A study was made of t he thermal behavior in a vac uum of polystyrcne, polytetra fluoroethvlcne, poly (a-m et h y 1 s tyrcne), polypropylene, polyisobutylen(', and poly (meth yl methacrylate), when pyrolized at 500, 800, and 1,200 .0C. The v olatile products of degradation were collected and fractionated, and the fractlOns analyzed by mass-spectrometn c and microcryoscopic methods. Generally, the results from 500 °0 pyrolysis resemble those obtained prev ious ly from t he same polymer at lower temperatures. The r es uILs at 800° and 1 :200° indicate a much greater fragmentation of the pyrolys is products than at lower temp~ratures. Thus, for example, at 1,200° polystyrene yields less monomer but co nsidcrable greater amounts of 0 2H2, 0 21 -14, 0 3H" and OsI-Is than at lower te mperatures. Similarly, poly(a-methylstyrcnc) yields 100 percent monomer below 500 °0 , but at 800 and 1,200 °0 t he yields are 88 p ercen t an d 34 percent, res pec t ively. A lso at the higher temperatures, pronounced amounLs of Hz, 0I-I4, OzH 2, 0 21-14, 0 3H" 0 3HS, O,H" 0 6I-I6, O,Hs, and OsT -l s are formed.