Biphasic calcium phosphate (BCP)scaffolds comprising hydroxyapatite (HA) and β-tricalcium phosphate (β-TCP) were produced from ultra-pure precursors and processed under an α-TCP–avoiding schedule (1100 °C, 2 h). Quantitative X-ray diffraction (Rietveld/Profex) detected no α-TCP above the ~1 wt% limit of detection and quantified post-sintering phase fractions (wt% HA/β-TCP): 99.26/0.74, 68.51/31.49, and 27.57/72.43. Across compositions, SEM/ImageJ yielded similar mean macropore sizes (≈71–80 µm), while open porosity increased with the HA fraction (27.5 ± 1.8%, 39.1 ± 2.0%, 57.1 ± 2.4%). Compressive strength decreased accordingly (1.07 ± 0.25, 0.24 ± 0.01, 0.05 ± 0.02 MPa), consistent with non-load-bearing use. In ISO-compliant simulated body fluid (28 d), medium pH remained stable (7.33–7.43); mass loss and early Ca²⁺ depletion increased with β-TCP content, consistent with more extensive surface apatite formation in β-TCP-rich scaffolds. Collectively, these data are consistent with a composition-dependent sequence—β-TCP content → densification/porosity → strength → degradation/apatite kinetics—within the tested conditions and inform parameter-based tuning of BCP scaffolds for non-load-bearing indications (e.g., alveolar ridge preservation, craniofacial void filling).