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Article
Peer-Review Record

Structural Changes of the Interface Material of Scallop Adductor under Ultra-High Pressure

Processes 2023, 11(2), 521; https://doi.org/10.3390/pr11020521
by Xue Gong 1,2, Jiang Chang 3, Yinglei Zhang 1, Danting Li 1, Ning Xia 2, Jing Wang 1 and Zhihui Sun 4,*
Reviewer 1:
Reviewer 3: Anonymous
Processes 2023, 11(2), 521; https://doi.org/10.3390/pr11020521
Submission received: 20 December 2022 / Revised: 2 February 2023 / Accepted: 6 February 2023 / Published: 8 February 2023

Round 1

Reviewer 1 Report

This manuscript is a good start to better understanding ultra-high pressure can potentially be used to improve shellfish processing in China due to its impact on the scallop shell’s interior coating. However, this manuscript needs to be improved for MDPI Coatings since the connection between use of ultra-high pressure and the improvement of scallop processing is not clearly presented so that it is clear to the reader why the exploratory research results would make scallop processing easier. I would be willing to review this manuscript for continuous improvement after this is done. The co-authors need to make the following TEN substantive edits as well as minor line-number specific edits to optimize the chance for more favorable peer review of the manuscript:

    1)      Include a new Figure 1 showing the scallop, interior of the scallop, particularly where the adductor joins the interior of the scallop shell. 

    2)      There are several places where there is no blank space before the [#] so for example on L35-36, L43, L49, etc.

    3)      Any paragraph needs to have a minimum of 3 sentences. There is a sub-section for example that only has one sentence (e.g., L81-82) so for this particular sentence, please add two more sentence to complete the paragraph or merge the sentence with another sub-section and rename the sub-section. 

    4)      Much of the Methods section have sentences that read as bullet points one would expect to find on a laboratory instruction list and not a journal article. These sentences also lack a noun to accompany the verb. You need to tell the story of how the research was done. There is also writing that needs to be broken up into shorter paragraphs especially in the Results section.

    5)      Any acronym (e.g., CH on L154) or measurement unit (e.g, MPa) needs to be defined at the start of its first use in every major section (e.g., Introduction, Methods, Results, Discussion, Conclusion) of the manuscript. Most readers do not read from start to finish. 

    6)      Make sure there is a blank row above and below tables and figures.

    7)      For all figures, the y-axis is not defined. Is it frequency? There is no labeled y-axis label for Figure 1. For the other figures, there is no y-axis label nor any y-axis for that matter. Any axis label needs to have the first word capitalized. 

    8)      Please ADD the section 4. Discussion on L383:

a.       Expand on the contrasts and linkages between your results and results of prior literature. You need to compare and contrast your results to similar studies in the literature. Title this sub-section “4.1. Contrasts to Previous Studies”.

b.      Discuss major themes or limitations to the implications of your research results. Please add this sub-section and title this “4.2. Research Implications” and you need to add this sub-section. In this newly added sub-section you need to break down your technical results by clearly explaining how the results make scallop processing easier. This is a great opportunity to also potentially answer other questions. For example, what are potential challenges to up-scaling this new processing technology? What is the comparative cost? Can the benefit-cost of this new ultra-high pressure technology be quantified? Meaning what is the benefit? Speed of processing? Minimizing yield loss? What are the variable and fixed costs? 

    9)      Make sure the number of references cited is around 50. The added references will primarily be from addressing 6) above. 

    10)  The format for the references require two corrections. First, the journal names need to be abbreviated with common abbreviations. Just type in the journal name and then the word
“abbreviation” in a Google search. Second for journal articles, you need to add the DOI link at the end of the reference so the page proof editor can inset the CrossRef hyperlink.

 

Specific Line Number of Manuscript Figure/Table comments (note that requested change of word(s) in quotations where NO edits need to be made for writing before/after each “…”):

L18 – Change to “…increased. A small…” and please do not use ; in this way elsewhere in the manuscript

L31-32 – Is that English “tons” or “metric tons”?

L32 – Change to “…tons [1,2].” and make similar changes on L35, etc.

L204 – Other small case letters a, b, and c need to be in bold just like d

L212 – The font size of the figure needs to be increased since it is hard to read

L215-245 – Break up into two or more paragraphs

L253-254 – Small case letters need to be in bold for picture (d) as well as all letters in caption

L268-269 – Sub-header caption needs to all be in italics

L316 – Add space after the number 864 and correct similar mistakes in the rest of the manuscript

L396-400 – The Author Contributions section on needs to have co-authors names in initial format (e.g., X.G.)

Also, throughout the manuscript the headers and footers listing of the journal year and volume need to be changed to 2023 and 13 respectively.

Author Response

Please see the attachment

Author Response File: Author Response.pdf

Reviewer 2 Report

Comments on the manuscript “Structural changes of the interface material of scallop adductor under ultra-high pressure” authored by Gong et al. (Ref: coatings_2140679)

In this paper, the authors have proposed a scheme through which the removal process of shell of shellfish can be made easier by using the high pressure of the order of 200 to 300 MPa. This proposed scheme will have advantages in seafood processing industry. The reviewer has the following comments.

1)    The paper has been written like a laboratory manual. Example: Page-2, line 74-77

“Clean the surface of scallops purchased carefully, and put scallops in the PE packag-74 ing bags that are filled in with dilute salt water. And then put the sealed scallops into the 75 ultra-high pressure equipment and process it at a test pressure of 100 MPa, 200 MPa and 76 300 MPa respectively.”

The procedure followed in the work and the results should be presented by writing these in passive sentences. Hence, it is recommended that the manuscript should be edited thoroughly keeping in mind the grammatical errors, sentence construction, syntax etc. Otherwise, reading the manuscript is cumbersome.

2)    Abstract: Check the line-17 of page-1.
“….was most sensitive to the pressure of 200MPa β- More folds α- The elasticity of the adductor”
 
This sentence doesn’t make any sense. What is the meaning of “200MPa β- More folds α- The elasticity”?

The abstract doesn’t convey the novelty of the work carried out in this paper. Please discuss the important results along with the evidences as observed in your work. You are suggesting that the shell gets detached easily from the adductor muscle due to structural changes induced because of high pressure. Why are you mentioning the pressure as 200 MPa only? In the results section, spectroscopy data is shown for 300 MPa also. What happens at 300 MPa? Is it not suitable for processing scallops? If so, why is it so?

3)    Section 2.2.1 (Page-31): Data regarding excitation wavelength, range of detection wavelength and other parameters are provided. How are these values chosen for the analysis? What is the basis of selection? Is there any reference for these data? Please elaborate.
4)    Sections 2.1.4, 2.2.1, 2.2.3 and 2.2.3: The make of many instruments are written and elaborated. These are not necessary in a scientific paper. This looks like some kind of advertisement. It is suggested that the manufacturer details of the instruments be removed from the paper and make the discussion more professional.
5)    Fig. 1: What is the Y-axis of Fig. 1? The wave numbers corresponding to untreated sample is only provided in this figure. Please show the peaks of 200 and 300 MPa data also. Moreover, it is seen that the peak is very high for 200 MPa processed sample. For 300 MPa processed sample, it reduces again. What is the reason for this? Please discuss.
6)    How are sample obtained after processing at high pressures. Is it sectioned near the interface of shall or away from it? Please draw sketches and show it. This is important because the spectroscopic data shall not be uniform. It depends upon the location of sampling. Please elaborate on this aspect.
7)    How many samples have been analyzed for Raman spectroscopy? It may be noted that one data may not be sufficient as it may not represent the molecular level changes that occurs in the muscle or shell of the shell fish. It is suggested that data from more samples be presented in order to make it more statistically representative. Moreover, in order to make the results more credible, the structural changes with application of pressure and the corresponding changes in the arrangement of fibres and other microstructures should be documented in an elaborate manner.
8)    Page-4, second paragraph: There are discussions regarding correlation of wavelength with deformation of different kinds of chemical bonds, such as N-H, C-N, C=O, C-C etc. Please show some sketches of a typical macromolecule of the representative muscles of shellfish and its associated bond deformation with application of ultra-pressure. Moreover, it is not clear if bond deformation increases only upto 200 MPa and then decreases. If so, why? What is the mechanism of bond deformation, as observed from the spectroscopy data? These aspects should be elaborated further.
9)    Fig. 2: Page-6: What are different curves? No legend is provided, though several curves are drawn. What is the x-axis and y-axis of these curves? How are these obtained? How is the theoretical value obtained? Please elaborate.
10)    Fig. 3: The structural changes for 200 MPa is very different for 100 MPa, 300 MPa and untreated conditions? What is the reason for this? What is reason for the percentage of alpha-helix to decrease and beta-sheet to increase? Please elaborate.
11)    Page-7, Line-219.
“…Hydrogen bonds between protein molecules are damaged when the pressure reaches an ultra-high level of 200 MPa.”
If hydrogen bond breaks at 200 MPa, it should also break at 300 MPa. Why do you have different observations for 300 MPa pressure? Moreover, where is the data supporting the assumption that 200 MPa pressure is required to break the hydrogen bond between protein molecules of the muscle?
12)    The SEM data for 200 MPa is similar to 300 MPa processed muscle. The 200 MPa data shows more breakage of ligaments compared to 300 MPa. Please provide SEM images from other places for confirmation of this observation. Please elaborate the reason for differences of 200 MPa and 300 MPa data.
13)    Fig. 5: What is y-axis for this data? Here the amplitudes of spectra are different compared to Fig. 1. Spectra of untreated interface is in-between those spectra of 200 and 300 MPa. According to your analysis, the spectra of 200 MPa should be very different from untreated spectra. It is not clear from this figure.
14)    One of the important aspect of the results of this work is analysis of spectra samples after application of pressure. When untreated sample is prepared, some pulling or cutting force is also applied on the muscle. It is not clear how is force alters the data regarding spectra for untreated sample. Please elaborate.
15)    Data of Table-1 should be combined with Fig. 5 in order to make it more meaningful.
16)    Table-2: fourth column: What is the source of this assumption? Is it assumption or the conclusions regarding the deformations have some basis. For example, how do we know that such as such wave number corresponds to stretching of such and such bonds? This requires extensive deformational analysis at molecular length scales. Have you taken it from such literature? If yes, please include it in Table-2.
17)    Fig. 6(d): The scallop interface at 300 MPa seems to be relatively clean compared to 200 MPa sample. Does it mean 300 MPa provides for better removal of shell?
18)    Conclusions: Please check this statement.
“At the same time, it is stretched to the maximum extent to form the maximum tension between the two shells; Under the ultra-high pressure above 200MPa, the minerals in the shell become brittle, which weakens the adhesion of the scallop interface to some extent;”

How do you know that the tension is maximum and the shell becomes brittle? In order to know if the shell become brittle after application of high pressure, tensile tests need to be carried out and the conclusions should be supported by experimental data. In the conclusion section, I don’t find sufficient evidence for many of the sentences. Hence, it is recommended that this section should be re-written completely. Only relevant conclusions should be included, which are duly supported by spectroscopic or other data.

Author Response

Please see the attachment

Author Response File: Author Response.pdf

Reviewer 3 Report

The work concerns structural changes of the organic and inorganic materials under high pressures. The idea of the work is quite original. The English language is correct, the structure of the manuscript is logical. However, changes are necessary before publication.

- an important part of the work is the structure of shellfishes. Authors should include in the manuscript a figure containing basic information about the structure of these shellfishes,

- the Materials and Methods section should be a bit more extensive, for example what means: "and other equipment" (line 89); it is in this section that photos of samples (shellfishes) could be placed,

- to what extent Raman spectroscopy was carried out (in the figure, the scale is up to 3000, in the descriptions it is different, it should be specified),

- for FTIR research, it would be worth providing the spectrum for calcium carbonate crystals

"The Raman spectrum characteristic bands affili-158 ation of the adductor muscle of scallops [19-21] is as shown in Table 1." I believe Table 1 contains FTIR data?

- "meanwhile, such an uneven surface has increased the surface friction for the connection between the shell and the adductor muscle, and increased the interface strength" - Why this conclusion? This statement needs to be backed up by research.

"As more stress concentrations appear, the more significant the effect grows, and the greater the interface failure expands" - A similar situation as above, the authors draw far-reaching conclusions based on microscopic examinations,

- Several sentences start with lower case letters,

 

The purpose of the study is unclear, the authors did not sufficiently substantiate the need to conduct such research. Why and for whom are such results needed? The conclusions are quite general - among others because the authors did not define a specific research problem. Despite these shortcomings, the presented material is interesting, which is why I believe that the authors should be given a chance to improve the manuscript. The entire article should be redrafted and given the character of a scientific work.

Author Response

Please see the attachment.

Author Response File: Author Response.pdf

Round 2

Reviewer 1 Report

This manuscript is a good start to better understanding ultra-high pressure can potentially be used to improve shellfish processing in China due to its impact on the scallop shell’s interior coating. However, this manuscript needs to be improved for MDPI Coatings since the connection between use of ultra-high pressure and the improvement of scallop processing is not clearly presented so that it is clear to the reader why the exploratory research results would make scallop processing easier. I would be willing to review this manuscript for continuous improvement after this is done. The co-authors need to make the following TEN substantive edits as well as minor line-number specific edits to optimize the chance for more favorable peer review of the manuscript:

    1)      The (a) picture added to Figure 1 is missing. 

    2)      This still at least one place where there is no blank space before the [#] on L48. Please double check this throughout the manuscript. 

    3)      Any paragraph needs to have a minimum of 3 sentences. For example, please do this on L94-98 and L100-104. These need to be 3 shorter sentences.

    4)      Any acronym (e.g., CH on L154) or measurement unit abbreviations (e.g, MPa) needs to be defined at the start of its first use in every major section (e.g., Introduction, Methods, Results, Discussion, Conclusion) of the manuscript. Most readers do not read from start to finish. For example, if MPa is a megapascal which is a unit of pressure, then this needs to be explained in a sentence when the unit is first introduced. Write it out the first time as “megapascal” and then if this is used shortly thereafter for a second or more time, then write out “megapascal (MPa)” the second time so you can use “MPa” afterward. If this is used again further into the manuscript, define the term again so the reader does not have to turn back earlier to remember what this stands for. Do the same for other acronyms and abbreviations. 

    5)      Make sure there is a blank row above and below tables and figures. There is still a case of this that needs correction on L315.

    6)      So on L34-35, the use of billion kg is an uncommon unit. What was wrong with metric tons (t)? 

    7)      There should not be any spaces between paragraphs (this is a Word format issue where you specify do not add blank row after choosing single spacing) so correct this on L237-238 and L244-245. 

    8)      a) While sub-section headers are in italics, the sub-sub-section headers are not in italics and the remaining first letter of words after the first word are not capitalized unless they are naturally capitalized (e.g., China). So for example on L282-283, this should “3.2.1. Infrared spectroscopic analysis” and note that the titles should be SIMPLE and CLEAR so I edited this one. Similar edits need to be made on L87, L93, L99, L106, L116, L125, L147-149, L194-195, L258-259, L282-283, L345-346, and L404-405.

b) Note that sub-section headers require capitalization of all major words. So L280-281 should be “3.2. Structural Changes of Scallop Shells under Ultra-High Pressure” and again note that I simplified this so it is more clear since the title of 3.2.1. flows from reading 3.2. Please make similar edits elsewhere. 

    9)      The MDPI citation format requires a comma for two references and not a dash so please change on L35 to [1,2] and make similar changes on L38 for [3,5] and [6,7] and on L39 for [8,9] and on L48 for [11,12] and on L299 for [35,36]. 

    10)  Sentences end with periods and not semi-colons (;) under normal circumstances. You only do that if there are two very closely related sentences and it is absolutely essential to tie the two sentence together like that. So please change L121 end of sentence to a period “.” from a semi-colon “;”.

 

Specific Line Number of Manuscript Figure/Table comments (note that requested change of word(s) in quotations where NO edits need to be made for writing before/after each “…”):

L18-20 – Need to define what MPa is

L56 – Change to “…calcium carbonate (CaCO3)…”

L64 – Change to “shellfish food, previous researchers [13] consider…”

L68 – Change start of sentence to “Certain fibers of…”

L69 – Change to “…high strength. Moreover based on”

L70-71 – Change to “…muscle interface, prior research found that there…”

L74 – Change end of sentence to “…connection system [14].”

L79-80 – Move [16-18] to end of sentence

L91-92 – Change end of sentence to “…weight of 48 grams (g) ± 5 g and the longest axis diameter of about 97 millimeters (mm) ± 5 mm.”

L94 – What does PE stand for?

L96 – Define MPa

L99 – Do not start sentences with a number so please re-write

L100 – Change start of sentence to “A 2.5% glutaraldehyde solution with a 0.2 mol/liter phosphate buffer, plus ethanol and other reagents”

L102 – Change to “…equipment. These equipment included field emission…”

L103 – Change to “…microscope, Raman spectrum analyzer, Fourier transform…”

L104 – Only one period at the end even if the last word is etc.

L109 – Change to “…wavelength of 515.4 nanometers (nm) and the slit at 200 micrometers (μm).”

L110 – What does mW mean? Megawatts?

L110 – Change to “…exposure time of 60 seconds was used…”

L118 – Change to “…with 0.2 mol/liter”

L120-121 – Change to “…into powder. The surface of…”

L130 – Change to “…spectrometer to 400 to 4000 waves/centimeter (cm), the scanning frequency to 4 waves/cm,”

L163 – Change to “…area, the 500 waves/cm to 1800 waves/cm, which mainly…”

L166-167 – Change to “…refers to the carbon-hydrogen bong (C-H) stretching vibration area of 2800 to 3050 waves/cm [21].”

L172-173 – Change to “…amide III bands (1335 waves/cm) and the amide I band (1657 waves/cm) [22-24].”

L171-193 – Too long paragraph so break up into shorter paragraphs

L186-187 – Change to “…shown at 942 waves/cm. As shown in Figure 1, the peak intensity…”

L209-212 – Add to the end of paragraph above since only 2 sentences

L212-213 – The font size of the figure still needs to be increased since it is hard to read

L288 – In the figure y-axis label, delete the -1 since not using that format

L292-294 – Change sentence to “…scallop shells. Previous studies found that the free-state CO32-anion refers to the symmetrical regular triangle configuration of the D3h point group [32-34]. Moreover, four…”

L296-303 & L311 & L319 & L325 & L330 – Change “cm-1” to “waves/cm”

L309-313 – Add to the end of paragraph above since only 2 sentences

L359-360 – Change to “…of scallop shells, we followed the method outlined in Surewica et al. 2012 [49]. The C=O vibrational…”

L379-398 – Please break up this writing into shorter sentences that follow a logical flow

L396-400 – The Author Contributions section requires deleting the space between initial letters (e.g., X.G.) where you note there is NO SPACE.

L451 – Change to “4. Discussion and Conclusions

L462 – Change to “obtained by Choi and Ma (2007) [51] and Zhang et al. (2019) [28]. Under ultrahigh pressure, the calcium carbonate (CaCO3) crystal structure…”

L465-466 – Change to “…microstructure, we found that the originally homogeneous stress was at the organic-inorganic interface. This trend…”

L469-481 – The paragraph writing should not be in italics and also please make into one paragraph and not two paragraphs

L472-473 – What does UHP stand for? Ultra-high pressure? If so, change to “…cost of ultra-high pressure (UHP) processing have limited the upscaling of UHP processing.” and note here the word I think you want to use is “upscaling” since this means you are doing this processing at industrial scale and no longer in a laboratory.

Author Response

Please see the attachment

Author Response File: Author Response.pdf

Reviewer 2 Report

The authors have addressed all'the comments of the reviewers and hence, the revised version of the  manuscript may be accepted for publication in this journal.

 

Author Response

Many thanks to the reviewers for their understanding and support

Reviewer 3 Report

The authors have significantly improved the work and addressed my comments. I believe the work can be published.

Author Response

Many thanks to the reviewers for their understanding and support

Round 3

Reviewer 1 Report

This manuscript is a good start to better understanding ultra-high pressure can potentially be used to improve shellfish processing in China due to its impact on the scallop shell’s interior coating. The co-authors have improved this manuscript so that it is acceptable for publication in MDPI Processes. The co-authors need to make the following minor line-number specific edits:

Specific Line Number of Manuscript Figure/Table comments (note that requested change of word(s) in quotations where NO edits need to be made for writing before/after each “…”):

L34-35 – Change to “…of 14.6 million metric tons (t), including scallop production of 2 million t [1,2].”?

L119 – Delete end quote and period so end of sentence should read (μm).

L101 – Unbold UHP

L102 – Change to “The pretreated sample was treated according…”

L104 – Change to “regents were used after…”

L104-107 – Change entire sentence to “Ultra-high voltage equipment, a field emission scanning electron microscope, a Raman spectrum analyzer, and additional experimental equipment such as a Fourier transform infrared spectrometer and a freeze dryer were used for our research.”

L229-230 – The font size of the figure still needs to be increased since it is hard to read

L230 – In the figure y-axis labels for both graphs above, delete the -1 since not using that format so should read wave number / centimeter for all 4 graphs

L301-307 – Unbold

L313 – The -2 needs to be superscripted since it is the anion charge so CO32

L382 – Subscript the 3 so change to CaCO3

L399-400 – Everything but the Figure 7. needs to be unbolded

L401-417 – Combine into one paragraph

Please submit as a pdf with all track changes accepted.

Author Response

Please see the attachment

Author Response File: Author Response.pdf

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