The use of carbons in sample preparation techniques such as solid phase extraction (SPE) and air sampling has been ongoing for several decades. Recent advancements in sample preparation techniques have led to the use of carbons in micro-SPE (i.e., pipette tips packed with particles), solid phase microextraction (SPME) techniques and carbon coatings for both gas and liquid sample preparation techniques. Improvements in carbon purities, particle size distribution, pore structure and surface chemistries have led to the ability to analyze trace levels of the respective analytes. The preparation of spherical, high-purity 2 micron carbon molecular sieves (CMS) with a large microporous regime allowed for the preparation of coated surfaces for environmental applications. The applications focused on a range of analytes from light gases to the semi-volatiles.