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EXPERIMENT 2-Purification and Melting Point Determination
EXPERIMENT 2-Purification and Melting Point Determination
3. Place the beaker in a sand bath such that about 1/3 of the beaker is immersed.
4. Heat the sand bath in a hot plate. Continue heating until needle-like crystals
deposit on
on the filter paper and at the sides of the beaker.
5. Carefully remove the filter paper and scrape the sublimate into a previously
weighed
vial. Report the weight and the %recovery of pure benzoic acid.
C. Sublimation of Caffeine
1. Weigh all the isolated caffeine left from Expt 1 in a weighing cup and transfer in
an
evaporating dish.
2. Prepare a simple heating set-up with Iron stand, iron ring, Bunsen burner and
wire
gauze and heat the weighed caffeine.
3. Cover the evaporating dish with a watch glass and wait until caffeine sublimes
from the
Evaporating dish into the watch glass.
4. Scrape all the sublimate into a previously weighed weighing cup.
5. Report the weight of the sublimate and the %recovery of pure caffeine.
D. Melting point determination of Benzoic Acid
1. Pulverize a small amount of recovered pure benzoic acid from Part B with the aid
of a
clean watch glass and a stirring rod.
2. Make a heap of the powder. Gently thrust the open end of a capillary tube (a
glass
capillary closed at one end) into this heap. Tap the capillary tube gently to cause
the
sample to collect at the bottom of the capillary tube. Repeat this step until a
sample
1-2 mm high has collected in the bottom of the tube.
3. Assemble the melting point determination set-up as shown in Figure 1.
4. Heat the oil with a moderate Bunsen flame. Allow the temperature to rise fairly
rapidly
to within 15 to 20 degrees below the expected melting point of the sample.
Then adjust
the flame size so that the temperature rises no more than 2-3 degrees per
minute just
before, during and just after the period in which the compound melts.
5. Record the range of temperature from the first visible evidence of liquid (the
sample
appears moist, or a tiny drop of liquid is observed) to the complete liquefaction
of the
sample.