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Article
Peer-Review Record

Contamination Fingerprints in an Inactive W (Sn) Mine: The Regoufe Mine Study Case (Northern Portugal)

Minerals 2023, 13(4), 497; https://doi.org/10.3390/min13040497
by Helena Sant’Ovaia 1,2,*, Cláudia Cruz 1,2, Alexandra Guedes 1,2, Helena Ribeiro 1,2, Patrícia Santos 1,2, Sónia Pereira 1,2, Jorge Espinha Marques 1,2, Maria dos Anjos Ribeiro 1,2, Catarina Mansilha 3,4, Helena Cristina Brites Martins 1,2, Bruno Valentim 1,2, Joana Torres 2,5, Ilda Abreu 2,6, Fernando Noronha 1,2 and Deolinda Flores 1,2
Reviewer 1:
Reviewer 2: Anonymous
Minerals 2023, 13(4), 497; https://doi.org/10.3390/min13040497
Submission received: 14 March 2023 / Revised: 26 March 2023 / Accepted: 27 March 2023 / Published: 31 March 2023
(This article belongs to the Special Issue Geochemistry, Environmental Impact and Remediation of Mining Areas)

Round 1

Reviewer 1 Report

The manuscript entitled “Contamination Fingerprints in a Former W (Sn) Mine: the Regoufe Mine Study Case (Northern Portugal)is a case study, concerning the assessment of environmental pollution in the close vicinity of a former tungsten mine (Portugal).

The manuscript is quite concise, written in a good layout and in a clear language.

Below you can find some remarks that should be taken into account when revising the manuscript:

Title:

The title should be redrafted, especially the phrase ” a Former W (Sn) Mine”.

Abstract:

Line 33: Please remove: “(for example a forge)”.

Introduction:

- lines 47-54: References must be cited throughout the introduction. The authors write about phenomena that have been perfectly described and published already, e.g.

Kicińska A. 2016. Risk assessment of children's exposure to potentially harmful elements (PHE) in selected urban parks of the Silesian agglomeration. E3S Web of Conferences, 10, Art. No. UNSP 00035, doi: 10.1051/e3sconf/20161000035

Kicińska A., Smreczak B., Jadczyszyn J. 2019. Soil Bioavailability of Cadmium, Lead, and Zinc in the Areas of Zn-Pb Ore Mining and Processing (Bukowno, Olkusz). Journal of Ecological Engineering, 20, 1: 84-92, doi: 10.12911/22998993/93794

-          lines 72-74: Please reconstruct the sentence: first what was done and then by what methods.

Geological setting:

- Fig. 1: Please correct the legend to the figure, a significant part of it is currently missing.

Material and Methods:

Subchapter 3.2.:

-          lines 216-217: What acids were used for the decomposition? please complete the information, what was the ratio f. of the solid to the solution?

-          lines 222-226: Please indicate the literature in which the calculated indicators were described, or provide the formulas, how the individual parameters were calculated?

Subchapter 3.3.:

-          line 240 and 250: Please enter the numbers for the patterns.

Results and Discussion:

-          Line 308: Why the content of Sn and W was not analyzed, the ores of these elements were exploited, isn’t it?

-          Tab. 2. There is no such measurable value “0.000”. Please replace "0.000" with values below detection limit (b.d.l.).

-          Tab. 3. What is the unit for cations and anions?

-          Tab. 4. What does the dot mean? Why are the results given with different accuracy?

Author Response

 Dear Reviewer

Thank you very much for your valuable feedback on this article. Your insightful comments were all considered and have been incredibly helpful in improving the quality and clarity of the article.

All answers are presented in detail below.

 

Sincerely,

Helena Sant’Ovaia

______________________________________

  • Title:

The title should be redrafted, especially the phrase “a Former W (Sn) Mine”.

Answer: The title was rewritten to: “Contamination fingerprints in an inactive W (Sn) Mine: the Regoufe mine study case (Northern Portugal)”

  • Abstract:

Line 33: Please remove: “(for example a forge)”. Answer: Removed.

  • Introduction:

Lines 47-54: References must be cited throughout the introduction. The authors write about phenomena that have been perfectly described and published already, e.g.

KiciÅ„ska A. 2016. Risk assessment of children's exposure to potentially harmful elements (PHE) in selected urban parks of the Silesian agglomeration. E3S Web of Conferences, 10, Art. No. UNSP 00035, doi: 10.1051/e3sconf/20161000035

KiciÅ„ska A., Smreczak B., Jadczyszyn J. 2019. Soil Bioavailability of Cadmium, Lead, and Zinc in the Areas of Zn-Pb Ore Mining and Processing (Bukowno, Olkusz). Journal of Ecological Engineering, 20, Ecological Engineering, 20, 1:84-92,doi: 10.12911/22998993/93794

 

Answer: The references were included.

Lines 72-74: Please reconstruct the sentence: first what was done and then by what methods.

Answer: The paragraph was rewritten to:

“To trace anthropogenic pollution, by applying environmental magnetism techniques, namely identifying ferromagnetic minerals in soils and waste mining tails sampled in the surrounding area of Regoufe mine”.

 

Geological setting:

Fig. 1: Please correct the legend to the figure, a significant part of it is currently missing.

Answer: Sorry, the map has gone out of place; the problem has been solved and the whole map and legend are now visible.

  • Material and Methods:

Subchapter 3.2.:

Lines 216-217: What acids were used for the decomposition? please complete the information, what was the ratio f. of the solid to the solution?

Answer: Text was included with the information (in bold)

This analysis was carried out at ACME Analytical Laboratories (Vancouver, BVC, Canada) using the method Four Acid digestion Ultratrace ICP-MS analysis. A sample weight of 0.25 g was heated to fuming in a tri-acid mixture (HF–HClO4–HNO3) and taken to dryness. Subsequently, the residue was dissolved in HCl. Resulting solutions were then analysed by ICP-MS. Analytical results of certified reference materials (STD OREAS45H and STD OREAS501D), blanks and random duplicate samples were used for quality control of the analytical procedure.

 

Lines 222-226: Please indicate the literature in which the calculated indicators were described, or provide the formulas, how the individual parameters were calculated?

Answer: This information was already included in the Supplementary File.

 

  • Subchapter 3.3.:
  • line 240 and 250: Please enter the numbers for the patterns.

Answer: numbers were inserted.

  • Results and Discussion:

Line 308: Why the content of Sn and W was not analyzed, the ores of these elements were exploited, isn’t it?

Answer: These metals were analyzed. However, they were not included in this work because the purpose was to study only the PTE’s

Tab. 2. There is no such measurable value “0.000”. Please replace "0.000" with values below detection limit (b.d.l.).

Answer: Table 2 was corrected.

- Tab. 3. What is the unit for cations and anions?

Answer: The units are mg/L; units were included on the table.

-Tab. 4. What does the dot mean? Why are the results given with different accuracy?

Answer: Results are given with the same accuracy and were corrected on the table.

Author Response File: Author Response.pdf

Reviewer 2 Report

The manuscript deals with the environmental impact assessment of the mining activity in a former W (Sn) mine (Northern Portugal), closed about 50 years ago. The manuscript is interesting, robust, well written and in order to achieve the proposed objective, the authors used a wide battery of analyses and tests (magnetic characterization and geochemistry of soils, mining waste tails and plants, and hydrogeo- chemistry).

In my opinion, the manuscript needs some further improvements, as follows:

Please translate in English the affiliations for all authors.

Figure 1: please reduce the size of the figure, to include the entire legend.

The authors should add briefly the digestion method for soil samples, prior to ICP-MS analysis.

Quality control: the authors should add the results obtained for CRMs (STD OREAS45H and STD OREAS501D) in relation to the certified reference concentrations.

Table 3: measure units are missing for the anions and cations.

Please add the limits of quantifications for metals in water, especially for Cu, using atomic absorption spectrometry.

As a personal curiosity: Water samples were groundwaters from mine galleries (P1, P3) and surface water downstream of the mine drainage gallery (P2). The obtained concentrations for metals were compared with Parametric Value (PV) for drinking water purposes. Are those waters used for drinking?

References no. 2 and no. 24 seem to be the same.

Author Response

Answer to Reviewer2

 Dear Reviewer

Thank you very much for your valuable feedback on this article. Your insightful comments were all considered and have been incredibly helpful in improving the quality and clarity of the article.

All answers are presented in detail below.

Sincerely,

 

Helena Sant’Ovaia

______________________________________

 

  • Please translate in English the affiliations for all authors.

Answer: All the affiliations were translated.

  • Figure 1: please reduce the size of the figure, to include the entire legend.

Answer: Sorry, the map has gone out of place; the problem has been solved and the whole map and legend are now visible.

  • The authors should add briefly the digestion method for soil samples, prior to ICP-MS analysis.

Answer: text was included with the information (in bold).

This analysis was carried out at ACME Analytical Laboratories (Vancouver, BVC, Canada) using the method Four Acid digestion Ultratrace ICP-MS analysis. A sample weight of 0.25 g was heated to fuming in a tri-acid mixture (HF–HClO4–HNO3) and taken to dryness. Subsequently, the residue was dissolved in HCl. Resulting solutions were then analysed by ICP-MS. Analytical results of certified reference materials (STD OREAS45H and STD OREAS501D), blanks and random duplicate samples were used for quality control of the analytical procedure.

 

  • Quality control: the authors should add the results obtained for CRMs (STD OREAS45H and STD OREAS501D) in relation to the certified reference concentrations.

Answer: The results were included in table 1.

 

  • Table 3: measure units are missing for the anions and cations.

Answer: The units are mg/L; units were included on the table.

 

  • Please add the limits of quantifications for metals in water, especially for Cu, using atomic absorption spectrometry.

Answer: Result is below the detection limit of 1 µg/L Cu

  • As a personal curiosity: Water samples were groundwaters from mine galleries (P1, P3) and surface water downstream of the mine drainage gallery (P2). The obtained concentrations for metals were compared with Parametric Value (PV) for drinking water purposes. Are those waters used for drinking?

Answer: The groundwater from the mine drainage galleries may be used for drinking, especially by hikers and shepherds.

  • References no. 2 and no. 24 seem to be the same.

Answer: you are right! The mistake was corrected.

 

Author Response File: Author Response.pdf

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