This article is concerned with the determination of what transition elements are present in a sample and their concentration. After considering the general nature of the problems confronting the analyst, a historical overview is given describing the development of the analytical chemistry of the transition elements from biblical times through to the nascent technologies of the eighteenth and nineteenth centuries. After a brief consideration of the treatment required by materials to get them in a form suitable for analysis, for example, sampling and digestion, the classical methods of gravimetry and titrimetry are discussed, with special emphasis on the use of organic reagents and on complexometric determinations using ethylenediaminetetraacetic acid (EDTA). The role of organic reagents is also seen to be important in spectrophotometric analysis or absorptiometry. Consideration is next given to the various modern instrumental techniques available for analysis of the transition elements, starting with various forms of atomic emission spectroscopy but giving emphasis to the inductively coupled plasma (ICP) sources. The widely used technique of atomic absorption spectroscopy (AAS) is next described, along with its many applications for the determination of transition elements in many diverse materials, from body fluids to engine oils. The modern day importance of X-ray fluorescence (XRF) is highlighted in a discussion of X-ray methods, while the technique of neutron activation analysis dominates the section on activation methods, this approach being of particular importance where a nondestructive analysis is essential, for example, of a museum artifact. Finally, brief consideration is given to the importance of the platinum group metals (PGMs) and the special analytical problems that they present.