Structural Analysis of Interstratified Illite-Smectite by the Rietveld Method

Round 1

Reviewer 1 Report

Crystals 1124030 peer review

Structural Analysis of Interstratified illite-smectite by the Rietveld Method 

Line 30. Please explain what illite and smectite are, give chemical formulae and crystal structures

Line 102. Why were the samples ion-exchanged with CaCl2, please explain why this was done and the XRD/XRF analyses were not just done on the initial samples.

Line 111. What was the anode used for the Zetium XRF spectrometer (Rh, Ag, W?)

Line 112. What was the proportion of sample to lithium borate flux used to make glass beads? Please give more information, what temperature was used to melt the flux/sample mix to make the beads?

Line 117. How was Thermal Analysis used to discriminate the structure of the octahedral sheet? I am not an expert on this technique, why was it used and what information does this give?

Line 139. Why were AD and EG XRD data collected out to 40 degrees 2theta when the initial powder samples had XRD data collected out to 80 degrees. Were there any Bragg peaks past 40 degrees for AD and EG?

Line 195. R0, R1, R2 and R3 structure models were used for each sample, were any other models tried and why not? What were the space groups, lattice parameters and starting coordinates for these models? Give more information on the parameters used in the refinements. Presumably Tables 6 and 7 give the refinement results for the models which gave the best fit, how bad were the fits from the other models?

Line 200/258. Can positions of Bragg reflections be given in Rietveld difference plots?

Line 256. Were any preferred orientation parameters included in the Rietveld refinements?

 

 

 

Author Response

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Author Response File: Author Response.pdf

Reviewer 2 Report

The submitted study is very well-planned, described and scientifically sound. The introduction, though concise, is very informative. The aim of the study was stated clearly and the methods applied are adequate. My comments are rather minor issues, with a few major ones.

 

Line 13, „combined” not „combining”\

Line 41, Word „models” before „[8]” is missing.

Line 67, what about Reflex Plus from BIOVIA?

Line 68, it should be “three-dimensional”

Line 159, not “normalization showed” but „normalization are shown”

Line 166, not “It deduced” but „it was deduced”

Table 3, firstly LOI is not defined in the Table caption. Secondly, the data are presented without uncertainties. Were they somehow determined? I understand that WD-XRD is not so accurate (i.e. in comparison to ASA) but it should be stated somewhere how were the concentrations of elements determined. Have you used any calibration curves or was the analysis based solely on the feature which is usually part of the software used for XRF processing.

Figure 2, there is no x-axis label (2-theta, degrees).

Figure 5, what was the degree of polynomial used for background?

Line 196, so, I guess, you have used all the models (R0, R1, R2, R3) for each sample and then you have chosen the right model using the one for which the lowest Rwp was obtained, am I right? If yes, please create a Table with the Rwp for other models (R0, R1, R2, R3) to show if the choice was obvious (the differences between the Rwp obtained by fitting to different models).

Line 265, not “bigger” but “larger”.

Lines 337-349, please delete this text.

Author Response

Please see the attachment.

Author Response File: Author Response.pdf

Round 2

Reviewer 2 Report

The Authors have significantly improved their manuscript, following my suggestions. I find it now suitable for publication.