Peer Review History
| Original SubmissionSeptember 19, 2025 |
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Dear Dr. kavak, 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. All comments need to be addressed in detail before re-submission. ============================== Please submit your revised manuscript by Jan 08 2026 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.. 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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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, Peter F. Biehl, PhD 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 2. In your manuscript, please provide additional information regarding the specimens used in your study. Ensure that you have reported human remain specimen numbers and complete repository information, including museum name and geographic location. 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Please note that, though access restrictions are acceptable now, your entire data will need to be made freely accessible if your manuscript is accepted for publication. This policy applies to all data except where public deposition would breach compliance with the protocol approved by your research ethics board. If you are unable to adhere to our open data policy, please kindly revise your statement to explain your reasoning and we will seek the editor's input on an exemption. Please be assured that, once you have provided your new statement, the assessment of your exemption will not hold up the peer review process. 4. Please upload a copy of Figure 17, to which you refer in your text on page 14. If the figure is no longer to be included as part of the submission, please remove all reference to it within the text. 5. Please include captions for your Supporting Information files at the end of your manuscript, and update any in-text citations to match accordingly. Please see our Supporting Information guidelines for more information: http://journals.plos.org/plosone/s/supporting-information .. 6. If the reviewer comments include a recommendation to cite specific previously published works, please review and evaluate these publications to determine whether they are relevant and should be cited. There is no requirement to cite these works unless the editor has indicated otherwise. Additional Editor Comments: Your manuscript has now been seen by a referee, whose comments are appended below. You will see from these comments that while the referees find your work of potential interest, they have raised substantial concerns that must be addressed. In light of these comments, we cannot accept the manuscript for publication, but would be interested in considering a revised version that addresses these serious concerns. We hope you will find the referees' comments useful as you decide how to proceed. Should presentation of further data and analysis allow you to address these criticisms, we would be happy to look at a substantially revised manuscript. However, please bear in mind that we will be reluctant to approach the referees again in the absence of major revisions. [Note: HTML markup is below. Please do not edit.] Reviewer's Responses to Questions Comments to the Author 1. Is the manuscript technically sound, and do the data support the conclusions? Reviewer #1: Partly ********** 2. Has the statistical analysis been performed appropriately and rigorously? -->?> Reviewer #1: N/A ********** 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??> Reviewer #1: Yes ********** Reviewer #1: This paper presents a study on a sample of charred bread dating back to the Bronze Age and found in Anatolia. The sample was analysed using optical and electron microscopy techniques, but also subjected to chemical analysis using EDX, FTIR, Raman and TG-DSC. The purpose of the analysis was to determine the raw materials used and the methods of preparation. ABSTRACT: It seems clear to me, but I would add at least a mention of the type of analysis conducted, in order to make it more interesting for an audience with a more scientific background. INTRODUCTION: The introduction clearly presents the importance of bread in human history, citing the main discoveries of ancient bread and reconstructing the history of this food with its highly symbolic and ritualistic power. The introduction also describes the site of origin of the sample analysed. In my opinion, given the type of journal chosen for publication, at least one paragraph dedicated to the scientific analysis of ancient bread is missing. This addition would serve to outline the state of the art in this field and justify the choice of analytical techniques used. MATERIALS AND METHODS: In my opinion, all experimental details should be collected in this section and not in the discussion of results section. These details should also be completed, according to the instructions given in the specific comments. RESULTS AND DISCUSSION: This section presents the results divided by technique. The idea is good, but the sections on SEM-EDX, FTIR, Raman and TG-DSC analyses need to be revised in terms of the interpretation of the results. CONCLUSIONS: Perhaps a little long, some considerations could be brought forward to the ‘Results and discussion’ section. ENGLISH LANGUAGE: The text is sufficiently clear, but needs some revisions to correct typos or a few incomplete sentences. BIBLIOGRAPHY: There are only 2 self-citations out of 35 papers cited. As mentioned in the specific comments, I would suggest expanding the bibliography on the application of analytical techniques on similar samples of archaeological bread. Specific comments: 1) Line 107 "Plant remains were obtained from the soil samples using a flotation system" Please provide some more information about the flotation system used. 2) Lines 116-117 "The oval, flat bread measures 12 cm in diameter and 2.5 cm thick" In my opinion, these details should be included in the materials and methods section. 3) Lines 127-128 "Conducted microscopic and elemental analyses to determine the carbonized bread sample's composition, production method, and plant content" Please check this sentence, which appears to be incomplete. 4) Lines 128-132 Some instrumental details are missing, such as the energy used, the type of electrons used to collect the image, and the type of elemental analysis conducted (point? Area?). Was the sample metallised or observed as is? Were one or more fragments taken from the entire sample of bread found? 5) Lines 142-143 "Triticum dicoccum (emmer wheat) seed particles and bran were identified by the analysis (Fig. 7)." What are the distinctive features that allowed the plant structures observed to be identified as emmer wheat? 6) Lines 159-160 "A detailed SEM analysis revealed starch granules of different morphologies and sizes (Fig. 10)." Are the shape and size of these granules consistent with the identified plant species? 7) Lines 166-168 "The analysis revealed carbon (C) as the most dominant The element's concentration ranged from 49.4% to 59.8%, indicating that the organic structure was largely preserved through carbonization" This sentence needs to be revised from a grammatical point of view. Furthermore, even if the organic structure had not been preserved during carbonisation, the result would still be to have a lot of carbon. In my opinion, the amount of carbon present cannot be used to assess the state of preservation of the bread sample. 8) Lines 169-170 "The high concentration of these two elements indicates that heat treatment and burial stabilize the carbon-based organic molecules" The same considerations made in the previous point apply here. Even after exposure to heat, the initial carbon remains carbon... 9) Lines 176-177 "These multifaceted analyses demonstrate that the Küllüoba bread is not merely a carbonized residue but also preserves molecular-level traces of its plant components" As already specified, EDX analysis cannot provide information at the molecular level, but only at the elemental level. 10) Line 183 "Vibrational spectroscopy is a nondestructive characterization technique" That is not entirely correct. Some vibrational spectroscopy techniques are non-destructive, while others require, for example, grinding of the sample. 11) Line 184 "Fourier Transformed InfraRed (FTIR) spectra" Transform, not Transformed 12) Lines 186-195 "Both spectra are complementary since FTIR detects vibrations based on electrical dipole moment changes, while Raman detects vibrations based on electrical polarizability changes. In other words, FTIR is sensitive to polar bonds affected by connected atoms or surrounding molecules. On the other hand, Raman is sensitive to the ability of the electron cloud to distort the bond (nonpolar covalent bonds, symmetric vibrational bonds, aromatic and conjugated systems, or heavy atomic bonds). During Raman measurement, the molecule's vibrational energy level briefly reaches a high-energy collision state and returns to a lower energy state by emitting a photon. The difference between the emitted photon and the excitant laser frequencies provides the Raman shift. The Raman shift corresponds to the frequency of the fundamental IR absorbance band of the bonds" I am not sure it is necessary to introduce the theory of infrared and Raman spectroscopy in a paper of this kind. I assume that most readers know what we are talking about, or know where to find information if they do not already have it. However, specific information on the analyses carried out is completely missing: brand and model of the instruments, analysis intervals, types of sources and detectors, resolution, number of scans, etc. For infrared spectroscopy: was an ATR technique used? All this information is fundamental in a scientific article, much more so than the theory of spectroscopy. 13) Line 202 "spectra of breads investigated in the modern literature" Does the term ‘modern’ refer to literature or bread? From personal experience, I know that it is not easy to find studies that apply infrared spectroscopy to samples of ancient bread and that it is therefore common practice to compare the spectra obtained with those recorded on samples of modern bread. It also seems to me that the few studies of infrared spectroscopy on ancient bread have not been cited here. 14) Lines 205-206 "Deconvolution of the latter group of peaks shows that there are so many peaks that it is not possible to assign a meaning to specific molecules" To be precise, individual peaks are not associated with molecules, but with specific vibrations within a molecule. Only by grouping together the information provided by multiple peaks is it possible to identify the molecule that produced them. 15) Lines 208-209 "those between 1750-2400 cm⁻¹ represent conjugated double or triple bonds between C, N, and/or O" Looking at the spectrum, there do not appear to be any peaks in this region. The spectrum is extremely noisy, probably due to moisture in the sample or an unsatisfactory background correction. It would nevertheless be advisable to indicate at least the main peaks discussed in the text on the spectrum. 16) Lines 210-211 "but probably not all of them are related to the bread structure." On what basis can this statement be justified? 17) Lines 222-224 "The lack of carbonyls may be natural, but the presence of a large number of additives (grains, leaves…) also suggests that carbonyl groups have probably disappeared in the structure." This sentence is unclear. 18) Lines 242-244 "the attenuated C-H stretching modes suggest that the bread dough was prepared with a minimum amount of water and possibly without oil and/or salt." However, line 236 stated that the attenuation of these peaks was due to the presence of oil and/or salt. 19) Line 264 "The thermogravimetric analysis result (Setaram, Labsys Evo analyzer)" Here too, details such as heating rate and, above all, the type of atmosphere used (nitrogen, air, etc.) are missing. 20) Line 265 "shows a maximum mass loss of 13% when the temperature reaches 150°C." Please explain this sentence more clearly. 21) Lines 266-267 "Therefore, it can be assumed that the Küllüoba bread is above 150°C. " Please explain this sentence more clearly. 22) Lines 269-271 "which changes at endothermic values between 50 and 150°C, indicating that the chemical bonds in the bread are broken between these temperatures" It is not necessarily the case that bonds are broken; even the evaporation of moisture generates an endothermic peak in DSC. 23) Lines 271-273 "The exothermic heat flow observed when the temperature rises above 160°C may be due to the formation of new bonds, suggesting that the possibility is likely baked at this temperature." I honestly don't see the exothermic peak above 160°C. Could you indicate it clearly, perhaps with an arrow? On the contrary, I see a slight endothermic peak just before 250°C, linked to the corresponding weight loss. 24) Lines 315-317 "These samples, which show no significant differences compared to those inside the furnaces and are similar in content; they were probably scattered across the area as debris while cleaning the hearths" Please check this sentence because it seems incomplete. ********** what does this mean? ). If published, this will include your full peer review and any attached files.). 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? 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| Revision 1 |
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Archaeometric analysis of Early Bronze Age bread from Küllüoba Höyük PONE-D-25-50027R1 Dear Dr. kavak, 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 will be generated when your article is formally accepted. Please note, if your institution has a publishing partnership with PLOS and your article meets the relevant criteria, all or part of your publication costs will be covered. Please make sure your user information is up-to-date by logging into Editorial Manager at Editorial Manager® and clicking the ‘Update My Information' link at the top of the page. For questions related to billing, please contact and clicking the ‘Update My Information' link at the top of the page. For questions related to billing, please contact billing support .. 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, Enrico Greco Academic Editor PLOS One Additional Editor Comments (optional): Reviewers' comments: Reviewer's Responses to Questions Comments to the Author Reviewer #1: All comments have been addressed ********** 2. Is the manuscript technically sound, and do the data support the conclusions??> 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??> Reviewer #1: Yes ********** Reviewer #1: I have carefully re-read the paper and it has improved substantially, both in terms of content and in the structure and readability of the text. All the issues I previously raised appear to have been fully addressed. I have no further comments and believe the manuscript is now suitable for publication. ********** what does this mean? ). If published, this will include your full peer review and any attached files.). 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 For information about this choice, including consent withdrawal, please see our Privacy Policy .--> Reviewer #1: No ********** |
| Formally Accepted |
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PONE-D-25-50027R1 PLOS One Dear Dr. kavak, I'm pleased to inform you that your manuscript has been deemed suitable for publication in PLOS One. Congratulations! Your manuscript is now being handed over to our production team. At this stage, our production department will prepare your paper for publication. This includes ensuring the following: * All references, tables, and figures are properly cited * All relevant supporting information is included in the manuscript submission, * There are no issues that prevent the paper from being properly typeset You will receive further instructions from the production team, including instructions on how to review your proof when it is ready. Please keep in mind that we are working through a large volume of accepted articles, so please give us a few days to review your paper and let you know the next and final steps. Lastly, 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. You will receive an invoice from PLOS for your publication fee after your manuscript has reached the completed accept phase. If you receive an email requesting payment before acceptance or for any other service, this may be a phishing scheme. Learn how to identify phishing emails and protect your accounts at https://explore.plos.org/phishing. If we can help with anything else, please email us at customercare@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. Enrico Greco Academic Editor PLOS One |
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