ASTM D850 Standard Test Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials
9. Assembly of Apparatus
9.1 Manual Distillation Apparatus:
9.1.1 Remove any residual liquid in the condenser tube by swabbing with a piece of lint-free cloth attached to a cord or wire.
9.1.2 Assemble the apparatus as shown in Fig. 2. Mount the flask on the insulation board of appropriate dimensions, with the side tube extending through a tightly fitting silicone or cork stopper about 50 mm into the condenser tube.
9.1.3 Support the distillation thermometer in the neck of the flask by means of a cork or silicone stopper with the thermometer vertical and centered in the neck of the flask and in such a position that the top of the bulb (or top of contraction bulb if present) is level with the lowest point of juncture between the side tube and the neck of the flask (see Fig. 3).
9.1.4 Place the burner directly under the center of the hole in the insulation board.
9.2 Automatic Distillation Apparatus - For assembly of automatic distillation apparatus, consult the instrument manufacturer's operating manual.
NOTE 2 - The centering device must be as stated in 6.2.2.1 (Fig. 2).
9.3 Carefully measure a 100-mL specimen of the material to be tested in the 100-mL graduated cylinder at room temperature and transfer to the distillation flask, draining the cylinder at least 15 s. This is preferably done before mounting the flask in position, in order to prevent liquid from entering the side arm. Do not rinse out the graduated cylinder used to measure the sample for distillation, but place under the lower end of the condenser tube to receive the distillate.
9.4 Fit the flask vapor tube, provided with a snug fitting silicone rubber stopper, tightly into the condenser tube. Adjust the flask in a vertical position so that the vapor tube extends into the condenser tube for a distance of 25 to 50 mm (1 to 2 in.). Raise and adjust the flask support board to fit snugly against the bottom of the flask.
9.5 Place the cylinder which was used to measure the charge, without drying, into its position under the lower end of the condenser tube so that the end of the condenser tube is centered in the graduate and extends in for a distance of at least 25 mm (1 in.).