9.3.1.1
Flask—A 500-ml flask of the shape shown in the figure, made of high resistance glass, well annealed and as free as possible from striae and similar defects.
9.3.1.2
Reflux condenser—Water-cooled, glass reflux condenser, having a jacket approximately 400 mm long and an inner tube of 9.5 to 12.5 mm outside diameter. The tip of the condenser to be inserted in the trap may be ground at an angle of 30° from the vertical axis of the condenser. When inserted into the trap, the tip of the condenser is 6 to 7 mm above the surface of the liquid in the trap after distillation conditions have been established.
9.3.1.3
Receiver (otherwise called the trap)—Receiver of 5 ml capacity made of high resistance glass, well annealed and as free as possible from striae and similar defects, provided with ground-glass joints, with the shape, dimensions and tolerances given in Fig. 1 and consisting essentially of the upper chamber together with the tube and ground joint leading to the flask and the graduated tube. The graduated portion has a capacity of 5 ml when filled to the highest graduation mark. The scale covers the range of 0 to 5 ml and is graduated at intervals of 0.1 ml. The graduation marks corresponding to each millilitre are numbered and carried completely round the tube.
The graduation marks mid-way between the numbered marks are carried three-quarter-way and the remaining marks are carried half-way around the tube. The error at any indicated capacity should not exceed 0.05 ml.
9.3.1.4
Heat source—The source of heat may be either an oil-bath or an electric heater provided with a sliding rheostat or other means of heat control. The temperature of the oil in the bath should not be very much higher than the boiling point of toluene.
9.3.1.5
Copper wire—This should be long enough to extend through out the condenser with one end twised into a spiral. The diameter of the spiral should be such that it fits snugly within the graduated portion of the receiver and yet can be moved up and down.
9.3.1.1
Flask—A 500-ml flask of the shape shown in the figure, made of high resistance glass, well annealed and as free as possible from striae and similar defects.
9.3.1.2
Reflux condenser—Water-cooled, glass reflux condenser, having a jacket approximately 400 mm long and an inner tube of 9.5 to 12.5 mm outside diameter. The tip of the condenser to be inserted in the trap may be ground at an angle of 30° from the vertical axis of the condenser. When inserted into the trap, the tip of the condenser is 6 to 7 mm above the surface of the liquid in the trap after distillation conditions have been established.
9.3.1.3
Receiver (otherwise called the trap)—Receiver of 5 ml capacity made of high resistance glass, well annealed and as free as possible from striae and similar defects, provided with ground-glass joints, with the shape, dimensions and tolerances given in Fig. 1 and consisting essentially of the upper chamber together with the tube and ground joint leading to the flask and the graduated tube. The graduated portion has a capacity of 5 ml when filled to the highest graduation mark. The scale covers the range of 0 to 5 ml and is graduated at intervals of 0.1 ml. The graduation marks corresponding to each millilitre are numbered and carried completely round the tube.
The graduation marks mid-way between the numbered marks are carried three-quarter-way and the remaining marks are carried half-way around the tube. The error at any indicated capacity should not exceed 0.05 ml.
9.3.1.4
Heat source—The source of heat may be either an oil-bath or an electric heater provided with a sliding rheostat or other means of heat control. The temperature of the oil in the bath should not be very much higher than the boiling point of toluene.
9.3.1.5
Copper wire—This should be long enough to extend through out the condenser with one end twised into a spiral. The diameter of the spiral should be such that it fits snugly within the graduated portion of the receiver and yet can be moved up and down.
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