Volatile matter (VM) analysis of green petroleum coke is an important measurement for determining the calcination behavior and properties of calcined coke. Green cokes with high VM (>12%) are more difficult to calcine and result in a higher porosity and lower bulk density in calcined coke. This paper will review current methods for measuring the VM of green coke based on the ASTM quartz method, the platinum crucible method, and the macro thermo-gravimetric (TGA) method. Detailed experimental results comparing the quartz crucible and macro TGA methods are presented in the paper. When used in combination with a high speed rotor mill, automated TGA equipment offers significantly improved speed and precision, as well as the capability for simultaneous measurement of ash and moisture contents.