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Peer-Review Record

Corrosion Inhibition Evaluation of Chitosan–CuO Nanocomposite for Carbon Steel in 5% HCl Solution and Effect of KI Addition

Sustainability 2022, 14(13), 7981; https://doi.org/10.3390/su14137981
by Peace S. Umoren 1, Doga Kavaz 1,* and Saviour A. Umoren 2,*
Reviewer 1:
Reviewer 2: Anonymous
Reviewer 3:
Sustainability 2022, 14(13), 7981; https://doi.org/10.3390/su14137981
Submission received: 29 May 2022 / Revised: 25 June 2022 / Accepted: 25 June 2022 / Published: 30 June 2022
(This article belongs to the Section Sustainable Materials)

Round 1

Reviewer 1 Report

Comments:

(1) (c) CHT2.0-CuO nanocomposites are different from others in Figure.1. Please change the Figure.

(2) Why choose CHT-CuO nanocomposites containing 0.5, 1.0, and 2.0 g of chitosan? The optimum nanocomposite concentration is 0.5. Why not choose 0.25? Or less.

(3) The English should be improved. Such as Figure 2 shows that both in the absence and presence of the nanocomposites, the X60 carbon steel showed active dissolution in the corrosive media. The tense is wrong.

(4) The varying dosages of CHT-CuO nanocomposite are 0.1, 0.3, and 0.5%. Why choose only three dosages. It should be added more.

(5) Figure 2 lacks part of (a).

(6) The Figure 4 (c) blank and (d) 0.5% CHT0.5 - CuO nanocomposite is bad, it should be changed.  

(7) Figure 5 and Figure 6 should be redrawn.

(8) If added the 3 mM KI changes the pH of a solution? Why choose 3 mM?

 

(9) Figure 8 and Figure 10 should be redrawn. The Figures in this manuscript should be checked again and again.

Author Response

REVIEWER # 1

1. (c) CHT2.0-CuO nanocomposites are different from others in Figure.1. Please change the Figure.

RESPONSE: We want to thank the reviewer for the observation. All the figures have been drawn to be uniform

2. Why choose CHT-CuO nanocomposites containing 0.5, 1.0, and 2.0 g of chitosan? The optimum nanocomposite concentration is 0.5. Why not choose 0.25? Or less.

RESPONSE: Three nanocomposites were prepared and each of them contain different amount of chitosan (0.5 g, 1.0 g and 2.0 g). From each of the nanocomposite, three different concentrations (0.1, 0.3 and 0.5%) were selected to evaluate the effect of concentration of the different nanocomposites on the anticorrosion performance of the different nanocomposites. These concentrations were chosen for the purpose of consistency with earlier studies of the antibacterial activity of the nanocomposites in which the same concentrations were used.

3. The English should be improved. Such as Figure 2 shows that both in the absence and presence of the nanocomposites, the X60 carbon steel showed active dissolution in the corrosive media. The tense is wrong.

RESPONSE: The English has been modified as suggested by the reviewer (See lines 233 – 235).

4. The varying dosages of CHT-CuO nanocomposite are 0.1, 0.3, and 0.5%. Why choose only three dosages. It should be added more.

RESPONSE: We appreciate the concerns of the reviewer. These concentrations were chosen for the purpose of consistency with earlier studies of the antibacterial activity of the nanocomposites in which the same concentrations were used.

5. Figure 2 lacks part of (a).

RESPONSE: We want to thank the reviewer for the observation. The figure caption has been completed.

6. The Figure 4 (c) blank and (d) 0.5% CHT5- CuO nanocomposite is bad, it should be changed.

RESPONSE: We have tried our best to improve Figures 4(c) blank and (d) 0.5% CHT0.5 - CuO nanocomposite as suggested by the reviewer.

7. Figure 5 and Figure 6 should be redrawn.

RESPONSE: Figures 5 and 6 have been redrawn as suggested by the reviewer.

8. If added the 3 mM KI changes the pH of a solution? Why choose 3 mM?

RESPONSE: Addition of 3 mM KI did not change the pH of the solution. Normally KI is added as an enhancer in corrosion inhibitor formulations in small quantity. In the last we have tried different concentrations of KI (0.5, 1, 3 and 5 mM) and it was noted that inhibition efficiency improves further with increasing concentration of KI. However, the difference between the value obtained with 3 mM and 5 mM was marginal. Hence, we decided in the present work to use 3 mM instead of 5 mM to reduce wastage.

9. Figure 8 and Figure 10 should be redrawn. The Figures in this manuscript should be checked again and again.

RESPONSE: The figures (8 and 10) the reviewer mentioned were obtained directly from the instrument and was not drawn by us. However, we have tried to improve both Figures for clarity.

Reviewer 2 Report

This manuscript assesses the corrosion inhibition performance of OLE mediated synthesis of CHT – CuO nanocomposite containing different amounts of chitosan (0.5, 1.0, and 2.0 g) on X60 carbon steel in 5% HCl acid corrodent employing weight loss and electrochemical approaches. In addition, the effect of temperature and KI addition on the corrosion inhibitive efficacy of the nanocomposites was also examined. In my opinion, I see that the idea is sounded and attractive; however, some issues should be addressed according to the following comments:

1) The overall presentation, readability, and more analysis are mandatory. Please, correct the language problems, it is weak from the Grammarly and sequences of events, I catch 26 errors by using a personal program, and the authors should cure them carefully.

2) The "Abstract" section should be more intensively focused on the main idea directly and must contain the contribution of this manuscript supported with numerical result indicators. Also, I see there is no need for many abbreviations in the abstract part that were mentioned only one time (e.g., WL, EIS, LPR, PDP, SEM, and EDS).

3) The "Introduction" section should be made much more impressive by highlighting your contributions. The novelty of this manuscript must be explained simply and clearly in points at the end of the introduction section. Note that, the introduction section should consist of three parts, i.e., a general introduction to the topic, followed by a literature survey, then the contribution clarifications.

4) The introduction section should be enriched with up-to-date references by adding and citing the latest trends in the area of the influence of the nanoparticle's functionalization process on the morphology, structure, and characterization within the carbon steel matrix. E.g., Effect of functionalized TiO2 nanoparticles on dielectric properties of PVC nanocomposites & Recent Advances in Polymer Nanocomposites Based on Polyethylene and Polyvinylchloride for Power Cables & PVC Nanocomposites for Cable Insulation with Enhanced Dielectric Properties, PD Resistance & Development of Industrial Scale PVC Nanocomposites with Comprehensive Enhancement in Dielectric Properties.

5) It is mandatory to check all the citing references of equations (1): (7). Also, check carefully all the abbreviation definitions, symbols, and standard units in the whole manuscript. I catch some errors and the other symbols are not defined, please, define the abbreviations. Also, there are many standard tests without citing their references.

6) The resolution and quality of figures must be modified; they should be presented as close to the camera-ready format (e.g., Figs. 2.a and 5.a). Also, please don't use the symbol abbreviations on X-Y-axes, they must have the full name with their SI units.

 

7) The conclusion section should be more concentrated and supported by the numerical results. Also, the authors may propose some interesting problems as future work in the conclusion.

Author Response

REVIEWER # 2

This manuscript assesses the corrosion inhibition performance of OLE mediated synthesis of CHT – CuO nanocomposite containing different amounts of chitosan (0.5, 1.0, and 2.0 g) on X60 carbon steel in 5% HCl acid corrodent employing weight loss and electrochemical approaches. In addition, the effect of temperature and KI addition on the corrosion inhibitive efficacy of the nanocomposites was also examined. In my opinion, I see that the idea is sounded and attractive; however, some issues should be addressed according to the following comments:

RESPONSE: We want to thank the reviewer for the kind commendation. It is well appreciated.

1) The overall presentation, readability, and more analysis are mandatory. Please, correct the language problems, it is weak from the Grammarly and sequences of events, I catch 26 errors by using a personal program, and the authors should cure them carefully.

RESPONSE: Although the reviewer did not specifically point out the 26 errors which would have been very helpful, we have thoroughly read through the manuscript and modify the language appropriately.

2) The "Abstract" section should be more intensively focused on the main idea directly and must contain the contribution of this manuscript supported with numerical result indicators. Also, I see there is no need for many abbreviations in the abstract part that were mentioned only one time (e.g., WL, EIS, LPR, PDP, SEM, and EDS).

RESPONSE: As suggested by the reviewer, some portions of the abstract has been modified with numerical results. Also, the abbreviations such as WL, EIS, LPR, PDP, SEM and EDS have been removed from the abstract.

3) The "Introduction" section should be made much more impressive by highlighting your contributions. The novelty of this manuscript must be explained simply and clearly in points at the end of the introduction section. Note that, the introduction section should consist of three parts, i.e., a general introduction to the topic, followed by a literature survey, then the contribution clarifications.

RESPONSE: We want to thank the reviewer for this comment, As rightly suggested we have highlighted the novelty of the work at the end of the “Introduction” section of the manuscript (see lines 107 – 111)

4) The introduction section should be enriched with up-to-date references by adding and citing the latest trends in the area of the influence of the nanoparticle's functionalization process on the morphology, structure, and characterization within the carbon steel matrix. E.g., Effect of functionalized TiO2 nanoparticles on dielectric properties of PVC nanocomposites & Recent Advances in Polymer Nanocomposites Based on Polyethylene and Polyvinylchloride for Power Cables & PVC Nanocomposites for Cable Insulation with Enhanced Dielectric Properties, PD Resistance & Development of Industrial Scale PVC Nanocomposites with Comprehensive Enhancement in Dielectric Properties.

RESPONSE: Although it would have been helpful if the reviewer had given specific journal articles, we want to however differ with the reviewer on the areas suggested to be added and cited in the present work. It is well known that nanocomposites have wide areas of applications, and it is imperative that literature review in the introduction section of a manuscript should be confined to the research focused area and subject matter. We have cited relevant and up to date references on the application of polymer-metal/metal oxide nanocomposites as corrosion inhibitors. The areas suggested by the reviewer such as “Effect of functionalized TiO2 nanoparticles on dielectric properties of PVC nanocomposites & Recent Advances in Polymer Nanocomposites Based on Polyethylene and Polyvinylchloride for Power Cables & PVC Nanocomposites for Cable Insulation with Enhanced Dielectric Properties, PD Resistance & Development of Industrial Scale PVC Nanocomposites with Comprehensive Enhancement in Dielectric Properties” are outside the scope of this manuscript.

5) It is mandatory to check all the citing references of equations (1): (7). Also, check carefully all the abbreviation definitions, symbols, and standard units in the whole manuscript. I catch some errors and the other symbols are not defined, please, define the abbreviations. Also, there are many standard tests without citing their references.

RESPONSE:  All the issues raised by the reviewer has been addressed in the revised manuscript

6) The resolution and quality of figures must be modified; they should be presented as close to the camera-ready format (e.g., Figs. 2.a and 5.a). Also, please don't use the symbol abbreviations on X-Y-axes, they must have the full name with their SI units.

 RESPONSE: The quality of Figures 2a and 5a have been improved as suggested by the reviewer. The reviewer should have been very specific on where symbol abbreviations are used in the X-Y axes in the figures. We believe that standard scientific symbols are used that is widely understood and acceptable by the researchers in the field.

7) The conclusion section should be more concentrated and supported by the numerical results. Also, the authors may propose some interesting problems as future work in the conclusion.

RESPONSE: As suggested by the reviewer, the conclusion has been modified with numerical results introduced. Also, we have proposed the evaluation of the prepared nanocomposites as sweet (CO2) and sour (H2S) corrosion inhibitors as well as biocides for microbial influenced corrosion (MIC) mitigation for future work.

Reviewer 3 Report

The manuscript report detailed, systematic study of the chitosan-CuO composite system for anti-corrosion applications. The results are of interest to industrial communities. With some minor revisions as indicated as follows, the reviewer has no objection for acceptance. 

A) The composite preparation need to be given. It can be a brief one, as apparently this is a follow-up research. It will leave too much blank if simply referencing the method to the previous publications. 

B) Olive-leave extract was used as a reducing agent, please justify the reason of this choice.

C) KI was added to the composite to test its influence on the anti-corrosion capability. Please justify the hypothesis: why KI is considered as a factor in the first place. 

Author Response

REVIEWER # 3

The manuscript report detailed, systematic study of the chitosan-CuO composite system for anti-corrosion applications. The results are of interest to industrial communities. With some minor revisions as indicated as follows, the reviewer has no objection for acceptance. 

RESPONSE: We want to thank the reviewer for the kind commendation. It is well appreciated

A) The composite preparation need to be given. It can be a brief one, as apparently this is a follow-up research. It will leave too much blank if simply referencing the method to the previous publications. 

RESPONSE: The method of the composite preparation has been given briefly in line with the suggestion of the reviewer (See lines 132 – 139)

B) Olive-leave extract was used as a reducing agent, please justify the reason of this choice.

RESPONSE: Olive-leave extract was used as reducing because it contains important phytoconstituents like Secoiridoids such as oleuropein, ligstroside, 1-methyloleuropein, and oleoside; flavanoids such as apigenin, kaempferol, luteolin, and chrysoeriol; and phenolic compounds such as caffeic acid, tyrosol, and hydroxytyroso. These phytoconstituents could have played important role in the reduction process.

C) KI was added to the composite to test its influence on the anti-corrosion capability. Please justify the hypothesis: why KI is considered as a factor in the first place. 

RESPONSE: KI is a well-recognised enhancer or intensifier. It is normally added as an enhancer in corrosion inhibitor formulations in small quantity to improve corrosion inhibition capacity of active corrosion inhibitors. It is most preferred to other intensifiers like formic acid, copper iodide because of its eco-friendly nature.

 

Round 2

Reviewer 1 Report

It can be accepted now.

Author Response

thanks

Reviewer 2 Report

Most of my concerns are adjusted.

Author Response

thanks

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