Air void size and spatial distribution have long been regarded as critical parameters in the frost resistance of concrete. In cement-based materials, entrained air void systems play an important role in performance as related to durability, permeability, and heat transfer. Many efforts have been made to measure air void parameters in a more efficient and reliable manner in the past several decades. Standardized measurement techniques based on optical microscopy and stereology on flat cut and polished surfaces are widely used in research as well as in quality assurance and quality control applications. Other more automated methods using image processing have also been utilized, but still starting from flat cut and polished surfaces. The emergence of X-ray computed tomography (CT) techniques provides the capability of capturing the inner microstructure of materials at the micrometer and nanometer scale. X-ray CTâ s less demanding sample preparation and capability to measure 3D distributions of air voids directly provide ample prospects for its wider use in air void characterization in cement-based materials. However, due to the huge number of air voids that can exist within a limited volume, errors can easily arise in the absence of a formalized data processing procedure. In this study, air void parameters in selected types of cement-based materials (lightweight concrete, structural concrete elements, pavements, and laboratory mortars) have been measured using micro X-ray CT. The focus of this study is to propose a unified procedure for processing the data and to provide solutions to deal with common problems that arise when measuring air void parameters: primarily the reliable segmentation of objects of interest, uncertainty estimation of measured parameters, and the comparison of competing segmentation parameters.Ph.D