A reappraisal of the ink-bottle effect and pore structure of cementitious materials using intrusion-extrusion cyclic mercury porosimetry

Reliable characterization of the pore structure is essentially important for transport-related durability studies of cementitious materials. Mercury intrusion porosimetry has been commonly used for pore structure measurement while the ink-bottle effect significantly affects the trustworthiness of pore size features of cementitious materials. Pressurization-depressurization cycling mercury intrusion porosimetry (PDC-MIP) is an alternative approach previously reported with the purpose to provide better estimates of pore size results. It is found however that the PDC-MIP greatly overestimates the ink-bottle pore volume owing to the incomplete extrusion of mercury in throat pores after the pressurization-depressurization cycle. Intrusion-extrusion cyclic mercury porosimetry (IEC-MIP), as a further improvement, is then described, which can reliably capture the ink-bottle effect and obtain a clear picture of the distribution of the ink-bottle pores in cementitious materials. The ink-bottle effect of cement pastes is observed being pore size-dependent and the role of critical pores is emphasized. Water-cement ratio primarily changes the effective porosity while plays a minor role in the ink-bottle porosity. The addition of reactive blends substantially enhances the ink-bottle effect during mercury penetration into small pores. IEC-MIP tests, together with a unique data analysis, enable to obtain a more truthful pore size distribution.

Automated summary

Reliable characterization of the pore structure in cementitious materials is crucial for durability studies. Commonly used mercury intrusion porosimetry is affected by the ink-bottle effect, which affects the accuracy of pore size measurement. Two alternative methods, pressurization-depressurization cycling and intrusion-extrusion cyclic mercury porosimetry, have been developed to improve pore size estimation in cementitious materials.