FIB-SEM Study of Archaeological Human Petrous Bones: 3D Structures and Diagenesis
<p>Plot of the SFs versus the full width at half maximum (FWMH) of the main peak of the mineral infrared spectrum of the inner (triangles) and outer (squares) layers of each of the 9 bones listed in <a href="#minerals-14-00729-t001" class="html-table">Table 1</a>. Dotted lines connect the different layers from the same petrous bone specimen. Samples selected for FIB-SEM imaging are indicated by sample number.</p> "> Figure 2
<p>FIB-SEM image of the outer layer obtained from one surface of the image stack from Sample 10610. (<b>A</b>) A 2D ESB image showing aligned lineations attributed mainly to the less-mineralized collagen fibrils. (<b>B</b>) A 3D image of the Eigenvector projections viewed in the same orientation as the image in (<b>A</b>). (<b>C</b>) A 3D image of the Eigenvector projections viewed top-down, i.e., orthogonal to the other views. The presence of only two colors shows that the collagen fibril bundles are oriented in two different directions within one plane. Vector directions parallel to the X-axis direction are blue, vectors parallel to the Y-axis are red, and vectors parallel to Z-axis are represented in green. Scale bar and grid size = 1 µm.</p> "> Figure 3
<p>A 3D representation of the FIB-SEM analysis using Eigenvectors for the outer layer of sample 10619. (<b>A</b>) A 2D ESB image of one of the surfaces. (<b>B</b>) Eigenvectors in 3D as viewed in the milling plane. <a href="#minerals-14-00729-f002" class="html-fig">Figure 2</a>B shows a 1µm thick layer where the collagen bundle follow the direction of the <span class="html-italic">X</span>-axis (blue), whereas the rest of the bundles follow the direction of the <span class="html-italic">Z</span>-axis (green). (<b>C</b>). A 3D image of the Eigenvector projections viewed top-down i.e. orthogonal to the other views. The color code for the EV directions is shown along each axis. Scale bar and grid size = 1 µm.</p> "> Figure 4
<p>The 2D and 3D images obtained from sample 10610 inner layer. (<b>A</b>) A 2D ESB image from the original milling plane. (<b>B</b>) A 3D image showing the Eigenvector from the same plane as in (<b>A</b>). The color code of the Eigenvectors shows the directions of the vectors which follows the axis colors, namely the x-axis direction is indicated by the blue color, the y-axis is indicated by red, and the z-axis is indicated by green. (<b>C</b>). A 3D image of the Eigenvector projections viewed top-down, i.e., orthogonal to the other views. Note the color mixtures of the EVs and the lack of layer organization. Note the random distribution of the colors across the image. Scale bar = 1 µm.</p> "> Figure 5
<p>The 2D and 3D images of the FIB-SEM analysis using Eigenvectors for sample 10619 inner layer. (<b>A</b>) A 2D image obtained from ESB detector. (<b>B</b>) A 3D image showing the Eigenvectors analysis at the same position as in (<b>A</b>). The color code for the Eigenvectors shows collagen fibril bundle directions as shown in the axis indicator (<span class="html-italic">x</span>-axis blue, <span class="html-italic">y</span>-axis red, and <span class="html-italic">z</span>-axis green). Note that at least 3 different directions can be discerned by eye. Scale bar = 1 µm.</p> ">
Abstract
:1. Introduction
2. Materials and Methods
2.1. Materials
2.2. Methods
2.2.1. Collagen Extraction
2.2.2. Fourier Transform Infrared (FTIR) Spectroscopy
2.2.3. Focused Ion Beam–Scanning Electron Microscopy (FIB-SEM)
2.2.4. Image Processing and Directionality Analysis
2.2.5. Volumes of the Less Mineralized Collagen Fibrils
3. Results
3.1. Determining of the Preservation States
Sample No. | Site | SF | Gelatin | C % | C/N | pMC ± 1σ |
---|---|---|---|---|---|---|
(RTD) | wt.% | |||||
10610* | Birgi | 2.73 | 13.2 | 44.26 | 2.80 | 78.7 ± 0.33 |
11184 | Birgi | 3.42 | 8.7 | 43.58 | 2.74 | 76.0 ± 0.38 |
10611 | Birgi | 2.76 | 6.8 | 43.62 | 2.76 | 72.9 ± 0.24 |
11198 | Birgi | 3.43 | 2.7 | 43.25 | 2.77 | 73.4 ± 0.22 |
11199 | Birgi | 3.30 | 2.4 | 46.73 | 2.78 | 73.0 ± 0.22 |
11183 | Birgi | 3.69 | 1.3 | 43.24 | 2.77 | 77.6 ± 0.41 |
11158 | Selinunte | 3.97 | 10.2 | 43.58 | 2.76 | 88.5 ± 0.34 |
10619* | Selinunte | 4.16 | 6.0 | 43.94 | 2.78 | 75.9 ± 0.33 |
11187 | Lilibeo | 3.48 | 1.9 | 43.3 | 2.78 | 77.0 ± 0.20 |
3.2. Petrous Bone Structure Using FIB-SEM
3.2.1. Outer Petrous Bone Layers
3.2.2. Inner Petrous Bone Layers
4. Discussion
5. Conclusions
Supplementary Materials
Author Contributions
Funding
Data Availability Statement
Acknowledgments
Conflicts of Interest
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Sample | Petrous Layer | Average (vol.%) | Std. Dev. |
---|---|---|---|
10610 | Outer | 1.0 | 0.2 |
Inner | 0.7 | 0.2 | |
10619 | Outer | 7.3 | 3.2 |
Inner | 4.3 | 0.8 |
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Ibrahim, J.; Mintz, E.; Regev, L.; Regev, D.; Gronau, I.; Weiner, S.; Boaretto, E. FIB-SEM Study of Archaeological Human Petrous Bones: 3D Structures and Diagenesis. Minerals 2024, 14, 729. https://doi.org/10.3390/min14070729
Ibrahim J, Mintz E, Regev L, Regev D, Gronau I, Weiner S, Boaretto E. FIB-SEM Study of Archaeological Human Petrous Bones: 3D Structures and Diagenesis. Minerals. 2024; 14(7):729. https://doi.org/10.3390/min14070729
Chicago/Turabian StyleIbrahim, Jamal, Eugenia Mintz, Lior Regev, Dalit Regev, Ilan Gronau, Steve Weiner, and Elisabetta Boaretto. 2024. "FIB-SEM Study of Archaeological Human Petrous Bones: 3D Structures and Diagenesis" Minerals 14, no. 7: 729. https://doi.org/10.3390/min14070729