A Surface Morphological Study, Poly(Vinyl Chloride) Photo-Stabilizers Utilizing Ibuprofen Tin Complexes against Ultraviolet Radiation
, Mohammed H. Al-Mashhadani 1, Alaa Mohammed 1, Dina S. Ahmed 2, Mohammed Kadhom 3 and Ali H. Jawad 4Round 1
Reviewer 1 Report
In this study the authors have undertaken "A Surface Morphological Study, Poly(Vinyl Chloride) Photo-stabilizers Utilizing Ibuprofen Tin Complexes Against Ultraviolet Radiation”
I have some comments with the present of manuscript which are highlighted below.
- This manuscript has no novelty
- The authors repeated this work in previous research articles using similar compounds as photostabilizers
- Why ibuprofen (used mainly in medications) was used to prepare its complexes to apply as photostabilizers
- The authors did not apply a reference photostabilizer as hydroxyphenyl benzophenones or hydroxyphenyl benzotriazoles to compare with the prepared photostabilizers.
- Regarding the preparation of the PVC-photostabilizaers films; I want to ask about the solubility of the complexes in THF and hence the homogeneity of the prepared films.
Author Response
Dear Reviewers,
We really appreciate your time and efforts to evaluate our work and improve its quality. Bellow, are our comments to your concerns.
With Regards
Reviewer 1
In this study the authors have undertaken "A Surface Morphological Study, Poly(Vinyl Chloride) Photo-stabilizers Utilizing Ibuprofen Tin Complexes Against Ultraviolet Radiation”
I have some comments with the present of manuscript which are highlighted below.
- This manuscript has no novelty
Answer: The novelty of this work is to synthesize new organotin complexes containing an ibuprofen moiety using simple procedures. These could be used as effective inhibitors for the PVC photodegradation.
- The authors repeated this work in previous research articles using similar compounds as photostabilizers
Answer: This work continuation designing and synthesizing new additives for PVC photostabilization. We now report the synthesis of new organotin complexes containing an ibuprofen moiety using simple procedures. The reported additives were not reported previously, which have new properties and impact.
- Why ibuprofen (used mainly in medications) was used to prepare its complexes to apply as photostabilizers.
Answer: Ibuprofen and its tin complexes are highly aromatic and absorb the UV light directly to protect the polymer against photodegradation. In addition, they can form coordination bonds with the polarized C-Cl bonds in PVC, which stabilizes these polymeric materials to a significant extent.
- The authors did not apply a reference photostabilizer as hydroxyphenyl benzophenones or hydroxyphenyl benzotriazoles to compare with the prepared photostabilizers.
Answer: Lucki, J.; Rabek, J.F.; Rånby, B.; Qu, B.J.; Sustic, A. Vogl, O. Surface photografting of polymerizable 2-(2-hydroxyphenyl)2H-benzotriazoles as ultra-violet stabilizers. Polymer, 31, 1772-1781. (Reference 12) is covering this issue.
- Regarding the preparation of the PVC-photostabilizaers films; I want to ask about the solubility of the complexes in THF and hence the homogeneity of the prepared films.
Answer: All Ibuprofen complexes are soluble in the THF and homogeneity with PVC.
Reviewer 2 Report
This work aimed to discuss the stability property and relevant mechanism of synthesized organotin complexes with complexed with PVC film. The most interesting part of this work should be the changes of molecular group and chemical bond after the irradiation. Several queries should be cleared as below. Line 33. should be smoother. Also, many cacography should be checked. Line 66. What have been reported in many works? And, what's the relation or precondition for this work? Line 68-69. I think the authors should tell us more information about the objective of this research. Line 127. Did, and how, the the purity of synthesized complex affect the stability property? The authors didn't tell the PVC was weight with what instrument. The weighing method was not accurate for examine the weight loss of PVC before and after irradiation. Fig. 7 didn't show the PVC with Photo-stabilizers before UV exposure, and thus we did not get information about the original morphology of them, or we didn't know if adding Photo-stabilizers would change the surface of PVE film or not. The dose of irradiation should be shown concerning Fig.8.Author Response
Reviewer 2
This work aimed to discuss the stability property and relevant mechanism of synthesized organotin complexes with complexed with PVC film. The most interesting part of this work should be the changes of molecular group and chemical bond after the irradiation.
Several queries should be cleared as below:
- Line 33. should be smoother. Also, many cacography should be checked.
Answer: Thank you for noticing this, it was corrected. Also, the following sentence was re-written as follows. " Finally, it seems possible that such synthesized ibuprofen tin complexes can work as excellent photo-stabilizers of PVC ".
- Line 66. What have been reported in many works? And, what's the relation or precondition for this work?
Answer: To address the comment, a new paragraph has been added at Line 66 as follows. "Herein, we reported the synthesis of Ibuprofen tin complexes and the evaluation of the activity of these complexes as photo-stabilizer for PVC"
- Line 68-69. I think the authors should tell us more information about the objective of this research.
Answer: This sentence was added at the end of introduction "Ibuprofen tin complexes are electron rich and act as UV absorbers. Therefore, these complexes are expected to absorb UV irradiation and protect PVC against photodegradation".
- Line 127. Did, and how, the purity of synthesized complex affect the stability property?
Answer: The high purity ibuprofen tin complexes made them more stable.
Ibuprofen contain heteroatoms that react with tin-containing reagents to produce highly stable complexes.
- The authors didn't tell the PVC was weight with what instrument. The weighing method was not accurate for examine the weight loss of PVC before and after irradiation.
Answer: PVC films have been weighted by a 4 digits sensitive balance before and after irradiation.
- 7 didn't show the PVC with Photo-stabilizers before UV exposure, and thus we did not get information about the original morphology of them, or we didn't know if adding Photo-stabilizers would change the surface of PVE film or not. The dose of irradiation should be shown concerning Fig.8.
Answer: The caption of fig. 8 was changed " Figure 8. FESEM PVC surface images. (a) PVC (b) PVC + 1 (c) PVC + 2 and (d) PVC + 3 after 300 hours of UV light exposure at intensity of 6.43 × 10 -9.ein dm-3.S-1.
The addition of the photo-stabilizers would not change the surface of PVC film because its small quantity.
Reviewer 3 Report
I am in favor of publishing this manuscript containing a good number of interesting data and relevant analysis. My comments are given below for a major revision:
- Abstract: When using for the 1st time, please use the elaboration of the abbreviation used (e.g., FTIR, NMR and so on).
- Abstract: “Using Field-emission scanning electron microscopy (FESEM) and microscopic images technique demonstrated that…” – Please correct the language.
- There are 19 self-citations in this work out of 50 references. Among those, 3-5, 12, 13, 15, 17-23, 31 and 32 are used either in the introduction section literature survey or in the experimental section standard equation only. It is highly recommended that authors consider replacing these references with the pioneer works in this field from other researchers. For standard equations, references from the books would be more appropriate, if considered.
- “The PVC films were formed by dissolved 5 g of the polymer…” – Please correct the language.
- Section 2.1: Please provide more details on the NMR experiment (sample preparation, test temperature, no. of scans, and so on).
- “All prepared films were died using vacuum to remove…” – Please correct the language “died”.
- Section 3.1: Please provide all of the FTIR and NMR spectra in a supplementary information file with proper legend and peak assignment.
- “The of PVC solution viscosity is used to measure the…” – Please correct the language.
- Fig. 7: Include same 200 nm scale SEM images of all four samples as Fig 7(b-e) after exposure. I agree that Fig. 8 provides lot more details because of the zoomed in view, however, it doesn’t help with the direct comparison to visualize the effect of irradiation.
- Please make sure that Fig. 8 scale information are available.
- “Obviously, it has demonstrated that the surface of the polymer became rougher and has more cracks, bigger spots after exposure to UV light in comparison to its surface before exposure to UV light.” – This is hard to follow. Please provide arrow marks to show the roughness and cracks.
- Fig 9: Please provide scale.
- Language: The English language of this manuscript needs improvement. I have mentioned some corrections in my comments, however, there are many more in the manuscript need correction. I am recommending a proofread of the manuscript thoroughly using a language editing service.
Author Response
Reviewer 3
I am in favor of publishing this manuscript containing a good number of interesting data and relevant analysis. My comments are given below for a major revision:
- Abstract: When using for the 1st time, please use the elaboration of the abbreviation used (e.g., FTIR, NMR and so on).
Answer: They were amended " Fourier Transform Infrared, 1H, 119Sn-Nuclear Magnetic Resonance"
- Abstract: “Using Field-emission scanning electron microscopy (FESEM) and microscopic images technique demonstrated that…” – Please correct the language.
Answer: Already amended "Field-emission scanning electron microscopy (FESEM) and optical microscope"
- There are 19 self-citations in this work out of 50 references. Among those, 3-5, 12, 13, 15, 17-23, 31 and 32 are used either in the introduction section literature survey or in the experimental section standard equation only. It is highly recommended that authors consider replacing these references with the pioneer works in this field from other researchers. For standard equations, references from the books would be more appropriate, if considered.
Answer: The unnecessary references were changed
- “The PVC films were formed by dissolved 5 g of the polymer…” – Please correct the language.
Answer: The sentence has been changed to " PVC (5.0 g) in tetrahydrofuran (THF; 100 mL) was stirred at room temperature"
- Section 2.1: Please provide more details on the NMR experiment (sample preparation, test temperature, no. of scans, and so on).
Answer: This sentence was added “using tetramethylsilane as the internal standard in deuterated dimethyl sulfoxide and.."
Proton nuclear magnetic resonance (1H-NMR) spectra (500 MHz) were recorded on a Bruker DRX500 NMR Spectrometer (Bruker, Zürich, Switzerland) in DMSO-d6 related to tetramethylsilane.
- “All prepared films were died using vacuum to remove…” – Please correct the language “died”.
Answer: Corrected "dried"
- Section 3.1: Please provide all of the FTIR and NMR spectra in a supplementary information file with proper legend and peak assignment.
Answer: They were attached
- “The of PVC solution viscosity is used to measure the…” – Please correct the language.
Answer: Corrected
- Fig. 7: Include same 200 nm scale SEM images of all four samples as Fig 7(b-e) after exposure. I agree that Fig. 8 provides lot more details because of the zoomed in view, however, it doesn’t help with the direct comparison to visualize the effect of irradiation.
Answer: Small quantity of additive didn't affect on surface morphology. Therefore, PVC (blank) film helps us to understand the surface
- Please make sure that Fig. 8 scale information are available.
Answer: Already changed with clear scale information
- “Obviously, it has demonstrated that the surface of the polymer became rougher and has more cracks, bigger spots after exposure to UV light in comparison to its surface before exposure to UV light.” – This is hard to follow. Please provide arrow marks to show the roughness and cracks.
Answer: Arrows were added.
- Fig 9: Please provide scale.
Answer: It was added.
- Language: The English language of this manuscript needs improvement. I have mentioned some corrections in my comments, however, there are many more in the manuscript need correction. I am recommending a proofread of the manuscript thoroughly using a language editing service.
Answer: The manuscript had another round of revision.
Reviewer 4 Report
The manuscript entitled: "A Surface Morphological Study, Poly(Vinyl Chloride) Photo-stabilizers Utilizing Ibuprofen Tin Complexes Against Ultraviolet Radiation" is a very nicely written work dealing with the packaging of Ibuprofen Tin complexes. The results presented are fascinating, while the study for the influence of UV irradiation is complete. I could not locate any significant issue and therefore, I recommend the manuscript to get accepted only after some minor points.
The first has to do with the errors and statistics of the measurements presented. Please include some statistics. Many diagrams are presented with absolute values, something that can be slightly different with different experiments.
Additionally, some details and scalebar of the light microscopy images are missing.
Last but not least, please include the methods for sample preparation for microscopy experiments.
Author Response
Reviewer 4
The manuscript entitled: "A Surface Morphological Study, Poly(Vinyl Chloride) Photo-stabilizers Utilizing Ibuprofen Tin Complexes Against Ultraviolet Radiation" is a very nicely written work dealing with the packaging of Ibuprofen Tin complexes. The results presented are fascinating, while the study for the influence of UV irradiation is complete. I could not locate any significant issue and therefore, I recommend the manuscript to get accepted only after some minor points.
The first has to do with the errors and statistics of the measurements presented. Please include some statistics. Many diagrams are presented with absolute values, something that can be slightly different with different experiments.
Answer: Thank you for your note. We'll take it in consideration in future study
Additionally, some details and scalebar of the light microscopy images are missing.
Answer: The scale bar of the light microscopy images has been added "400X magnification"
Last but not least, please include the methods for sample preparation for microscopy experiments.
Answer: the method for sample preparation for microscopy experiments were added "The film was cut into 1 × 1 cm dimensions and placed into a device".
Round 2
Reviewer 3 Report
Following recommendations are missing from the 1st round review. It is suggested that authors revise the manuscript carefully:
1.
- Section 2.1: Please provide more details on the NMR experiment (sample preparation, test temperature, no. of scans, and so on).
Round 2 comment: Please provide some essential details on the NMR experiment such as test temperature and no. of scans.
2.
- Section 3.1: Please provide all of the FTIR and NMR spectra in a supplementary information file with proper legend and peak assignment.
Answer: They were attached
Round 2 comment: Please upload the file. I don't see any supplementary file uploaded in this round.
3.
- Please make sure that Fig. 8 scale information are available.
Answer: Already changed with clear scale information
Round 2 comment: Please check and correct. The scales are not clear and units are not legible at all.
4.
- Fig 9: Please provide scale.
Answer: It was added.
Round 2 comment: Authors added magnification information in the title, however, scale is still missing. It was recommended to add scale on the image (as an example, 200 nm scale in Fig. 7) which will help the reader to get an idea about the particle and agglomeration size. Please add.
5.
- Language: The English language of this manuscript needs improvement. I have mentioned some corrections in my comments, however, there are many more in the manuscript need correction. I am recommending a proofread of the manuscript thoroughly using a language editing service.
Answer: The manuscript had another round of revision.
Round 2 comment: Agreed, however, it is not clear what were the corrections in this round. I am recommending a proofread of the manuscript thoroughly using a language editing service.
Author Response
Dear Reviewer,
Thank you for your efforts and time to improve the quality of our work, we really appreciate that. The followings are our answers to your comments.
With regards
Following recommendations are missing from the 1st round review. It is suggested that authors revise the manuscript carefully:
1.
- Section 2.1: Please provide more details on the NMR experiment (sample preparation, test temperature, no. of scans, and so on).
Round 2 comment: Please provide some essential details on the NMR experiment such as test temperature and no. of scans.
Answer: The following paragraph was added: “The sample was shaken or ultrasonic was used if necessary until full dissolving was achieved. 500 MHz 1H NMR and 107 MHz 119Sn NMR was used to identify the substance with 16 scans. The samples were irradiated at room temperature with a maximum wavelength of 365 nm.”
- Section 3.1: Please provide all of the FTIR and NMR spectra in a supplementary information file with proper legend and peak assignment.
Answer: They were attached
Round 2 comment: Please upload the file. I don't see any supplementary file uploaded in this round.
Answer: A supplementary file was added as requested. Sorry for didn’t upload it due to of a technical issue.
3.
- Please make sure that Fig. 8 scale information are available.
Answer: Already changed with clear scale information
Round 2 comment: Please check and correct. The scales are not clear and units are not legible at all.
Answer: The scales were clarified.
4.
- Fig 9: Please provide scale.
Answer: It was added.
Round 2 comment: Authors added magnification information in the title, however, scale is still missing. It was recommended to add scale on the image (as an example, 200 nm scale in Fig. 7) which will help the reader to get an idea about the particle and agglomeration size. Please add.
Answer: The scale bars were added. Thanks for your comment.
5.
- Language: The English language of this manuscript needs improvement. I have mentioned some corrections in my comments, however, there are many more in the manuscript need correction. I am recommending a proofread of the manuscript thoroughly using a language editing service.
Answer: The manuscript had another round of revision.
Round 2 comment: Agreed, however, it is not clear what were the corrections in this round. I am recommending a proofread of the manuscript thoroughly using a language editing service.
Answer: The language was revised carefully and changes were made at every single row, including rewriting sentences. Now, the manuscript should be in better shape regardless of where the previous mistakes were at. It is very hard to point out the previous mistakes; however, if there are any suggestions to improve the language, we will be more than happy to do so.
