Adsorption of Chromium, Copper, Lead, Selenium, and Zinc ions into ecofriendly synthesized magnetic iron nanoparticles

Mutairah S. Al Shammari; Hussein M. Ahmed; Fatehy M. Abdel-Haleem; Nowarah J. Almutlq; Mohamed A. El-Khateeb

doi:10.1371/journal.pone.0289709

Peer Review History

Original SubmissionFebruary 27, 2023
29 Mar 2023 Decision Letter - Vusumzi Pakade, Editor PONE-D-23-05787Adsorption of Chromium, Copper, Lead, Selenium, and Zinc Ions into Ecofriendly Synthesized Magnetic Iron NanoparticlesPLOS ONE Dear Dr. El-Khateeb, Thank you for submitting your manuscript to PLOS ONE. After careful consideration, we feel that it has merit but does not fully meet PLOS ONE’s publication criteria as it currently stands. Therefore, we invite you to submit a revised version of the manuscript that addresses the points raised during the review process. Please submit your revised manuscript by May 13 2023 11:59PM. If you will need more time than this to complete your revisions, please reply to this message or contact the journal office at plosone@plos.org. When you're ready to submit your revision, log on to https://www.editorialmanager.com/pone/ and select the 'Submissions Needing Revision' folder to locate your manuscript file. Please include the following items when submitting your revised manuscript: A rebuttal letter that responds to each point raised by the academic editor and reviewer(s). You should upload this letter as a separate file labeled 'Response to Reviewers'. A marked-up copy of your manuscript that highlights changes made to the original version. You should upload this as a separate file labeled 'Revised Manuscript with Track Changes'. An unmarked version of your revised paper without tracked changes. You should upload this as a separate file labeled 'Manuscript'. If you would like to make changes to your financial disclosure, please include your updated statement in your cover letter. Guidelines for resubmitting your figure files are available below the reviewer comments at the end of this letter. If applicable, we recommend that you deposit your laboratory protocols in protocols.io to enhance the reproducibility of your results. Protocols.io assigns your protocol its own identifier (DOI) so that it can be cited independently in the future. For instructions see: https://journals.plos.org/plosone/s/submission-guidelines#loc-laboratory-protocols. Additionally, PLOS ONE offers an option for publishing peer-reviewed Lab Protocol articles, which describe protocols hosted on protocols.io. Read more information on sharing protocols at https://plos.org/protocols?utm_medium=editorial-email&utm_source=authorletters&utm_campaign=protocols. We look forward to receiving your revised manuscript. Kind regards, Vusumzi Pakade Academic Editor PLOS ONE Journal Requirements: When submitting your revision, we need you to address these additional requirements. 1. Please ensure that your manuscript meets PLOS ONE's style requirements, including those for file naming. The PLOS ONE style templates can be found at https://journals.plos.org/plosone/s/file?id=wjVg/PLOSOne_formatting_sample_main_body.pdf and https://journals.plos.org/plosone/s/file?id=ba62/PLOSOne_formatting_sample_title_authors_affiliations.pdf 2. We noticed you have some minor occurrence of overlapping text with the following previous publication(s), which needs to be addressed: Review of Green Methods of Iron Nanoparticles Synthesis and Applications - https://doi.org/10.1007/s12668-018-0516-5 Synthesis and Characterization of Iron Oxide Nanoparticle by Precipitation Method - https://www.arcjournals.org/pdfs/ijarps/v2-i8/6.pdf (among others) In your revision ensure you cite all your sources (including your own works), and quote or rephrase any duplicated text outside the methods section. Further consideration is dependent on these concerns being addressed. 3. 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Please include your amended statements within your cover letter; we will change the online submission form on your behalf. 5. We note that you have stated that you will provide repository information for your data at acceptance. Should your manuscript be accepted for publication, we will hold it until you provide the relevant accession numbers or DOIs necessary to access your data. If you wish to make changes to your Data Availability statement, please describe these changes in your cover letter and we will update your Data Availability statement to reflect the information you provide. 6. Please ensure that you refer to Figure 1 in your text as, if accepted, production will need this reference to link the reader to the figure. Additional Editor Comments: Academic Editor's comments: 1) Provide a conclusion in the abstract 2) pH is one of the most critical parameters influencing the adsorption of contaminants as it affects the surface chemistry and ionization of species among other things. In the current paper, various metal ions were studies and these may have different optimum pH for the removal by the nanoparticles composites. I strongly suggest that authors include a pH study in their manuscript. 3) Also, it is important that experiments are reproducible. How many replicates were used by the authors? 4) SEM and TEM analysis must be included in the revised manuscript. 5) Section 2.2 must reference Figure 1. 6) Section 2.3, describe the filter used. Is there any chance that it might have participated in the adsorption? Also considering that low concentrations of pollutants were investigated? 7) Standardize the units throughout the manuscript. 8) Sections 2.3.1, 2.3.2 and 2.3.3 can all be combined into one section. 9) Section 3.1.2. Delete the repeating sentence 10) The mechanism of the adsorption process must be explained/ 11) Kinetic models and adsorption isotherms must be used to interpret the data. [Note: HTML markup is below. Please do not edit.] Reviewers' comments: Reviewer's Responses to Questions Comments to the Author 1. Is the manuscript technically sound, and do the data support the conclusions? The manuscript must describe a technically sound piece of scientific research with data that supports the conclusions. Experiments must have been conducted rigorously, with appropriate controls, replication, and sample sizes. The conclusions must be drawn appropriately based on the data presented. Reviewer #1: No ******** 2. Has the statistical analysis been performed appropriately and rigorously? Reviewer #1: No ****** 3. Have the authors made all data underlying the findings in their manuscript fully available? The PLOS Data policy requires authors to make all data underlying the findings described in their manuscript fully available without restriction, with rare exception (please refer to the Data Availability Statement in the manuscript PDF file). The data should be provided as part of the manuscript or its supporting information, or deposited to a public repository. For example, in addition to summary statistics, the data points behind means, medians and variance measures should be available. If there are restrictions on publicly sharing data—e.g. participant privacy or use of data from a third party—those must be specified. Reviewer #1: No ****** 4. Is the manuscript presented in an intelligible fashion and written in standard English? PLOS ONE does not copyedit accepted manuscripts, so the language in submitted articles must be clear, correct, and unambiguous. Any typographical or grammatical errors should be corrected at revision, so please note any specific errors here. Reviewer #1: Yes ****** 5. Review Comments to the Author Please use the space provided to explain your answers to the questions above. You may also include additional comments for the author, including concerns about dual publication, research ethics, or publication ethics. (Please upload your review as an attachment if it exceeds 20,000 characters) Reviewer #1: The manuscript “Adsorption of Chromium, Copper, Lead, Selenium, and Zinc Ions into Ecofriendly Synthesized Magnetic Iron Nanoparticles” does not meet the minimum required scientific standard for publication in PLOS ONE. Although the work is very specific, the synthesis of magnetic Iron nanoparticles using eco-friendly methods is well studied in previous publications. The following major comments can be clarified to improve acceptability. See the comments below: 1. Section 1. The author suggests “The particle size, magnetic properties, and morphology of Fe-NPs depend on the conditions of the material” but fails to prove the statement in the characterization. SEM and /or TEM are strongly recommended for morphology and particle size measurement. 2. Section 2.2 “The production of extracts and the synthesis of Fe-NPs were carried out according to Niraimathee et al [19]”. Include the method and modification done. 3. Section 2.3 – it is not clear whether the adsorption of heavy metals was simultaneous or individual. 4. Section 3.1.2 - The inclusion of SEM results will show how morphology changes with different modifications. 5. Section 3.1.4 - “The change in the position of the absorption peak of the iron colloidal nanoparticles may be due to the change in the size of the colloidal nanoparticles [18]”. TEM results will support the changes in particle size. 6. Section 3.1.5 – The author should include EDX spectra after adsorption. 7. The author should include TGA results to assess the thermal stability of adsorbents. 8. Section 3.2.1 and 3.2.2 – Explain a significant drop in copper adsorption in figure 7 (17.26 & 20.00% respectively). 9. Can the authors compare the adsorption capacity of the adsorbents with other reported similar adsorbents? 10. The author should include pH and temperature studies as heavy metals behave differently in solution. 11. The authors should give some more information on the mechanism of interaction of the heavy metals with adsorbents, which could be in terms of the ionic forms present and the surface of the powder since they are pH dependent. The author should include the isotherm model, kinetics and thermodynamics to understand the adsorption mechanism. 12. Are these results reproducible with different batches of the adsorbents? Have you done the error analysis? Is there any effect on the size of the powder? 13. A regeneration study is important to evaluate the cost-effectiveness of the adsorbents. ****** 6. PLOS authors have the option to publish the peer review history of their article (what does this mean?). If published, this will include your full peer review and any attached files. If you choose “no”, your identity will remain anonymous but your review may still be made public. Do you want your identity to be public for this peer review? For information about this choice, including consent withdrawal, please see our Privacy Policy. Reviewer #1: No ******** [NOTE: If reviewer comments were submitted as an attachment file, they will be attached to this email and accessible via the submission site. Please log into your account, locate the manuscript record, and check for the action link "View Attachments". If this link does not appear, there are no attachment files.] While revising your submission, please upload your figure files to the Preflight Analysis and Conversion Engine (PACE) digital diagnostic tool, https://pacev2.apexcovantage.com/. PACE helps ensure that figures meet PLOS requirements. To use PACE, you must first register as a user. Registration is free. Then, login and navigate to the UPLOAD tab, where you will find detailed instructions on how to use the tool. If you encounter any issues or have any questions when using PACE, please email PLOS at figures@plos.org. Please note that Supporting Information files do not need this step. <quillbot-extension-portal></quillbot-extension-portal> Attachments Attachment Submitted filename: The manuscript comment.docx https://doi.org/10.1371/journal.pone.0289709.r001
Revision 1
9 May 2023 Author Response Dear Valued Reviewers Thank you for your valuable comments. All the comments were responded within the text with highlights. Also a separate file is submitted. PONE-D-23-05787 Adsorption of Chromium, Copper, Lead, Selenium, and Zinc Ions into Ecofriendly Synthesized Magnetic Iron Nanoparticles Academic Editor's comments: Provide a conclusion in the abstract (Done) 2) pH is one of the most critical parameters influencing the adsorption of contaminants as it affects the surface chemistry and ionization of species among other things. In the current paper, various metal ions were studies and these may have different optimum pH for the removal by the nanoparticles Done 2.3.4 Effect of pH 3) Also, it is important that experiments are reproducible. How many replicates were used by the authors? (Three time) Done 4) SEM and TEM analysis must be included in the 3.1.6 Scanning Electron Microscopy (SEM) and TEM not applicable 5) Section 2.2 must reference Figure 1. Done 6) Section 2.3, describe the filter used. Is there any chance that it might have participated in the adsorption? Also considering that low concentrations of pollutants were investigated? Done 7) Standardize the units throughout the manuscript. Done 8) Sections 2.3.1, 2.3.2 and 2.3.3 can all be combined into one section. Done 9) Section 3.1.2. Delete the repeating sentence Done 10) The mechanism of the adsorption process must be explained/ isotherm, kinetic Done, 2.4 Batch studies using adsorbent 11) Kinetic models and adsorption isotherms must be used to interpret the data. Done 2.5 Kinetic Study Reviewer #1: 1. Section 1. The author suggests “The particle size, magnetic properties, and morphology of Fe-NPs depend on the conditions of the material” but fails to prove the statement in the characterization. SEM and /or TEM are strongly recommended for morphology and particle size measurement. 3.1.6 Scanning Electron Microscopy (SEM) and TEM not applicable 2. Section 2.2 “The production of extracts and the synthesis of Fe-NPs were carried out according to Niraimathee et al [19]”. Include the method and modification done. 3. Section 2.3 – it is not clear whether the adsorption of heavy metals was simultaneous or individual. All metals dissolved in same solution (simultaneous) 4. Section 3.1.2 - The inclusion of SEM results will show how morphology changes with different modifications. Done 3.1.6 Scanning Electron microscope 5. Section 3.1.4 - “The change in the position of the absorption peak of the iron colloidal nanoparticles may be due to the change in the size of the colloidal nanoparticles [18]”. TEM results will support the changes in particle size. TEM, not available 6. Section 3.1.5 – The author should if include EDX spectra after adsorption. The EDX for materials FeNPs before done but after absorption Not, available 7. The author should include TGA results to assess the thermal stability of adsorbents. TGA,Not,available 8. Section 3.2.1 and 3.2.2 – Explain a significant drop in copper adsorption in figure 7 (17.26 & 20.00%respectively) The removal efficiency opuntia is low due to in the vacant site for adsorption and free electrons for the degradation process is very low other than adsorbents. 9. Can the authors compare the adsorption capacity of the adsorbents with other reported similar adsorbents? Table 6: Adsorption efficiencies of some selected adsorbents 10. The author should include pH and temperature studies as heavy metals behave differently in solution 2.3.4 Effect of pH, and temperature not applicable 11. The authors should give some more information on the mechanism of interaction of the heavy metals with adsorbents, which could be in terms of the ionic forms present and the surface of the powder since they are pH dependent. The author should include the isotherm model, kinetics and thermodynamics to understand the adsorption mechanism. 2.5 Kinetic Study 2.4 Batch studies using adsorbent 2.3.4 Effect of pH 12. Are these results reproducible with different batches of the adsorbents? Done, Three time Have you done the error analysis? Is there any effect on the size of the powder? Not applicable 13. A regeneration study is important to evaluate the cost-effectiveness of the adsorbents Done 3.6 Cost of adsorbents Best Regards Attachments Attachment Submitted filename: Respond to Reviewers.docx https://doi.org/10.1371/journal.pone.0289709.r002
30 May 2023 Decision Letter - Vusumzi Pakade, Editor PONE-D-23-05787R1Adsorption of Chromium, Copper, Lead, Selenium, and Zinc Ions into Ecofriendly Synthesized Magnetic Iron NanoparticlesPLOS ONE Dear Dr. El-Khateeb, Thank you for submitting your manuscript to PLOS ONE. After careful consideration, we feel that it has merit but does not fully meet PLOS ONE’s publication criteria as it currently stands. Therefore, we invite you to submit a revised version of the manuscript that addresses the points raised during the review process. Please submit your revised manuscript by Jul 14 2023 11:59PM. If you will need more time than this to complete your revisions, please reply to this message or contact the journal office at plosone@plos.org. When you're ready to submit your revision, log on to https://www.editorialmanager.com/pone/ and select the 'Submissions Needing Revision' folder to locate your manuscript file. Please include the following items when submitting your revised manuscript: A rebuttal letter that responds to each point raised by the academic editor and reviewer(s). You should upload this letter as a separate file labeled 'Response to Reviewers'. A marked-up copy of your manuscript that highlights changes made to the original version. You should upload this as a separate file labeled 'Revised Manuscript with Track Changes'. An unmarked version of your revised paper without tracked changes. You should upload this as a separate file labeled 'Manuscript'. If you would like to make changes to your financial disclosure, please include your updated statement in your cover letter. Guidelines for resubmitting your figure files are available below the reviewer comments at the end of this letter. If applicable, we recommend that you deposit your laboratory protocols in protocols.io to enhance the reproducibility of your results. Protocols.io assigns your protocol its own identifier (DOI) so that it can be cited independently in the future. For instructions see: https://journals.plos.org/plosone/s/submission-guidelines#loc-laboratory-protocols. Additionally, PLOS ONE offers an option for publishing peer-reviewed Lab Protocol articles, which describe protocols hosted on protocols.io. Read more information on sharing protocols at https://plos.org/protocols?utm_medium=editorial-email&utm_source=authorletters&utm_campaign=protocols. We look forward to receiving your revised manuscript. Kind regards, Vusumzi Pakade Academic Editor PLOS ONE Journal Requirements: Please review your reference list to ensure that it is complete and correct. If you have cited papers that have been retracted, please include the rationale for doing so in the manuscript text, or remove these references and replace them with relevant current references. Any changes to the reference list should be mentioned in the rebuttal letter that accompanies your revised manuscript. If you need to cite a retracted article, indicate the article’s retracted status in the References list and also include a citation and full reference for the retraction notice. [Note: HTML markup is below. Please do not edit.] Reviewers' comments: Reviewer's Responses to Questions Comments to the Author 1. If the authors have adequately addressed your comments raised in a previous round of review and you feel that this manuscript is now acceptable for publication, you may indicate that here to bypass the “Comments to the Author” section, enter your conflict of interest statement in the “Confidential to Editor” section, and submit your "Accept" recommendation. Reviewer #1: All comments have been addressed Reviewer #2: (No Response) ******** 2. Is the manuscript technically sound, and do the data support the conclusions? The manuscript must describe a technically sound piece of scientific research with data that supports the conclusions. Experiments must have been conducted rigorously, with appropriate controls, replication, and sample sizes. The conclusions must be drawn appropriately based on the data presented. Reviewer #1: Yes Reviewer #2: Partly ****** 3. Has the statistical analysis been performed appropriately and rigorously? Reviewer #1: Yes Reviewer #2: No ****** 4. Have the authors made all data underlying the findings in their manuscript fully available? The PLOS Data policy requires authors to make all data underlying the findings described in their manuscript fully available without restriction, with rare exception (please refer to the Data Availability Statement in the manuscript PDF file). The data should be provided as part of the manuscript or its supporting information, or deposited to a public repository. For example, in addition to summary statistics, the data points behind means, medians and variance measures should be available. If there are restrictions on publicly sharing data—e.g. participant privacy or use of data from a third party—those must be specified. Reviewer #1: Yes Reviewer #2: Yes ****** 5. Is the manuscript presented in an intelligible fashion and written in standard English? PLOS ONE does not copyedit accepted manuscripts, so the language in submitted articles must be clear, correct, and unambiguous. Any typographical or grammatical errors should be corrected at revision, so please note any specific errors here. Reviewer #1: Yes Reviewer #2: Yes ****** 6. Review Comments to the Author Please use the space provided to explain your answers to the questions above. You may also include additional comments for the author, including concerns about dual publication, research ethics, or publication ethics. (Please upload your review as an attachment if it exceeds 20,000 characters) Reviewer #1: The authors have addressed major concerns raised and the manuscript is recommended for publication in PLOS. Reviewer #2: This manuscript evaluates the ability of synthesized sorbents (Magnetic Iron Nanoparticles, Fe-NPs) derived from the peel extracts of banana, pomegranate, opuntia, orange, potato, and onion for efficient removal of Pb, Se, Cu, Zn, and Cr from aqueous solutions. The authors claimed that the prepared Fe-NPs adsorbents were effective in removing the studied heavy metals. However, the following technical aspects of the present work are lacking and were note appropriately addressed: ****** 7. PLOS authors have the option to publish the peer review history of their article (what does this mean?). If published, this will include your full peer review and any attached files. If you choose “no”, your identity will remain anonymous but your review may still be made public. Do you want your identity to be public for this peer review? For information about this choice, including consent withdrawal, please see our Privacy Policy. Reviewer #1: No Reviewer #2: No ******** [NOTE: If reviewer comments were submitted as an attachment file, they will be attached to this email and accessible via the submission site. Please log into your account, locate the manuscript record, and check for the action link "View Attachments". If this link does not appear, there are no attachment files.] While revising your submission, please upload your figure files to the Preflight Analysis and Conversion Engine (PACE) digital diagnostic tool, https://pacev2.apexcovantage.com/. PACE helps ensure that figures meet PLOS requirements. To use PACE, you must first register as a user. Registration is free. Then, login and navigate to the UPLOAD tab, where you will find detailed instructions on how to use the tool. If you encounter any issues or have any questions when using PACE, please email PLOS at figures@plos.org. Please note that Supporting Information files do not need this step.<quillbot-extension-portal></quillbot-extension-portal> Attachments Attachment Submitted filename: Review PLOS ONE.pdf https://doi.org/10.1371/journal.pone.0289709.r003
Revision 2
24 Jun 2023 Author Response There are file attached reveals the respond to the comments of the reviewers. Attachments Attachment Submitted filename: Response to Reviewers.docx https://doi.org/10.1371/journal.pone.0289709.r004
27 Jun 2023 Decision Letter - Vusumzi Pakade, Editor PONE-D-23-05787R2Adsorption of Chromium, Copper, Lead, Selenium, and Zinc Ions into Ecofriendly Synthesized Magnetic Iron NanoparticlesPLOS ONE Dear Dr. El-Khateeb, Thank you for submitting your manuscript to PLOS ONE. After careful consideration, we feel that it has merit but does not fully meet PLOS ONE’s publication criteria as it currently stands. Therefore, we invite you to submit a revised version of the manuscript that addresses the points raised during the review process. I was tempted to accept this manuscript as the reviewers have suggested but upon inspection I noted a number of details that need to be addressed. Hence, I am sending it back to major revision. I advise that authors pay due diligence to the comments made and address them as best as they could. Also, I suggest that authors find a critical reader to assist them with the manuscript packaging.Here are my concerns:1) The comments about quantitative data and conclusion in the abstract were not addressed.2) The Ce in the abstract is 1.0 mg/L, in the conclusion is 3.0 mg/L and in the authors response narrative is 6.0 mg/L. So which is which?3) Section 2.4, what is qmax?4) Section 2.4.1, Equation 3 is incorrect.5) The KL and KF values of the Langmuir and Freundlich must be properly addressed, not loosely as K.6) Table 1 title, that is XRF data not XRD.7) Table 2, the data shown there is incorrect.8) Table 3 and 4, why only show R2 values? Why not other parameters are not shown? Consider putting other data in the supporting document.9) Section 3.5 does not have data and it should be omitted and reported as such that reusability studies were not done. Also, in the authors comments, it is suggested repeatability was done 5.72 times. How is this possible? Fraction?10) Table 6 should compare the adsorption capacity of the current study to literature not just listing the literature values alone.11) What significant FTIR peaks were observed? This can be used to suggest successful synthesis and/ or adsorption. This value (s) can be quoted in the conclusion and abstract.12) Again, what properties of Fe-NPs were explored or came to the fore during adsorption? This was asked before by a reviewer and needs to be included in the conclusion.13) Authors are advised to scrutinize their manuscript even for comments not made here and make necessary adjustments. Please submit your revised manuscript by Aug 11 2023 11:59PM. If you will need more time than this to complete your revisions, please reply to this message or contact the journal office at plosone@plos.org. When you're ready to submit your revision, log on to https://www.editorialmanager.com/pone/ and select the 'Submissions Needing Revision' folder to locate your manuscript file. Please include the following items when submitting your revised manuscript: A rebuttal letter that responds to each point raised by the academic editor and reviewer(s). You should upload this letter as a separate file labeled 'Response to Reviewers'. A marked-up copy of your manuscript that highlights changes made to the original version. You should upload this as a separate file labeled 'Revised Manuscript with Track Changes'. An unmarked version of your revised paper without tracked changes. You should upload this as a separate file labeled 'Manuscript'. If you would like to make changes to your financial disclosure, please include your updated statement in your cover letter. Guidelines for resubmitting your figure files are available below the reviewer comments at the end of this letter. If applicable, we recommend that you deposit your laboratory protocols in protocols.io to enhance the reproducibility of your results. Protocols.io assigns your protocol its own identifier (DOI) so that it can be cited independently in the future. For instructions see: https://journals.plos.org/plosone/s/submission-guidelines#loc-laboratory-protocols. Additionally, PLOS ONE offers an option for publishing peer-reviewed Lab Protocol articles, which describe protocols hosted on protocols.io. Read more information on sharing protocols at https://plos.org/protocols?utm_medium=editorial-email&utm_source=authorletters&utm_campaign=protocols. We look forward to receiving your revised manuscript. Kind regards, Vusumzi Pakade Academic Editor PLOS ONE Additional Editor Comments: All comments are provided in the email above. [Note: HTML markup is below. Please do not edit.] [NOTE: If reviewer comments were submitted as an attachment file, they will be attached to this email and accessible via the submission site. Please log into your account, locate the manuscript record, and check for the action link "View Attachments". If this link does not appear, there are no attachment files.] While revising your submission, please upload your figure files to the Preflight Analysis and Conversion Engine (PACE) digital diagnostic tool, https://pacev2.apexcovantage.com/. PACE helps ensure that figures meet PLOS requirements. To use PACE, you must first register as a user. Registration is free. Then, login and navigate to the UPLOAD tab, where you will find detailed instructions on how to use the tool. If you encounter any issues or have any questions when using PACE, please email PLOS at figures@plos.org. Please note that Supporting Information files do not need this step. <quillbot-extension-portal></quillbot-extension-portal> https://doi.org/10.1371/journal.pone.0289709.r005
Revision 3
3 Jul 2023 Author Response Dear Valued Editor, Thank you for your help and support. Your comments are helpful and improving the article a lot. The following Table shows the response to these comments. 1 The comments about quantitative data and conclusion in the abstract were not addressed. 2 The Ce in the abstract is 1.0 mg/L, in the conclusion is 3.0 mg/L and in the authors response narrative is 6.0 mg/L. So which is which? 3.0 mg/L modified 3 Section 2.4, what is qmax qe (mg/g) modified 4 Section 2.4.1, Equation 3 is incorrect Done - delete 5 The KL and KF values of the Langmuir and Freundlich must be properly addressed, not loosely as K. Done 6 Table 1 title, that is XRF data not XRD Done Table 1: The XRF analysis of Fe-NPs (%) 7 Table 2, the data shown there is incorrect. Done modified Table 2: The Fe-NPs adsorbent's maximal adsorption capacity is compared to that of other adsorbents used in the removal of metal ions 8 Table 3 and 4, why only show R2 values? Why not other parameters are not shown? Consider putting other data in the supporting document. Done Table 3: The parameters of Langmuir and Freundlich isotherm models for Cu, Se, Zn, Pb, and Cr adsorption on the banana, potato, orange, onion, opuntia, and pomegranate Table 4: The parameters of pseudo-second-order model parameters of Cu, Se, Zn, Pb, and Cr adsorption onto iron nanoparticles of banana, potato, orange, onion, opuntia, and pomegranate 9 Section 3.5 does not have data and it should be omitted and reported as such that reusability studies were not done. Also, in the authors comments, it is suggested repeatability was done 5.72 times. How is this possible? Fraction? Done – delete 10 Table 6 should compare the adsorption capacity of the current study to literature not just listing the literature values alone. Table 6 was deleted and corporated into Table 2 11 What significant FTIR peaks were observed? This can be used to suggest successful synthesis and/ or adsorption. This value (s) can be quoted in the conclusion and abstract. Done The functional groups were examined and responsible for adsorption process by nanoparticle powder sample, these peaks are 3400 cm−1, 2900 cm-1, 1600 cm−1,1000 cm−1, and 1550 cm−1. 12 Again, what properties of Fe-NPs were explored or came to the fore during adsorption? This was asked before by a reviewer and needs to be included in the conclusion. Done The preparation of iron nanoparticles was characterized many distinct magnetic properties, the ability to control their size, morphology, and high surface area properties, have many functions group responsible for adsorption process 13 13) Authors are advised to scrutinize their manuscript even for comments not made here and make necessary adjustments. Done Table 1: The XRF analysis of Fe-NPs (%) Component Fe-NPs banana Fe-NPs Potato Fe-NPs Onion Fe-NPs Orange Fe-NPs Opuntia Fe-NPs Pomegranate Fe2O3 58.9 53.9 67.3 46.6 49 46.6 Na2O 14 16.1 8.39 22.1 20.1 22.1 MnO 0.46 0.53 0.63 0.46 0.46 0.46 CaO 0.28 0.3 0.47 0.27 0.27 0.27 SiO2 0.25 0.37 0.38 0.36 0.36 0.36 Al2O3 0.1 0.09 0.08 0.07 0.07 0.07 K2O 0.05 0.05 0.14 ---- 0.07 0.07 SO3-- 0.08 0.09 0.05 0.07 ---- ---- Cr2O3 0.05 0.05 0.05 ---- 0.04 0.04 MgO 0.04 0.04 0.04 0.04 ----- ----- Cl- 16.1 9.63 11.6 14.9 13.9 14.9 LOI 9.61 18.8 9.51 15.1 15.1 15.1 Total 99.94 99.98 99.94 99.99 99.37 99.99 Table 2: The Fe-NPs adsorbent's maximal adsorption capacity is compared to that of other adsorbents used in the removal of metal ions Adsorbents Adsorbants Q max Reference Untreated rice husk Direct dyes 2.4 (Abdelwahab, El Nemr et al. 2005) Activated rice husk Direct dyes 4.3 (Abdelwahab, El Nemr et al. 2005) Red-mud Ni+2 0.0018 (Lakshmi Narayan, Govindan et al. 2013) Peanut Hulls Fe+3 and Cu+2 79.28 and 96.58 mg/g for Fe+3 and Cu+ (Salam, Reiad et al. 2011) Zeolite derived from fly ash Cu+2 14.7 (Mishra and Tiwari 2006) Ag nanoparticle-loaded activated carbon (Ag-NP-AC) Cu+2 60 (Shahamirifard, Ghaedi et al. 2016) Iron oxide coated eggshell powder Cu+2 6.7 (Liu, Liang et al. 2005) Chitosan Cu+2 62.4 (Crini 2005) Figure 11: Effect of pH on removal of Cu, Pb, Se, Zn, and Cr by iron nanoparticles of banana, potato, orange, onion, opuntia, and pomegranate, the other conditions kept constant, the during the adsorption processes dose=04 g/L, Initial conc.= 3.0 mg/L and rpm 150/45 min 3.3 Adsorption Isotherms The adsorption isotherms of the studied metals on the iron nanoparticles for extracts of banana, potato, orange, onion, opuntia, and pomegranate, were based on the optimum operating conditions which were 0.4 g at pH 6.0 Figure 12. The linearization was performed according to the mathematical models of Freundlich. Table 3 shows the parameters of Langmuir and Freundlich models obtained and the correlation coefficients of adsorption data. The experimental results of Cu, Pb, Cr, Zn, and Se adsorption on the banana, potato, orange, onion, opuntia, and pomegranate comply with the Freundlich isotherm model according to R2 studied (Gonçalves Junior, Meneghel et al. 2013). The model that best fitted for metal adsorption was Freundlich, indicating that the adsorption occurred in multiple layers(Gonçalves Junior, Meneghel et al. 2013). The calculated parameters for the Langmuir and Freundlich models are shown in Table 3, along with the correlation coefficients for the adsorption data. According to the experimental results of Cu, Pb, Cr, Zn, and Se adsorption on the iron nanoparticles of banana, potato, orange, onion, opuntia, and pomegranate, the adsorption took place in multiple layers and was consistent with the Freundlich isotherm model (Gonçalves Junior, Meneghel et al. 2013). The metals Cu, Cr, Se, and Zn have higher adsorption capacities (qm) and the highest binding energies with the adsorbent in the Langmuir linearization. As the adsorbents ranged from 1.3 to 388 (mg/g), the values of KF for Cu, Se, Zn, Pb, and Cr were calculated from Table 3. The characteristics of each metal and the manner of interaction with the adsorbents can be linked to this adsorption sequence. The magnitudes of KF demonstrate the simple removal of metal ions from the aqueous solution and suggest an advantageous adsorption process (Kumar and Kirthika 2009, Gonçalves Junior, Meneghel et al. 2013, dos Santos, de Toledo Gomes et al. 2019). Figure 12: The Langmuir and Freundlich isotherms models of Pb; Cr Se Cu, and Zn onto iron nanoparticles of banana, potato, orange, onion, opuntia, and pomegranate, the other conditions kept constant, the during the adsorption processes dose=04 g/L, and rpm 150/45 min Table 3: The Langmuir and Freundlich isotherm models for Cu, Se, Zn, Pb, and Cr adsorption on the banana, potato, orange, onion, opuntia, and pomegranate Langmuir isotherm models R2 qmax KL Pb Cu Cr Zn Se Pb Cu Cr Zn Se Pb Cu Cr Zn Se Fe NPs (Banana) 0.7345 0.7767 0.7954 0.8237 0.9674 25000 33333 33333 23 22 0.0002 0.66 0.76 0.73 0.75 Fe NPs (Potato) 0.4878 0.9621 0.9621 0.4749 0.4709 25000 33653 33245 49595 50000 0.0003 0.0002 0.0002 0.0002 0.0002 Fe NPs (Orange) 0.6942 0.6439 0.6436 0.6955 0.6936 33333 33457 34873 34332 33333 0.0002 0.0002 0.0002 0.0002 0.0002 Fe NPs (Onion) 0.8393 0.6949 0.6949 0.8667 0.0017 25000 34233 33333 21 20 0.0002 0.0014 0.13 0.16 0.81 Fe NPs (Opuntia) 0.3581 0.2771 0.2778 0.9704 0.9478 20000 44 43 20 20 0.0006 0.0005 0.13 0.98 1.0 Fe NPs (Pomegranate) 0.964 0.9661 0.966 0.941 0.9869 58 55 58 21 22 0.18 0.16 0.18 0.64 0.62 R2 N KF Freundlich isotherm models Pb Cu Cr Zn Se Pb Cu Cr Zn Se Pb Cu Cr Zn Se Fe NPs (Banana) 0.8554 0.9791 0.9792 0.9056 0.9789 5.53 5.33 6.33 7.01 7.22 9.0 9.40 9.13 8.7 6.5 Fe NPs (Potato) 0.889 0.977 0.9873 0.7134 0.7042 0.24 0.34 0.42 0.98 1.55 343 12.3 66 54 44 Fe NPs (Orange) 0.876 0.8702 0.8679 0.8701 0.8661 0.21 0.33 0.54 6.98 6.87 345 12.3 22 14 13 Fe NPs (Onion) 0.9449 0.8722 0.8679 0.9332 0.1545 0.20 6.8 7.40 7.35 7.44 388 12.3 55 14 12 Fe NPs (Opuntia) 0.9757 0.9772 0.4986 0.988 0.9767 0.64 4.4 4.46 3.65 3.98 55 1.3 1.3 1.5 1.3 Fe NPs (Pomegranate) 0.9831 0.9775 0.9725 0.9726 0.9961 0.59 1.7 1.72 1.56 1.66 66 13 11 1.4 11 3.4. Kinetic study Figure 13 shows the kinetics models for Cu, Pb, Se, Zn, and Cr ion adsorption onto banana, potato, orange, onion, opuntia, and pomegranate. The relation between log (qeq-qt) and t. The K1 and qe are obtained from the slope and intercept, respectively. The correlation coefficients (R2) of the pseudo-first-order kinetic model are non-linear but the pseudo-second-order kinetic model linear line, the correlation coefficients (R2) of the pseudo-second-order is shown in Table 4:. The results suggested that the overall rates of adsorption of Cu, Pb, Se, Zn, and Cr ions onto banana, potato, orange, onion, opuntia, and pomegranate were controlled by chemisorption (Ibrahim Hegazy 2021). Besides, the value of R2 (linear correlation) around 1 in pseudo-second-order confirms that the adsorption kinetics is controlled by this order and that there is a strong interaction between adsorbent and adsorbate. Figures 13 showed the kinetics models for Cu, Pb, Se, Zn, and Cr ion adsorption onto banana, potato, orange, onion, opuntia, and pomegranate. The pseudo-first-order kinetic model shows in Figure 13, that’s shows the relation between log (qeq-qt) and t, and through this relation the values K1 and qe could be deduced from the slope and intercept, respectively. The correlation coefficients (R2) of the pseudo-second-order kinetic model are higher than the pseudo-first-order kinetic model, and qe values calculated from the pseudo-second-order kinetic model are very close to the experimental with freundlich isotherm model. The results suggested that the overall rates of adsorption of Cu, Pb, Se, Zn, and Cr ion onto adsorption onto banana, potato, orange, onion, opuntia, and pomegranate by physical adsorption [46]. Figure 13: The pseudo-first-order and pseudo-second-order of Pb, Cr, Se, Cu, and Zn onto iron nanoparticles of banana, potato, orange, onion, opuntia, and pomegranate, the other conditions kept constant, the during the adsorption processes dose=04 g/L, initial concentration 3.0 mg/L, and speed 150 rpm Table 4: The parameters of pseudo-second-order model parameters of Cu, Se, Zn, Pb, and Cr adsorption onto iron nanoparticles of banana, potato, orange, onion, opuntia, and pomegranate Adsorbents/ metal R2 q K2 Pb Cu Cr Zn Se Pb Cu Cr Zn Se Pb Cu Cr Zn Se FeNPs/Potato 0.9974 0.9974 0.9974 0.9134 0.9001 10.8 10.75 7.14 7.14 7.78 0.001 0.001 0.015 0.01 0.01 FeNPs/Banana 0.9425 0.9712 0.9567 0.9223 0.9113 10.43 10.30 1.88 1.88 1.98 0.001 0.001 0.007 0.007 0.007 FeNPs/Onion 0.9325 0.9711 0.225 0.9012 0.913 9.11 9.01 8.33 8.33 8.76 0.003 0.004 0.0008 0.0008 0.0007 FeNPs/Opuntia 0.9911 0.9468 0.9911 0.915 0.9563 0.87 0.83 11.11 100 101 0.011 0.013 0.0016 0.00001 0.00001 FeNPs/Orang 0.9971 0.9717 0.9442 0.9334 0.9553 11.28 11.23 3.03 3.03 3.12 0.001 0.001 0.003 0.003 0.004 FeNPs/pomegranate 0.9974 0.9525 0.9627 0.9011 0.991 11.87 11.36 8.33 8.33 8.34 0.001 0.0015 0.005 0.003 0.003 Attachments Attachment Submitted filename: response 30-6 .docx https://doi.org/10.1371/journal.pone.0289709.r006
25 Jul 2023 Decision Letter - Vusumzi Pakade, Editor Adsorption of Chromium, Copper, Lead, Selenium, and Zinc Ions into Ecofriendly Synthesized Magnetic Iron Nanoparticles PONE-D-23-05787R3 Dear Dr. El-Khateeb, We’re pleased to inform you that your manuscript has been judged scientifically suitable for publication and will be formally accepted for publication once it meets all outstanding technical requirements. Within one week, you’ll receive an e-mail detailing the required amendments. When these have been addressed, you’ll receive a formal acceptance letter and your manuscript will be scheduled for publication. An invoice for payment will follow shortly after the formal acceptance. To ensure an efficient process, please log into Editorial Manager at http://www.editorialmanager.com/pone/, click the 'Update My Information' link at the top of the page, and double check that your user information is up-to-date. If you have any billing related questions, please contact our Author Billing department directly at authorbilling@plos.org. If your institution or institutions have a press office, please notify them about your upcoming paper to help maximize its impact. If they’ll be preparing press materials, please inform our press team as soon as possible -- no later than 48 hours after receiving the formal acceptance. Your manuscript will remain under strict press embargo until 2 pm Eastern Time on the date of publication. For more information, please contact onepress@plos.org. Kind regards, Vusumzi Pakade Academic Editor PLOS ONE Additional Editor Comments (optional): Improve the quality of the graphs. Reviewers' comments: <quillbot-extension-portal></quillbot-extension-portal> https://doi.org/10.1371/journal.pone.0289709.r007
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2 Oct 2023 Acceptance Letter - Vusumzi Pakade, Editor PONE-D-23-05787R3 Adsorption of Chromium, Copper, Lead, Selenium, and Zinc Ions into Ecofriendly Synthesized Magnetic Iron Nanoparticles Dear Dr. El-Khateeb: I'm pleased to inform you that your manuscript has been deemed suitable for publication in PLOS ONE. Congratulations! Your manuscript is now with our production department. If your institution or institutions have a press office, please let them know about your upcoming paper now to help maximize its impact. If they'll be preparing press materials, please inform our press team within the next 48 hours. Your manuscript will remain under strict press embargo until 2 pm Eastern Time on the date of publication. For more information please contact onepress@plos.org. If we can help with anything else, please email us at plosone@plos.org. Thank you for submitting your work to PLOS ONE and supporting open access. Kind regards, PLOS ONE Editorial Office Staff on behalf of Prof. Vusumzi Pakade Academic Editor PLOS ONE https://doi.org/10.1371/journal.pone.0289709.r008

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