Use an apparatus consisting of the following parts:
A round-bottom distilling flask, of heat-resistant glass, of 200-mL capacity, and having a total length of 17 to 19 cm and an inside neck diameter of 20 to 22 mm. Attached about midway on the neck, approximately 12 cm from the bottom of the flask, is a side-arm 10 to 12 cm long and 5 mm in internal diameter, which forms an angle of 70
with the lower portion of the neck.
A straight glass condenser 55 to 60 cm in length with a water jacket about 40 cm in length, or a condenser of other design having equivalent condensing capacity. The lower end of the condenser may be bent to provide a delivery tube, or it may be connected to a bent adapter that serves as a delivery tube.
Two pieces of insulating board, 5 to 7 mm thick and 14 to 16 cm square, suitable for confining the heat to the lower part of the flask. Each board has a hole in its center, and the two boards differ only with respect to the diameter of the hole, i.e., the diameters are 4 and 10 cm, respectively. In use, the boards are placed one upon the other, and resting on a tripod or other suitable support, with the board having the larger hole on top.
A 100-mL cylinder graduated in 1-mL subdivisions.
In order to avoid the necessity for an emergent stem correction, an accurately standardized, partial-immersion thermometer having the smallest practical subdivisions (not greater than 0.2
) is recommended. Suitable thermometers are available as the ASTM E-1 series 37C through 41C, and 102C through 107C (see Thermometers 21
). When placed in position, the stem is located in the center of the neck and the top of the contraction chamber (or bulb, if 37C or 38C is used) is level with the bottom of the outlet to the side-arm.
A small Bunsen burner or an electric heater or mantle capable of adjustment comparable to that possible with a Bunsen burner.
Assemble the apparatus, and place in the flask 100 mL of the liquid to be tested, taking care not to allow any of the liquid to enter the side-arm. Insert the thermometer, shield the entire burner and flask assembly from external air currents, and apply heat, regulating it so that between 5 and 10 minutes elapse before the first drop of distillate falls from the condenser. Continue the distillation at a rate of 4 to 5 mL of distillate per minute, collecting the distillate in the receiver. Note the temperature when the first drop of distillate falls from the condenser, and again when the last drop of liquid evaporates from the bottom of the flask or when the specified percentage has distilled over. Correct the observed temperature readings for any variation in the observed ambient barometric pressure from the normal (760 mm), adding if the pressure is lower or subtracting if the pressure is higher than 760 mm, and apply the emergent stem correction where necessary. Unless otherwise specified in the individual monograph, allow 0.1
for each 2.7 mm (0.037
per mm) of variation.