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Article
Peer-Review Record

Impregnation of Medium-Density Fiberboard Residues with Phase Change Materials for Efficient Thermal Energy Storage

Forests 2023, 14(11), 2175; https://doi.org/10.3390/f14112175
by Gustavo E. Rodríguez 1,*, Cecilia Bustos Ávila 1,*, Romina Romero 2 and Alain Cloutier 3
Reviewer 1: Anonymous
Reviewer 2: Anonymous
Reviewer 3: Anonymous
Forests 2023, 14(11), 2175; https://doi.org/10.3390/f14112175
Submission received: 20 September 2023 / Revised: 27 October 2023 / Accepted: 30 October 2023 / Published: 1 November 2023

Round 1

Reviewer 1 Report

Comments and Suggestions for Authors

Interesting idea to use a side-stream of wood processing as a substrate for a novel product. More background information on the substrate, the PCM and the resulting impregnated product possibilities would be useful.

MDF residues contain adhesive - what challenges or opportunities does this provide?

L48 ‘waste’ implies no value, or negative value (pay to handle/dispose). Surely most of that ‘waste’ ends up being used for something (e.g. being burned for heat generation)? Better to speak of low-value by products and the opportunities for increased value…]

L74 when reading that concrete and bricks have problems with loss of PCM but that (solid?) balsa wood is good because it traps it, I am wondering which material is closer to MDF?

For a reader not very familiar with PCM, the references to specific latent heat and encapsulation values are not very useful. It would be helpful to give some reference points, e.g to other materials that are not considered to provide a good substrate (concrete and bricks mentioned above?)

L97 at what stage of the production of MDF are the residues that you used formed? After refining but before blending? Later on it is clear that these are post blending residues that contain adhesive. That should be made clearer earlier.

L207 This explanation doesn’t make sense to me. Cellulose is relatively stable in processing, it seems likely that thermally induced losses are more likely in the hemicellulose component. Maybe just a measurement error?

L409 You can get the PCM into a powder, but what use will be made of the impregnated powder?

Also some discussion of the potential cost/benefit of the material and other practicalities would be useful. Just because you can do something doesn’t necessarily mean you should!

 

Author Response

Dear Reviewer, Thank you for your review. A complete revision of the paper was performed considering your comments. The following changes were made in track mode:

- MDF residues contain adhesive – what challenges or opportunities does this provide?

Response:

* Line 127, “As a by-product of MDF panels, the residues contain small UF adhesive particles. This would mean fewer voids in the wood fibers to impregnate other materials. However, as demonstrated below, it is possible to impregnate them with PCM.”

- L48 “waste” implies no value, or negative value (pay to handle/dispose). Surely most of that “waste” ends up being used for something (e.g., being burned for heat generation)? Better to speak of low-value by-products and the opportunities for increased values

Response:

* Line 57, “wood waste” was changed to “wood residues”

- L74 when reading that concrete and bricks have problems with loss of PCM but that (solid?) balsa wood is good because it traps it, I am wondering which material is closer to MDF?

Response:

- In the text I express: “However, it is important to mention that one of the main challenges faced by researchers is the loss of PCM during phase transition”. This problem applies to all materials used as matrix. However, wood porous structure can mitigate this effect and improve it. MDF boards are made of wood fibers, so it is possible, as demonstrated, that they can be impregnated. Line 94 indicates that the thermal properties (latent heat) of balsa wood are better than some experience with cement and gypsum.

-  For a reader not very familiar with PCM, the references to specific latent heat and encapsulation values are not very useful. It would be helpful to give some reference points, e.g. to other materials that are not considered to provide a good substrate (concrete and bricks mentioned above?)

Response:

- Line 94, “The latent heat obtained is tenfold higher than that reported by Frazzica et al. [26], who integrated PCM into cement, and about sevenfold higher than the gypsum-PCM composite developed by Yaras et al [14]. It is important to note that the heat storage capacity of the composite depends on the thermal attributes of the PCM used. However, impregnating wood has shown to provide better performance.”

- L97 at what stage of the production of MDF are the residues that you used formed? After refining but before blending? Later on it is clear that these are post blending residues that contain adhesive. That should be made clearer earlier.

Response:

* Line 123, “These residues, which look like dust flour, consist of small fibers (0.15 – 1.19 mm). They originated from…” and Line 127, “As a by-product of MDF panels, the residues contain small UF adhesive particles.”

- L207 This explanation doesn’t make sense to me. Cellulose is relatively stable in processing; it seems likely that thermally induced losses are more likely in the hemicellulose component. Maybe just a measurement error?

Response:

- There was no measurement error. We agree with your assessment and it was eliminated. However, although the result is lower than that reported by Ariete Merino, it is similar to that of other authors. Line 239, “However, it is similar to the value reported by Cruz et al. [38], who obtained 38,4% cellulose.”

- L409 You can get the PCM into a powder, but what use will be made of the impregnated powder?

Response:

* Line 445, “The composites obtained can be used in the development of novel materials. An interesting challenge would be to use them to produce wood-based panels with improved thermal properties.”

- Also, some discussion of the potential cost/benefit of the material and other practicalities would be useful. Just because you can do something doesn’t necessary mean you should.

Response:

* Line 440, “A potential utilization of such composites is in building construction for walls, ceiling, and partition systems enhancing their passive thermal energy storage property.”

Reviewer 2 Report

Comments and Suggestions for Authors

Here are my comments on the strengths and weaknesses of this article:

 

Strengths:

- The article addresses an important and relevant issue - valorizing wood residues from the MDF industry by developing thermal energy storage materials. This provides a novel application for wood waste and contributes to the circular economy. 

- The experiments are well designed and executed. The methods for preparing and characterizing the composites are sound. A good variety of analytical techniques are utilized.

- The results demonstrate successful impregnation of the MDF residues with PCMs to create composites capable of storing latent heat. In particular, the R+PCM1 composite showed favorable thermal properties. 

- The article is clearly written overall. The introduction provides good context and the results are presented in a logical manner. Figures and tables are appropriate.

 

Weaknesses: 

- The abstract could provide more specific details on the best performing composite developed rather than mentioning all 3 PCMs.

- The introduction's explanation of the need for PCM composites is a bit vague. More details on their utility for thermal energy storage applications would help.

- The authors could expand the discussion of the chemical characterization results which showed higher than expected lignin content. This point needs more explanation.

- The practical implications of the research could be expanded on more in the conclusion - e.g. how might the composites be applied at scale?

- The quality of the figures could be improved - increasing their size and resolution.

 

 

 

 

Comments on the Quality of English Language

- There are some minor grammatical mistakes, such as missing articles ("the" or "a/an"), incorrect prepositions, and subject-verb agreement issues. These occur sporadically throughout the text.

- Some sentences are overly long or convoluted. Breaking down complex sentences into shorter, clearer ones would improve readability.

- Word choice could be more precise in certain places. For example, using "determined" vs "realized", "indicate" vs "show", etc.

- The flow and logic between sentences needs to be smoothed out in some paragraphs. Better transitions between ideas would help with coherence.

- There is inconsistent verb tense in some parts - switching between past and present tense. It should be past tense throughout for completed work.

- Some phrases are awkward or repetitive. Varying word choice would help. For example, repeatedly saying "it was observed that..."

- The paper would benefit from thorough proofreading to catch minor typos/spelling errors.

- The writing is generally clear overall, but some portions could be reworded or restructured to improve clarity and concision.

Author Response

Dear Reviewer,

Thank you for your review.

A complete revision of the paper was performed considering your comments. The following changes were made in track mode:

- The abstract could provide more specific details on the best-performing composite developed rather than mentioning all 3 PCMs.

Response:

* Line 31, “This better thermal performance is attributed to a higher encapsulation ratio compared to the other compounds developed (31.4%). Furthermore, R+PCM1 showed an absorption capacity of 142.8%.”

- The introduction’s explanation of the need for PCM composites is a bit vague. More details on their utility for thermal energy storage applications would help.

Response:

* Line 77, “The main strength of thermal energy storage with PCMs is the use of one of the largest renewable energy sources: solar energy. It is possible, for example, to store excess heat in buildings and release it when temperatures are lower. This concept would help to reduce the current energy consumption in homes due to the use of cooling and heating systems. Using PCMs within building structures for thermal energy storage serves to mitigate energy intermittency. Therefore, it would help to keep the indoor temperature consistent, effectively regulating temperature fluctuations.”

- The authors could expand the discussion of the chemical characterization results which showed higher than expected lignin content. This point needs more explanation.

Response:

* Lines 249, “Since the UF adhesive was not removed before the chemical analysis process, the UF particles add to the overall oven-dry mass of the sample, leading to an overestimation of the real lignin content. This study aimed to assess the impregnation of the residues without any prior modifications.”

- The practical implications of the research could be expanded on more in the conclusion – e.g. how might the composites be applied at scale?

Response:

* Line 445, “The composites obtained can be used in the development of novel materials. An interesting challenge would be to use them to produce wood-based panels with improved thermal properties.”

- The quality of the figures could be improved – increasing their size and resolution.

Response:

* All the figures were improved in size and resolution except Figure 4. Due to the format constraints, it's not possible to enlarge Figure 4. It may be necessary to split it into multiple figures. However, We believe its current size and presentation are adequate.

Reviewer 3 Report

Comments and Suggestions for Authors

The topic of the research work and manuscript is really interesting and provides new information. However there are some issues to be addressed towards its quality improvement. In the abstract, it is not at all clear in what form is the referred inital "MDF board-residue" (in powder/mdf densified piece/solid wood material)?Please, clarify this. That is clear neither in abstact, nor in introduction-chapter end (line 92). In line 93, you talk about fibrous material, though it is not clear since you referred in the abstract the vacuum impregnation method (which is usually not necessary in fibres, but applied mainly in solid wood), therefore, it would be necessary to specify. In line 99, you refer to "MDF panels" (materials-methods chapter). The potential future applications of such materials are not presented neither in abstract, nor in introduction end, conclusions etc.

Erase the dot before the reference parentheses. In line 47, please add as a reference the relevant work of https://doi.org/10.1002/bbb.2291 . Try to provide more plain words instead of phrases in the key words area, in order to contribute to the readability and detectability of the manuscript. In the introduction chapter it would be useful to refer to the nature of these residual material (MDF residues generated in the fiberboard molding industry), since it is the raw material to be utilized in the present research work. Provide the scientific name of the wood species used in italics. Which were the reagents used in Karl-Fisher method? Did you use any other standards for the processes applied in this experimental work? For the vacuum oven, provide details (manufacturer, country). Now that the experiment has been completed, a brief comment on the number of 5 replicates/samples produced for each material-category, was that adequate? The chapter 2.3. of characterization should be presnted earlier in the raw materials before the description of impregnation method in my opinion. Check the TAPPI standards, some of them have been withdrawn and updated. In more detail, what kind of statistical analysis has been applied (explain in 2.4.chapter). For the decimals, dot is widely/internationally used instead of commas (since it is an international journal). The authors have used both dots and commas for decimals separation in the text and this should be corrected.  In 301 line, are you sure about the term of "crystallization temperature"? Which could be the meaning/consequence of not developing chemical bonds between the wood powder and the PCL materials? Why are we talking in the whole text for MDF-fibers and not wood fibers? (is there any difference between them concerning the chemical composition?did you include also adhesive in the fibers coming from the process of MDF production)? In the future it would be nice to examine the recycled mdf fibres potential to be utilized in the proposed PCL composite materials. 

Comments on the Quality of English Language

In line 15, probably it should be changed to "needs"? The use of English language is more than satisfying.

Author Response

Dear Reviewer,

Thank you for your review. A complete revision of the paper was performed considering your comments. The following changes were made in track mode:

- In the abstract, it is not at all clear in what form is the referred initial “MDF board-residue” (in powder/mdf densified piece/solid wood material)? Please clarify this.

Response:

* Line 14, “These residues consist of fine fibers with sizes between 0.15 mm and 1.19 mm.  A…”

- That is clear neither in the abstract nor in introduction-chapter end (line 92)

Response:

* Line 46, “The manufacturing of moldings from MDF panels is a particularly important source of wood residues. These residues consist mainly of wood fibers, smaller in size (0.15 – 1.19 mm) than those used in MDF board production. Some of these residues are utilized for power generation in the panel industry. A very small fraction of it serves as filler material in the production of new panels. Nevertheless, most of it is stockpiled in the mill yards and eventually buried after an extended period.”

- In line 93, you talk about fibrous material, thought it is not clear since you referred in the abstract the vacuum impregnation method (which is usually not necessary in fibers, but applied mainly in solid wood), therefore, it would be necessary to specify.

Response:

* It is more common to impregnate solid wood. However, it is also possible to perform them on particles or fibers, as in our case. An example of this is the study by Jiang et al. cited in line 107. In the sentence "This study aimed to develop a PCM impregnation process in fibrous MDF panel residues to obtain a shape-stabilized composite suitable for thermal energy storage" (Line, 116); it is clear that an impregnation process was carried out on the fibrous MDF residues.

- In line 99, you refer to “MDF panels” (materials-methods chapter). The potential future applications of such materials are presented neither in abstract, nor introduction and, conclusions etc.

Response:

* We wanted to explain that the residues used in the present work came from MDF boards produced under those conditions. Therefore, the following was added to Line 123: “These residues, which look like dust flour, consist of small fibers (0.15 – 1.19 mm). They originated from…”

- Erase the dot before the reference parentheses. In Line 47, please add as a reference the relevant work of https://doi.org/10.1002/bbb.2291.

Response:

* Line 57, “A zero-waste program is implemented in the European Union which aims to reduce the use of virgin raw materials. A reduction of around 25% is estimated for the year 2030, with the target to reduce greenhouse gas production by 40%. One of the most relevant applications is the use of residues as bio-insulation in housing [4].”. Also, the dot was erased.

- Try to provide more plain words instead of phrases in the key word area, in order to contribute to the readability and detectability of the manuscript.

Response:

* We changed “shape-stabilized phase change material” to “thermal properties”. We consider the other keywords to be appropriate.

- In the introduction chapter it would be useful to refer to the nature of these residual materials (MDF residues generated in the fiberboard molding industry) since it is the raw material to be utilized in the present research work. 

Response:

* Line 46, “The manufacturing of moldings from MDF panels is a particularly important source of wood residues. These residues consist mainly of wood fibers, smaller in size (0.15 – 1.19 mm) than those used in MDF board production. Some of these residues are utilized for power generation in the panel industry. A very small fraction of it serves as filler material in the production of new panels. Nevertheless, most of it is stockpiled in the mill yards and eventually buried after an extended period.”

- Provide the scientific name of the wood species used in italics.

Response:

* Line 121, 253, and 431; radiata pine was changed to Pinus radiata

- Which were the reagents used in Karl-Fisher method?

Response:

* Line 137, “(A solution of iodine in methanol and pyridine as a water-sequestering agent was used)”

- Did you use any other standards for the processes applied in this experimental work?

Response:

* Only the standards mentioned in the text were used.

- For the vacuum oven, provide details (manufacturer, country).

Response:

* Line 157, Vacucell-22-Standard blue line vacuum oven (MMM group, Semmelweisstrasse 6 D-82152 Planegg / München – Germany).

- Now that the experiment has been completed, a brief comment on the number of 5 replicates/samples produced for each material-category, was the adequate?

Response:

* We consider that a good result was obtained with 5 replicates. The ANOVA yielded an R2: 0.996 which indicates that the model is reliable and explains in a good way the influence exerted by the factors on absorption.

- The chapter 2.3 of characterization should be presented earlier in the raw materials before the description of impregnation method in my opinion.

Response:

* We consider that only section 2.3.1 is the one that should be moved to the raw material section. It was moved to line 141 and was denoted as section 2.1.1. The other characterizations involving the developed compound should be after the impregnation process description.

- Check the TAPPI standards, some of them have been withdrawn and updated.

Response:

  • TAPPI standards were reviewed and are correct.

- In more detail, what kind of statistical analysis has been applied (explain in 2.4 chapter)

Response:

* Line 207, “(two-way ANOVA).” and “on the data obtained for the properties studied…”.

- For the decimals, dot is widely/internationally used instead of commas (since it is an international journal). The authors have used both dots and commas for decimals separation in the text and this should be corrected.

Response:

* Commas were replaced by dots in Tables 1, 2, and 3. Located in Lines 266, 343, and 354 respectively. In the text, all decimals are separated by dots.

- In Line 301, are you sure about the term of “crystallization temperature”?

Response:

* Yes, the term is well used. There are synonyms such as "solidification temperature" or “freezing temperature”. It is at the discretion of the researcher which one to use.

- Which could be the meaning/consequence of not developing chemical bonds between the wood powder and the PCM material?

Response:

* Line 331, “The physical bonding between the PCM and the residues prevents the formation of new compounds by chemical reaction. The initial chemical composition of both components is maintained and improves their heat storage capacity.” The non-formation of chemical bonds is not a disadvantage, nor does it have any consequences.

- Why we are talking in the whole text for MDF-fibers and not wood fibers? (Is there any difference between them concerning the chemical composition? Did you include also adhesive in the fibers coming from the process of MDF production)?

Response:

* In the text, the term "MDF fibers" is employed to denote the fibers conventionally utilized in the manufacturing of MDF panels (Line 257). Conversely, "MDF residues" are utilized to describe the "recycled MDF fibers," mentioned by the evaluator in their last comment, which originates from molding production, with UF particles and used in this work.

- In Line 15, probably it should be changed to “needs”

Response:

* The correction was made.

Other modifications were made.

- Line 15, “residues” was erased.

- Line 16, “These residues can be reused as raw materials for manufacturing new products using the circular economy approach” to “Using the circular economy approach, these residues can be reused as raw materials for manufacturing new products”

- Line 52, “this” to “the”

- Line 85, “successfully incorporated” to “incorporated successfully”.

- Line 87, “face” to “faced by”

- Line 89, “anatomical” to “porous”

- Line 108, “demonstrated” to “showed”.

- Line 121, “The Solid” to “Solid”.

- Line 124, “were prepared” to “manufactured”.

- Line 125, “percent” to “content”.

- Line 126, “gluing ratio” to “resin content” and “%”

- Line 132, “phase change materials” to “PCMs”.

- Line 139, “in” to “of”.

- Line 142, “A granulometric analysis and chemical characterization were…” to “Granulometric and chemical analyses were…”

- Line 143, “In the granulometric characterization,” was added.

- Line 155, “Then, the MDF residue was added…” to “Then, the MDF residues were added…”.

- Line 198, “MDF residues-PCM” was added.

- Line 206, “on” to “in”.

- Line 212, “fiber” was erased.

- Line 213, “fiber” to “fine particles”

- Line 216, “of fine particles” was added.

- Line 217, “residues” was added.

- Line 218, “residue” was added.

- Line 219, “of fine particles” was added.

- Line 221, “in” to “to” and “manufacturing” to “manufacture”.

- Line 222, “The more significant fraction of fibers in MDF is…” to “A more significant fraction of MDF fibers is…”.

- Line 224, “fibers” to “particles”

- Line 225, “fibers” to “fine material”.

- Line 226, “residual fibers” to “MDF residues”.

- Line 233, “…materials underutilized by industries” to “underutilized materials.”.

- Line 239, “content” was added.

- Line 277, “phase change materials” to “PCMs”.

- Line 301, “clearly” was eliminated.

- Line 330, “phase change materials” to “PCMs”

Round 2

Reviewer 2 Report

Comments and Suggestions for Authors

Here is my assessment of the strengths and weaknesses of this article:

Strengths:

- The article addresses an important issue of finding useful applications for wood residues from the MDF industry. Reusing these residues to develop thermal energy storage materials aligns with circular economy principles.

- The experimental methodology is sound. The authors utilized appropriate characterization techniques (SEM, FTIR, DSC, TGA) to analyze the materials. The statistical analysis adds rigor.

- Impregnating the MDF residues with PCMs to improve their thermal storage capacity is an original idea. The R+PCM1 composite showed good thermal performance.

- The article is well-structured overall with sufficient details provided in the methods and results sections. Figures and tables are clear.

 

Weaknesses: 

- The introduction could be strengthened by more clearly highlighting the novel contributions and knowledge gaps addressed. The current summary of general PCM concepts should be more concise. Please use the following ref.     https://doi.org/10.1007/s10924-009-0155-6

 

- Certain parts of the results and discussion are repetitive and could be condensed for brevity and clarity. For example, the full FTIR spectra for all samples are shown when the key points could be conveyed with less.

- There are some language issues throughout that need editing for clarity and grammar. Academic tone and style should also be made more consistent.

- The practical implications of the research could be expanded on in the discussion and conclusions. How might the developed composites actually be applied?

- References are comprehensive but the formatting is inconsistent in some cases. 

Flow Issues:

- The transitions between ideas can be abrupt in places. Using more linking words/phrases could improve logical flow. 

- Organization is clear overall but some paragraphs in the results/discussion jump between topics without a smooth progression. 

- Repetition in the text causes it to lose forward momentum. Condensing this excess verbiage would give better flow.

- The interplay between the results and cited literature is not always smoothly integrated. Tighter connections are needed.

- The conclusions do not always logically follow from the evidence presented earlier. Strengthening these ties would improve flow.

 

 

 

Comments on the Quality of English Language

Here are some of the key weaknesses I see in terms of English language and flow of the article:

English Language Issues:

- There are some grammatical errors throughout, such as incorrect verb tenses, missing words, etc. The writing would benefit from careful proofreading.

- Certain sentences are awkwardly phrased or overly long, making them difficult to parse. Simplifying language and sentence structure could improve clarity.

- Some discipline-specific terminology is used inconsistently or incorrectly. For example, "anatomical structure" should be "anatomical features" when referring to wood.

- There is inconsistent use of British/American spelling in cases like "valorise" vs. "valorize." Academic writing should adhere to one style.

- Some parts use informal phrasing not typical of a scientific publication, such as "this phenomenon was not observed..."

 

Author Response

We would like to thank the review for your time and recommendations. The actions taken following your comments are described below:  

- The introduction could be strengthened by more clearly highlighting the novel contributions and knowledge gaps addressed. The current summary of general PCM concepts should be more concise.

Response:

* Line 115, we rewrite “The context provides an opportunity to valorize MDF residues generated in the fiberboard molding industry. This study aimed to develop a PCM impregnation process in fibrous MDF panel residues to obtain a shape-stabilized compo-site suitable for thermal energy storage.” To Line 119: “To our knowledge, there is no published literature reporting the impregnation of PCMs in MDF residues to produce a compound material with improved thermal properties. The above context provides an opportunity to valorize the MDF residues generated in the MDF molding industry. This novel study aims to develop a process to impregnate MDF residues with PCMs to obtain shape-stabilized compounds that are suitable for thermal energy storage.”

* To reduce the summary of general PCM concepts, we eliminated: Line 67, “From a thermodynamic perspective, PCM absorbs or releases thermal energy, or heat, by changing its entropy. The amount of heat is directly associated with the mass of the material and is defined as its latent heat [11]”

 

- Please use the following ref.     https://doi.org/10.1007/s10924-009-0155-6

Response:

* The reference suggested by the evaluator is not relevant to the current manuscript. It describes the manufacture of a polypropylene composite reinforced with newspaper fibers and wood flour. In no case does it include PCM.

 

- Certain parts of the results and discussion are repetitive and could be condensed for brevity and clarity. For example, the full FTIR spectra for all samples are shown when the key points could be conveyed with less

Response:

* We do not consider the analysis and discussion made for the FTIR analysis to be repetitive. Each part provides different information since each PCM shows different behavior in its interaction with the residues. However, the following was eliminated: Line 326, “The main difference between the two PCMs, both being petroleum derived, lies in the intensity of their characteristic peaks”; and Line 330, “Instead, differences in the intensities of the peaks related to the constituent material can be observed (Figure 4-D)”.

 

- The practical implications of the research could be expanded on in the discussion and conclusions. How might the developed composites actually be applied?

Response:

* Line 451. We added the following: “The compounds that have been developed could be utilized in the manufacturing of panels, which could function as integral wall components. They could regulate the temperature inside buildings by absorbing and releasing thermal energy, thereby improving indoor thermal comfort. Therefore…” and we eliminated Line 460, “An interesting challenge would be to use them to produce wood based panels with improved thermal properties”.

 

- References are comprehensive but the formatting is inconsistent in some cases.

Response:

* The references located in Table 1 were modified (Line 271). The rest of the document maintains the same format for citing references.

 

- The conclusions do not always logically follow from the evidence presented earlier. Strengthening these ties would improve flow.

Response:

* We considered that the conclusions are structured according to the characterizations and findings made during the paper. However, the following was added on Line 445, “both” and “encapsulation ratio and the highest…”; and Line 446, “In general, all the compounds demonstrated commendable thermal stability.”

 

- Some discipline-specific terminology is used inconsistently or incorrectly. For example, "anatomical structure" should be "anatomical features" when referring to wood.

Response:

* We changed it to "anatomical features" which is more appropriate in this case. The changes were made in Lines 252, 334, 375, and 383.

 

- There is inconsistent use of British/American spelling in cases like "valorise" vs. "valorize." Academic writing should adhere to one style.

Response:

* In the text only "valorize" is used, and this corresponds to the American style, which is how the article is written. In no case was "valorise" used.

 

- Some parts use informal phrasing not typical of a scientific publication, such as "this phenomenon was not observed..."

Response:

* We added in Line 222 “particle size” and we eliminated “phenomenon”.

 

- There are some language issues throughout that need editing for clarity and grammar. Academic tone and style should also be made more consistent. The transitions between ideas can be abrupt in places. Using more linking words/phrases could improve logical flow. Organization is clear overall but some paragraphs in the results/discussion jump between topics without a smooth progression. Repetition in the text causes it to lose forward momentum. Condensing this excess verbiage would give better flow. The interplay between the results and cited literature is not always smoothly integrated. Tighter connections are needed. There are some grammatical errors throughout, such as incorrect verb tenses, missing words, etc. The writing would benefit from careful proofreading. Certain sentences are awkwardly phrased or overly long, making them difficult to parse. Simplifying language and sentence structure could improve clarity.

Response.

* To address various language-related issues and enhance the overall fluency of the manuscript, the text underwent a comprehensive revision process conducted by a professional editor. Significant changes were implemented, leading to a discernible enhancement in the paper's quality. This revised version maintains an academic and formal style while presenting the information more clearly and concisely.

Reviewer 3 Report

Comments and Suggestions for Authors

As I have checked the authors have implemented the proposed changes in the revised verion of manuscript towards the improvement of their work. Almost all the changes have been implemented and in my opinion, the manuscript is well-prepared and organized enough. 

Author Response

Thank you for your revision

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