PONE-D-20-19845

Characterization of structural changes in modern and archaeological burnt bone: Implications for differential preservation bias

PLOS ONE

Dear Dr. Gallo,

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 Sep 28 2020 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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We look forward to receiving your revised manuscript.

Kind regards,

Justin W. Adams, Ph.D.

Academic Editor

PLOS ONE

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2. In your manuscript, please provide additional information regarding the specimens used in your study. Ensure that you have reported specimen numbers and complete repository information, including museum name and geographic location.

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Additional Editor Comments (if provided):

Thank you for your submission.

In reviewing the feedback from all three Reviewers, several major factors have been highlighted that will need to be considered with the manuscript in its current form. Setting aside some of the suggestions to provide greater literature integration, restructure of the manuscript to improve clarity, and potentially to reduce the background content into supplementary materials to improve readability, the primary concerns raised by the reviewers focus on: 1) providing sufficient supporting data (particularly SEM data) to support the argument and interpretations made within the manuscript; and 2) greater integration of the prmary study topic (characterisation of burnt bone) with other taphonomic processes that co-vary in assemblages and impact interpretability. I encourage you to read these comments carefully, particularly those from Reviewer 1 and 3 when revising the manuscript for resubmission. I'd also note that I would expect, given the scope of the comments and requests for greater integration and expansion of data presentation, that the resubmission will require another round of peer-review.

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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

Reviewer #2: Yes

Reviewer #3: Partly

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

Reviewer #1: N/A

Reviewer #2: Yes

Reviewer #3: Yes

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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

Reviewer #2: Yes

Reviewer #3: No

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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: No

Reviewer #2: Yes

Reviewer #3: 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: The paper is very interesting and suitable for Plos One, of broader utility. However, the originality of the paper needs to be more explicitly described, crystallinity changes are referred to burning but very little if any is referred to diagenetic influence in burnt archaeological specimens (which is the objective of the paper but finally not clearly discussed). A reorganization of the text and more clear statements and aspects to be discussed to demonstrate the goals of the paper is needed.

All referred to burnt effects from modern collection applied to fossils is well and clearly described. I believe that the inference of all analyses is that bones below carbonization are underrepresented in the fossil site T-17 unit 3. I believe the problem is to better describe what the Unit 3 of T17 is characterized for. One apparent conclusion is that burning is the cause of fragmentation, but this is not true. Burning alone does not cause fragmentation, a subsequent movement or effort may produce fragmentation, but indication of which movement or effort acted after burning is not described. Further, fragmentation before and after burning can be caused by a large number of taphonomic agents (e.g. butchery, trampling, weathering, corrosion...). None of them are described in the paper. Definitively, the paper needs a better and more exhaustive description of the fossil assemblage: number of specimens, size of fossils, surface modifications, how many fossils are in each burning stage or which have also been affected by any other taphonomic agent both before and after burning should be described or included in a table...

All should be described more in detail, all should be reorganized and described in a more organized way according to objectives and conclusions, right now it is very disorganized, lacks basic information and conclusions are not clear enough, rather an act of faith...and the paper needs several reading to follow the conclusions.

Some suggestions to the authors are included in the file attached.

Reviewer #2: The article "Characterization of structural changes in modern and archaeological burnt bone:

Implications for differential preservation bias" by Gallo et colleagues is certainly interesting, well written and argued and with a correct methodology.

Although the performed methodological procedures are well known, the modern bone analysis and the discussion involving the possible preservation bias is quite interesting.

I think that the article can be published in PlosOne after some minor revisions:

1. I like very much the introductory part, it is a very good compilation/resume of the state of the art of bone transformation research. I will suggest to try to resume all the information in a graph where the X axe is the burning temperature/time (qualitative and/or quantitative) and all the mentioned parameter-changes (Y axe) are depicted.

2. First paragraph of page 13: Describe better the sedimentological/postdepositional features indicating the mentioned features/processes. Any images of the deposits and/or bone remains? They will be very welcome.

3. Include/discuss more FTIR-ATR related references for archaeological studies in the discussion, please reivew this recent work and references therein:

Iriarte, E., García-Tojal, J., Santana, J., Jorge-Villar, S.E., Teira, L.C., Muñiz, J.R., Ibañez, J.J. (2020). Geochemical and spectroscopic approach to the characterization of earliest cremated human bones from the Levant (PPNB of Kharaysin, Jordan). Journal of Achaeological Science: Reports, 30. 102211. doi: https://doi.org/10.1016/j.jasrep.2020.102211.

Reviewer #3: The manuscript by Gallo et al discusses an interesting topic related to the behaviour and diagenesis of archaeological bones after exposition at different T. Authors compare mineralogical data from modern samples and archaeological ones. The results are interesting, but the manuscript needs more work before it can be suitable for publication. I summarise my suggestions in the following bullet points.

- The abstract is not informative about the results but mostly talk about methods. I suggest to rewrite it.

- Introduction: you explain the aims of your study, but I think that a major implication of your work is not considered in this paper. I suggest to discuss in the introduction section (and maybe in the discussion or conclusion) a further implication: are your results relevant in the field of radiocarbon dating on bones or collagen and DNA extraction? I think that you may discuss the importance of changes in crystallinity of bone apatite in the context of radiocarbon dating of archaeological bones.

-The Background section is really too long. It seems a summary of the background chapters of a PhD dissertation. I suggest to strongly reduce this section and possibly to add some parts to supplementary material or add a new table summarising available information about bones, porosity, diagenesis, solubility. All information reported in this part is very interesting but are redundant in a scientific paper.

- Looking to the cited references, I noted that you completely missed the many papers published by Gregorio dal Sasso of the University of Padua (Italy). His PhD project was dedicated to the issue of archaeological bones diagenesis after burying and he investigated in details the behaviour of buried bones in terms of changes in crystallinity and interaction with water in the archaeological deposit. I strongly suggest especially to consider the paper elaborating an universal curve for apatite crystallinity (https://www.nature.com/articles/s41598-018-30642-z).

- In the method section, please explain how you selected samples from the archaeological sequence of Tolbor. Moreover, In the result section I strongly suggest to add information about collected bones. For instance, the description of bones and their preservation is missing. The same for the model bone samples. Also, some pictures would help.

- I would also suggest to add (maybe in supplementary material) the section of Tolbon indicating the stratigraphic position of sampled bones. Please condor also that if bones come from different parts of the archaeological despots, they may have suffered different (I mean local) diagenetic process (e.g. related to water percolation or variations of pH values of the host archaeological layer); can this influence your results? the sole map of the study region is completely useless if you don't supply data on the stratigraphy of the site. Finally, it is not clear why you selected this specific archaeological sequence to carry out your experiments.

- The description of methods is also very long and many informations are very basic. I suggest to shorten this part of the manuscript or move some parts to supplementary material.

- I think the corpus of data described in the result section is robust and it is a good starting point for your discussion. Unfortunately, you do not present and discuss results of SEM investigation. Scanning microscope, I guess, may inform about the modification of apatite crystals of your samples; for instance changes in crystal shape or orientation, or can explain the evolution of diagenesis recording the process of recrystallization (evidence of dissolution and recrystallisation are very evident under the SEM). As you cited SEM in the Methods section, I think you should have interesting data to show. The only SEM images are in Fig. 7, but they are not discussed. SEM data would increase also the quality of discussion.

- Discussion: at the moment the discussion is mostly the comparison between data from modern samples and the archaeological ones. I suggest to expand the discussion also because the interaction between water and buried bones is not very clear. What is the specific potential influence of circulating water on bones heated at different T? As I already said, this may have huge implication intern in radiocarbon dating. Bone apatite is used in dating, but it is not the best, because it often underwent recrystallisation or contamination by CaCO3 (see Cherkinsky and di Lernia, Radiocarbon 2013 and some of the papers by Dal Sasso). Also, water circulating in an archaeological deposit is generally quite rich in dissolved CaCO3 and there are major exchanges of Ca2+ between fluids and bone apatite; you can also have deposition of CaCO3 along with recrystallisation of bone apatite. What is the interaction of Ca-rich fluids and bones heated at different T? You shall consider this fundamental interaction and discuss it on the basis of your data. Two main points are laking in the discussion, but they are mandatory, the interaction between CaCO3 rich water and archaeological bones, and the implication of your study to the field of radiocarbon dating of archaeological bones.

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Reviewer #1: Yes: Yolanda Fernández-Jalvo

Reviewer #2: No

Reviewer #3: No

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Attachments

Attachment

Submitted filename: PONE-D-20-19845_reviewer1_27july.pdf

PONE-D-20-19845R1

Characterization of structural changes in modern and archaeological burnt bone: implications for differential preservation bias

PLOS ONE

Dear Dr. Gallo,

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 Apr 30 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.

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: http://journals.plos.org/plosone/s/submission-guidelines#loc-laboratory-protocols

We look forward to receiving your revised manuscript.

Kind regards,

Justin W. Adams, Ph.D.

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.

Additional Editor Comments (if provided):

On behalf of myself and the reviewers I would like to thank you for resubmitting your manuscript and addressing the minor and major points raised during the first peer review.

Having received a second round of reviews from the original reviewers, there are very few minor points which have been raised and should be easily addressed.

Based on my own independent evaluation, I agree with Reviewer 2 that the current Discussion could very easily be expanded. I appreciate and understand that there is the intent to provide a more expanded faunal analysis of the T17 sample in the future, nor does every individual publication have to include comprehensive coverage of all topics and content. However, given the general audience of PLOS One, it is equally critical to highlight to broader significance and importance of results. And as this presents novel data that has immediate relevance towards the archaeological sample under analysis, it would seem to be a significant missed opportunity to take these results on burnt bone and contextualise them in light of a larger consideration as to what significance this result will have to site-based interpretations. The introductory segment highlights (pages 7-8) the significance of the site for human biogeography, use of fire, the minimal archaeological/faunal record in the region, etc. Yet the Discussion (and separate Conclusions) fail to pick up on the significance of this locality and what the presented results can inform on in the planned future research. This lends the impression that the site itself, or the descriptions of results from the site, have no particular interpretative significance (and any site therefore could have been picked); and therefore is a missed opportunity to provide a reinforcement of the significance of the results for the T17 site in addition to the broader experimental outcomes. I don't view this as a onerous task but strongly recommend expanding the Discussion to revisit the site and how these results assist in framing understandings of the deposits (and their significance as alluded to in the first description of the materials).

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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)

Reviewer #3: 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

Reviewer #2: Partly

Reviewer #3: Yes

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

Reviewer #1: N/A

Reviewer #2: N/A

Reviewer #3: Yes

**********

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

Reviewer #3: Yes

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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

Reviewer #3: 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: There are very minor changes suggested included in the pdf file attached. These refer to including a reference, be more precise in the sample size and delete a sentence from conclusions that is not really conclusion form the manuscript

Reviewer #2: Dear Authors,

I am quite surprised with the reviewed version of the manuscript. In my opinion, all the suggestions made by the reviewers were pertinent and most of them, apparently, easily realizable. But instead of reviewing and completing the manuscript with new information/discussion, it seems that the authors have choosen to rewrite and reorganize the text, it is better organized and better understood now, but they have not include new discussions or even explain the archaeological and stratigraphical context of archaeological remains analysed... or include sample´s photographs (as requested).

I feel that the analytical work and data is very OK, but the manuscript lacks a proper discussion. The nice analytical data support what already previous papers has published regarding the mineralogical, textural and compositional evolution of burned bone and it is a good starting point for a dscussion; but the discussion is just focused in comparing experimental results with results from archaeological data, it is OK, but which are the implications of having burnt bones in T17 ? Why it is important to have burned bones? How is archaeologically interpreted Unit 3?

In the same way, in the title "differential preservation bias" is mentioned, but it is not discussed in the text...which bias is detected in T17 collection? Why?

If the revisions of the reviewers are not tackled and the above mentioned comments corrected (they are easily realizable minor to moderate revisions) I think that this manuscript it is not suitable for PlosONE, it would be more appropiate for a more methodlogical/archaeometrical journal as e.g. Archaeometry or similar journals.

Reviewer #3: (No Response)

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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

Reviewer #2: No

Reviewer #3: 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.

Attachments

Attachment

Submitted filename: PONE-D-20-19845_R1_reviewer1.pdf

Characterization of structural changes in modern and archaeological burnt bone: implications for differential preservation bias

PONE-D-20-19845R2

Dear Dr. Gallo,

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.

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Kind regards,

Justin W. Adams, Ph.D.

Academic Editor

PLOS ONE

Additional Editor Comments (optional):

Thank you for your careful consideration of the minor amendments that arose during your resubmission. I appreciate your attention to the comments from the reviewers and myself as part of that process. I'm happy to recommend acceptance of the submission.

Reviewers' comments: