Supramolecular dynamic binary complexes with pH and salt-responsive properties for use in unconventional reservoirs

Bhargavi Bhat; Shuhao Liu; Yu-Ting Lin; Martin L. Sentmanat; Joseph Kwon; Mustafa Akbulut

doi:10.1371/journal.pone.0260786

Peer Review History

Original SubmissionJuly 5, 2021
2 Sep 2021 Decision Letter - Jay D. Schieber, Editor PONE-D-21-21931 Supramolecular dynamic binary complexes with pH and salt-responsive properties for use in unconventional reservoirs PLOS ONE Dear Dr. Akbulut, Thanks for your submission. As you see the reviewer is quite positive, but has several minor comments. Please take these into account for your revision. I do not anticipate a need to request a second review from the reviewer, provided the points are taken into account. Please make modifications to the manuscript clear. Please submit your revised manuscript by Oct 09 2021 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. 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Please see the following video for instructions on linking an ORCID iD to your Editorial Manager account: https://www.youtube.com/watch?v=_xcclfuvtxQ 4. 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 If you have cited papers that have been retracted, please include the rationale for doing so in the manuscript text, or remove these references and replace them with relevant current references.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 If you need to cite a retracted article, indicate the article’s retracted status in the References list and also include a citation and full reference for the retraction notice.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. 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 ******** 2. Has the statistical analysis been performed appropriately and rigorously? Reviewer #1: Yes ****** 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: Yes ****** 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: Article: Supramolecular dynamic binary complexes with pH and salt-responsive properties for use in unconventional reservoirs Overall Rating: publish with minor revision required This article by Bhargavi Bhat et al. presents rheological measurements on a dynamic binary complex (DBC) solution with PH and salt-responsive properties with the potential to be used in hydraulic fracturing of unconventional reservoirs. The rheological properties of samples depend on PH and salinity. They also have done sand settling experiments to check the possibility of holding the sand particles up. The manuscript is rather well written, and the results are also correctly discussed. I think that this study is worth interest for the PLOS ONE after some modifications. The following comments may help the authors to improve their manuscript: 1. Line 88: . --> , 2. Line 104: in your plots, the minimum shear rate is 10^-4 instead of 0.001 1/s. 3. Line 110: in cone- plate geometry, it is not possible to adjust the gap. How do you adjust the gap to 1 mm? 4. Line 110-112: “Dynamic shear frequency sweep measurements were performed on all of the samples at a strain amplitude of 1-10% over an angular frequency range from 0.1 to 100 rad s‒1.” Strain amplitude is constant in oscillatory frequency sweep tests. It is not correct to have a region of 1-10% for strain amplitude. Would you please clarify it? 5. Line 119: Why do you choose 7wt% of sand particles for the settling tests? Any calculation according to the real situation? Or randomly was chosen? 6. Line 143: shear rate’s unit is 1/s, not HZ! 7. Line 144: increasing the viscosity at a shear rate of 10^-3 s^-1, is not 30-fold by increasing salinity from 0wt% to 3wt%. Please check the amount of viscosity from the plot. 8. Line 223: What is the amount of the imposed shear strain/stress in the angular frequency sweep (fig 4)? 9. How the error bars are calculated in Fig. 1? Do you repeat the test several times? 10. Could you provide higher resolution images in Fig 5? Good luck! ****** 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. https://doi.org/10.1371/journal.pone.0260786.r001
Revision 1
14 Sep 2021 Author Response Dear Dr. Scheiber, We thank the reviewer for judiciously reading our manuscript and for their constructive comments and suggestions on our manuscript, “Supramolecular dynamic binary complexes with pH and salt-responsive properties for use in unconventional reservoirs.” We have carefully considered these comments/suggestions. In light of the feedback we have received, we have revised the article accordingly. Below are our responses to the comments (Changes are marked with red in the revised main text). Editorial Comments: The funding information has been removed from the acknowledgements section of the manuscript. We are fine with the current funding statement, and it does not have to be updated. The ORCID ID of the corresponding author has been linked. The reference list was judiciously reviewed, and it was ensured that there were no retracted articles. However, reference 67 (now 70) was noticed to be incomplete and that has been corrected. 3 new references regarding supramolecular systems to adequately capture the state-of-art in this area have been added to the manuscript as well. For Figure 5, we have uploaded a higher resolution image (<10 MB size limit). However, if the 10 MB can be waived, we can upload even higher resolution image that can satisfy the reviewer’s request. Kindly use the high-resolution image if possible. Reviewer Comments 1. Line 88: --> , Thank you for pointing out this typographical error. The period in this line has been replaced with a comma, as it is more appropriate. 2. Line 104: in your plots, the minimum shear rate is 10^-4 instead of 0.001 1/s. We appreciate this comment and see the issue with the axes of the figures. In order to address this, we have changed the figures (Fig1 and Fig2) to ensure that the labelled axes start at a shear rate of 10^-3 (0.001 1/s). 3. Line 110: in cone- plate geometry, it is not possible to adjust the gap. How do you adjust the gap to 1 mm? Thank you for this observation. We realized that there is an error in this sentence. In fact, we used a 40 mm parallel plate, Peltier plate steel for which gap adjustment is possible. This line has been corrected in the manuscript. 4. Line 110-112: “Dynamic shear frequency sweep measurements were performed on all of the samples at a strain amplitude of 1-10% over an angular frequency range from 0.1 to 100 rad s‒1.” Strain amplitude is constant in oscillatory frequency sweep tests. It is not correct to have a region of 1-10% for strain amplitude. Would you please clarify it? Thank you for your comments. We meant to say that the strain amplitude chosen was 1% for certain samples (pH 11 and 12) and greater values for the others (4%/10%). This is because a larger amplitude seemed necessary for the instrument to effectively detect the modulus values of less viscous samples. Furthermore, it was possible to have a larger strain amplitude for pH 9 and 10 samples because they have a larger limit of linear viscoelasticity. The above statement has been modified in the manuscript to elucidate this point. 5. Line 119: Why do you choose 7wt% of sand particles for the settling tests? Any calculation according to the real situation? Or randomly was chosen? Thank you for your question. In literature, proppant settling tests have been conducted with a wide variety of concentration of sand, as low as 5 wt% [1]. Sometimes, the approach has been to just use a single particle of sand and see how fast it settles down after travelling through the fluid [2]. This particular value of 7wt% was chosen as a good starting point which would allow us to gain a visual picture of how well sand is being captured by the matrix of the fluid. 6. Line 143: shear rates unit is 1/s, not HZ! This has been corrected in the updated manuscript 7. Line 144: increasing the viscosity at a shear rate of 10^-3 s^-1, is not 30-fold by increasing salinity from 0wt% to 3wt%. Please check the amount of viscosity from the plot. Thank you for this correction. A more accurate statement would be that there is a ~260 fold increase in viscosity at 10^(-3) s^(-1) upon changing the salinity from 0 wt% to 3 wt%. This correction has been made in the main text. 8. Line 223: What is the amount of the imposed shear strain/stress in the angular frequency sweep (fig 4)? This has been addressed in question 4. The corrected statement in the manuscript provides this information in a better fashion under the ‘Materials and Methods’ section 9. How the error bars are calculated in Fig. 1? Do you repeat the test several times? Thank you for your question. Each measurement was performed 3 times for statistical analysis. The error bars represent the standard error from the mean of the 3 measurements. We recognize this has not been mentioned clearly in the text. Hence, we have added an explanation in the materials and methods section. 10. Could you provide higher resolution images in Fig 5? Due to the image size limit, Figure 5 had to be compressed. Some resolution was lost because of this. A slightly better version that is under 10 MB has been uploaded. The link for the original high resolution file has been shared with the PLOS One as well. 1. Ahmad FA, Miskimins JL. Proppant Transport and Behavior in Horizontal Wellbores Using Low Viscosity Fluids. 2019. doi:10.2118/194379-MS 2. Shah SN. Proppant Settling Correlations for Non-Newtonian Fluids Under Static and Dynamic Conditions. Soc Pet Eng J. 1982;22: 164–170. doi:10.2118/9330-PA Sincerely, Attachments Attachment Submitted filename: Response Letter v2.docx https://doi.org/10.1371/journal.pone.0260786.r002
17 Nov 2021 Decision Letter - Jay D. Schieber, Editor Supramolecular dynamic binary complexes with pH and salt-responsive properties for use in unconventional reservoirs PONE-D-21-21931R1 Dear Dr. Akbulut, 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, Jay D. Schieber, Ph.D. Academic Editor PLOS ONE https://doi.org/10.1371/journal.pone.0260786.r003
Formally Accepted
24 Nov 2021 Acceptance Letter - Jay D. Schieber, Editor PONE-D-21-21931R1 Supramolecular dynamic binary complexes with pH and salt-responsive properties for use in unconventional reservoirs Dear Dr. Akbulut: 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. Jay D. Schieber Academic Editor PLOS ONE https://doi.org/10.1371/journal.pone.0260786.r004

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