Vacuum system, design vibration

Schematic diagrams of the apparatus, designed in our lab at< y, are shown in Fig. 1. Polymer flakes are placed, with a balls of about 5 mm dieter, in a glass an oule A about 4 cm in diameter and 7 cm in length. To the other end of the ampoule an ESR sample tube B is attached. Through connector C, the ampoule can be connected to a vacuum system and then evacuated to 10 mm Hg. After evacuation the connector is sealed off and the ampoule is removed from the vacuum system. The evacuated ampoule is now placed on a vibrator, wWch moves vertically at about 4 cycle per second. The procedure can be carried out in a Dewar flask containing coolant, such as liquid nitrogen, to fix the temperature. After some hours of this vibration, the crushed flakes are transferred to the ESR sample tube without raising the temperature of the sample. Ihen, sample tube containing the fractured flakes is placed in an ESR cavity at controlled temperature. The ball-mill apparatus permitted polymeric materials to be crushed in vacuum at low temperature and the ESR spectrum to be observed without contamination of oxygen.

---