Synthesis and Characterization of a Nano-Adsorbent Derivative Derived from Grape Seeds for Cadmium Ion Removal in an Aqueous Solution

Round 1

Reviewer 1 Report

This manuscript demonstrates the synthesis of iron-based nanoparticles using grape seed and FeCl2 for Cd removal. It needs a major revision before publication according to the following comments.

1. nano-adsorbent is too broad to be highlighted in the Title. According to the manuscript, it looks like an iron (hydro)oxide with nano scales. However, critical characterization of this nano adsorbent using other methods like TEM is missing.
2. There are too many typo errors in the manuscript. For example, Line 15, FeCl2; Line 18, Cd (II); Line 22, adsorption site (II); Line 28, (Cd) (Cd). Check through the manuscript carefully.
3. Introduction part is too long and missing some advanced and important works. Here are some references for help. (Environmental Science & Technology 2021 55 (8), 4287-4304; ACS ES&T Engineering 2021 1 (4), 623-661; Journal of Cleaner Production 2019, 232, 774-783.)
4. All the figures presented are of low quality. Figure 3 and 4 can be all in one.
5. The identification of crystalline should be validated by PDF card and previous reports. (Applied Catalysis B: Environmental, 2021, 286, 119859; Chemical Engineering Journal, 2021, 404, 127075)
6. The kinetic study is missing.
7. Comparison with other adsorbents is also missing. 

Author Response

1. nano-adsorbent is too broad to be highlighted in the Title. According to the manuscript, it looks like an iron (hydro)oxide with nanoscales. However, critical characterization of this nano adsorbent using other methods like TEM is missing.

Due to the shortage in laboratories because the lockdown due to varus corona

 

2. There are too many typo errors in the manuscript. For example, Line 15, FeCl2; Line 18, Cd (II); Line 22, adsorption site (II); Line 28, (Cd) (Cd). Check through the manuscript carefully.

(Done)

3. The introduction part is too long and missing some advanced and important works. Here are some references for help. (Environmental Science & Technology 2021 55 (8), 4287-4304; ACS ES&T Engineering 2021 1 (4), 623-661; Journal of Cleaner Production 2019, 232, 774-783.)

(Done)

4. All the figures presented are of low quality. Figures 3 and 4 can be all in one.

(Done)

5. The identification of crystalline should be validated by PDF card and previous reports. (Applied Catalysis B: Environmental, 2021, 286, 119859; Chemical Engineering Journal, 2021, 404, 127075)

6. The kinetic study is missing.

Not available

7. Comparison with other adsorbents is also missing. 

(Done)

 

 

Author Response File: Author Response.pdf

Reviewer 2 Report

The present article studied the grape seed extract mediated nano-adsorbent for cadmium removal. The manuscript lack significant basics of material preparation, novelty, and clarity in its applications for cadmium adsorption. The manuscript did not fit for the Journal Water. I have the following major comments;

1. What is the rationale behind selecting grape seed extract for the process?
2. Authors applied material for cadmium adsorption, however, authors need to compare it with recently reported materials, and explain how this material is working better.
3. The authors should give the kinetics data and models for the adsorption process.
4. Very poor English writing in the manuscript. The spelling/presentation of units (g, ml, etc.) is very poor.
5.  The authors did not report the synthesis mechanism clearly. 
6. Authors not discussed the magnetic properties of the material by MPMS analysis.
7. Difficult to understand the chemistry of the process, how this material formed.
8. Very poor SEM image, it's very difficult to get an idea about morphology.
9. The authors have not explained the mechanism of the adsorption. The studied adsorption process is poorly usderstood.
10. The authors should report the RL factor values and favourability of the adsorption process. 

Author Response

1. What is the rationale behind selecting grape seed extract for the process?

            We working on converting agriculture waste to useful materials and we found that grape seeds can use as starting material for the preparation of bio adsorbent   

2. Authors applied material for cadmium adsorption, however, authors need to compare it with recently reported materials, and explain how this material is working better.

(Done)

3. The authors should give the kinetics data and models for the adsorption process.

It is not available now

4. Very poor English writing in the manuscript. The spelling/presentation of units (g, ml, etc.) is very poor.

(Done)

5. The authors did not report the synthesis mechanism clearly.

(Done) 

6. Authors not discussed the magnetic properties of the material by MPMS analysis.

(Done)

7. Difficult to understand the chemistry of the process, how this material formed.

(Done)

8. Very poor SEM image, it's very difficult to get an idea about morphology.

Due to the shortage in laboratories because the lockdown due to varus corona

8. The authors have not explained the mechanism of the adsorption. The studied adsorption process is poorly understood.

(Done) 

9. The authors should report the RL factor values and favorability of the adsorption process. 

      (Done)

Author Response File: Author Response.pdf

Reviewer 3 Report

I prepared the manuscript review Synthesis and characterisation of a nano-adsorbent derivative derived from grape 2 seeds for cadmium ion removal in aqueous solution written by Alaa J. Mohammed, Mohd Hafiz Ibrahim, Syaizwan Z. Zulkifli and Jasim M. Salman.

The study is clear and adequately described.

In my opinion this manuscript is acceptable for publication after minor revision.

As for details:

page 3 line 116: As an adsorbent ???, Scharlaw Chiemi, S. A., Barcelona, Spain, provided technical grade Cadmium Cd (II) 117 at a concentration of 1000 ppm.

This error should be corrected.

page 5 line 185: Figure 2: UV-Visible spectroscopy absorbance of iron oxide nanoparticles synthesized by 185 grape seeds extract mixing with ferrous chloride pH, 3.8, ratio of (2:1).

The peaks numbered in the graph should be described in the text

I propose to add some sentences to explain these informations.

Author Response

1. page 3 line 116: As an adsorbent ???, Scharlaw Chiemi, S. A., Barcelona, Spain, provided technical grade Cadmium Cd (II) 117 at a concentration of 1000 ppm.

This error should be corrected.

(Done): Technical grade of cadmium Cd (II) at a concentration of (1000 mg/l) used as adsorbent which provided from Scharlaw Chiemi, S. A., Barcelona, Spain.

2. page 5 line 185: Figure 2: UV-Visible spectroscopy absorbance of iron oxide nanoparticles synthesized by 185 grape seeds extract mixing with ferrous chloride pH, 3.8, the ratio of (2:1).

The peaks numbered in the graph should be described in the text

I propose to add some sentences to explain this information.

(Done)

Author Response File: Author Response.pdf

Reviewer 4 Report

Article: Synthesis and characterization of a nano-adsorbent derivative derived from grape seeds for cadmium ion removal in aqueous solution for publication in Water is good. The subject is interesting. In this work, Grape seeds were discovered to be a source for nanoparticle adsorbent production. The goal of the research was to create and describe a Nano adsorbent made from grape seeds (GS) and FeCl2. The physical and chemical prop- erties of grape seed ferrous oxide nanoparticles (GS-IONPs) were investigated. Batch adsorption was used to investigate the removal of cadmium ion from aqueous solutions in relation to beginning concentrations, contact time, and pH. The adsorption of Cd (II) onto GS-IONPs was studied using three isotherm models: Langmuir, Freundlich, and Temkin. The data obtained fit the Langmuir model well, with a maximum adsorption capacity of 16.3 mg/g. The removal of cadmium decreased from 98.0 to 88.0 percent as the initial concentration increased. This is because the surface area and adsorption  sites are very high at low initial concentrations, resulting in an increase in Cd(II) removal, whereas the availability of  binding sites at higher concentrations is limited, resulting in no additional Cd(II) adsorption site (II). The presented article is interesting and a construction of article is logical. Scientific merit is good. The work is relevant and practical. Clarity of expression and communication of ideas, readability and discussion of concepts is good.

 

However some corrections are needed:

 

1. More discussion should be presented in every part in this manuscript.
2. Should the quality of drawings 2, 4, 5 be improved?
3. If it is possible, an interesting addition to this publication could be the calculated size of crystallites from XRD results by, for example, Scherrer equation.
4. It would be necessary to unify units according to the Si system
5. If possible, it would be good to propose some cadmium ions adsorption mechanism.
6. Novelty elements should be better highlighted in the introduction. Papers should be cited in Introduction section; for example:

Hydroxyapatite with magnetic core: Synthesis methods, properties, adsorption and medical applications Advances in Colloid and Interface Science 291 (2021) 102401

Adsorption of Cd (II) ions at the hydroxyapatite/electrolyte solution interface Separation Science and Technology (Philadelphia) 51(1) 2016 11-21

The effect of  adsorption of Pb(II) and Cd(II) ions in the  presence  of EDTA on  characteristic of electrical double layer at the  ion exchanger/NaCl electrolyte solution  interface”  J. Colloid and Interface Sci. 333(2009) 448-456

Author Response

1. More discussion should be presented in every part in this manuscript.

(Done)

2. Should the quality of drawings 2, 4, 5 be improved?

(Because of the lockdown and the shortage in laboratories due to virus corona, we  did the characterization of materials  only for one time)  3.If it is 3. possible, an interesting addition to this publication could be the calculated size of crystallites from XRD results by, for example, Scherrer equation.

(Not available)

4. It would be necessary to unify units according to the Si system

(Done)

5. If possible, it would be good to propose some cadmium ions adsorption mechanism.

(Done)

6. Novelty elements should be better highlighted in the introduction. Papers should be cited in the Introduction section; for example:

Hydroxyapatite with magnetic core: Synthesis methods, properties, adsorption and medical applications Advances in Colloid and Interface Science 291 (2021) 102401

Adsorption of Cd (II) ions at the hydroxyapatite/electrolyte solution interface Separation Science and Technology (Philadelphia) 51(1) 2016 11-21

The effect of  adsorption of Pb(II) and Cd(II) ions in the  presence  of EDTA on  characteristic of electrical double layer at the  ion exchanger/NaCl electrolyte solution  interface”  J. Colloid and Interface Sci. 333(2009) 448-456

(Done)

Author Response File: Author Response.pdf

Round 2

Reviewer 1 Report

There are still some typo errors. Please carefully check the manuscript again.

Author Response

- There are still some typo errors. Please carefully check the manuscript again.

(Done) we revised and check the language of the manuscript

Thanks a lot for your comments  

 

Author Response File: Author Response.pdf

Reviewer 2 Report

The authors not provided enough details. The manuscript does not match with the standards of journal water.

Author Response

The authors not provided enough details. The manuscript does not match with the standards of journal water.

We re-checked the manuscript carefully and corrected the language

Thanks for your comments  

Author Response File: Author Response.pdf

Reviewer 4 Report

I accept publication in this form.    

Author Response

Comments and Suggestions for Authors

I accept publication in this form.    

Thanks a lot 

Author Response File: Author Response.pdf

Round 3

Reviewer 2 Report

I still think that the manuscript is not suitable for the journal water. As the synthesis mechanism is unclear, and magnetic properties of the materials were not studied. Also, the authors not provided the JCPDS number file which compared the peaks. The authors did not compare the XRD peaks with many reported gamma Fe₂O₃ particles. This proves the poor validation of the material synthesized. Thus due to lack of mechanism and validation, I recommend the rejection of the manuscript. 

Author Response

We submitted this manuscript to water journal and we did all the comments suggested by reviewers.

We re-checked the manuscript again according to your comments.

Thanks a lot for your considerations, sir.

Author Response File: Author Response.pdf

This manuscript is a resubmission of an earlier submission. The following is a list of the peer review reports and author responses from that submission.