Several recent review articles have been concerned with the topic of polymers at interfaces from the theoretical standpoint. This reflects the extensive effort made in this area over the last 10 – 15 years. However, new experimental techniques for studying polymers at interfaces have also begun to appear in recent years; so have better defined model systems. This article is therefore directed more to a survey of these experimental aspects of the subject. However, a short review of the current state of the theory is given first as background and to define concepts. In the following chapter, details of the modern experimental methods are given. The last chapter comprises an extensive comparative review of results obtained using these techniques with model systems, covering homopolymers, copolymers and polyelectrolytes.