Ultrathin two-dimensional (2D) materials have profound interest from recent years due to its extraordinary physical and chemical properties. Within these different 2D materials, transition metal nitrides/carbides, generally known as MXenes have more preference in accordance to their structure and other properties. An analysis of their properties making them suitable for multifunctional applications is necessary to introduce. Thus, there are various characterization techniques used to distinguish their properties in order to meet these application requirements. Among different characterization techniques used for MXenes, surface characterization techniques have more preference, in order to achieve details on the presence of functional groups, surface active sites, structural tunability, etc. Here in the present chapter, we establish an outline on the basic and major surface characterization techniques used in MXene films and powders.