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Question 2.5
The details of the analytical techniques used as well as the procedure used to analyze your
products should be provided. The experimental procedure of the preparation of the mixtures
AP supplemented with different catalysts needs to be well elaborated.
- The test DSC performed in the research is explained comprehensively in the revised paper.
In the experiment, the sample's release or capture of heat is checked. The samples examined
in the paper are a combination of ammonium perchlorate plus different catalysts, which is
the purpose of testing the catalytic effect on the thermal decomposition of ammonium
perchlorate (AP). In the thermal decomposition of ammonium chlorate, two points are
essential: the starting temperature of the thermal decomposition and the amount of heat
released. The paper focuses on the heat released during the use of catalyst 3, which is very
high. DSC analysis (or Differential Scanning Calorimetry) is a thermal analysis and one of
the most widely used methods for analyzing polymer and mineral materials. In thermal
analysis, the characteristics or changes in the characteristics of materials due to heat are
measured. A wide range of physical properties of materials can be obtained by interpreting
DSC results. Temperature and heat of phase change (such as melting and crystallization
temperature), chemical changes (decomposition and oxidation), and temperature of
transformations and reactions are among these properties. DSC analysis, compared to DTA
thermal analysis, has the advantage that in this analysis, the heat produced or absorbed can
moreover be determined. Mahamax provides the most comprehensive DSC analysis services.
The temperature range of up to 1000 degrees and the possibility of reading with both return
and return cycles is a unique service from Mahamax. Now, the DSC device used in the
experiment is SDT Q600 which is tested under Argon gas and the thermal treatment of 10℃
per minute.
Question 2.6
The authors didn't mention in the main text the results reported in the supplementary
materials. These latter should be carefully discussed in the main part of the text to confirm
the quality of the obtained products. Nevertheless, if the data were already published, provide
the references employed for that. A schematic presentation is highly recommended.
- Thanks for your comment; the outcomes of the supplementary materials are discussed and
analyzed in the manuscript. The references are cited in the right places if necessary. Actually,
the materials extracted from the previous studies are cited otherwise they are defined without
reference. A schematic image is in adition presented for indicating the processes of
conducting the project in detail. furthermore the explanations regarding materials of the
supporting file are given and highlighted in red.
Question 2.7
Please state if your DSC is previously calibrated because it is an important factor to get
consistent results.
- Thanks for your comment; the supplementary information has been added to the discussion
part of the revised paper. As stated in the revised manuscript, DSC is previously calibrated.
Question 2.8
Further characterizations of the obtained catalysts such as Raman as well as some
micrographs using SEM are welcome.
- Thanks for your comment; we moreover conducted this test to prepare the manuscript based
on your valuable comments. The results related to Raman are discussed before section 3.3
and more information is added.
The three compounds 1, 4 and 6 have a charectristich Raman direction as shown in Figure
7. Accordingly, the peaks related to the identification of copper are observed in the range of
400 and 1500 cm-1. moreover, the framework containing cobalt metal in the regions of 500,
700 and 900 cm-1, indicating the structure of this compound. In the spectrum of the
framework containing manganese, peaks relevant to manganese are observed at 400 and
600. furthermore, Figures S13-19 in Supporting Information shows the analytical results of
Raman for compounds 1-6.
Question 2.9
The sign Exo/Endo should be provided in DSC figures.
- The DSC figures have been edited based on your comment. Figures 1-6 have been improved
significantly in the revised version such as below:
Question 2.10
What is the amount of the catalyst employed?
- The amount of the catalyst is 5%, as written in the text and figures. Notably, in Figure 6 and
related explanations, 2 and 8 % are used to evaluate the amount of catalyst less and more.
Question 2.11
If the authors can add some TGA analyses of AP supplemented with different catalysts, they
can consolidate their discussion.
- Table 1 demonstrates the TGA analyses of AP with the various catalysts. To represent the
result clearly, more a comparison is made between the thermodynamic date presented in the
table 1, as can be seen from table 1, while the highest Wt.% value is relevant to Cu-Mtta +
Ap, its ∆H/J.g-1 value is much lower than the gighest obtained data ( 1470 ∆H/J.g -1 compared
to 2120 ∆H/J.g-1). Generally combined catalysts presented in the Table 1, improves the
enthalpy values to can siderabled amounts when compared to other Catalyst found in the
litrature. Cu-AzTO + AP has the acceptable value of enthalpy before and is now a good
candidate for accelerating the AP thermal decomposition. However, the use of the proposed
combination is more recommended here.
Table 1. Catalytic activity resulting from various additives on AP thermal decomposition
Sample Wt% TL/oC TH/oC ∆H/J.g-1 References
CuO NPs + 4 317 359 1360 [1]
AP
Cu/CNT + 5 282 316 1345 [1]
AP
Cu/GO + AP 5 303 354 1721 [1]
Hkust-1 + 5 300 345 1470 [1]
AP
Cu-AzTO + 5 297 328 2120 [43]
AP
Cu-Mtta + 25 - 318 1470 [44]
AP
3 + AP 5 - 309 2435 This work
In addition, more comparison is made in Section 3.2 above Table 1 to represent the outcomes
well.
Question 2.12
How about the Ea of pure AP, and which contains other catalysts? Why do the authors
determine only 1 activation energy? I can see the various heating rate 2 decomposition
processes, which means that the LTD and the HTD are shifted to lower temperatures.
- In some samples, such as samples 1, 4, 5 and 6, LTD is not seen. furthermore, in real
burning conditions (in the presence of fuel), due to the released heat, the temperature rises
rapidly and the reaction conditions pass through LTD. moreover, Because HTD is crucial
and the reaction temperature is usually within the range of HTD, only its activation energy
can be calculated. For more explanations, see references 4, 10-15 and 41.
Question 2.13
Eqns. 4– 7 originate from Eyring's theory of the activated complex. In addition, they have
been derived for gas-phase reactions and do not directly apply to condensed-phase
decomposition
- The required explanations are given below Equations 4-7 based on the used references.
Notably, we attempted to make clear any ambiguity in the text by giving supplementary
information. Hence we added this sentence in the revised paper as it was moreover consistent
with our investigation. Reference 46 has been added.
Question 2.14
The decomposition products released during both processes of the decomposition of AP
(LTD and HTD) need to be deeply discussed. An interesting review paper can be used to well
do that (Applied Spectroscopy Reviews 55 (8), 724-777, 2020).
- Thanks for your comments; we need a DSC-GC device for conducting this analysis which is
not currently available in Iran. As our products have explosive nature and as result there are
difficulties with shipment, we didn’t consider DSC-GC analysis in other countries with such
equipments.
Question 2.15
Conclusions need more improvement and the references part needs to be updated because it is
not exhaustive.
- Thanks for your comment; to make the conclusions and refrences parts all-inclusive, edited
these parts both technically and qualitatively by mentioning the major findings and giving
interesting suggestions for future works. The references have furthermore been updated using
aticles published in 2022 and 2023.
We hope that with all these changes made, you may now find the manuscript suitable
for publication. Lastly, we would like to thank you and the panel of reviewers for their
suggestions resulting in the overall improvement of the manuscript.
With kind regards and thanks for your kind cooperation,