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J. Atoms and Molecules / 3(2); 2013 / 509–519

Iloamaeke IM et al

Research Article

Journal of Atoms and Molecules

AnAnAnAn InternationalInternationalInternationalInternational OnlineOnlineOnlineOnline JournalJournalJournalJournal

ISSNISSNISSNISSN –––– 2277227722772277 –––– 1247124712471247

–––– 2277227722772277 –––– 1247124712471247 A COMPARATIVE STUDY OF VITEX DONIANA AND PTEROCARPUS

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

Revised on: 20-03-2013

Accepted on: 16–04–2013

ABSTRACT:

Corrosion inhibition of mild steel using Vitex doniana (VD) and Pterocarpus soyauxi (PS) leaves extract were studied using thermometric and gasometric methods at 30 o C and 60 o C. 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 30 o C. 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, ΔH and ΔG was calculated and all indicated physical adsorption.

KEY WORDS: corrosion, inhibition, mild steel, Vitex doniana and Pterocarpus soyauxi

* Corresponding author

I. M. Iloamaeke,

Email: ifeomailoamaeke@yahoo.com

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,

J. Atoms and Molecules / 3(2); 2013 / 509–519

Iloamaeke IM et al

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 π 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 (-NH 2 , -NO 2 , -CHO or –COOH), it’s 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 30 o C and 60 o C.

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

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 3×2×0.14cm. 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 ( 0 C min -1 ) =

(1)

Where T m is the maximum temperature attained by the system, T t 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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Gasometric Method:

Mild steel of 2 x 3 x 0.144cm was used here and this experiment was carried out at 30 o C and 60 o C.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 (θ) were calculated using equation 3 & 4

I%

θ

=

=

1 −

100

I –

(3)

(4)

Where V 1 Ht and V 0 Ht are the volume of H 2 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)

Where H R is the rate of hydrogen evolution, V t and V i are the volume of hydrogen evolved at time T t and T i 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 0.03827 o Cmins -1 to 0.02058 o Cmins -1 as the inhibition efficiency increases from 41.23% to 68.49% while PS decreases from 0.0345 o Cmins -1 to 0.0191 o Cmins -1 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.

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

Inhibition

Reaction number

Degree of surface

inhibitor in (g/l)

Efficiency

(%)

( o C Mins -1 )

coverage (θ)

0.1

41.23

0.03827

0.03659

0.2

43.71

0.02393

0.02133

0.3

63.55

0.02048

0.4123

0.4

67.18

0.4371

0.6355

0.5

68.49

0.6718

0.6849

Concentration of PS inhibitor in (g/l)

0.1

0.2

0.3

0.4

0.5

45.38

46.92

66.00

68.15

70.67

0.0355

0.0345

0.0221

0.0207

0.0191

0.4538

0.4692

0.6600

0.6815

0.7067

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Gasometric Method:

Fig.1, 2, 3 and 4 showed the variation in volume of H 2 evolved with time at 30 0 C and 60 0 C with different concentrations of the VD and PS extract. It could be observed from the plot that volume of H 2 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

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

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 30 o C

7 6 30 O C 5 blank at 30oC 4 0.1g/l 0.2g/l 3 0.3g/l 2
7
6
30
O C
5
blank at 30oC
4
0.1g/l
0.2g/l
3
0.3g/l
2
0.4g/l
1
0.5g/l
0
0
5
10
15
20
time (mins)
volume of hydrogen evolume (cm 3 )

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 30 o C

J. Atoms and Molecules / 3(2); 2013 / 509–519

Iloamaeke IM et al

50 40 blank 30 0.1g/l 0.2g/l 20 0.3g/l 10 0.4g/l 0 0.5g/l 0 5 10
50
40
blank
30
0.1g/l
0.2g/l
20
0.3g/l
10
0.4g/l
0
0.5g/l
0
5
10
15
Time (mins)
Volume of hydrogen evolved
3 )
(cm

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 60 o C

50 40 blank at 60oC 60 O C 30 0.1g/l 20 0.2g/l 0.3g/l 10 0.4g/l
50
40
blank at 60oC
60
O
C
30
0.1g/l
20
0.2g/l
0.3g/l
10
0.4g/l
0
0.5g/l
0
5
10
15
Time (mins)
Volume of hydrogen
evolved (cm 3)

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 60 o C.

Table 2: Shows the concentration of the VD and PS extract and inhibition efficiencies at 30 o C and 60 o C from gasometric method.

Concentration of the inhibitors in(g/l)

Inhibition efficiency (%) from VD extract at

Inhibition efficiency (%) from PS extract at

 

30 o C

60 o C

30 o C

60 o C

0.1

23.51

21.11

50.64

47.41

0.2

38.35

30.20

60.16

57.03

0.3

45.13

38.39

62.08

58.96

0.4

51.06

42.29

68.22

64.25

0.5

68.22

54.98

69.28

67.80

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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/θ = C +1/k

(6)

Taking the logarithm of equation 6, equation 7 is obtained

Log C/θ = log C – log K

(7)

Where C is the concentration of the inhibitor in the electrolyte, θ is the degree of surface coverage of the inhibitor and k is the equilibrium constant of adsorption.

The plot of C/ θ 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(-2aθ) = kC

(8)

Where “a” is the Tempkin interaction parameter, θ 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.

θ = .

-

.

Slope=

.

, while intercept =

(9)

.

Fig.6 and 7: Shows plot of θ 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 Freundlich’s 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)

= kc 1/n

(10)

Log

= log k +

log c

(11)

The fraction 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 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 y = 1.464x + 0.3462 R² = 0.994 1 0.8 y = 1.025x
2008c)
1.2
y = 1.464x + 0.3462
R² = 0.994
1
0.8
y = 1.025x + 0.3323
0.6
R² = 0.9616
30oC
0.4
60oC
0.2
0
0
0.2
0.4
0.6
C
C/θ

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

J. Atoms and Molecules / 3(2); 2013 / 509–519

Iloamaeke IM et al

0.8 0.7 y = 0.5714x + 0.7864 R² = 0.9203 0.6 0.5 30oC 0.4 60oC
0.8
0.7
y = 0.5714x + 0.7864
R² = 0.9203
0.6
0.5
30oC
0.4
60oC
y = 0.3708x + 0.5746
R² = 0.9927
0.3
0.2
0.1
0
-1.2
-1
-0.8
-0.6
-0.4
-0.2
0
logC
θ

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

y = 0.2683x + 0.7775 R² = 0.9752 0.8 0.7 0.6 y = 0.28x +
y = 0.2683x + 0.7775
R² = 0.9752
0.8
0.7
0.6
y = 0.28x + 0.7546
R² = 0.979
0.5
0.4
30oC
0.3
60oC
0.2
0.1
0
-1.2
-1
-0.8
-0.6
-0.4
-0.2
0
logC
θ

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

1.86 y = 0.1964x + 1.9049 R² = 0.9743 1.84 1.82 1.8 1.78 1.76 30oC
1.86
y = 0.1964x + 1.9049
R² = 0.9743
1.84
1.82
1.8
1.78
1.76
30oC
y = 0.2137x + 1.8932
R² = 0.9807
1.74
1.72
60oC
1.7
1.68
1.66
-1.2
-1
-0.8
-0.6
-0.4
-0.2
0
logC
log I%

Fig.8: Freundlich isotherm for the adsorption of PS extract on the surface of the mild steel.

J. Atoms and Molecules / 3(2); 2013 / 509–519

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Thermodynamics Studies

The value of activation energy Ea was calculated using Arrhenius equation.

Log

=

. ( -

)

(12)

Where H R1 and H R2 are the hydrogen evolution rate at temperature T 1 and T 2 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

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 ΔH ads . The values of heat of adsorption were calculated using equation (13). (Quraish et al., 2009; Okafor et al., 2010; Eddy et al., 2008).

ΔH ads = 2.303R [log (

) – log (

)] x

(13)

Where θ 1 and θ 2 are degree of surface coverage at temperatures T 1 and T 2 respectively. Table 3: enumerated the values of ΔH ads at different concentrations of inhibitors. ΔH ads 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 (R 2 ) 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 (ΔG ads ) according to equation 14

ΔG ads = -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 ΔG ads according to equation 14 and the result in Table 4 and 5.

From the result, ΔG ads 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 ΔH for VD and PS extract at different concentrations

Concentration of VD and PS inhibitor in g/l.

Ea from VD inhibitor in KJ/mol

Ea from PS inhibitor in KJ/mol

ΔH from VD inhibitor in KJ/mol

ΔH from PS inhibitor in KJ/mol

Blank

54.19

54.19

-------

-------

0.1

31.18

64.30

-3.88

-3.63

0.2

41.24

58.76

-10.39

-3.69

0.3

36.38

59.95

-7.72

-3.65

0.4

38.30

59.69

-9.91

-3.70

0.5

37.42

59.09

-17.05

-1.94

J. Atoms and Molecules / 3(2); 2013 / 509–519

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

(

o C)

Log k

Slope

ΔG (KJ/mol)

R 2

 

Langmuir

 

30

0.4785

1.0250

-7.3444

0.9616

 

60

0.4606

1.4640

-8.1840

0.9940

 

Tempkin

a

 

30

1.3764

-2.0151

-9.5141

0.9203

 

60

1.5410

-3.1050

-9.5870

0.9927

Table 5: Freundlich and Tempkin adsorption isotherm parameters for adsorption of PS extract on the surface of the mild steel.

Temperature

(

o C)

Log k

Slope

ΔG (KJ/mol)

R 2

 

Freundlich

 

30

1.9049

0.1964

-11.743

0.9743

 

60

1.8932

0.2137

-12.889

0.9807

 

Tempkin

a

 

30

0.1573

-0.2330

-9.4860

0.9752

 

60

0.1594

-0.2432

-10.3420

0.9790

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.

The mechanism of physical adsorption was proposed from the calculated values of Ea, ΔH ads , and ΔG ads, obtained.

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