Procedure: Observations:

1. Obtain unkown macro-scale

compound, record letter designation.
2. Weigh out approximately 1.00 g. Make
note of appearance, color, and solid
crystalline or amorphous.
3. Use (melting point apparatus) to obrain
crude melting point range. Report this
range (to 0.1 degree). Make note if it
all melted, sharp or broad range, clean
phase transition or discolored
(decomposition).
4. Check list of possible unknowns to
narrow down the possibilities and
determine suggested solvent.
5. Dissolve a small amount of compound
by adding a small amount of suggested
solvent (heat the solvent).
6. Begin recrystallization:
a. 1solvent system, slowly cool
b. 2 solvent system, room-temp to
cold solvent slowly added to
hot solvent, when swirled it
should remain cloudy when
fully recrystallized.
7. If solution is discolored, add a little
charcoal to decolorize.
8. If there are solids in the solution that
will not dissolve, then begin hot gravity
filtration. Use stem-less funnel and
filter paper.
9. Recrystallize via vacuum filtration:
Make note of solvent or solvent combo,
heating or icing, scratching of glass wall,
time for crystals to appear. Compare
the appearance to the initial sample.
10. Isolate purified product. Sketch
(picture) of vacuum filtration. Record
the solvent used to wash crystals, was it
hot/cold. Describe filtrate and
appearance of final product.
11. Calculate and report percent recovery.
12. Record melting point of final product.
13. Repeat steps 1-12 with about 100 mg of
micro-scale unknown.