ASTM D2569 Standard Test Method for Distillation of Pitch
7. Sample Preparation
7.1 Hard Pitch - If the pitch can be crushed at room temperature, prepare a working sample of approximately 150 g by crushing, mixing, and quartering a representative portion of the dry sample. Crushing may be done with a small jaw crusher and a mullite mortar and pestle. No particle of the crushed sample shall be larger than 10 mm in any dimension.
7.2 Soft Pitch - Heat a portion of the dry sample to the lowest temperature at which it can be mixed and poured.
7.3 Preservation of Samples - Store samples as large lumps or solidified melts in closed containers. Do not save crushed samples for future testing since changes in composition may occur in pulverized pitch.
8. Preparation of Apparatus
8.1 Assemble the apparatus shown in Fig. 2 as follows:
8.1.1 Place the refractory on the heater with the larger opening facing upwards. Center the asbestos-cement plate with the hole on the refractory and place the distillation shield on the plate.
8.1.2 Insert the thermometer through a new, rolled, tightly fitting cork in the neck of the flask, with the bottom of the cork 24 to 27 mm above the lowest point of the juncture between the side-arm tubulature and the neck of the flask. The top of the thermometer bulb must be level with this point. Align the stem of the thermometer on the axis of the bulb of the flask.
8.1.3 Place the flask within the shield so that it is seated in the hole in the non-asbestos containing cement board, and connect the condenser tube to the side arm of the flask with a tight cork so that the side arm projects 30 to 50 mm beyond the cork. The distance from the neck of the flask to the outlet of the condenser tube shall be not more than 600 nor less than 500 mm. Support the flask and condenser tube so that the latter is aligned with the side arm and the thermometer is vertical. Place the cover on top of the shield around the neck of the flask.
