721 DISTILLING RANGE
To determine the range of temperatures within which an official liquid distills, or the percentage of the material that distills between two specified temperatures, use Method I or Method II as directed in the individual monograph. The lower limit of the range is the temperature indicated by the thermometer when the first drop of condensate leaves the tip of the condenser, and the upper limit is the Dry Point, i.e., the temperature at which the last drop of liquid evaporates from the lowest point in the distillation flask, without regard to any liquid remaining on the side of the flask, or the temperature observed when the proportion specified in the individual monograph has been collected.
NoteCool all liquids that distill below 80 to between 10 and 15 before measuring the sample to be distilled.
Apparatus Use apparatus similar to that specified for Method II, except that the distilling flask is of 50- to 60-mL capacity, and the neck of the flask is 10 to 12 cm long and 14 to 16 mm in internal diameter. The perforation in the upper insulating board, if one is used, should be such that when the flask is set into it, the portion of the flask below the upper surface of the insulating material has a capacity of 3 to 4 mL.
Procedure Proceed as directed for Method II, but place in the flask only 25 mL of the liquid to be tested.
Apparatus Use an apparatus consisting of the following parts:
Distilling Flask 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 to 75 with the lower portion of the neck.
Condenser 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.
Insulating Boards 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 cm and 10 cm, respectively. In use, the boards are placed one upon the other, and rest on a tripod or other suitable support, with the board having the larger hole on top.
Receiver A 100-mL cylinder graduated in 1-mL subdivisions.
Thermometer 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.
Heat Source A small Bunsen burner or an electric heater or mantle capable of adjustment comparable to that possible with a Bunsen burner.
Procedure 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. Unless otherwise specified in the individual monograph, apply when necessary the emergent stem correction and report the temperatures adjusting the barometric pressure by the following formula:
t = t0 + [(t0104 + 0.033)(760 p)]in which t is the corrected boiling temperature, in Celsius scale; t0 is the measured boiling temperature, in Celsius scale; and p is the barometric pressure at the time of measurement, in mm Hg.
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