3 Facteur C T Et E 2018

Materials Research Express
ACCEPTED MANUSCRIPT
Constitutive modeling for prediction of optimal process parameters in

corrosion inhibition of austenitic stainless steel (Type 316) /acidic
medium
To cite this article before publication: Omotayo Sanni et al 2018 Mater. Res. Express in press https://doi.org/10.1088/2053-1591/aad98f
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Page 1 of 28 AUTHOR SUBMITTED MANUSCRIPT - MRX2-100899.R2
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3 CONSTITUTIVE MODELING FOR PREDICTION OF OPTIMAL PROCESS
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5 PARAMETERS IN CORROSION INHIBITION OF AUSTENITIC STAINLESS STEEL
6 (TYPE 316) /ACIDIC MEDIUM
7 SANNI, O., POPOOLA, A.P.I. and KOLESNIKOV, A
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Tshwane University of Technology, Department of Chemical, Metallurgical and
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10 Materials Engineering, Pretoria, South Africa
11 Corresponding author: tayo.sanni@yahoo.com
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ABSTRACT
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16 Corrosion is a major concern in the industrial application of ferrous alloys due to
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18 enormous cost involved in damages, maintenance and corrosion control. Material
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20 scientists increasingly use statistical methods to speed up material design, due to the
21 need for several process parameters in corrosion inhibition method. This study focuses
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on optimization of three main contributing parameters; inhibitor concentration, exposure
time and temperature on the austenitic stainless steel (SS) Type 316 corrosion inhibited
through a novel eco-friendly waste material. Response surface method (RSM) was used
for evaluation of experimental process variables influencing SS corrosion. The effect of
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30 changes in the level of these variables on stainless steel corrosion was studied using
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32 Box Behnken design. The optimum levels of process parameters were studied using
33 quadratic regression model coupled with desirability approach. The relationship
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35 between predicted and experimental values shows the accuracy of the developed
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37 model. Morphologies of the corroded surfaces are examined via scanning electron
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microscope equipped with energy dispersive X-ray spectroscopy (SEM/EDX). The study
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40 showed that RSM is an effective statistical method to predict optimum operating
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42 parameters of the inhibitor studied in acid solution required to reduce corrosion rate of
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44 stainless steel.
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46
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47 Keywords: Inhibition, Stainless steel, Response surface method, Corrosion rate,

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49 Optimization, Morphology
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AUTHOR SUBMITTED MANUSCRIPT - MRX2-100899.R2 Page 2 of 28
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INTRODUCTION
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8 Stainless steel posses an excellent corrosion resistance in environments where carbon
9 steels and other engineering metals cannot withstand due to the presence of high
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11 chromium contents and other alloying elements. However, stainless steel is not
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13 impermeable to degradation in acidic environments which is a fundamental industrial
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and academic concern as a result of failure of material components in this environment
16 [1-6]. Various methods used in preventing corrosion includes; painting, material
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18 selection, anodic and cathodic protection, lubrication and application of inhibitor [7].
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20 Corrosion inhibitor is a globally accepted method owing to its tendency to decrease
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corrosion rate in corrosive environment, low cost and easy application [8]. The use of
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organic and inorganic substances has been proved by many researchers to inhibit
corrosion of metals [8-21], but recently many inorganic inhibitors has been found to be
toxic, expensive and scarce [21] which limits their use. Efforts have been made to
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replace these inhibitors with eco-friendly, cheap and non-toxic inhibitors [8, 20-23]. The
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30 conventional method of performing experiments is fast becoming out-dated because it
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32 involves varying one variable at a time while having other variables fixed at specific
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34
conditions. In recent time, egg shell powder has been studied by our research group
35 [21] as corrosion inhibitor, and has been found efficient in acidic environment but the
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37 use of response surface method on stainless steel Type 316 to evaluate the inhibitory
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effects of egg shell powder statistically to the best of our knowledge has not been
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reported which call for this work. Previous efforts have been made towards modeling of
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42 pitting corrosion which was reviewed by [24]. The limitation of these models was later
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44 observed by [25]. Mechanistically-based and atomistic models using partial differential
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46 equations and theoretical principles was tried to further tackle this drawback [26-29].
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47 Recently, progress in computational competences has facilitated the simulation of

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49 pitting corrosion via new modeling standards; Monte Carlo [30, 31], artificial neural
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51 networks [32, 33] and response surface methodology [34-45]. From the above literature,
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it is clear that no research have been carried out to study the effect of process
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54 parameters on the use of inhibition tendency of egg shell powder for stainless steel
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56 corrosion. As a result, this study examines the influence of corrosion inhibitor, exposure
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3 time and temperature on the inhibitory effectiveness of egg shell powder on stainless
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5 steel corrosion. Box-behnken design was used to study empirical model and parametric
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7 analysis of the process. Process parameters interaction was investigated with response
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surface method and optimized using desirability approach. Scanning electron
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10 microscope was employed to examine stainless steel surface morphology.
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14 2. EXPERIMENTAL PROCEDURES
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Experiments are conducted using stainless steel (Type 316) sample rectangular shape
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17 of 10mm diameter cut into size 2 mm x 2 mm x 1 mm specimens for corrosion tests
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19 according to [21]. After cutting, the specimens used for the corrosion tests were de-
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21 scaled by wire brush, ground using different grades of emery paper and followed by
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polishing. To remove any corrosion products, the specimens were further rinsed in de-
ionized water and cleaned with acetone. The samples were kept in a desiccator in order
to prevent it from been further exposed to atmospheric moisture. The prepared
specimens were suspended using a thread in beakers containing 250 ml of 0.5 molar
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29 sulphuric acid in the absence and presence of egg shell powder with varying
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31 concentrations (2, 4, 6, 8 and 10 g). Each specimen after corrosion test was rinsed with
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33 de-ionized water, put in methanol solution to remove remaining acid residual and
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inhibitor. Rinse again using de-ionized water and then dried in acetone prior to reweigh.
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38 2.1 Materials
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40 Table 1 Chemical composition of studied stainless steel Type 316 (wt%)
41 Element C S P Mn Si Cr Ni Mo N
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43 Composition 0.030 0.030 0.045 2.000 0.750 18.000 14.000 3.000 0.100
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18 Figure 1 Chemical structure of egg shell powder
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41 Figure 2 Microstructure of raw egg shell powder
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Figure 3 EDX of the raw egg shell powder
Table 2 Properties of the egg shell powder

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Chemical Constituents Percentage composition Wt(%)
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30 C 37.3
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32 O 35.7
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Ca 25.6
35 K 0.8
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37 Cl 0.4
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S 0.3
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Mg 0.3
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42 Na 0.2
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44 P 0.1
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46 Si 0.1
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3 2.2 Inhibitor efficiency determination
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5 For the weight loss experiment, cleaned weighed stainless steel samples with a hole of
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7 1 mm diameter drilled at the centre were completely immersed in a 250 ml beaker
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containing the inhibitor and 0.5M H2SO4 with the aid of hooks and glass rod. After a
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10 period of time, the test samples were taken out of the test solution, scrubbed with bristle
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12 brush, thoroughly washed with distilled water, dried in acetone and weighed. The weight
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14 loss, corrosion rate and inhibitor efficiency were determined. The tests without inhibitor
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were carried out for comparison with the tests with inhibitor. The difference between the
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17 initial weight and final weight of the samples were determined using the equation below;
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19 W = WO − WF DDDDD.. (1)
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21 Where :
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W = weight loss (mg )
WO = initial weight (mg )
WF = final weight (mg )
 87.6W 
Corrosionrate(CR) =  
an (2)
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29  DAT  DDDDDDDDDDDDDDDDDDDD.
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31 Where :
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W = weight loss (mg )
34 D = specimen density ( g / cm3 )
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36 A = specimen area (cm2 )
37 T = exp osure time (h)
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39 The percentage inhibition efficiency (% IE ) of egg shell used as inhibitor in the solution
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41 was calculated using the relationship:
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43 CR o − CR 100
44 IE (%) = x (3)
CR o 1 DDDDDDDDDDDDDDDDDDD.
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Where CR and CR O are corrosion rates of the stainless steel in the presence and
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49 absence of inhibitor respectively in the corrosive medium (0.5 M H2SO4).
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3 2.3 Experimental design using response surface method (RSM)
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5 RSM is a statistical model technique used for multiple regression analysis in which
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7 quantitative data are acquired from experimental design [15]. This method is useful in
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optimizing complex procedures by reducing experimental number trails in order to
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10 assess several independent variables plus their interactions. Design expert software
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12 version 6.0.8 (Stat-Ease Inc., Minneapolis, USA) was utilized in this study. It has the
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14 profound ability to optimize the response function and predict future responses after it
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has developed a regression model statistically from appropriate experimental data. It
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17 has been widely reported that inhibitor concentration, exposure time and temperature
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19 are significant factors affecting corrosion of metals. RSM was used in this study to
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21 examine the simultaneous effects of the independent variables (inhibitor temperature,
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exposure time and temperature) on stainless steel corrosion in H2SO4 environment as
previously studied experimentally by our research group [21]. Process parameters used
in this study are inhibitor concentration, exposure time and temperature. The
experimental set up was supported by box behnken design (BBD) [16] at different levels
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29 – 1 (low), 0 (mid) and + 1(high) (as shown in Table 3). The coding of variables follows
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31 equation 4.
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33 Xi − Xo
xi =
34 ∆X
35 DDDDDDDDDDDDDDDDDDDDDDDDDDD(4)
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37 xi = dimensionless value
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Xi = real value
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Xo = real value of an independent variable at the centre point
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42 ∆X = step change value of the variable
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46 The number of experiments for BBD follows equation 5
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47 N = 2k (k − 1) + Co DDDDDDDDDDDDDDDDDDDDDDDD(5)
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49 k = number of factors and C number of central point
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2.4 Third-order regression model
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54 Response surface method was used to develop mathematical models in the form of
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56 multiple regression equations for corrosion of stainless steel Type 316. The main
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3 interaction effects of all possible factor combinations have been estimated. Third-order
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5 polynomial equation was applied to develop regression equations related to the
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7 corrosion process to fit the experimental data.
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9 Y = β o + β A A + β B B + β C C + β D D + β AA A 2 + β BB B 2 + β CC C 2 + β DD D 2 + β AB AB + β AC AC + β AD AD
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10 + β BC BC + β BD BD + β CD CD + β AAA A 3 + β BBB B 3 + β CCC C 3 + β DDD D 3 + β AAB A 2 B + β AAC A 2 C
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12 + β AAD A 2 D + β ABB AB 2 + β ACC AC 2 + β ADD AD 2 + β ABB AB 2 + β BCC B 2 C + β BBD B 2 D + β BCC BC 2
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14 + β BDD BD 2 + β CCD C 2 D + β CDD CD 2 + β ABC ABC + β ABD ABD
15 + β ACD ACD + β BCD BCD
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19 DDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDD(6)
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21 Y is fitted response
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βo is offset term
βA, βB, βC, βD is linear effect terms
βAA, βBB, βCC, βDD is squared effect
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βAB, βAC, βAD, βBC, βBD, βAAB, βAAC, βAAD, βABB, βACC, βADD, βABB, βBCC is interaction
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30 βBBD, βBCC, βBDD, βCCD, βCDD, βABC, βABD, βACD, βBCD is effects
31 βAAA, βBBB, βCCC, βDDD is cubed effect
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35 2.5 Variable coding
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Response plots and analysis of variance was used to analyze the results. Experimental
38 data sets of 17 runs were used as design points for the modeling (as shown in Table 4).
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40 The three factors; inhibitor concentration, exposure time and temperature indicate the
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42 conditions of the acid environment with their low, mid and high values set with respect
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to experimental data sets range. The operational parameters, response and
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45 experimental range are tabulated in Table 4. The experimental design of the operational
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47 parameters with the observed values for the response is also depicted in Table 4.
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50 3 RESULTS AND DISCUSSION
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52 The presence of different components of egg shell powder given in Table 2 enhanced
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54 the inhibiting process of stainless steel. This verdict was in agreement with previous
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report [21]. Calcium, carbon and oxygen molecules contained in egg shell powder are
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3 found to inhibit stainless steel by forming a protective layer on its surface thereby
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5 preventing the steel corrosion.
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8 3.1 Regression model fitting for weight loss, corrosion rate and inhibition
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10 efficiency
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A regression model was obtained for the response data (weight loss, corrosion rate and
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13 inhibition efficiency) from the historical data design of RSM used, which recommended
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15 a third-order polynomial model fitted to the response data. The model is a modified
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17 cubic model obtained by manual reduction and simplification of the model which
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20 actual factors as shown in Equations 7 to 9.
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ܹ‫ = ܮ‬2.2 − 1.23 ∗ ‫ ܣ‬+ 1.92 ∗ ‫ ܤ‬+ 0.18 ∗ ‫ ܥ‬− 0.24 ∗ ‫ܣ‬ଶ + 0.21 ∗ ‫ܤ‬ଶ + 0.16 ∗ ‫ ܥ‬ଶ − 0.73 ∗ ‫ ܤܣ‬−
0.025 ∗ ‫ ܥܣ‬+ 0.025 ∗ ‫ ܥܤ‬− 0.7 ∗ ‫ܣ‬ଶ ‫ ܤ‬+ 0.05 ∗ ‫ܣ‬ଶ ‫ ܥ‬− 0.15 ∗ ‫ܤܣ‬ଶ DDDDDDDDD(7)
‫ = ܴܥ‬0.17 − 0.093 ∗ ‫ ܣ‬− 0.004414 ∗ ‫ ܤ‬+ 0.10 ∗ ‫ ܥ‬+ 0.022 ∗ ‫ܣ‬ଶ + 0.029 ∗ ‫ܤ‬ଶ − 0.037 ∗ ‫ ܥ‬ଶ − 0.053 ∗
‫ ܤܣ‬− 0.001323 ∗ ‫ ܥܣ‬+ 0.048 ∗ ‫ ܥܤ‬− 0.066 ∗ ‫ܣ‬ଶ ‫ ܤ‬+ 0.088 ∗ ‫ܣ‬ଶ ‫ ܥ‬− 0.015 ∗ ‫ܤܣ‬ଶ DDDD(8)
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32 ‫ = ܧܫ‬72.15 + 15.35 ∗ ‫ ܣ‬− 16.57 ∗ ‫ ܤ‬− 1.33 ∗ ‫ ܥ‬+ 2.37 ∗ ‫ܣ‬ଶ − 0.19 ∗ ‫ܤ‬ଶ − 0.11 ∗ ‫ ܥ‬ଶ + 5.01 ∗ ‫ ܤܣ‬−
33 0.31 ∗ ‫ ܥܣ‬− 0.82 ∗ ‫ ܥܤ‬+ 7.55 ∗ ‫ܣ‬ଶ ‫ ܤ‬− 0.14 ∗ ‫ܣ‬ଶ ‫ ܥ‬+ 1.06 ∗ ‫ܤܣ‬ଶ ……………………………(9)
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38 Multiple regression analysis method was used to obtain the coefficients of the empirical
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40 model. The model coefficients with positive sign represent synergistic effect, while
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42 negative sign represents antagonistic effect. A, B, C, A2, B2, C2, AB, AC, BC, A2B,
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44 A2C, AB2 are found to be the significant model terms.
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49 ANOVA was another statistical parameter used in analyzing model adequacy. ANOVA
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51 results for the model in Equations (7 to 9) are tabulated in Table 5. The p-value (Prob>
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F) of < 0.0001 for the model indicates that the model is significant. As can be observed
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54 in Table 5, thirteen (13) of the seventeen (17) p-values of the model are less than 0.05,
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56 signifying that about 76.47% of the model parameters are significant. As earlier stated,
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3 majority of the insignificant terms were purposely eliminated for improvement of model
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5 performance.
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9 Table 3 Central composite design factor levels of independent variables
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11 Independent Unit level
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13 variables
14 Low factor Mid-point High factor
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16 level (-1) factor level level (+1)
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18 (0)
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20 Inhibitor (g) 2 6 10
21 concentration
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Exposure time
Temperature
(Hour)
(oC) an
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168
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29 Table 4 Experimental design of the independent variables with the observed values for
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32 Response
33 Factor 1 Factor 2 Factor 3 1 Response 2 Response 3
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A:Conc B:Time C:Temp Wt loss Corrosion rate
36 Std Run (g) (Hours) (oC) (mg) (mm/yr) IE (%)
37 8 1 10 96 35 1.1 0.071372 86.99
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9 2 6 24 15 0.5 0.013386 87.92
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40 10 3 6 168 15 4.3 0.100815 56.43
41 1 4 2 24 25 1.6 0.485453 71.93
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4 5 10 168 25 1.3 0.056347 86.73
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44 3 6 2 168 25 5.5 0.238392 43.88
45 13 7 6 96 25 2.2 0.166874 72.15
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17 8 6 96 25 2.2 0.166874 72.15
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48 15 9 6 96 25 2.2 0.166874 72.15
49 14 10 6 96 25 2.2 0.166874 72.15
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51 2 11 10 24 25 0.3 0.091022 94.74
52 11 12 6 24 35 0.8 0.313496 86.91
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55 12 14 6 168 35 4.7 0.208412 52.13
56 16 15 6 96 25 2.2 0.166874 72.15
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6 16 10 96 15 0.7 0.046364 90.53
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5 7 17 2 96 35 3.6 0.260713 56.9
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8 Table 5 ANOVA for response surface reduced cubic model
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Sum of Mean F
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12 Source Squares DF Square Value Prob > F
13 Model 37.34 12 3.11 6.37E+07 < 0.0001 significant
14 A 6 1 6 6.37E+07 < 0.0001 significant
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16 B 14.82 1 14.82 6.37E+07 < 0.0001 significant
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17 C 0.12 1 0.12 6.37E+07 < 0.0001 significant
18 A2 0.24 1 0.24 6.37E+07 < 0.0001 significant
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B2 0.19 1 0.19 6.37E+07 < 0.0001 Significant
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21 C2 0.11 1 0.11 6.37E+07 < 0.0001 Significant
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AB
AC
BC
A2B
A2C
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2.50E-03
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2.1 6.37E+07 < 0.0001
2.50E-03 6.37E+07 < 0.0001
2.50E-03 6.37E+07 < 0.0001
0.98 6.37E+07 < 0.0001
5.00E-03 6.37E+07 < 0.0001
Significant
Significant
Significant
Significant
Significant
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AB2 0.045 1 0.045 6.37E+07 < 0.0001 significant
30 Pure Error 0 4 0
31 Cor Total 37.34 16
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According to the model, all the operational parameters have been identified as
36 significant terms and as such influence the response. Therefore, it is proven statistically
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38 that the corrosion rate of stainless steel is dependent on the operational parameters:
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40 inhibitor concentration, exposure time and temperature based on the frequency of
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occurrence of each parameter in the model.
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45 3.3 Factor plots
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The behavior of the effect of each of the three variables considered individually on
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48 weight loss, corrosion rate and inhibition efficiency is presented in Figures 4 to 6. The
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50 Figures show the effect of inhibitor concentration (A), exposure time (B) and
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52 temperature (C) on weight loss, corrosion rate and inhibition efficiency at constant
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inhibitor concentration (A) of 6 g, exposure time (B) of 96 h and temperature (C) of
55 25oC. There was a decrease in the value of corrosion rate from 0.16 to 0.046 mm/year
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3 with increase in A from 6 to 10. However, from C 25 and B 24, the corrosion rate slightly
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5 increased to 0.09 mm/year. Figure 4 shows that the relationship between the weight
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7 loss, A, B and C is an inverse relationship. The corrosion rate increased with an
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increase in exposure time and temperature, while a slight increase in corrosion rate was
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10 observed when the temperature was increased, leading to a corrosion rate value of
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12 0.261 mm/year at inhibition efficiency of 56.9 %. Illustrated in Figures 4 to 6 is the effect
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14 of increase in inhibitor concentration from 2 to 10 g, exposure time of 24 hours and
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temperature of 15oC. The corrosion rate decreased linearly from 0.48 to 0.01 mm/year
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21 3.4 3D Response surface plots
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The surface behavior of combination of variables on corrosion rate was described in
Figures 7 to 9. Figure 7 describes the behavior of weight loss and temperature at
constant inhibitor concentration and exposure time. From the plot, weight loss rate
decreased from 5.5 to 0.3 mg when the exposure time decreased from 168 to 24 hours
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29 at inhibitor concentration of 2 to 10g. At high immersion time, there was a similar trend
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31 in behavior at low concentration only that the corrosion rate was 0.238 mm/year at
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33 temperature of 25oC and 0.208 mm/year at temperature of 35oC. Figure 9 shows the
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behavior of inhibitor efficiency and temperature at constant immersion time and inhibitor
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36 concentration. It is apparent from the plot that inhibition efficiency rate decreased from
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38 91 to 56 % with increase in exposure time from 96 to 168 hours at low concentration of
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40 6 g. At low immersion time, the corrosion rate decreased on increasing inhibitor
41 concentration. When concentration decreased, corrosion rate increased leading to low
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43 inhibition efficiency value.
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4 DESIGN-EXPERT Plot DESIGN-EXPERT Plot
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5 WL 5.5 2
B: Time
WL 5.5
C: Temp
6 X = A: Conc (g) X = A: Conc (g)

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7 Y = B: Time (hrs) Y = C: Temp ( C)
8 Design Points 4.18978 Design Points 4.18978
9 B- 24.000 C- 15.000
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B+ 168.000 C+ 35.000
10 Actual Factor Actual Factor 2
WL2.87956 WL2.87956
11 C: Temp = 25.00 B: Time = 96.00
12 5 5
13
2
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1.56934 1.56934
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2
2
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0.259125 2 0.259125
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18 2.00 4.00 6.00 8.00 10.00 2.00 4.00 6.00 8.00 10.00
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A: Conc A: Conc
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DESIGN-EXPERT Plot
WL
X = B: Time (hrs)
o
Y = C: Temp ( C)
Design Points
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5.5
4.18978
C: Temp
2
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C- 15.000
C+ 35.000
29 Actual Factor
30 A: Conc = 6.00 WL2.87956
31 5
32
33
1.56934
34 2
35 0.259125
2
36
37 24.00 60.00 96.00 132.00 168.00
38
B: Time
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44 Figure 4 Effect of factor interactions on weight loss for first historical data
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4 DESIGN-EXPERT Plot DESIGN-EXPERT Plot
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5 CR 0.485453
C: Temp
CR 0.485453 2
B: Time
6 X = B: Time (hrs)
o
X = A: Conc (g)
7 Y = C: Temp ( C) Y = B: Time (hrs)
8 Design Points 0.36701 Design Points 0.36701
9 C- 15.000 B- 24.000
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C+ 35.000 B+ 168.000
10 Actual Factor Actual Factor
CR0.248568 CR0.248568
11 A: Conc = 6.00 C: Temp = 25.00
2
12 2
13 5 5
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0.130125 0.130125
2
2
15 2
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0.0116822 2 0.0116822
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18 24.00 60.00 96.00 132.00 168.00 2.00 4.00 6.00 8.00 10.00
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B: Time A: Conc
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DESIGN-EXPERT Plot
CR
X = A: Conc (g)
o
Y = C: Temp ( C)
Design Points
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0.485453
0.366343
C: Temp
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C- 15.000
C+ 35.000
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CR0.247233 2
30 B: Time = 96.00
2
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32 5
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0.128123
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35 0.0090124
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37 2.00 4.00 6.00 8.00 10.00
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A: Conc
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44 Figure 5 Effect of factor interactions on corrosion rate for first historical data
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4 Interaction Graph Interaction Graph
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A: Conc
94.74
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6 A+
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7 2 C-22
C+
8 82.025 82.025
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IE
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69.31 69.31
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13 A-2
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56.595 56.595 2
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C: Temp B: Time
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94.74
82.025
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A: Conc
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41 Figure 6 Effect of factor interactions on inhibition efficiency (%) for first historical data
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0.259125
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15 168.00
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B: Time 60.00 4.00
19 24.00 2.00
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WL
WL
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0.259125 0.259125
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34 35.00 35.00
35 30.00
10.00
30.00
168.00
36 25.00
8.00
25.00
132.00
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6.00 96.00
C: Temp 20.00 C: Temp 20.00
4.00 60.00
38 15.00 2.00
A: Conc
15.00 24.00
B: Time
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41 Figure 7 3D Response surface plots of factor interactions for weight loss (mg)
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0.378176
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0.163624
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CR
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0.056347
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15 168.00
16 10.00
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132.00
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8.00
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6.00
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19 24.00 2.00
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0.283841
0.215142
an 0.313496
0.238056
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0.0777444 0.0871755
CR
CR
31
0.00904549 0.0117354
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34 35.00 35.00
35 30.00
10.00
30.00
168.00
36 25.00
8.00
25.00
132.00
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6.00 96.00
C: Temp 20.00 C: Temp 20.00
4.00 60.00
38 15.00 2.00
A: Conc
15.00 24.00
B: Time
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41 Figure 8 3D Response surface plots of factor interactions for corrosion rate (mm/year)
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56.595
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43.88
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19 24.00 2.00
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90.5747
82.156
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79.4669
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IE
IE
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56.9 52.13
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34 35.00 35.00
35 30.00
10.00
30.00
168.00
36 25.00
8.00
25.00
132.00
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6.00 96.00
C: Temp 20.00 C: Temp 20.00
4.00 60.00
38 15.00 2.00
A: Conc
15.00 24.00
B: Time
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41 Figure 9 3D Response surface plots of factor interactions for inhibition efficiency (%)
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43
44
3.5 Optimization using desirability approach (DBA)
45 Optimal process parameters prediction in reducing corrosion rate of stainless steel
46
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47 using inhibitor is a difficult task as a result of large number of independent variables.

48
49 Therefore, RSM using desirability optimization method was applied in which rate of
50
corrosion was found to reduce and independent variables were found to be within
51
52 range. From the DBA, best varied solutions are attained. The most excellent optimized
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54 conditions are attained at desirability of 1.00 for minimal inhibitor concentration of 9.97g:
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56 exposure time 24.02 hours and temperature of 16.62 as observed in desirability slope
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1
2
3 function (Figure 10). The dot of each slope on the desirable plot indicates parameter
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5 setting reflection and height of the dot indicates the desirability amount. The optimum
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7 region at the left corner of the graph shows the desirability value (1.00). To verify and
8
9
predict the identified optimal process parameters to determine weight loss, corrosion
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10 rate and inhibition efficiency, verification experiments were carried out. Each of the
11
12 verification experiments was carried out different times and the average values have
13
14 been reported. Table 6 indicates the actual and predicted values of weight loss,
15
corrosion rate and inhibition efficiency. The results imply that the difference between
16
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17 actual and predicted value is below 5% indicating that the model developed is suitable
18
19 for predicting the weight loss, corrosion rate and inhibition efficiency of stainless steel
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21 corrosion in acid solution.
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40 Figure 10 Desirability ramp function of numerical optimization
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45 Table 6 Actual and predicted values of weight loss, corrosion rate and inhibition
46 efficiency
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48 Actual values Predicted values
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50 Weight loss (mg) 0.2501 0.2658
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52 Corrosion rate (mm/year) 0.0120 0.0133
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55 Inhibition efficiency (%) 97 95
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5 3.7 SEM/EDX analysis
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7 The SEM/EDX analysis of the studied stainless steel after corrosion test is shown in
8
9 Figures 11-13. The optimal processing conditions of stainless steel surface shown in
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10 Figure 13 illustrates the accumulation of the egg shell powder as observed from the
11
12 EDX. The particles agglomeration observed in the surface with inhibitor is reduced due
13
14 to enhanced fusion of powder constituent which produces dense structure with reduced
15
corrosion rate. The sample without inhibitor showed smeared layer and micro cracks in
16
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17 their worn surface as shown in Figure 12. This is as a result of inadequate protective
18
19 layer in the acid medium which leads to increase in corrosion process. The increased
20
21 deformation and cracks observed in the surface without inhibitor could be caused due to
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the presence of sulphuric acid. The SEM/EDX results validate the response trend
examined in 3D surface plots (Figures 7-9) and show that the corrosion rate increased
linearly with increased temperature, but decrease with inhibitor concentration.
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Figure 11 SEM/EDX images of as-received stainless steel sample
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3 Figure 12 SEM/EDX images of stainless steel immersed in 0.5 M H2SO4 solution in the
4
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Figure 13 SEM/EDX images of stainless steel immersed in 0.5 M H2SO4 solution in the
presence of inhibitor
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31
4 CONCLUSIONS
32
33 The resulting response surface model, obtained as a function of virtually
34 significant effects, was statistically proven to be realistic. The result of the
35
ANOVA demonstrated that the model was highly significant and that immersion
36
37 time was the most significant factor affecting the corrosion of stainless steel Type
38 316 in 0.5 M H2SO4 solution. Moreover, strong interaction has been found
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39 between inhibitor concentration, exposure time and temperature.

40
41 Corrosion rate decreased in the presence of inhibitor (egg shell powder),
42 whereas it increased with increase in temperature and exposure time.
43 The SEM micrographs of stainless steel surface in the absence of inhibitor
44
45 illustrate the corroded surface and micro cracks due to exposure to the acidic
46 environment.
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47 The compliance of predicted results shows that the proposed RSM-desirability

48
49 approach can be effectively used in determining and evaluating optimal corrosion
50 inhibition process parameters.
51 The two factor interactions were revealed with 3D response surface plots. In
52
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53 minimizing corrosion rate, optimum operating conditions of the acid environment

54 were obtained at inhibitor concentration (9.97g), immersion time (24 hours), and
55 temperature (16.62oC). Therefore, it is apparent that RSM not only gives valuable
56
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1
2
3 insight on interactions between the factors, but also helps in the recognition of
4
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5 possible optimum values of the same. It is concluded that RSM is a promising
6 statistical method that could be used to predict optimum operating conditions of
7 H2SO4 environments that would minimize corrosion rate of stainless steel Type
8
9 316 in the acid industry.
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10
11 Acknowledgements
12
13 This work is based on research supported by National Research Foundation of South
14 Africa.
15
16
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17
18
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Materials Research Express

Constitutive modeling for prediction of optimal process parameters in

Manuscript version: Accepted Manuscript

This Accepted Manuscript is © 2018 IOP Publishing Ltd.

View the article online for updates and enhancements.

This content was downloaded from IP address 196.11.235.237 on 15/08/2018 at 00:22

47 Keywords: Inhibition, Stainless steel, Response surface method, Corrosion rate,

47 Recently, progress in computational competences has facilitated the simulation of

Table 2 Properties of the egg shell powder

47 3.2 Analysis of variance (ANOVA) and statistical significance of the model

53 5 13 2 96 15 3.1 0.230411 59.21

6 X = A: Conc (g) X = A: Conc (g)

8 Design Points 4.18978 Design Points 4.18978

8 Design Points 0.36701 Design Points 0.36701

47 using inhibitor is a difficult task as a result of large number of independent variables.

39 between inhibitor concentration, exposure time and temperature.

47 The compliance of predicted results shows that the proposed RSM-desirability

53 minimizing corrosion rate, optimum operating conditions of the acid environment

53 extract on corrosion and kinetics of corrosion process of aluminium in HCl solution.

39 Environmental Technology, (2017), 14-22.

47 Science, (2014), 144-149.

39 Wiley & Sons, New York, USA. 1997; 427–510.

47 Operating Conditions Affecting Microbiologically Influenced Corrosion of Mild Steel

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