The remarkable electrical, thermal, mechanical, and optical properties of graphene and its derivative grapheme oxide have recently gained great importance, along with the large surface area and single-atoms thickness. In this respect, several techniques of synthesis such as chemical exfoliation, mechanical exfoliation, or chemical synthesis have been discovered. However, the development of graphene with fewer defects and on a large scale poses major challenges; therefore, it is increasingly necessary to produce it in large proportions with high quality. This paper reviews the top-down synthesis approach of graphene and its well-known derivative graphene oxide. Furthermore, characterization of graphene oxide nanomaterial is a critical component of the analysis. The characterization techniques employed to determine the quality, defects intensity, number of layers, and structures for graphene oxide nanomaterial at the atomic scale. This article focuses on the different involved characterization methodology for graphene oxide with their percentage utilization for the past 11 years. Additionally, reviewing all of the characterization literature for the last 11 years would be a difficult task. Therefore, the aim is to outline the existing state of graphene oxide by different characterization techniques and provide a comparative analysis based on their percentage utilization.