Nitrogen reduction reaction (NRR) and nitrate reduction reaction (NO3−RR) provide a potential sustainable route by which to produce ammonia, a next-generation energy carrier. Many studies have been conducted over the years, mainly emphasizing material design and strategies to improve catalytic performance. Despite significant achievements in material design and corresponding fundamental knowledge, the produced ammonia is still very limited, which makes it prone to bias. The presence of interferants (e.g., cations and sacrificial reagents), the pH of the solution, and improper analytical procedure can lead to the over or underestimation of ammonia quantification. Therefore, the selection of the appropriate ammonia quantification method, which meets the sample solution condition, along with the proper analytical procedures, is of great importance. In this review, the state-of-the-art ammonia quantification method is summarized, emphasizing the advantages, limitations, and practicality for NRR and NO3−RR studies. Fundamental knowledge of the quantification method is introduced. Perspective on the considerations for selecting the suitable quantification method and for performing the quantification process is also provided. Although non exhaustive, this focused review can be useful as a guide to design the experimental setup and procedure for more reliable ammonia quantification results.