Issue 74

N. Meddour et alii, Fracture and Structural Integrity, 74 (2025) 227-261; DOI: 10.3221/IGF-ESIS.74.16

Appendix A2: Test technical specifications. A2-1: X-ray diffraction (XRD) analysis  Tools and software used : For the XRD analysis, the procedure involved the use of the PDF-ICDD database and HighScore Plus software for diffractogram interpretation.  Objective : The XRD analysis was employed to identify the crystalline phases present in the samples. A2-2: Scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy (SEM-EDX) analysis  Tools and software used : For the SEM-EDX analysis, the procedure involved the use of a Zeiss Gemini 300 equipped with an Oxford X-MaxN 80 EDX detector, operating at accelerating voltages of 5–20 kV in variable pressure modes, with working distances of 5–15 mm.  Objective : The SEM-EDX analysis was employed to characterize the surface topography, pore network architecture, and mineralogical constituents of lithic samples at nanoscale resolution ( ≤ 1 nm) with an elemental sensitivity of approximately 0.1 wt%. A2-3: X-Ray fluorescence (XRF) spectrometry analysis  Tools and software used : For the XRF analysis, the procedure involved the use of a SciAps X-200 spectrometer equipped with a high-performance silicon drift detector (SDD) with an active area of 20 mm² and a resolution of <140 eV FWHM at the 5.95 keV Mn K-alpha line, operating with a 40 kV Rh anode (for alloys) or a 50 kV Au anode (for geochemical, soil, RoHS, and other applications), achieving count rates exceeding 125,000 cps with >90% live time.  Objective : The XRF analysis was employed to determine the elemental composition of the samples with high sensitivity. A2-4: Petrographic Analysis  Tools and Software Used : For the petrographic analysis, the procedure involved using polarized light microscopy (Leitz ORTHOPLAN, 40–1000×) to characterize the chemical and mineralogical composition of lithic specimens.  Objective : The petrographic analysis was employed to reveal textural attributes, intragranular microporosity, bonding matrix integrity, and secondary mineralization phases, critical for understanding weathering mechanisms in heritage materials. Tools and software used : For porosity measurement, the procedure involved drying samples at 70 ± 5 °C to constant mass (Md), followed by vacuum saturation at 2.0 ± 0.7 kPa for 2 ± 0.2 hours, and immersion in deionized water at 20 ± 5 °C for 24 ± 2 hours. Hydrostatic (Mh) and saturated (Ms) masses were measured.  Objective : The porosity measurement procedure was employed to determine the porosity of the samples, as presented in Fig. A2-5. A2-5: Porosity measurement 

(a) (f) Figure A2-5: Test procedure: Open porosity and bulk density. (a) drying samples to constant mass,(b) weighing samples (M d), (c) samples in a vacuum vessel and reduction gradually of the pressure,(d) introduction slowly of demineralized water at (20 ± 5) °C until sample immersion ,(e) maintain a pressure of (2.0 ± 0.7) kPa ,(f) weighing the sample underwater (M h) (b) (c) (d) (e)

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