Milk is a highly nutritious food. However, it is susceptible to microbial growth and degradation due to its high moisture content (86–88%) and water activity (aw ~ 0.995). Therefore, milk products are dried for long-term storage. Conversion of powder also helps in lowering of transportation costs. Milk powders are great source of proteins, fat, minerals, lactose, and sometimes fortified vitamins. Thus, proper quantification and analysis of milk powders is necessary for meeting the standards laid down by the regulatory agencies like Food and Drug Administration (FDA) and Codex Alimentarius Commission (CAC) to name a few. Organizations like International Organization for Standardization (ISO), International Dairy Federation, etc., have introduced several analytical methods for determination of proximate composition and physicochemical characteristics for analysis of milk powders. This chapter aims to bring together all the analytical procedures for determination of composition and physicochemical characteristics of several powdered dairy products