Peer Review History

Original SubmissionNovember 28, 2020
Decision Letter - Yongjun Sun, Editor

PONE-D-20-37253

Design of facile technology for the efficient removal of hydroxypropyl guar gum from fracturing fluid

PLOS ONE

Dear Dr. Dong,

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Kind regards,

Yongjun Sun

Academic Editor

PLOS ONE

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"This project was funded by the Study on Fracturing Fluid Destabilization

Technology (XJYT-gcjsyjy-2018-JS-618)."

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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

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2. Has the statistical analysis been performed appropriately and rigorously?

Reviewer #1: N/A

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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

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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

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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: This paper involves and put forward the hydroxypropyl guar gum (HPG) removal technologies for the efficient removal of HPG from fracturing fluid. This is a meaningful work, but significant improvements need to be made in the quality and clarity of the writing. Please check the manuscript and refine the language carefully. Also, in some places the authors need to refine and improve some of the technical content. These technical issues are listed below. If the authors make properly corrections and addressed the technical content, I think the material would be publishable.

1. Is the frozen sample (solid) still having same surface microstructures of the original fracturing fluid (fluid)? It is important for the reliability of the SEM results.

2. Experimental Section, the experiment errors and accuracy should be illustrated.

3. The HPG removal technologies in this paper should be clearly specified. It also need to show in Abstract and Conclusion.

4. The adding scheme of PAC+ PAM (polyaluminium chloride + polyacrylamide) was missing. Please check and revise.

5. What are the set of requirements for “gel-breaking, coagulation and precipitation”? On the other hand, the choice basis of potassium bicarbonate (KHCO3), PAC, PAM and natural polymer flocculation (chitosan) and the adding concentration basis of the above compounds should be elucidated.

6. HPG and crude oil can be seen as organic compound. Then the organic flocculant (PAM) has a good effect in coagulation and precipitation process, which had been proved by the results in Fig. 6. What are the modes of action of inorganic flocculant (PAC) and chitosan in coagulation and precipitation process? Please add enough discuss with good reason about their results.

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Reviewer #1: No

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Revision 1

Response to Reviewers

Dear Professor,

Thank you for giving us a chance to revise the paper and the reviewer’s comments concerning our manuscript entitled “Design of facile technology for the efficient removal of hydroxypropyl guar gum from fracturing fluid” (Manuscript number: PONE-D-20-37253). Those comments are valuable and very helpful in depth to improve the quality of the paper. We have studied comments carefully and have made corrections according to the reviewer’s suggestions.

We will be greatly honored by your approval of the corrections. Thank you very much!

With best regards,

Dr. Bin Dong

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Response to Reviewers' comments:

The following is a point-to-point response to the reviewer’s comments.

Reviewer #1:

This paper involves and put forward the hydroxypropyl guar gum (HPG) removal technologies for the efficient removal of HPG from fracturing fluid. This is a meaningful work, but significant improvements need to be made in the quality and clarity of the writing. Please check the manuscript and refine the language carefully. Also, in some places the authors need to refine and improve some of the technical content. These technical issues are listed below. If the authors make properly corrections and addressed the technical content, I think the material would be publishable.

1. Is the frozen sample (solid) still having same surface microstructures of the original fracturing fluid (fluid)? It is important for the reliability of the SEM results.

Answer: Thank the reviewer for the good comments. We chose to use vacuum freeze-drying technology to convert the sample into a solid state because the original fracturing fluid cannot be directly used to characterize the surface microstructure. It is well-known that the vacuum freeze-drying is carried out at low temperature and vacuum environment, and the dried sample is very stable and convenient for long-term storage. Compared with other drying methods, the original structure of sample is almost unchanged since the drying process of the sample is completed in a frozen state. More importantly, the surface microstructure and organizational structure appearance of sample are well preserved, which means that the surface microstructure of freeze-dried fracturing fluid (solid) is the same as the that of original fracturing fluid (fluid).

2. Experimental Section, the experiment errors and accuracy should be illustrated.

Answer: Thank the reviewer for the good comments. The further explanations related to the experiment errors and accuracy have been added and marked red in the experimental section (Section 2.4.2).

3. The HPG removal technologies in this paper should be clearly specified. It also need to show in Abstract and Conclusion.

Answer: Thank the reviewer for the good comments. The more detailed description about HPG removal technologies have been improved and marked red in the revised abstract and conclusion.

4. The adding scheme of PAC+PAM (polyaluminium chloride + polyacrylamide) was missing. Please check and revise.

Answer: Thank the reviewer for the good comments. These mistakes have been carefully examined and corrected in the experimental section 2.3. The adding scheme of PAC+PAM have been described and marked red in detail in the revised manuscript.

5. What are the set of requirements for “gel-breaking, coagulation and precipitation”? On the other hand, the choice basis of potassium bicarbonate (KHCO3), PAC, PAM and natural polymer flocculation (chitosan) and the adding concentration basis of the above compounds should be elucidated.

Answer: Thank the reviewer for the good comments. As we all know, the outstanding fracturing operation requires that fracturing fluid not only has a high viscosity, but also can quickly complete the step of gel-breaking; at the same time, it must be economically feasible. In view of the characteristics of the above fracturing fluid and the in-depth study of gel-breaking and coagulation processes, the treatment plan of "gel breaking, coagulation, precipitation" was finally finalized. Moreover, the fracturing fluid used contains various complex inorganic salts, and potassium bicarbonate (KHCO3) is one of them in the actual oil field. More explicitly, one of the most important tasks is to highly simulate the fracturing fluid in actual environment. The selection of the types and concentrations of inorganic salt are based on the actual value in the real fracturing fluid. In addition, the most important step in our research is coagulation, and the difficulty is the selection of suitable flocculants. Therefore, we selected the most representative PAC, PAM and chitosan from the categories of inorganic, organic, and natural polymer flocculants. The above flocculants exhibited not only typical and representative properties, but also the more ideal treatment effects comparing with other similar flocculants in the preliminary experiment stage. Finally, the combination of different types of flocculants were applied to this technology to achieve the HPG removal. Meanwhile, through countless times optimization of the proportion of the flocculants added while considering cost, we got the final flocculants ratio as depicted in the experimental section. This ratio and concentration can not only meet the requirements for efficient removal of HPG, but also achieve the target of lowest cost.

6. HPG and crude oil can be seen as organic compound. Then the organic flocculant (PAM) has a good effect in coagulation and precipitation process, which had been proved by the results in Fig. 6. What are the modes of action of inorganic flocculant (PAC) and chitosan in coagulation and precipitation process? Please add enough discuss with good reason about their results.

Answer: Thank the reviewer for the good comments. The HPG removal technology is a series of designed processes including gel-breaking, coagulation and precipitation towards the treatment of fracturing fluids. It should be noted that coagulation was achieved through the flocculation of clever combination of different types of flocculants. They achieved the HPG removal by compressing the electric double layer, charge neutralization, adsorption bridging mechanisms and trap precipitation, which make colloidal particles form floc to precipitate and separate from the fracturing fluids. Reasonable combination of different types of flocculants can play a synergistic effect during the coagulation process. It is widely believed that adsorption bridging and charge neutralization play a major role for organic flocculant, and these mechanisms including compression of electric double layers, adsorption bridging and trap precipitation play an important role for inorganic or natural polymer flocculant. Some explanations and enough discussion have been added and marked red in the revised manuscript.

Attachments
Attachment
Submitted filename: Response to Reviewers.docx
Decision Letter - Yongjun Sun, Editor

Design of facile technology for the efficient removal of hydroxypropyl guar gum from fracturing fluid

PONE-D-20-37253R1

Dear Dr. Dong,

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,

Yongjun Sun

Academic Editor

PLOS ONE

Additional Editor Comments (optional):

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

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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

**********

3. Has the statistical analysis been performed appropriately and rigorously?

Reviewer #1: N/A

**********

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

**********

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

**********

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 made sufficient modifications according to the modification comments, and I suggest that this paper be accepted.

However, there are two suggestions to the authors:

1. It needs to emphasize that the application of natural polymer flocculation have a clear environment-friendly characteristic. As far as I’m concerned, it is a seductive choose over PAC or PAM.

2. For further in-depth research, it could be thought about how to tackle the environmental problems in coagulation and precipitation process.

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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

Formally Accepted
Acceptance Letter - Yongjun Sun, Editor

PONE-D-20-37253R1

Design of facile technology for the efficient removal of hydroxypropyl guar gum from fracturing fluid

Dear Dr. Dong:

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

Dr. Yongjun Sun

Academic Editor

PLOS ONE

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