Chem Lab 7 Procedure

Melting Point Determination

1. Prepare a capillary tube 1 mm in diameter and about 6 cm in length. Seal one

end by melting in an open flame.
2. Ensure that your sample, the mortar and pestle, and your capillary tube, are
dry. Pulverize a pinch of your sample using a mortar and pestle.
3. Introduce the powdered sample into the capillary tube by pushing the open
end of the capillary tube into the powder and tapping the closed end on the
tabletop. The powder should occupy a height of about 1 cm in the capillary.
4. Use a rubber band to attach the capillary tube to the bulb-end of a
thermometer as illustrated in the figure below.
5. Dip the setup in the oil bath.
6. Slowly heat the oil bath, gently stirring and observing the thermometer and
capillary tube.
7. Record the temperatures when the sample starts to liquefy (T​m,1​) and when
all remaining solids disappear (T​m,2​).
8. Report the melting point value as a range.

OPTIONAL

● Vegetable oils typically boil or decompose at 200​o​C. Likewise, lab

thermometers are limited to only a maximum of 100​o​C (Alcohol
thermometers) or 200o​ ​C (Mercury thermometers). ​For samples which melt
beyond this range, you may use a ​melting point apparatus​ which makes
use of a digital thermometer.

Boiling Point Determination

1. Prepare a capillary tube 1 mm in diameter and about 6 cm in length. Seal one

end by melting in an open flame.
2. Use a rubber band to attach a 5-mL test tube to the bulb-end of a
thermometer.
3. Add about 10 drops of liquid sample into the test tube.
4. Insert the capillary tube into the test tube containing the sample with the
capillary's open end immersed in the liquid sample.
5. Dip the setup in the oil bath.
6. Slowly heat the oil bath, gently stirring and observing the setup. Random
intermittent bursts of bubbles will be observed as you approach the boiling
point.
7. Record the temperature when you observe a rapid and continuous stream of
bubbles (T​b,1​). Turn off the heating. Record the temperature at the moment
the liquid sample enters the capillary tube (T​b,2​).
8. Report the boiling point value as a range.