Laboratory Experiment

Cite This: J. Chem. Educ. XXXX, XXX, XXX−XXX pubs.acs.org/jchemeduc

Enhancing the Teaching of Corrosion to Chemical-Engineering

Students through Laboratory Experiments
Javier Llanos,* Á ngel Peŕ ez, and Antonio de Lucas-Consuegra
Chemical Engineering Department, Facultad de Ciencias y Tecnologías Químicas, University of Castilla−La Mancha, Edificio
Enrique Costa Novella, Avenida Camilo José Cela no. 12, 13071 Ciudad Real, Spain
*
S Supporting Information

ABSTRACT: This work presents a laboratory to help chemical-engineering students

understand the basic concepts of corrosion. This laboratory has been performed since
academic year 2011−2012 in the framework of the subject “Design of equipment and
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installations” for the third year of the Chemical Engineering Degree of the University of
Castilla−La Mancha (Spain). It is based on calculating the corrosion rates of six different
samples in order to evaluate the effects of the corrosion environment, the material of the
sample, and the application of corrosion-prevention methods. The performance of the laboratory to enhance the teaching−
learning methodology was evaluated by asking the students to answer a test before and after completing the laboratory. The
results show that the laboratory improves the understanding of the students and also their confidence in their answers, although
room for improvement was found in relation to the application of corrosion-prevention methods, for which corrective actions
are proposed.
KEYWORDS: Upper-Division Undergraduate, Chemical Engineering, Hands-On Learning/Manipulatives, Electrochemistry,
Oxidation/Reduction, Electrolytic/Galvanic Cells/Potentials
J. Chem. Educ.

C orrosion is one of the most relevant issues in regard to

the economy of many different key sectors. According to
the calculations of the US National Association of Corrosion
Engineers (NACE), the cost of corrosion worldwide is
estimated to be US$2.5 trillion, which is equivalent to 3.4%
of the 2013 global GDP.1 Thus, the study of corrosion
principles is a matter of major importance in many sectors,2
including aerospace engineering,3 medicine,4,5 and, of course,
chemical engineering.6−8
The fundamentals of corrosion cover several disciplines,
including materials engineering, physical chemistry, electro-
chemistry, and others. This causes students of chemical
engineering to show certain difficulties in understanding the
main concepts of corrosion science; it is especially important
to include laboratory practices for teaching the basic principles
of electrochemical corrosion, as it is possible to design visual,
quick, and affordable practices that enhance the teaching−
learning process.9−12
The present work describes a laboratory developed to
explain the principles of corrosion in the subject “Design of
equipment and installations” in the third year of the Chemical
Engineering Degree of the University of Castilla−La Mancha
(Spain). This laboratory was designed and placed to give
support to the corrosion concepts previously explained in the
theoretical classes. Moreover, the assessment of the teaching−
learning process was made by asking the students to answer a
questionnaire twice (before and after performing the
laboratory). This survey evaluates not only the knowledge
but also the degree of certainty in the answers, thus helping to
find out if the activity is effective as well as the possible weak
© XXXX American Chemical Society and
Division of Chemical Education, Inc.
points to be further improved. In addition, correcting actions
to improve the weaknesses detected are proposed.
■ BACKGROUND
Although the definition of the term corrosion is wide, in the
vast majority of practical cases corrosion is a chemical process
in which the metal is oxidized. When an electrolyte (e.g.,
water) is present (the general case for environmental
corrosion), corrosion is called electrochemical corrosion or
wet corrosion. In this particular case, an electrochemical cell is
formed; the dissolution of the metal (M) is the anodic reaction
(eq 1), and either the reduction of oxygen (for neutral or basic
pH, eq 2) or the reduction of protons (for acidic conditions, eq
3) is the cathodic reaction.9,13
M(s) → Mn +(aq) + ne− (1)
O2 (g) + 2H 2O(l) + 4e− → 4OH−(aq) (2)
2H+(aq) + 2e− → H 2(g) (3)
In this laboratory, the students evaluate the average
corrosion rates of iron and stainless steel in different acidic
corrosion environments. Moreover, they perform two tests in
which two different methods for corrosion prevention are
applied (metallic coating and cathodic protection by impressed
current).
Received: October 9, 2018
Revised: March 6, 2019
A DOI: 10.1021/acs.jchemed.8b00803
J. Chem. Educ. XXXX, XXX, XXX−XXX
Journal of Chemical Education
Table 1. Comparison of Student Results for Exposure of the Probes to Different Environments
Material Solution Protection Method
Test 1 Iron 0.1 M HNO3 None
Test 2 Iron 0.1 M HCl None
Test 3 Iron 0.1 M HNO3 Zinc coating
Test 4 Iron 0.1 M HNO3 Cathodic protection by impressed current
Test 5 Stainless steel 5.0 M HNO3 None
Test 6 Stainless steel 5.0 M HCl None
a
The exposure time was 20 min, and the total attack volume was 200 mL.
■ LEARNING OUTCOMES
This laboratory is designed to help the students improve their
basic knowledge on the following:
• The reactions taking place in electrochemical corrosion
• The roles of the type of material and the corrosion
environment on the rate of the corrosion process
• The effectiveness of the application of two methods of
corrosion prevention (metal coating and cathodic
protection by impressed current)
This laboratory lasts approximately 3 h, is performed in
groups of 4 students, and has been performed by an average of
40 students per year since academic year 2011−2012 in the
framework of the subject “Design of equipment and
installations”. The students have scored an average of 64.8%
in this subject from the course in 2011−2012 to the course in
2017−2018. After completing the laboratory, the students are
asked to perform the calculations and discuss the results by
answering four questions (explained in the Supporting
Information). This work of calculation and discussion of the
results may take 3 h of additional work for the students.
According to the students’ answers to the surveys about the
teaching activities (made by the University of Castilla−La
Mancha), the students have a good opinion of the laboratory
(average mark of 2.23/3 from the courses in 2011−2012 and
2013−2014 and average mark of 4.43/5 from the courses in
2014−2015 to 2017−2018).
■ HAZARDS
Splash goggles and gloves should be worn while handling the
acid solutions. The power supply used is of a very low power,
and it is protected by a fuse, so no important hazards from
electric shocks are expected. An important aspect to remember
is placing both electrodes far enough away to avoid short-
circuits.
■ RESULTS AND DISCUSSION
Basically, the laboratory consists of performing the attack on
six samples (four of iron and two of stainless steel) with
different acid solutions (nitric acid and hydrochloric acid) over
20 min. After this exposure time, the concentration of iron is
measured by inductively coupled plasma−atomic-emission
spectroscopy (ICP-AES), and the average rate of corrosion is
calculated on the basis of the total volume of the solution and
the external area of the sample. Two of the iron samples are
subjected to methods for corrosion prevention in order to test
the influence in the overall corrosion rate. One of them
(sample 3) is covered by a zinc coating, and the second
(sample 4) is connected to the cathode of a power supply with
a fix intensity of 0.4 A in order to promote its cathodic
protection by impressed current. A detailed description of the
B DOI: 10.1021/acs.jchemed.8b00803
Laboratory Experiment
Sample Area Average Ratea
[Fe] (mg L−1) (cm2) (mg cm−2 min−1)
134 ± 2.01 4.20 3.18 × 10−01
6.80 ± 0.09 4.18 1.63 × 10−02
96.7 ± 1.38 3.60 2.69 × 10−01
40.9 ± 0.52 4.20 9.74 × 10−02
0.001 ± 0.0005 4.56 2.19 × 10−06
5.56 ± 0.07 4.84 1.15 × 10−02
laboratory and the calculations is included in the Supporting
Information.
Table 1 shows a real example of the iron-concentration
results obtained by one group together with the conditions of
the tests.
The first result that the students can obtain from these data
is that the rate of corrosion of iron in nitric acid is higher than
that obtained in hydrochloric acid. This can be explained by
the nature of the acid, as nitric acid can be considered
oxidizing, whereas hydrochloric acid is nonoxidizing. The nitric
ion can be reduced to several chemical species in acidic media,
including HNO2, NO, or N2O4. The standard reduction
potentials of nitric ions to these species (0.934 V for HNO2,
0.957 V for NO, or 0.803 V for N2O4, in all cases vs SHE) are
higher than the standard reduction potentials of Fe2+ to
metallic iron (−0.440 V vs SHE). In contrast, chloride ion
cannot be further reduced to any other chemical species. This
means that the anion of nitric acid can contribute to the
oxidation of iron, whereas the chloride anion is not able to
oxidize the metal, thus giving a lower rate of oxidation.
Next, by comparing the rate of test 1 with the rates of tests 3
and 4, the students can check whether applying a method for
corrosion prevention diminishes the rate of corrosion. An
additional conclusion that can be obtained from these results is
that neither the Zn coating nor cathodic protection can
completely reduce the corrosion of iron in this environment.
This is generally one of the matters that creates higher
confusion among the students, as they are expecting full
protection of the base metal and not just a partial reduction in
the corrosion rate. In this case, the explanation can be found in
the fact that neither a galvanic coating nor cathodic protection
are the best protection methods in aggressive corrosion
environments, such as those tested in the present work. On
the contrary, both methods are generally applied in environ-
mental corrosion, in which the aggressiveness of the environ-
ment is not as high as in the laboratory.14,15
Finally, two main conclusions can be obtained from
analyzing the results of tests 5 and 6. The first one is that
the rate of corrosion with stainless steel is far below that
registered for iron, even considering that the concentrations of
the acids are 50 times higher for the attack on stainless steel.
This is expected as stainless steel is able to form a passive layer
that hinders the evolution of the oxidation process. The second
conclusion from this part of the laboratory is that the
aggressiveness of these corrosion environments on stainless
steel is the opposite of that observed for iron. In this case, the
concept of pitting corrosion (previously explained in the
theoretical classes) is the key to finding the answer to this
behavior. Chloride ions have the ability to locally dissolve the
passive layer of stainless steel, thus allowing protons to attack
the base material.16 In contrast, nitrate ions cannot dissolve the
J. Chem. Educ. XXXX, XXX, XXX−XXX
Journal of Chemical Education Laboratory Experiment

passive layer, but the the strongly oxidizing environment of

nitric acid is perfect for forming and maintaining this
protective film,17 thus resulting in a negligible corrosion rate
(the measured iron concentration is almost zero). In this case,
the students are also required to visually inspect the samples to
observe the incipient pitting formed for the probe immersed in
HCl. An example of this is shown in Figure 1, in which an

Figure 1. Microscope analysis of the stainless-steel probes: original

(a), after test 5 (HNO3, b), after test 6 (HCl, c). The original and
HNO3-treated stainless steel (a,b) have similar aspects, whereas
incipient pitting corrosion is observed on the stainless steel treated
with HCl (c). The figures were obtained with an Optika SZM-D
digital microscope.

original sample of stainless steel (Figure 1a) and the final

aspects of stainless-steel pieces in both nitric acid (Figure 1b)
and hydrochloric acid (Figure 1c) are compared. The aspect of
Figure 1b is visually similar to that of the original piece (Figure
1a), whereas incipient pitting corrosion can be observed in
Figure 1c.

■ ASSESSMENT OF THE TEACHING−LEARNING

METHODOLOGY
Figure 2. Questionnaire designed to evaluate the effect of the
laboratory on the knowledge and confidence of the students.
To assess the teaching−learning methodology, the students
were asked to answer a questionnaire (Figure 2) before and
after performing the laboratory.
In this questionnaire, the students answered four questions
related to the three main concepts developed in the laboratory
and were asked to state their confidence rating for each
question, according to the work of Hoe and Subramaniam.18
Figures 3 and 4 compare the percentages of correct answers
(Figure 3) and the confidence ratings (Figure 4) before and
after completing the laboratory.
As can be observed, performing the laboratory has a marked
positive effect on the percentage of correct answers (from 63.2
to 97.4% for question 1, from 45.6 to 83.5% for question 2,
from 31.6 to 68.4% for question 3, and from 52.6 to 65.8% for
question 4). Regarding Figure 4, performing the laboratory
also has a positive effect on the confidence of the students.
Nevertheless, it is worth mentioning that more than 30% of the
students who answered question 4 incorrectly had a high Figure 3. Success ratios of the answers to questions 1−4 (Q1−Q4)
degree of certainty, which indicates that something is wrong. before (white bars) and after (gray bars) the laboratory practices. The
According to these results, it seems clear that, after sample included 76 chemical-engineering students from two
completing the laboratory, the students have improved their consecutive academic years. A clear increase in the success ratio is
knowledge of the roles of the corrosion environment and the observed after completion of the laboratory.
material (questions 1 and 2). Regarding the application of a
metallic coating (question 3), the percentage of correct
answers more than doubled, although 30% of the answers brief explanation of the nature and basic operation of a power
were still incorrect. Concerning the application of an supply will be included in the theoretical classes prior to the
electrochemical method for corrosion prevention (question laboratory period in order to help students take the best
4), this is the field in which the laboratory has room for possible advantage of the laboratory.
improvement. To work on these points, special attention will
be paid to giving deeper explanations of the experimental
procedures of tests 3 and 4, and their relation to the theoretical
■ CONCLUSION
The main conclusion to be obtained from this work is that a
concepts previously explained in master classes. Moreover, a simple laboratory practice was effectively designed to improve
C DOI: 10.1021/acs.jchemed.8b00803
J. Chem. Educ. XXXX, XXX, XXX−XXX
Journal of Chemical Education
Figure 4. Confidence rating of the answers to questions 1−4 (Q1−
Q4) before (white bars) and after (gray bars) the laboratory practices.
The sample included 76 chemical-engineering students from two
consecutive academic years. A clear increase in the confidence rating
is observed after completion of the laboratory.
the understanding of basic corrosion concepts for chemical-
engineering students. The laboratory helps to increase both
their knowledge of corrosion concepts and their confidence in
their answers. The results suggest that it is possible to improve
the design of the laboratory in regard to the field of the
application of corrosion-prevention methods. On the basis of
this, special attention will be paid in the future to the
explanation of the experimental tests related to this concept
and new theoretical concepts will also be included in the
master classes prior to the laboratory.
■
*
ASSOCIATED CONTENT
S Supporting Information
The Supporting Information is available on the ACS
Publications website at DOI: 10.1021/acs.jchemed.8b00803.
Student handout with a detailed explanation of the
experimental procedures, questions, and examples of the
calculations needed (PDF, DOC)
Answers to the postlab questions (PDF, DOCX)
Instructor notes, including a list of the chemicals used
with CAS numbers, the materials needed, and the prelab
explanations (PDF, DOCX)
■
AUTHOR INFORMATION
Corresponding Author
*E-mail: javier.llanos@uclm.es.
ORCID
Javier Llanos: 0000-0001-6404-3577
Antonio de Lucas-Consuegra: 0000-0001-8080-8293
Notes
The authors declare no competing financial interest.
■ ACKNOWLEDGMENTS
The authors want to acknowledge the collaboration of the
students in performing the practice.
D DOI: 10.1021/acs.jchemed.8b00803
■
Laboratory Experiment
REFERENCES
(1) National Association of Corrosion Engineers (NACE) website.
http://impact.nace.org/economic-impact.aspx (accessed Feb 2019).
(2) Winkleman, A.; Svedberg, E. B.; Schafrik, R. E.; Duquette, D. J.
Preventing corrosion from wearing our future away. Adv. Mater.
Process. 2011, 169 (3), 26−31.
(3) Abrahami, S. T.; de Kok, J. M. M.; Terryn, H.; Mol, J. M. C.
Towards Cr(VI)-free anodization of aluminum alloys for aerospace
adhesive bonding applications: A review. Front. Chem. Sci. Eng. 2017,
11 (3), 465−482.
(4) Nagaraja, S.; Di Prima, M.; Saylor, D.; Takai, E. Current
practices in corrosion, surface characterization, and nickel leach
testing of cardiovascular metallic implants. J. Biomed. Mater. Res., Part
B 2017, 105 (6), 1330−1341.
(5) Gao, A.; Hang, R.; Bai, L.; Tang, B.; Chu, P. K. Electrochemical
surface engineering of titanium-based alloys for biomedical
application. Electrochim. Acta 2018, 271, 699−718.
(6) Viertel, J.; Neuer, L.; Mauch, B.; Czyborra, T. Project RepaKorr:
Development of a novel single coat, direct to metal repair coating with
outstanding protection and colour retention performance for offshore
structures. Mater. Corros. 2017, 68 (12), 1321−1325.
(7) Khadom, A. A.; Farhan, S. N. Corrosion inhibition of steel in
phosphoric acid. Corros. Rev. 2018, 36 (3), 267−280.
(8) An, S.; Lee, M. W.; Yarin, A. L.; Yoon, S. S. A review on
corrosion-protective extrinsic self-healing: Comparison of micro-
capsule-based systems and those based on core-shell vascular
networks. Chem. Eng. J. 2018, 344, 206−220.
(9) Sanders, R. W.; Crettol, G. L.; Brown, J. D.; Plummer, P. T.;
Schendorf, T. M.; Oliphant, A.; Swithenbank, S. B.; Ferrante, R. F.;
Gray, J. P. Teaching Electrochemistry in the General Chemistry
Laboratory through Corrosion Exercises. J. Chem. Educ. 2018, 95 (5),
842−846.
(10) Silva, M. V. F.; Pereira, M. C.; Codaro, E. N.; Acciari, H. A.
Carbon steel corrosion: An everyday approach for chemistry teaching.
Quim. Nova 2015, 38 (2), 293−296.
(11) Malel, E.; Shalev, D. E. Determining the effect of environmental
conditions on iron corrosion by atomic absorption. J. Chem. Educ.
2013, 90 (4), 490−494.
(12) Moraes, E. P.; Confessor, M. R.; Gasparotto, L. H. S.
Integrating mobile phones into science teaching to help students
develop a procedure to evaluate the corrosion rate of iron in simulated
seawater. J. Chem. Educ. 2015, 92 (10), 1696−1699.
(13) Cicek, V.; Al-Numan, B. Corrosion Chemistry; John Wiley &
Sons, Hoboken, NJ, 2011.
(14) Garrity, K. C.; Urbas, M. Cathodic protection of external tank
bottoms. Mater. Perform. 2018, 57 (9), A40−A44.
(15) Cole, I. S. Recent progress and required developments in
atmospheric corrosion of galvanised steel and zinc. Materials 2017, 10
(11), 1288.
(16) Solorza, O.; Ibanez, J. G.; Olivares, L. Experimental
demonstration of corrosion phenomena: the corrosion, passivation
and pitting of iron in aqueous media. J. Chem. Educ. 1991, 68, 175−
177.
(17) Arce, E. M.; Ramírez, R.; Cortés, F.; Ibanez, J. G. Experimental
demonstration of corrosion phenomena. part ii. corrosion phenomena
of steel in aqueous media. J. Chem. Educ. 1991, 68, 351−352.
(18) Hoe, K. Y.; Subramaniam, R. On the prevalence of alternative
conceptions on acid−base chemistry among secondary students:
insights from cognitive and confidence measures. Chem. Educ. Res.
Pract. 2016, 17 (2), 263−282.
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