Multi-Analytical Techniques to Define the Mineralogical and Petrophysical Characteristics and Provenance of Siliceous Lithic Findings: The Case Study of La Calvera Rock Shelter (Cantabria, Spain)
<p>Geological map of the Peña de Oviedo sector (west territory of Camaleño village) at scale 1:50.000 from Sheet 81—Potes modified, Instituto Geològico y Minero de España web site at link: <a href="http://info.igme.es/cartografiadigital/geologica/Magna50Hoja.aspx?language=es&id=81" target="_blank">http://info.igme.es/cartografiadigital/geologica/Magna50Hoja.aspx?language=es&id=81</a> (accessed on 15 March 2023). The inlets show the position of the study area in Spain (red rectangle) and a sketch map of the tectonic units in which the area is subdivided. The numbers of the formations are taken from the original map (sheet 81—Potes); those in bold indicate the formation hosting cherts and/or quartzites.</p> "> Figure 2
<p>Main representative samples of cherts, rock crystals and chunk raw materials analysed from La Calvera rock shelter: (<b>a</b>) grey chert of AR12.1 sample; (<b>b</b>) grey chert of AR18.2 sample; (<b>c</b>) grey-ochre chert of AR21; (<b>d</b>) raw material chunk of RM3.4 sample; (<b>e</b>) yellow chert of AR37 sample; (<b>f</b>,<b>g</b>) quartzite of AR29 and AR34 samples; (<b>h</b>,<b>i</b>) Domeño cherts of AN5.1 and AN1.2 samples (from Andilla, Valencia); (<b>l</b>) rock-crystal of AR10 sample. Red line is 1 cm.</p> "> Figure 3
<p>BSE images representative of analysed samples: (<b>a</b>) AR12.1 (grey chert) at low magnification, showing an apparent compact texture with cracks, holes (sometimes filled by phyllosilicates) and bright spots of zircon and metal oxides; (<b>b</b>) millimetres-long trail of Fe and Ti oxides within the quartz matrix (AN5.1,Grey-beige chert from Domeño); (<b>c</b>) AR37 (yellow chert) at moderate magnification that shows the rough surface covered by small crystals and plagues of light-grey phyllosilicates; (<b>d</b>) quartz matrix of AR29 (dark quartzite) hosting a REE-phosphate grain and Ti oxide; (<b>e</b>) compact and homogeneous surface of AR10 (rock crystal) samples with dark-grey stains due to carbon (organic?) impurities; (<b>f</b>) phyllosilicate in quartz matrix (AR34).</p> "> Figure 4
<p>BSE images representative of analysed samples: (<b>a</b>) corroded crystal of Ti-oxide and zircon in AR18.2 (grey chert); (<b>b</b>) Fe-oxide encrustation on the surface of the sample RM3.4 (grey chert); (<b>c</b>) framboidal pyrite on a calcite crystal at high magnification (AN1.2, blackish chert, Domeño); (<b>d</b>) negative crystal shape on the AN5.1 (grey-beige chert, Domeño) surface, formerly hosting calcite, whose remains are still preserved; (<b>e</b>) negative crystal shape of calcite, now totally removed; (<b>f</b>) NaCl patinas with particular snowflake-like habitus on the AR10 (rock crystal) surface.</p> "> Figure 5
<p>XRD patterns of the selected samples of cherts (AR12.1, AR18.2, AR21, AR29, AR34, AR37), rock crystal (AR10), raw material (RM03.4) and geological samples (AN1.2, AN5.1). Abbreviations followed by question marks corresponds to phases for which a clear assignment was not possible (see text).</p> "> Figure 6
<p>Positive correlation between the matrix crystallinity determined by comparing of the background signals of each sample with the background of a reference known crystallinity of the AR10 crystal rock and the grain size means determined by SEM analysis (see <a href="#minerals-13-00666-t003" class="html-table">Table 3</a>).</p> "> Figure 7
<p>Petrophysical and mechanical properties of archaeological and geological samples: (<b>a</b>) real density vs. bulk density; (<b>b</b>) real density vs. matrix crystallinity; (<b>c</b>) open helium porosity vs. bulk density; (<b>d</b>) helium open porosity vs. phase size mean; (<b>e</b>) helium open porosity vs. water open porosity; (<b>f</b>) open helium porosity vs. PLT punching strength index.</p> "> Figure 8
<p>Petrophysical and mechanical properties of archaeological and geological samples: (<b>a</b>) phase size mean vs. PLT punching strength index; (<b>b</b>) matrix crystallinity vs. PLT punching strength index.</p> "> Figure 9
<p>Mean (•) and standard deviation (♦) of the elemental concentrations for the six classes of samples (DC: Domeño chert; GCC: grey chert chunks; GCF: grey chert fragments; OC: other cherts; QZ: quartzite; RC: rock crystal).</p> ">
Abstract
:1. Introduction and Aims
2. Geological Setting and Natural Chert Occurrences
3. Materials and Methods
4. Results
4.1. Compositional Characteristics
4.1.1. SEM-EDS Analysis
4.1.2. XRD Analysis
4.2. Petrophysical Properties
4.3. Preliminary Results of Multielement Analysis
5. Discussion
6. Conclusions
Supplementary Materials
Author Contributions
Funding
Acknowledgments
Conflicts of Interest
References
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Sample | Rock type | Classification | Origin |
---|---|---|---|
AR10 | Rock crystal | Chunk | La Calvera rock shelter |
AR12.1 | Grey chert | Flake | La Calvera rock shelter |
AR18.2 | Grey chert | Flake | La Calvera rock shelter |
AR21 | Ochre chert | Flake | La Calvera rock shelter |
AR29 | Quartzite | Flake | La Calvera rock shelter |
AR34 | Quartzite | Flake | La Calvera rock shelter |
AR37 | Yellow chert | Chunk | La Calvera rock shelter |
RM03.4 | Grey chert | Chunk | La Calvera rock shelter |
AN1.2 | Domeño chert | Outcrop sample | Andilla (Valencia) |
AN5.1 | Domeño chert | Outcrop sample | Andilla (Valencia) |
Sample | Classification | Description |
---|---|---|
AR10 | Rock crystal | Colourless hyaline quartz with yellowish hues |
AR12.1 | Grey chert | Blackish surface with shiny appearance, compact but very rich in micro-grain alterations giving a porous appearance |
AR18.2 | Grey chert | Blackish with shiny appearance, compact with micro-grain alterations (similar to sample AR12.1) |
AR21 | Grey-ochre chert | Grey-beige, compact with conchoid-type fracturing and with porous appearance |
AR29 | Dark quartzite | Presence of dark-to-light colour gradient in thickness: dark side more porous and altered, light side shiny as formed by microcrystals (similar to sample AN5.1) |
AR34 | Dark quartzite | Dark in colour, porous and altered (similar to the dark side of sample ARCH29 but shinier) |
AR37 | Yellowish chert | Yellow-brown colour, with varied surface appearance: from smooth and firm in some places, to extremely porous in others |
RM03.4 | Grey chert | Black colour, shiny, almost obsidian-like appearance, with conchoid fractures, rich in alterations and also in diffuse patina (similar to sample 12.1) |
AN1.2 | Blackish chert | Blackish colour, compact with conchoid fracturing, low porosity, clean surface (no soil residue on the surface) |
AN5.1 | Grey-beige chert | Grey-beige surface with no soil residue on the surface, porous but compact appearance with conchoid-type fracturing |
Sample | Classif. | Textural/Structural Description | Qtz | Si-Al | Cal | Fe-ox | Ti-ox | Notes | Grain-Size Frequency Range (μm) | |
---|---|---|---|---|---|---|---|---|---|---|
AR10 | Rock crystal | Extremely compact, conchoid fractures, common Si-Al micro-grains, Fe oxide, gypsum, Zn oxide, Sn and P-REE, presence of NaCl surface patina | X | X | X | X | Zn oxide, Sn, Gyp, P-REE, NaCl | 25 | 120 | |
AR12.1 | Grey chert | Cribrous and rough appearance with microcavities filled by alteration phases, abundant metal oxides | X | X * | X | X | Zircons; Fe, Ni, Cr oxides | 8 | 50 | |
AR18.2 | Grey chert | Cribrous, rough appearance with microcavities filled by alteration phases, with many diffuse oxides | X | X | X | X | X | Gypsum and abundant Ti | 5 | 30 |
AR21 | Grey-ochre chert | Compact homogeneous surface, with diffuse niches rich in Si-Al phases and few metal oxides | X | X | X | / | 1 | 12 | ||
AR29 | Dark quartzite | Partly compact and clean and partly covered with earthy sediment, with scattering of Si-Al phases and metal oxides | X | X | X | X | P-REE | 10 | 80 | |
AR34 | Dark quartzite | Partly compact and clean and partly covered with earthy sediment, with scattering of Si-Al phases, metal oxides and P-REE | X | X | X | X | P-REE, Zircon, phyllosilicate | 30 | 150 | |
AR37 | Yellowish chert | Cribrous or locally smooth surface with scantily scattered light spots (without the presence of oxides or Si-Al phases) | X | X | Traces | / | 8 | 20 | ||
RM03.4 | Grey chert | Cribrous, rough appearance resulting from the presence of oxide patinas, with portions of the surface clean and smooth, unaltered quartz | X | X | XX | X | / | 10 | 40 | |
AN1.2 | Blackish chert | Compact appearance but appearing earthy at medium magnifications, covered with microparticles, and scattered with oxides of Fe, Ti and framboids | X | X | X | X | X | Pyrite framboids | 3 | 15 |
AN5.1 | Grey-beige chert | Compact appearance but earthy at medium magnifications, covered with microparticles, scattered with oxides of Fe, Ti and Cr | X | X | X | X | X | Fe-Cr grains and Ni oxides | 2 | 10 |
Sample | Type | Classification | Main Minerals | Minor or Accessory Minerals | Crystallinity | |||||
---|---|---|---|---|---|---|---|---|---|---|
α-Qtz | Cal | Ant | Phyl | Py | Rt | Dol | % | |||
AR10 | Archaeological find (artefact) | Rock crystal | X | 100 | ||||||
AR12.1 | Archaeological find (artefact) | Grey chert | X | X | X | X | 84 | |||
AR18.2 | Archaeological find (artefact) | Grey chert | X | X | X | X | X | 88.5 | ||
AR21 | Archaeological find (artefact) | Grey-ochre chert | X | (X) | 61.6 | |||||
AR29 | Archaeological find (artefact) | Dark quartzite | X | 99 | ||||||
AR34 | Archaeological find (artefact) | Dark quartzite | X | X | (X) | 95 | ||||
AR37 | Archaeological find (artefact) | Yellowish chert | X | 80 | ||||||
RM03.4 | Raw material (chunk) | Grey chert | X | 86 | ||||||
AN1.2 | Geological sample | Blackish chert | X | X | 65.3 | |||||
AN5.1 | Geological sample | Grey-beige chert | X | (X) | X | 84 |
Sample | Origin | Type | ρR | ρB | ΦO He | ΦO H2O | ICW | SI | Is(50) | RC | RT | |
---|---|---|---|---|---|---|---|---|---|---|---|---|
(g/cm3) | (g/cm3) | (%) | (%) | (%) | (%) | (MPa) | (MPa) | (MPa) | ||||
AR21 | Artefact | Grey-ochre chert | Group 1 | 2.56 | 2.41 | 5.9 | 5.3 | 2.2 | 89.8 | 9.8 | 195.2 | 7.8 |
AN1.2 | Geolog. samples from Domeño (Andilla) | Blackish chert | 2.54 | 2.41 | 5.1 | 2.5 | 1.0 | 49.2 | 15.2 | 303.1 | 12.1 | |
AN5.1 | Grey-beige chert | 2.52 | 2.38 | 5.8 | 5.6 | 2.3 | 96.6 | 8.0 | 160.1 | 6.4 | ||
AR12.1 | Artefact | Grey chert | Group 2 | 2.65 | 2.59 | 2.1 | 1.8 | 0.7 | 85.8 | 8.6 | 171.6 | 6.9 |
AR18.2 | Artefact | Grey chert | 2.63 | 2.56 | 2.9 | 2.8 | 1.1 | 97.2 | 11.5 | 230.3 | 9.2 | |
AR37 | Artefact | Yellowish Chert | 2.58 | 2.50 | 3.2 | 3.1 | 1.3 | 96.7 | 7.0 | 140.5 | 5.6 | |
AR10 | Artefact | Rock-crystal | 2.64 | 2.61 | 1.2 | 1.0 | 0.4 | 83.5 | 4.9 | 99.0 | 4.0 | |
AR29 | Artefact | Dark quartzite | 2.65 | 2.61 | 1.8 | 1.7 | 0.6 | 96.8 | 15.3 | 306.9 | 12.3 | |
AR34 | Artefact | Dark quartzite | 2.65 | 2.62 | 1.2 | 1.2 | 0.5 | 97.6 | 8.3 | 165.5 | 6.6 | |
RM03.4 | Raw material (chunk) | Grey chert | 2.65 | 2.58 | 2.7 | 1.4 | 0.6 | 52.7 | 7.5 | 149.6 | 6.0 |
Class | Al | K | Ca | Ti | Fe | Zr | |
---|---|---|---|---|---|---|---|
Raw material chunks | Mean | 0.88 | 0.21 | 0.05 | 0.066 | 0.33 | 59 |
(n = 10) | SD | 0.23 | 0.05 | 0.05 | 0.014 | 0.08 | 22 |
Grey chert | Mean | 1.15 | 0.26 | 0.035 | 0.06 | 0.30 | 55 |
(n = 24) | SD | 0.55 | 0.16 | 0.019 | 0.02 | 0.14 | 30 |
Other cherts | Mean | 0.38 | 0.045 | 0.03 | 0.008 | 0.07 | <LD |
(n = 6) | SD | 0.08 | 0.019 | 0.02 | 0.002 | 0.05 | |
Quartzite | Mean | 1.5 | 0.28 | 0.045 | 0.09 | 0.5 | 185 |
(n = 15) | SD | 0.7 | 0.14 | 0.019 | 0.04 | 0.6 | 115 |
Rock crystal | Mean | <LD | 0.022 | 0.023 | 0.020 | 0.053 | <LD |
(n = 6) | SD | 0.007 | 0.009 | 0.007 | 0.013 | ||
Domeño chert | Mean | 0.30 | 0.07 | 1.9 | 0.016 | 0.16 | 9 |
(n = 11) | SD | 0.05 | 0.02 | 1.1 | 0.004 | 0.02 | 2 |
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Columbu, S.; Fancello, D.; Gallello, G.; Ramacciotti, M.; Diez-Castillo, A. Multi-Analytical Techniques to Define the Mineralogical and Petrophysical Characteristics and Provenance of Siliceous Lithic Findings: The Case Study of La Calvera Rock Shelter (Cantabria, Spain). Minerals 2023, 13, 666. https://doi.org/10.3390/min13050666
Columbu S, Fancello D, Gallello G, Ramacciotti M, Diez-Castillo A. Multi-Analytical Techniques to Define the Mineralogical and Petrophysical Characteristics and Provenance of Siliceous Lithic Findings: The Case Study of La Calvera Rock Shelter (Cantabria, Spain). Minerals. 2023; 13(5):666. https://doi.org/10.3390/min13050666
Chicago/Turabian StyleColumbu, Stefano, Dario Fancello, Gianni Gallello, Mirco Ramacciotti, and Agustin Diez-Castillo. 2023. "Multi-Analytical Techniques to Define the Mineralogical and Petrophysical Characteristics and Provenance of Siliceous Lithic Findings: The Case Study of La Calvera Rock Shelter (Cantabria, Spain)" Minerals 13, no. 5: 666. https://doi.org/10.3390/min13050666