Volatilomics studies the emission of volatile compounds from living organisms like plants, flowers, animals, fruits, and microorganisms, using metabolomics tools to characterize the analytes. This is a complex process that involves several steps like sample preparation, extraction, instrumental analysis, and data processing. In this chapter, we provide balanced coverage of the different theoretical and practical aspects of the study of the volatilome. Static and dynamic headspace techniques for volatile capture will be discussed. Then, the main techniques for volatilome profiling, separation, and detection will be addressed, emphasizing gas chromatographic separation, mass spectrometry detection, and non-separative techniques using mass spectrometry. Finally, the whole volatilome data pre-processing and multivariate statistics for data interpretation will be introduced. We hope that this chapter can provide the reader with an overview of the research process in the study of volatile organic compounds (VOCs) and serve as a guide in the development of future volatilomics studies.