Stability of Mesoporous Silica Using Ricinoleic Methyl Ester as a Template with the Addition of HCl and Application of Cd2+ Adsorption Optimized by Box–Behnken Design

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3/14/23, 12:56 PM Email Universitas Sumatera Utara - Acknowledgement of your Submission to RSC Advances - RA-ART-11-2022-006973

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Acknowledgement of your Submission to RSC Advances - RA-ART-11-2022-006973

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RSC Advances <[email protected]> 3 November 2022 pukul 16.37 Balas Ke: [email protected]

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Dear Dr .:

TITLE: Stability of mesoporous silica using ricinoleic methyl ester as a template with the addition of HCl and application of the adsorption Cd2+ optimized by Box–Behnken design

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3/14/23, 12:55 PM Email Universitas Sumatera Utara - Decision on submission to RSC Advances - RA-ART-11-2022-006973

Decision on submission to RSC Advances - RA-ART-11-2022-006973

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RSC Advances <[email protected]> 5 Desember 2022 pukul 10.46 Balas Ke: [email protected]

Kepada: [email protected] 05-Dec-2022

Dear Dr .:

Manuscript ID: RA-ART-11-2022-006973

Thank you for your submission to RSC Advances, published by the Royal Society of Chemistry. I sent your manuscript to reviewers and I have now received their reports which are copied below.

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REVIEWER REPORT(S):

Referee: 1

Recommendation: Major revisions Comments:

1- In "optimization of the adsorption process" say "Cu" instead "Cd" besides, the authors should indicate the ion not metal heavy, for example "Cd2+2.

2- authors according to adsorption branch or hysteresis can describe the type of porous. Besides authors can explain Why is the graph given for the MS-50 sample further away from the trend than the rest of the prepared samples?

3- how can the authors explain the behavior shown in table 3. It is assumed that as the pore size decreases then the value of the surface area must increase, however, when the pore size is greater than 2 nm ( mesopore) the material exhibits a higher specific surface value (MS-50) and when the pore sizes are smaller than 2nm (micropores) the area value decreases considerably.

4- the authors indicate that the materials develop a determined symmetry, without basing it on any of the results obtained.

OCnsider that this should be reanalyzed and well-founded based on the results shown in the manuscript.

5- On page 6 the authors mention that they apply linear and non-linear models of the Langmuir and Freundlich isotherms, but in figure 9 only the application of linear models is observed. The authors should correct this statement and also suggest applying only nonlinear models for both kinetics and isotherms.

The rest of the design and results do not show relevant or novel information for the adsorption area.

Additional Questions:

Does the work significantly advance the understanding or development in this field?: Yes Is this work of relevance to the chemistry community?: No

Are the conclusions of the work convincing and sufficiently supported by experimental evidence?: Yes Does the data provided fulfil the journal’s data requirements?

See Journal specific guidelines: <a href="https://www.rsc.org/journals-books-databases/about-journals/rsc-advances/#

Characterisation-of-new-compounds" target="_new">https://www.rsc.org/journals-books-databases/about-journals/rsc- advances/#Characterisation-of-new-compounds</a>: Yes

Is the experimental section sufficiently detailed to allow others to reproduce the work?: Yes Are the reported claims adequately discussed in the context of the literature?: No

Are the number of tables and figures in the manuscript appropriate and clear?: Yes

Referee: 2

The manuscript titled “Stability of mesoporous silica using ricinoleic methyl ester as a template with the addition of HCl and application of the adsorption Cd2+ optimized by Box–Behnken design” provides synthesis of mesoporous silica and application of the adsorption Cd2+. There are following concerns need to be clarified firstly. Hence, I think it cannot be accepted for publication of RSC Advances in this present form.

1) The authors stated that the objectives of this study are to improve the medium's chemical stability and mechanical properties. However, I think these improvements are poorly supported by experimental data of chemical stability and

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https://mail.google.com/mail/u/1/?ik=2050c0a035&view=pt&search=all&permthid=thread-f%3A1751344232328132392&simpl=msg-f%3A1751344232… 3/6 mechanical properties. The authors should provide more results and discussion by comparing these properties of this

mesoporous silica with the reported ones.

2) Page 2 right line 5 from the bottom-page 3 left line 4: The authors explained the effect of the timing and the addition of alcohol. However, the authors did not explore any effect of the timing and alcohol. For the better understanding of the readers, the authors should provide some relevance of these statements to the author’s study.

3) Fig.1(a) ”- COOOCH3” It is not clear to me. The authors should explain the chemical structure (see Fig.1) in more detail.

4) Page 4 right line 1-12: The authors should provide particle size distribution and quantitatively interpret the SEM observation.

5) Page 5 left line 5-13: The author should determine the micropore size distribution by using the DFT method or HK method and so on and discuss the elimination of microporosity based on the micro and meso pore size distribution.

Besides, I failed to find any results by the t-method in this manuscript.

6) Page 5 right line 1-12: “Pm3n symmetry and Ia3d symmetry” and “hexagonal P6m symmetry”, “interconnections between mesopores” These statements are speculative, with the authors presenting no supporting evidence. For example, the XRD analysis results indicate the mesoporous silica has amorphous.

7) The authors stated as follows; (a) Page 6 left line 2 from the bottom-right line 2: “It was found that pH (A) does not affect the percentage of Cd2+ removal efficiency. It is probably because the adsorption process is not as sensitive to changes in pH.” Nevertheless, the authors stated as follows; (b) Page 6 right line 10-17 “In the experiments, the initial pH and concentration of Cd2+ were changed to show how well Cd2+ was removed. The results showed that the pH of the solution has an essential effect on how well the process works (Fig. 8a). The efficiency of Cd2+ adsorption decrease as pH increases. It is caused by changes in the surface charges of the adsorbent and Cd2+ as a function of the pH.”

These statements((a) (b)) regarding the effect of pH are inconsistent and remains unconvincing. The authors should carefully revise the section of results and discussions with more explanations and discussions. For the better understanding of the readers, the zeta potential might be helpful to clarify the surface chemistry of adsorbent.

8) Some typos were found. Please carefully check the manuscript.

Page 2 left line 22 and page 7 left line 13, “Cu2+”: It is not clear.

Page 2 left line 22, “temperature”: The authors did not explore an effect of temperature the in this manuscript.

Does the work significantly advance the understanding or development in this field?: Yes Is this work of relevance to the chemistry community?: Yes

Are the conclusions of the work convincing and sufficiently supported by experimental evidence?: No Does the data provided fulfil the journal’s data requirements?

Characterisation-of-new-compounds" target="_new">https://www.rsc.org/journals-books-databases/about-journals/rsc- advances/#Characterisation-of-new-compounds</a>: No

Is the experimental section sufficiently detailed to allow others to reproduce the work?: Yes Are the reported claims adequately discussed in the context of the literature?: Yes

Referee: 3

Comments: This work reports an experimental work related to synthesis of mesoporous silica with addition of a specific HCl volume to increase the porous of silica. The target of the authors is extract heavy metals, such as Cd. Overall, the work was conducted with care, concluding that in the synthesis conditions performed the mesoporous silica may be formed with a high surface area. However, there are some important points that need to be clarified. Therefore, the current version of this work cannot be accepted. Major revisions are necessary. In more details:

1. Introduction is very short. The authors should include explanations and citations related to the silica surface structure, interactions of other types of metals, water interface influences etc.

2. The authors analyzed the variation of pH. However, it would importantly evaluate the ratio of the components of the reaction mixture, solvent, and temperature that can affect the regularity of the pores.

3. If the XRD results show that “all silica are amorphous”, could the regularity of the pores affect the adsorption

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4. Some reaction mechanisms should be included in the text to make clear the results.

5. I can’t understand why exactly 20 mL of HCl can form mesoporous silica with a high surface area?

6. According to Figure 8, the “ideal” point of efficiency of Cd adsorption is through a high Cd concentration and low pH.

Do the authors agree that these conditions are too extreme? In these conditions, is it possible to evaluate if the silica surface could be poisoned by Cl impurities?

7. In “Abstract” and “Conclusion”, what is the applicability of the results of this work? The conclusions are a little confusing and do not show the main applicability of this work.

Is the experimental section sufficiently detailed to allow others to reproduce the work?: Yes Are the reported claims adequately discussed in the context of the literature?: No

Referee: 4

The manuscript entitled ‘Stability of mesoporous silica using ricinoleic methyl ester as a template with the addition of HCl and application of the adsorption Cd2+ optimized by Box–Behnken design’ deals with the synthesis of mesoporous silica and its application in the sorption of Cd2+ ions. The assumptions of the article seem reasonable, but the article itself is written carelessly and chaotically. My comments are as follows:

1. Firstly, this manuscript required significant/rigorous language editing.

2. ‘Characterization’ section – What technique was used to measure the FTIR spectra?

3. ‘Optimization of the adsorption process’ section - please provide formulas for calculating Cd concentration, % sorption, as well as formulas for isotherms and kinetics.

4. ‘Results and discussions’ - the process of synthesis and the quality of the obtained silica does not depend only on the amount of HCl added - please specify what other parameters the authors took into account.

5. Fig. 1 - figures a and b appear to be the same?

6. Fig. 2a - Please explain the origin of the bands at about 2400 and 1600cm-1.

7. The authors might consider doing a grain size distribution for the obtained material.

8. Can the authors specify what type of mesoporous silica they obtained?

9. Characterization of N2 adsorption isotherms is long-winded and sloppy, it is difficult to understand the cause-and- effect sequence. Please condense and simplify this part of the article. Tab 3 and Fig. 4 show almost the same data - please decide between table or figure.

10. Why is sorption best at pH 6? What are the Cd complexes and surface charge of the material at pH 6? Once the authors state that Cd sorption is insensitive to pH changes, and later that Cd sorption depends on pH? Please clarify this.

11. Why did the authors choose the BBD and ANOVA model and not neural networks?

12. Did the authors check the possibility of sorbent regeneration?

Does the work significantly advance the understanding or development in this field?: No Is this work of relevance to the chemistry community?: Yes

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Does the data provided fulfil the journal’s data requirements?

Is the experimental section sufficiently detailed to allow others to reproduce the work?: No Are the reported claims adequately discussed in the context of the literature?: No

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3/14/23, 12:54 PM Email Universitas Sumatera Utara - Acknowledgement of your revised manuscript submission to RSC Advances - RA-ART-11-20…

Acknowledgement of your revised manuscript submission to RSC Advances - RA- ART-11-2022-006973.R1

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RSC Advances <[email protected]> 20 Desember 2022 pukul 16.17 Balas Ke: [email protected]

Cc: [email protected], [email protected], [email protected], [email protected], [email protected] 20-Dec-2022

Dear Dr .:

AUTHORS: ., Andriayani; ., Marpongahtun; Muis, Yugia; Pakpahan, Jessica; Daulay, Amru

Thank you for your revised submission to RSC Advances, published by the Royal Society of Chemistry. This is an automatic acknowledgement that you have uploaded your files to our online submission system. Your manuscript ID is:

RA-ART-11-2022-006973.R1

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3/14/23, 12:53 PM Email Universitas Sumatera Utara - Decision on submission to RSC Advances - RA-ART-11-2022-006973.R1

Decision on submission to RSC Advances - RA-ART-11-2022-006973.R1

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RSC Advances <[email protected]> 4 Januari 2023 pukul 14.17 Balas Ke: [email protected]

Kepada: [email protected] 04-Jan-2023

Dear Dr .:

Manuscript ID: RA-ART-11-2022-006973.R1

Thank you for your submission to RSC Advances, published by the Royal Society of Chemistry. I sent your revised manuscript to one of the original reviewers and I have now received their report which is copied below.

I have carefully evaluated your manuscript and the reviewer's report, and the report indicates that major revisions are necessary.

Please submit a revised manuscript which addresses all of the reviewer's comments. Further peer review of your revised manuscript may be needed. When you submit your revised manuscript please include a point by point response to the reviewer's comments and highlight the changes you have made. Full details of the files you need to submit are listed at the end of this email.

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You should submit your revised manuscript as soon as possible; please note you will receive a series of automatic reminders. If your revisions will take a significant length of time, please contact me. If I do not hear from you, I may withdraw your manuscript from consideration and you will have to resubmit. Any resubmission will receive a new submission date.

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REVIEWER REPORT(S):

Referee: 2

This manuscript corresponds to a revised version of the manuscript entitled “Stability of mesoporous silica using ricinoleic methyl ester as a template with the addition of HCl and application of the adsorption Cd2+ optimized by Box–Behnken design”. Despite effort to better consider the literature date, the literature is often wrongly used. Hence, the questions raised by the reviewer were not well answered to enhance the innovation of the manuscript. Therefore, I am sure this manuscript would require a major revision.

1) Referee2 -3)

The condensation reaction between the ricinoleic methyl ester and APMS is described differently in the manuscript (page 4 left line 16-20) and Fig.1. The authors should revise Fig.1 to make these consistent. That is, the authors should clarify the relevance of the reactions (i.e., desorption of sodium ions, desertification of methyl ions, protonation of amine group, and interaction between COO- and NH3+) to the addition of HCl. Additionally, Fig.1 (d) should be moved separately to a new figure. The drawing of Cd adsorption in Figure 1(d) is different from the reaction drawing during the synthesis in Fig.1(a-c).

2) Referee2 -5)

Since the physical properties of micropore and mesopore are not included in the present form, the author’s statement in page 5-6 (regarding Table 3 and Figure 4) are strongly speculative. More direct evidence is needed.

Besides, the evacuated temperature (i.e.,350oC for 4 h) before the nitrogen adsorption is too high to occur the dehydration condensation of surface functional groups. And then I disagree with the following calculation: “the surface area is calculated using the t-plot method by subtracting the surface area of BET with surface area, the outer surface can be identified”. The inner and external surface area can be calculated from the first and second slopes of t-plot.

3) Revised parts: Page 1 left line 5 from the bottom right line 2: “The seed Ricinus communis extracts castor oil. Castor oil is unusual among vegetable oils because it is the sole source of hydroxylated fatty acids. Castor oil extracts from the castor plant by pressing or solvent extraction, forming methyl ester when vegetable oils or animal fats combine with alcohol in a chemical reaction. Methanol and ethanol are the most used alcohols.”

Since the authors do not provide the relevance of this statement to the chemical stability and mechanical properties. The authors should delete these statements in the present form. Alternatively, these statements should be moved to the results and discussions section for explanation of the ricinoleic methyl ester as a template (page 3 right line 15 from the bottom).

4) Revised parts: Regarding the references added in the revised version, the authors should provide an appropriate reference.(For example, “reference 35” in revised version, and so on ). The authors should carefully check the manuscript before submission. (For example, page 3 right line 7 “Cu2+”)

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Are the reported claims adequately discussed in the context of the literature?: No Are the number of tables and figures in the manuscript appropriate and clear?: Yes

Referee: 3

Recommendation: Minor revisions Comments:

It's hard to locate the main changes in new text. Please, the changes in text should be marked for the reviewers. There is also an edition problem with a figure on page 12.

************

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Acknowledgement of your revised manuscript submission to RSC Advances - RA- ART-11-2022-006973.R2

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Cc: [email protected], [email protected], [email protected], [email protected], [email protected] 18-Jan-2023

Dear Dr .:

AUTHORS: ., Andriayani; ., Marpongahtun; Muis, Yugia; Pakpahan, Jessica; Daulay, Amru

Thank you for your revised submission to RSC Advances, published by the Royal Society of Chemistry. This is an automatic acknowledgement that you have uploaded your files to our online submission system. Your manuscript ID is:

RA-ART-11-2022-006973.R2

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Decision on submission to RSC Advances - RA-ART-11-2022-006973.R2

1 pesan

Kepada: [email protected] 31-Jan-2023

Dear Dr .:

Manuscript ID: RA-ART-11-2022-006973.R2

Thank you for your submission to RSC Advances, published by the Royal Society of Chemistry. I sent your revised manuscript to one of the original reviewers and I have now received their report which is copied below.

I have carefully evaluated your manuscript and the reviewer's report, and the report indicates that major revisions are necessary.

Please submit a revised manuscript which addresses all of the reviewer's comments. Further peer review of your revised manuscript may be needed. When you submit your revised manuscript please include a point by point response to the reviewer's comments and highlight the changes you have made. Full details of the files you need to submit are listed at the end of this email.

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You should submit your revised manuscript as soon as possible; please note you will receive a series of automatic reminders. If your revisions will take a significant length of time, please contact me. If I do not hear from you, I may withdraw your manuscript from consideration and you will have to resubmit. Any resubmission will receive a new submission date.

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REVIEWER REPORT(S):

Referee: 2

This manuscript corresponds to a revised version of the manuscript entitled “Stability of mesoporous silica using ricinoleic methyl ester as a template with the addition of HCl and application of the adsorption Cd2+ optimized by Box–Behnken design”. The authors previously studied the mesoporous silica using ricinoleic methyl ester as a template with the addition of HCl (Ref.22, https://doi.org/10.1016/j.cscee.2022.100287) and it is hard to find a new aspect of this study. For example, the mesoporous silica had similar structures and surface areas: BET specific surface area of 250.78 m2/g for this study and that of 163.71 m2/g for the previous study (Ref. 22). It cannot be accepted for publication of RSC Advances in this present form.

Furthermore, there is still an open question that need to be answered.

Referee2 -3)

The authors should make sure you write down the source (Ref. 22) of Fig.1.

Despite effort to better take into account the explanation for Fig.2, I do not understand this explanation (page.4 left line 9 from the bottom-page 4 right line10: Yellow highlighted text). If necessary, please clarify.

Referee2 -5)

Fig. 5 (a) and (b) shows N2 adsorption−desorption isotherms and Fig.5(c) shows the pore size distribution using the BJH method. The figure legend is incorrect. Besides, the BJH method are not applied to the analysis for micropore (less than 2 nm). Therefore, the authors provide only information regarding the BET specific surface area and the size distribution of mesopore (between 2 nm and 50 nm). More direct evidence about the micropore(<2nm) is needed. If there is no evidence, the statement regarding the micropore should be deleted.

Does the work significantly advance the understanding or development in this field?: No Is this work of relevance to the chemistry community?: Yes

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This communication is from The Royal Society of Chemistry, a company incorporated in England by Royal Charter (registered number RC000524) and a charity registered in England and Wales (charity number 207890). Registered office: Burlington House, Piccadilly, London W1J 0BA. Telephone: +44 (0) 20 7437 8656.

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