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Article
Peer-Review Record

The Challenge of Grinding Ternary Blends Containing Calcined Clays and Limestone

Minerals 2022, 12(9), 1170; https://doi.org/10.3390/min12091170
by Juan Francisco Garces-Vargas 1,*, Yosvany Díaz-Cardenas 2, Franco Zunino 3, Juan Ribalta-Quesada 2, Karen Scrivener 3 and Fernando Martirena 2
Reviewer 1: Anonymous
Reviewer 2:
Minerals 2022, 12(9), 1170; https://doi.org/10.3390/min12091170
Submission received: 28 July 2022 / Revised: 21 August 2022 / Accepted: 6 September 2022 / Published: 16 September 2022
(This article belongs to the Special Issue Blended Cements Incorporating Calcined Clay and Limestone)

Round 1

Reviewer 1 Report

This manuscript describes the influence of co-grinding (LC3) and separate grinding (LC2) of OPC with clay, limestone, and gypsum.

Here are some comments:

- in the abstract, you mentioned the use of grinding aids from the family of TEA, while you only use one type (TEA-GLCR) at two different dosages in the study (3g and 4.5g). I would recommend only mentioning the one grinding aid in the abstract, as some readers might expect a study of several types of grinding aids. There should be a paragraph on why this particular grinding aid was selected for this study and no other.

- in the materials and methods section, the techniques and equipment are not described. The readers would like to know the type of equipment used for granulometry (PSD), with water or isopropanol, did you use ultrasound, etc. Same for quantitative XRD, XRF, Blaine fineness, calorimeter, what type of equipment was used, as well as the brand? What are the procedures used for each equipment: for example, the scan time for XRD, the software used for XRD interpretation, the ICDD files used? What kind of ball mill was used? What was exactly the sizes and materials of the balls used inside the ball mill? All of this information is important for any reader to be able to reproduce the experiments and the results.

- in the experimental procedure section:

- there is a mention of Table 5 summarizing the grinding times, which is absent from Table 5.

- Please, can you explain this sentence “in addition, the compressibility parameter was obtained”? Are you referring to the Blaine method?

- There is a paragraph duplicated within the section 2.3.2, when presenting the tests carried out for fresh concrete, before and after Table 6.

- Why was the TAM Air calorimeter calibrated at 30 C? Is there a justification for using this high temperature? If so, were all the tests performed on pastes, mortars, and concretes performed at 30 C as well?

- in the results section:

                - I would recommend zooming on the calorimeter data, Figures 7 and 10, maybe up to 100 hours, so the readers can clearly see the differences between the samples.

                - Figures 5, 6, 8, 9, 11, 12, 13, 14, and 15 repeat the results twice: once in the graph, and then under as numbers. I would recommend choosing one or the other.

                - Figure 9 is missing the PSD data.

                - Figure 11 is represented twice, as included in Figure 12 too. I suggest removing Figure 11.

                - Figure 13 and 14 might be combined for better clarity.

 

There might be an excessive number of self-citations, one third of the citations are self-citations:

- Zunino – in references: 18, 24, 25, 27

- Scrivener – in references: 5, 6, 8, 9, 10, 18, 24, 25, 27, 30

- Martinera – in references: 6, 8, 9, 30

 

Also, references 18 and 24 are the same.

 

Author Response

Please see attached file

Author Response File: Author Response.pdf

Reviewer 2 Report

 

Journal: Minerals (ISSN 2075-163X)

Manuscript ID: minerals-1864225

Type: Article

Title: The challenge of grinding ternary blends containing calcined clays and limestone.

Authors: Juan Francisco Garces-Vargas* , Yosvany Diaz-Cardenas, Franco Zunino, Juan Ribalta-Quesada, Karen Scrivener, Fernando Martirena.

 

a)           Line 156, how does the author measure the particle size of the samples used? Explain in detail.

b)          Figure 1 Delete the background from the figures and revise the Y axis in the other side.

c)           The author wrote “Both aggregates meet the specifications of Ecuadorian standards” add ref.

d)          Why the author didn’t use energy‒ dispersive X‒ray spectroscopy (EDX) to distinguish the elements of the sample?

e)           Why the author did not utilize XRD diffraction to construct the phases?

f)            Figure 2, the same note for figure 1 and revise the legend of the figure and the intervals of X-and Y axes.

g)          Figure 3 the same note as mentioned in f.

h)          Figure 4 the same note as mentioned in f.

i)             Figure 5 the same note as mentioned in f.

j)             Figure 6 the same note as mentioned in f.

k)          Figure 7, 8, 9, 10, 11, 12, 13, 14, and 15, the same note as mentioned in f.

l)             Why the author didn’t measure the compression Strength, thermal conductivity, roughness, and hardness of the samples used?

 

Best Regards

Author Response

Please see attached file 

Author Response File: Author Response.pdf

Round 2

Reviewer 1 Report

I would like to thank the authors for replying to the comments.

However, I still do not agree with not providing the techniques and equipment used during this project. Providing the name of the equipment (XRD), the way the samples were scanned by XRD, and the way the data was interpreted for XRD should not matter for the company.

Please, can you describe how you obtained the compressibility index exactly?

You mention that the TAM Air was run at 30C to take into account the working conditions. Did you perform all the other tests at 30C, such as compressive strength for mortar and concrete to take into account the working conditions?

Please, can you explain why it is not possible to enlarge the calorimeter data in Figure 7? Or at least provide an additional small graph with a zoom on the first 50 hours within the same graph?

 

 

Author Response

  1. However, I still do not agree with not providing the techniques and equipment used during this project. Providing the name of the equipment (XRD), the way the samples were scanned by XRD, and the way the data was interpreted for XRD should not matter for the company.

The recommendation was accepted and corrected.

Clay: The clay used was obtained from the mining area of the city of Cuenca (see Table 1). In this mining area a mixture of clay minerals of the 1:1 type is identified. Thermogravimetric Analysis (TGA) was used to quantify the kaolinite content of the clay by using the tangent method between 400 °C and 600 °C. 50 mg of powdered sample was analyzed using a Mettler Toledo TGA/SDTA 851 balance with a heating rate of 10 °C/min from 30 °C to 1000 °C under constant dinitrogen flow of 30 mL/min. The content of clay minerals of the kaolinite group was estimated as 55.27%. The Loss on Ignition (LOI) of the clay was also quantified by TGA and from the weight loss between 30 °C and 1000 °C. The CaCO3 content in the limestone was calculated from TGA as well, from the weight loss between 600 °C and 800 °C. The experimental protocols for LOI and CaCO3 quantification by TGA were the same as for kaolinite quantification.

X-Ray Fluorescence (XRF) measurements were performed by an external company using a Bruker AXS S4 Explorer spectrophotometer operating at a power of 1 kW and equipped with a Rh X-ray source. Crystals used were OVO55FC for Na with 0.46° divergence collimator, PET for Al and Si with 0,23 ° divergence collimator and LiF220, with 0,23° divergence collimator for all other elements.

  1. Please, can you describe how you obtained the compressibility index exactly?

To begin the test, the cement sample to be tested should be prepared and the cement should be placed or poured into the container so that it falls in a loose state until the container is filled with the screed, remove the excess, then place the full container on the scale and note the weight, this weight would be the loose volumetric weight. After this we repeat the emptying step, but in layers, it is recommended that it be 3 or 4 layers compacted with the rammer passing it 4 to 5 times, once the container is filled, we proceed to level it and place it on the scale. The weight is noted down, which would be the compacted volumetric weight.

The following equation is used to obtain the result of the compressibility percentage: 100

  1. You mention that the TAM Air was run at 30C to take into account the working conditions. Did you perform all the other tests at 30C, such as compressive strength for mortar and concrete to take into account the working conditions?

That is correct, all tests on both mortars and concrete were performed at 30°C.

  1. Please, can you explain why it is not possible to enlarge the calorimeter data in Figure 7? Or at least provide an additional small graph with a zoom on the first 50 hours within the same graph?

The recommendation was accepted and corrected.

Author Response File: Author Response.pdf

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