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H O S T E D BY

Alexandria University

www.elsevier.com/locate/aej

www.sciencedirect.com

SHORT COMMUNICATION

a Tafel region using Excel spreadsheets

Marco Alfaro

Departamento de Quı´mica, Campus Andre´s Bello, Facultad de Ciencias, Universidad de La Serena, Colina el Pino S/N, La

Serena, Chile

Available online 4 August 2014

KEYWORDS Abstract This paper describes the modeling of polarization curves not exhibiting a Tafel region

Lineal voltammetry; using Excel spreadsheets. Carbon steel in aerated NaCl unbuffered solutions was studied applying

Steel corrosion rate; a linear potential sweep technique. Current–potential curves were obtained from linear potential

Sodium chloride solution; sweep at a rate of 10 mV s1 in un-buffered 0.1, 0.4 and 0.9 M NaCl solutions, at a constant

Excel spreadsheet temperature of 25 C and potential sweeps that were conducted in a potential range 1.0 to

0.4 V vs. Ag/AgCl.

ª 2014 Production and hosting by Elsevier B.V. on behalf of Faculty of Engineering, Alexandria

University.

kinetic models have been reported, but the ﬁt of these models

The determination of the corrosion rate of steel is generally to the experimental data requires the development of computa-

conducted by using the extrapolation Tafel method from a tional programs [9,10]. An alternative method is by using the

potentiodynamic polarization curve of the metal in aqueous solver function in Excel for the ﬁtting of nonlinear functions

solution [1–4], but this method requires the preference that along with the nonlinear least squares method, which

the anodic and cathodic branches present Tafelian behavior minimizes the sum of the squared differences between the

[5]. Another method used to determine the corrosion rate from experimental values and the predicted by the model, and it

polarization curves with exclusive activation control for both has already been successfully used in electrochemical

anodic and cathodic branches is the adjustment of the Wagner kinetics [11]. The objective of this work was modeling of polar-

and Traud equation to the curve using a nonlinear least ization curves not exhibiting a Tafel region using Excel

squares method [6,7]. Much modern equipment give the corro- spreadsheets.

sion rate by using this method but do not provide any informa-

2. Materials and methods

tion about the goodness of ﬁtting the experimental data to the

polarization curve in case where clearly the curves do not

present Tafel region [8]. Moreover, several investigations that 2.1. Experimental

Peer review under responsibility of Faculty of Engineering, Alexandria electrode cell, where the working electrode was made of carbon

University. steel with a 4 mm diameter and an exposed area of 0.5027 cm2,

http://dx.doi.org/10.1016/j.aej.2014.07.005

1110-0168 ª 2014 Production and hosting by Elsevier B.V. on behalf of Faculty of Engineering, Alexandria University.

978 M. Alfaro

a platinum wire as a counter electrode and Ag/AgCl in 1 M the corrosion potential, obtained directly from the experimen-

KCl cell as a reference electrode. The composition of carbon tal polarization curve and electrochemical parameters of the

steel was SAE 1008 with chemical content wt% 98.5 Fe, 0.02 cathodic reaction for the reduction of oxygen under zero total

C, 0.15 Mn and traces of P, S, Si and Cr. The cell was current (it = 0) condition. The corrosion rate, it can be

immersed in a thermostatic Haake D1 bath operating at calculated using the expression given by Khaled and Amin

25 C. Measurements were conducted in water before air was [8] Eq. (4).

bubbled for about 15 min; air was bubbled into the water by CR ¼ 3; 28 icorr ðM=ndÞ ð4Þ

using a small ﬁsh-tank pump, this water was used to prepare

the test solutions. A PG 580 (Princeton Instrument) potentio- where CR is the corrosion rate (mm y1), M is the atomic

stat was employed with the software of the same company. weight of iron (55.85), n is the number of electrons transferred

Polarization curves were obtained from linear potential sweep in the corrosion reaction (2 in this case) and d is the density of

at a rate of 10 mV s1. Potential sweeps were conducted in the iron (7,88 g cm3).

potential range 700 to 100 mV/SHE in 0.1, 0.4 and 0.9 M

NaCl un-buffered solution. Unbuffered solutions were used 2.3. Adjustment of the kinetic model to the experimental data

to prevent adsorption of the buffer compounds and their com-

plexes on the surface of metal [12], because the Caceres model In this case in order to adjust Caceres model [13] to the exper-

does not evaluate compound adsorption effect. imental polarization curve a nonlinear least squares method

was used. This is an iterative method that estimates the mini-

2.2. Kinetic model mum of the function (SS), Eq. (5), via Excel solver function

[15].

The kinetic model chosen for this study was developed by and X N !2

i i

Caceres et al. [13], which uses the superposition model SS ¼ wi ð5Þ

proposed by Wagner and Traud in 1938 [14], method that con- i¼1

A exp A pred

siders that the total current density (it) is the algebraic sum of

where (i/A)exp is the experimental current density, (i/A)ﬁt is

the anodic (ia) and cathodic (ic) current, which is:

the current density predicted by the model and wi is a weight

h i

io;O2 exp 2:3

EEeq;O2 function, designed to improve the ﬁt, which in this case is

tc

ic ¼ h i ð1Þ deﬁned by Eq. (6), as [16].

i 2 EEeq;O2

1 þ io;Ol;O2

exp 2:3 tc 1

wi ¼ ð6Þ

E Eeq;Fe s2

ia ¼ io;Fe exp 2:3 ð2Þ

ta where s is the standard deviation of the data predicted, deﬁned

h i

EE

io;O2 exp 2:3ð tceq;O2 Þ by the Eq. (7) as:

E Eeq;Fe

it ¼ h i þ io;Fe exp 2:3 ð3Þ vﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃ

i 2 EEeq;O2 ta uX

1 þ io;O exp 2:3 tc u N i

i

2

l;O

2

u

t A Average;fit A i;fit

where iL,O2 (A cm2) is the limiting current density for oxygen s¼ i¼1

ð7Þ

reduction, io,O2 (A cm2) is the exchanged current density for N1

oxygen, Eeq,O2 (V) is the potential balance for oxygen reduc- where (i/A)Average, ﬁt is the average of the predicted current

tion, tc, is the pseudo Tafel slope for oxygen reduction,. io,Fe, density, (i/A)I, ﬁt is the current density of each point and N is

is the exchange current density for iron, Eeq,Fe is the potential the total number of points. The goodness of ﬁt of the data to

balance for iron and ta is the pseudo anodic Tafel slope. Cor- the model will be evaluated by using the regression coefﬁcient

rosion intensity (icorr) can be calculated from Eq. (3) by using (R2) [15]. The sum of squared errors (SSE), the root mean

Excel cell Formula Excel programming

B2 SHE = Ag/AgCl + 0,237 =A2 + 0,237

D2 i = I/A =C2/0.5027

E2 |i| =ABS(D2)

F2 Log i =LOG(E2)

EEeqO2

G2 ¼ i0O2 exp 2:3 tc =$M$1 * (EXP(2,3 * (B2 0,762)/$M$2))

i 2 EEeqO2

H2 ¼ 1 þ i0O lO2

exp 2:3 tc =1 + (($M$1/$M$3) * (EXP(2,3 * (B2 0,762)/$M$2)))

EEeqO

I2 ¼ 2 t

c

EEeqO

=G2/H2

i0 O2 2

1þ exp 2:3

ilO

2 tc

EEeq;Fe

J2 ¼ io;Fe exp 2:3 ta =$M$4 * (EXP(2,3 * (B2+0,614)/$M$5))

EEeq;O

io;O2 exp 2:3 2

EEeq;Fe

K2 ¼ c

EE

t

þ io;Fe exp 2:3 ta =G2 + H2

io;O eq;O

1þ 2 exp 2:3 2

il;O tc

2

P2 =((K2 D2)^2)/($K$94^2)

K94 =STDEVA(K2:K93)

Modeling of polarization curves not exhibiting a Tafel region 979

2 3

square error (RMSE) and chi-square (v2) [17], which compares XN !2 !=2

1 i i

the values of experimental current density (i/A)exp with those RMSE ¼ 4 5 ð10Þ

predicted by the model (i/A)pred and R2 that include the N i¼1

A exp A fit

experimental average current density (i/A)ave,exp.

N

X i

i

2

N

X i

i

2 A exp

A fit

i¼1

A exp A fit v2 ¼ ð11Þ

R2 ¼ 1 i¼1

ð8Þ Nz

N

X 2

i

i

A exp

A ave; exp

i¼1 2.4. Construction of the Excel spreadsheet

!2

1X N

i i To construct the Excel spreadsheet, the indications given in

SSE ¼ ð9Þ Table 1 and Figs. 1–3 must be followed. Once the spreadsheet

N i¼1 A exp A fit

is built, the solver function of Excel has to be installed by

980 M. Alfaro

following the procedure described by Brow [15]. Once 2.5. Sensitivity analysis of corrosion rate prediction Caceres

installed, its mode of execution is as follows: model

1. The option Data has to be clicked and then a dialog Parameters considered in the sensibility analysis for the corro-

box of the solver function of Excel should appear as sion rate prediction Caceres model are listed in Table 3. The

follows. sensibility parameter, S is given by:

2. The set target cell has to be marked, in this case the cell ½ðO2 O1 Þ=O12

S¼ ð12Þ

marked is $M$7. ½ðI2 I1 Þ=I12

3. Then Min has to be marked.

where I1 and I2 are the least and greatest values of input used,

4. After marking Min the cells that are marked are

respectively. I12 is the average of I1 and I2. O1 and O2 are the

$M$1:$M$5, these are the cells of the kinetic constants of

output for the two input values, and O12 is the average of the

Caceres model (Eq. (3)) and the ones that solver will change

two outputs [18,19].

to minimize the function SS (Eq. (5)).

5. Finally with this data, the spreadsheet shown in Fig. 4 is

3. Results and discussions

created, and replacing the experimental corrosion potential

value therein, icorr is obtained for the condition where the

total current is approximately zero, i.e. iﬁt = 0.001 and with Figs. 5–7 show the correlation of polarization curves of carbon

this the corrosion rate. steel in un-buffered 0.1, 0.4 and 0.9 M NaCl solutions, at a

Modeling of polarization curves not exhibiting a Tafel region 981

Figure 4 Excel spreadsheet showing the calculation of the corrosion rate from experimental corrosion potential, the electrochemical

parameters and the condition that the total current density is approximately zero (it = 0.001).

-0,1

-0,1

Experimental

-0,2 Caceres Model Experimental

-0,2

Caceres Model

-0,3

-0,3

E (V vs. SHE)

-0,4

E (V vs. SHE)

-0,4

-0,5 -0,5

-0,6 -0,6

-0,7 -0,7

-0,8 -0,8

-5,0 -4,5 -4,0 -3,5 -3,0 -2,5 -5,0 -4,5 -4,0 -3,5 -3,0 -2,5

-2 -2

Log (i/A) A cm Log (i/A) A cm

Figure 5 Experimental polarization curve (X) for carbon steel in Figure 6 Experimental polarization curve (X) for carbon steel in

aerated 0.1 M NaCl solution un-buffered and ﬁtted curve (con- aerated 0.4 M NaCl solution un-buffered and ﬁtted curve (con-

tinuous line) calculated from the Caceres model using Excel tinuous line) calculated from the Caceres model using Excel

spreadsheet. spreadsheet.

using excel spreadsheets to predict the total current density. 4. Conclusions

It can be appreciated that both, anodic and cathodic branches

of both curves do not present Tafel region and that the hydro- i. The experimental polarization curve was obtained from

gen evolution reaction is almost negligible. The Table 2 shows a stationary electrode of carbon steel in un-buffered 0.1,

the values of the electrochemical parameters, the corrosion 0.4 and 0.9 M NaCl solutions, at a constant temperature

rate and the statisticians to evaluate the quality of ﬁt of the of 25 C.

kinetic model of Caceres. The Fig. 8 shows that a higher molar ii. The superposition Wagner and Traud model was used to

concentration of NaCl to a higher corrosion rate. The results obtain the total current as an algebraic sum of the ano-

from sensitivity index analysis are summarized in Table 3. dic and cathodic currents.

Limiting current density for oxygen reduction, with the aver- iii. The nonlinear least squares method and the solver func-

age index value of 1.65, is the critical input parameter in Các- tion of Excel were used to calculate the electrochemical

eres model. parameters of a kinetic model.

982 M. Alfaro

-0,1

Table 3 Caceres model parameter values used for sensibility

Experimental analysis and parameter S.

-0,2

Caceres Model Parameter Base value Range of test S

-0,3 0.1 M NaCl

io,O2 8.84 * 104 1.0 * 104–1.77 * 103 1.03

E (V vs. SHE)

iL,O2 0.02 0.04–0.1 1.63

io,O2 1.48 * 103 1.0 * 104–2.96 * 103 0.94

-0,6

tc,O2 4.32 0.9–8.64 0.94

iL,O2 0.6 1.0 * 103–1.2 1.73

io,O2 9.53 * 104 1.0 * 104–1.91 * 103 1.00

tc,O2 2.00 0.1–4.00 0.96

-0,8

iL,O2 0.3 1.0 * 103–0.6 1.58

-4,5 -4,0 -3,5 -3,0 -2,5

-2

Log (i/A) A cm iv. An excel spreadsheet was developed that allowed the

determination of the corrosion rate from polarization

Figure 7 Experimental polarization curve (X) for carbon steel in curves that do not present Tafel region.

aerated 0.9 M NaCl solution un-buffered and ﬁtted curve (con- v. The limiting current density for oxygen reduction is the

tinuous line) calculated from the Caceres model using Excel critical input parameter in Cáceres model.

spreadsheet.

Acknowledgments

Table 2 Electrochemical parameters, corrosion rate and

statistical parameters of ﬁt of polarization curves. The generous support of the FAU (Universidad Friedrich-

Electrochemical parameters 0.1 M NaCl 0.4 M NaCl 0.9 M NaCl Alexander of Erlangen-Nuremberg, in Germany, Friedrich-

io,O2 (A cm2) 8.84 * 104 1.48 * 103 9.53 * 104 Alexander-Universität Erlangen-Nürnberg, shortened FAU)

tc,O2 (V dec1) 2.04 4.32 2.00 Germany. Project of Cooperation Universidad de Erlanger

iL,O2 (A cm2) 0.02 0.6 0.3 Universidad de La Serena, Chile is gratefully appreciated.

io,Fe (A cm2) 1.10 * 103 1.48 * 103 2.09 * 103 Thanks to Prof. Dr. Ulrich Nickel for all those encouraging

ta,Fe (V dec1) 0.96 1.23 1.14 discussions.

Ecorr (V) 0.283 0.403 0.359

icorr (A cm2) 2.41 * 103 2.74 * 103 3.41 * 103

CR (mm y1) 2.80 * 102 3.19 * 102 3.97 * 102

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