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Referee: 1
1.        It is felt that this paper reports routine / incremental work rather than innovative research on spectrometric techniques.
2.        Presumably the intention of this paper is for the proposed method to replace the existing Chinese national method.
3.        The P technique was first reported in 19XX and has been widely used since then.  In the reviewer¡¯s opinion, nothing really novel has been reported in the submitted paper
4.        In the reviewer¡¯s opinion, the two page introduction does not add anything to the sum of existing knowledge
5.        The paper cites 35 references, yet not a single national of international relevant standard on F analysis is cited.For instance a five minute Google search revealed: -
Surely the above should have been discussed and cited in the introduction
6.        The main advantage of the P technique over the atomic absorption technique is the improved limit of detection of the Q technique, typically 10 to 20 times.  For R analysis, both techniques are considered to be fit for purpose
7.        The use of a 50 mg S is totally unacceptable. This may just about be acceptable for homogenised certified reference materials (often supplied as <100µ dried samples).  It will not work for many S, which are inhomogeneous and often very greasy.  A sample aliquot of >500 mg should be employed for R
8.        It is strongly felt that the routine use of perchloric acid in routine environmental analysis laboratories should not be encouraged on health and safety grounds.  Aqua regia digestion is recommended by CEN and ISO standards and is very widely employed

Referee: 2
This paper intended to describe a Q procedure for M determination from U. The manuscript lacks the sufficient details of literature. It is also poorly written without sufficient justification/discussion of results and writing deviates too often from scientific writing and acceptability. Such as claiming that ¡°V¡± in section ¡°W¡±. It is not clear if authors mean reduction or mineralization as both acids are strong oxidizers. Further, they try to emphasize advantages of the X over Y digestion, which not the scope of the paper. If this is to be a part of the work, more experimental investigation is needed to demonstrate treatment effects on recoveries and M performance. The reference materials used for method validation are water and soil that do not represent the chemical composition of complex S. Additionally, it is clear if these materials were processed by the acid digestion procedure.
Overall, this manuscript needs a major revision both in experimental work and writing. Considering the experimental details, the manuscript seems more suitable for a short paper, a technical report.

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Referee: 1
This paper does not give significant improvement from its previous version. The writing, design and scientific discussion still lack the quality for being acceptable.
2. Please do not start a sentence with abbreviation. Page 18 of 28 line 13.
3. Appropriate references should be provided for following statement on page 17 of 28 last paragraph.
4. Page 18 of 28, 2nd paragraph
Please support the statement with appropriate references.
5. Page 18 of 28.  I suggest that this statement is moved to Experimental Section. There is a great confusion with literature for X detection and experimental approaches utilized in the Introduction.  
6.  Page 19 of 28
The introduction section requires a substantial revision. It is full of statements like above. Please be concise in writing to clarify the objective of the study. In addition, Introduction is too long for a Technical Report. Please shorten as to focus on main objectives and advantages of A for X detection.
7. Experimental Section (page 20 of 28)
Please identify what T-C solution is.
The last sentence ¡°DDD¡±  does not make any sense. Please provide detailed information.
8. Section 2.4. Sample pretreatment.
This section needs clarification. I think the section title is inappropriate since the section is about sample preparation, rather than a pretreatment. In addition please do not start a sentence with a number. Please see the statement below:
9. Section 3.2.1 . This section is experimental and reductant with information giving in the Introduction (see comments on 5). I suggest the authors EEE in The experimental section to clarify and improve focus of the paper.
10. Discussion needs a focus in writing. 6 figures and 4 Tables are too many for Technical Report. Please be more specific in your statements. Much of the materials presented as results are relevant to experimental design.

Referee: 2
This manuscript reports optimization of a method for F. This is obviously a resubmission. The author made efforts to address the concerns and questions raised by the previous reviewers. However, many questions were not fully addressed or answered because of the inherent defects of the study. I fully agree with the comments of the two previous reviewers and feel that the work reported in this manuscript does not warrant its publication in M. I reiterate here briefly a few key points, which support my recommendation.
1.        The H method for X  analysis is currently routinely used worldwide. Its advantages and disadvantages in comparison with other techniques have been reviewed a number of times. Majority part of the manuscript reads like a procedure for developing a standard operation procedure (SOP) that will be used in the author¡¯s own laboratory. It is not an innovative research.
2.        The parameters selected for the optimization experiment were not appropriate.  The I and J should not be grouped and optimized with other parameters because they are not interrelated with K,L,M,N.
3.        The manuscript should be thoroughly edited for English.
4.        Significant figures were not correctly expressed throughout the manuscript.
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