Rigour over R²: Defensible Practice in BET Surface Area and Adsorption Kinetic Analysis
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Abstrak
This comprehensive review synthesizes the theoretical foundations, core physical assumptions, and standardized experimental protocols required for defensible Brunauer–Emmett–Teller (BET) surface area determination and adsorption kinetic analysis. The work addresses critical methodological gaps in porous materials characterization, focusing on recurring pitfalls such as conflating mathematical goodness-of-fit (R²) with true physical mechanism and applying fixed relative-pressure windows or linearized regressions without regard to data error structure. A systematic review and critical evaluation framework was employed, compiling authoritative guidelines, IUPAC technical recommendations, ISO 9277:2022 standards, and interlaboratory consensus studies published between 2015 and 2026. The evaluation reveals that unstandardized sample degassing protocols and arbitrary pressure-interval selections can induce discrepancies exceeding 30% in reported BET surface areas. Furthermore, algebraic linearization of non-linear kinetic frameworks (pseudo-first-order, pseudo-second-order, Elovich, and Weber–Morris intraparticle diffusion) severely distorts error distributions, resulting in biased rate constants and flawed mechanistic interpretations. To establish rigorous characterization standards, BET analysis must objectively implement Rouquerol consistency criteria, select appropriate probe gases (e.g., argon at 87 K for micropores or krypton for low-area solids), and incorporate complementary porosity techniques such as t-plot or NLDFT kernels. For kinetic modeling, non-linear regression must be prioritized alongside multi-metric statistical evaluations (such as chi-squared and residual sum of squares) corroborated by independent spectroscopic or structural evidence. The study concludes that strict adherence to standardized reporting guidelines, complete metadata disclosure, and FAIR data principles using Adsorption Information File (AIF) repositories are essential for ensuring international comparability and academic integrity, particularly when evaluating locally sourced bio-derived adsorbents and novel functional porous materials for environmental and energy applications.
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