soyauxi at 30oC All rights reserved 2011 www.jamonline.in 512

J. Atoms and Molecules / 3(2); 2013 / 509519

Volume of hydrogen evolved (cm3) 50 40 30 20 10 0 0 5 Time (mins) 10 15

Iloamaeke IM et al

blank 0.1g/l 0.2g/l 0.3g/l 0.4g/l 0.5g/l

Fig.3: volume of hydrogen evolved with time for corrosion of mild steel in 2.5M HCl in the presence and absence of Vitex doniana at 60oC

50 Volume of hydrogen evolved (cm3) 40 30 20 10 0 0 5 Time (mins) 10 15

60OC blank at 60oC

0.1g/l 0.2g/l 0.3g/l 0.4g/l 0.5g/l

Fig.4: Volume of hydrogen evolved with time for the corrosion of mild steel in 2.5M of HCl in the presence and absence of ethanol extract of Pterocarpus soyauxi at 60oC.

Table 2: Shows the concentration of the VD and PS extract and inhibition efficiencies at 30oC and 60oC from gasometric method. Concentration of the Inhibition efficiency (%) from VD Inhibition efficiency inhibitors in(g/l) extract at from PS extract at 30oC 0.1 0.2 0.3 0.4 0.5 23.51 38.35 45.13 51.06 68.22 60oC 21.11 30.20 38.39 42.29 54.98 30oC 50.64 60.16 62.08 68.22 69.28 (%)

60oC 47.41 57.03 58.96 64.25 67.80

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J. Atoms and Molecules / 3(2); 2013 / 509519 Adsorption Consideration The adsorption behaviour of ethanol extract of VD and PS was also studied by fitting data obtained (gasometric method) from degree of surface coverage to different adsorption isotherms such as Langmuir, Tempkin, Freundlich and Flory Huggin. The test revealed that adsorption of VD extract on the surface of the mild steel is consistent with the assumption of Langmuir and Tempkin Isotherms. While the adsorption of PS extract on the surface of the mild steel obeyed Tempkin and Freundlich adsorption isotherms. Langmuir adsorption models can be represented as follows equation 6 (Agrawal et.al. 2003) C/ = C +1/k (6) =
. .

Iloamaeke IM et al .

(9)
.

Slope=

, while intercept =

Fig.6 and 7: Shows plot of versus log C. which was made from equation 8 and a linear graph was obtained which confirmed Tempkin adsorption isotherm for the adsorption of VD and PS extract on the surface of mild steel. Fig.8 revealed Freundlichs adsorption isotherm of PS extract on the surface of the mild steel and is given by the equation 10 and 11 (Sharma and Sharma, 1999)

= kc1/n

(10) log c (11)

Log = log k + The fraction

Taking the logarithm of equation 6, equation 7 is obtained Log C/ = log C log K (7)

in equation 11 has been found

to be approximate to the inhibition efficiency of the inhibitor, k and n is constant. Slope is equal to

Where C is the concentration of the inhibitor in the electrolyte, is the degree of surface coverage of the inhibitor and k is the equilibrium constant of adsorption. The plot of C/ versus C (fig 5) gave linear plots indicating that Langmuir adsorption isotherm is applicable to the adsorption of ethanol extract of VD on the surface of the mild steel. Tempkin isotherm was also found to occur according to this equation 8 (Abdullah, 2004; El etre, 2003; Ayssar et al., 2010) Exp(-2a) = kC (8)

and intercept =l og . Therefore,

from equation 11, a plot of log inhibition efficiency (I%) versus log c produces a straight line that obeyed Freundlich adsorption isotherm. (Umoren et al., 2006b; 2008c)
1.2 1 0.8 0.6 0.4 0.2 0 0 0.2 C 0.4 0.6 y = 1.025x + 0.3323 R = 0.9616 30oC 60oC C/ y = 1.464x + 0.3462 R = 0.994

Where a is the Tempkin interaction parameter, is the degree of surface coverage of the inhibitor. K is the equilibrium constant of adsorption and C is the concentration of the inhibitor in the bulk electrolyte. Rearranging and taking logarithm of equation 8, equation 9 is obtained.

Fig. 5: Langmuir isotherm for the adsorption of vitex doniana on the surface of mild steel. www.jamonline.in 514

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J. Atoms and Molecules / 3(2); 2013 / 509519

Iloamaeke IM et al

y = 0.5714x + 0.7864 R = 0.9203

y = 0.3708x + 0.5746 R = 0.9927

0.8 0.7 0.6 0.5 0.4 0.3 0.2 0.1 0 -0.2 0

30oC 60oC

-1.2

-1

-0.8

-0.6 logC

-0.4

Fig 6: Tempkin isotherm for adsorption of the extract of vitex doniana on the surface of the mild steel.

y = 0.2683x + 0.7775 R = 0.9752 y = 0.28x + 0.7546 R = 0.979

0.8 0.7 0.6 0.5 0.4 0.3 0.2 0.1 0 30oC 60oC

-1.2

-1

-0.8

-0.6 logC

-0.4

-0.2

Fig.7: Tempkin isotherm for the adsorption of Pterocarpus soyauxi extract on the surface of the mild steel.

log I% 30oC 60oC 0

y = 0.1964x + 1.9049 R = 0.9743

y = 0.2137x + 1.8932 R = 0.9807

1.86 1.84 1.82 1.8 1.78 1.76 1.74 1.72 1.7 1.68 1.66 -0.2

-1.2

-1

-0.8

-0.6 logC

-0.4

Fig.8: Freundlich isotherm for the adsorption of PS extract on the surface of the mild steel. All rights reserved 2011 www.jamonline.in 515

J. Atoms and Molecules / 3(2); 2013 / 509519 Thermodynamics Studies The value of activation energy Ea was calculated using Arrhenius equation. Log

Iloamaeke IM et al while that of PS extract increased when compared to the value obtained from Blank experiment which is 54.19KJmol-1. But since none of Ea reach up to the threshold value of 80KJmol-1 required for chemical adsorption therefore, the adsorption is by physical adsorption mechanism (Deepai Rani and Selvaraj, 2010). Heat of adsorption is approximately equal to enthalpy of reaction Hads. The values of heat of adsorption were calculated using equation (13). (Quraish et al., 2009; Okafor et al., 2010; Eddy et al., 2008).

(12)

Where HR1 and HR2 are the hydrogen evolution rate at temperature T1 and T2 respectively. Table 3 shows the values of Ea for VD and PS extract on the surface of mild steel. It could be inferred from the table that the values of Ea for VD extract decreased Hads = 2.303R [log (

) log (

)] x

(13)

Where 1 and 2 are degree of surface coverage at temperatures T1 and T2 respectively. Table 3: enumerated the values of Hads at different concentrations of inhibitors. Hads were found to be negative in all the concentrations of the VD and PS extract showing that the reactions are exothermic. Values of adsorption parameter deduced from Langumir, Tempkin and Freundlich isotherms are recorded in Table 4 and 5: From the Tables the degrees of linearity (R2) were also close to unity indicating strong adherence of the adsorption of VD and PS extract on the surface of the mild steel. The equilibrium constant of adsorption of VD and PS extract on the surface of the mild steel are related to the free energy of adsorption (Gads) according to equation 14

Gads= -2.303RTlog (55.5K)

(14)

Where R is the gas constant, T is the temperature, K is the equilibrium constant of adsorption, 55.5 is the molar heat of adsorption of water. Values of K obtained from intercept of Langumir, Tempkin and Freundlich isotherm were used to compute for Gads according to equation 14 and the result in Table 4 and 5. From the result, Gads values were found to be negative and less than the threshold value of -40KJmol-1 required for chemical adsorption hence the adsorption of VD and PS extract on the surface of mild steel is spontaneous and follows physical adsorption mechanism (Eddy et al., 2007; Saratha et al., 2011; Ihebrodike et al., 2010).

Table 3: Calculated values of Ea and H for VD and PS extract at different concentrations Concentration of VD and PS inhibitor in g/l. Blank 0.1 0.2 0.3 0.4 0.5 Ea from VD inhibitor in KJ/mol 54.19 31.18 41.24 36.38 38.30 37.42 Ea from PS inhibitor in KJ/mol 54.19 64.30 58.76 59.95 59.69 59.09 H from VD inhibitor in KJ/mol -------3.88 -10.39 -7.72 -9.91 -17.05 H from PS inhibitor in KJ/mol -------3.63 -3.69 -3.65 -3.70 -1.94

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J. Atoms and Molecules / 3(2); 2013 / 509519

Iloamaeke IM et al

Table 4: Langmuir and Tempkin adsorption isotherm parameters for adsorption of VD extract on the surface of the mild steel. Temperature (oC) 30 60 30 60 Log k Langmuir 0.4785 0.4606 Tempkin 1.3764 1.5410 Slope 1.0250 1.4640 a -2.0151 -3.1050 G (KJ/mol) -7.3444 -8.1840 -9.5141 -9.5870 R2 0.9616 0.9940 0.9203 0.9927

Table 5: Freundlich and Tempkin adsorption isotherm parameters for adsorption of PS extract on the surface of the mild steel. Temperature (oC) 30 60 30 60 CONCLUSION: VD and PS extract showed inhibitive effect on corrosion of mild steel in acidic environment. Inhibition efficiency increase with an increase in inhibitor concentration for both extracts. The adsorption of VD extract on the surface of the mild steel followed Langmuir and Tempkin, while that of PS extract obeyed Tempkin and Freundlich adsorption isotherms. PS extract proved to be better corrosion inhibitor than VD extract since it has higher inhibition efficiency in thermometric and gasometric method. Log k Freundlich 1.9049 1.8932 Tempkin 0.1573 0.1594 Slope 0.1964 0.2137 a -0.2330 -0.2432 G (KJ/mol) -11.743 -12.889 -9.4860 -10.3420 R2 0.9743 0.9807 0.9752 0.9790

The mechanism of physical adsorption was proposed from the calculated values of Ea, Hads, and Gads, obtained.

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