Recrystallization Page 3

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completely dissolves at elevated temperature, record that it is soluble in the hot solvent.
If some but not all dissolves, record that it is slightly soluble, and continue to add drops
of solvent until dissolution is complete. Once the substance has been dissolved in hot
solvent, allow the solution to cool to room temperature, then stick the test tube in ice. If
necessary, induce crystallization by rubbing the walls of the tube with a stirring rod.
Describe the nature of the crystals that form (for example, needles, plates or blocks). If
the solid remains undissolved even at elevated temperature, simply record it to be
insoluble in both the hot and cold solvent.
If the solid dissolves in methanol, ethanol, acetone or acetic acid at room
temperature, add a few drops of water to the solution to see if the solid precipitates. If it
does, heat the mixture in the water bath and observe if the solid re-dissolves. Adjust the
composition by adding drops of solvent and/or water as necessary until the solid has just
dissolved and the solution is saturated at the boiling point. Allow the solution to cool to
room temperature, then stick the test tube in ice. Describe the shape of the crystals which
form. Do not add water to either toluene or ligroin since it is not miscible with these
solvents.
Pour the mixtures contained in your test tubes into the Laboratory Byproducts
jar.
Notes:
• Acetic acid will freeze when placed in ice. Do not interpret frozen acetic acid
as crystal formation.
• Ligroin will evaporate quickly when placed in boiling water. Cool down your
water bath (by adding ice) before heating a test tube that contains ligroin.
Prepare a table in your notebook before coming to lab in which you will record
your observations. You will need to record the solubility at room temperature, the
solubility at elevated temperature, the result of adding water to a solution of the
compound (when applicable) and the appearance of the crystals.
In order to write a complete discussion for
Assignment
1, you will need to use the
Spartan software that can be found on the computers located in the lab. Bring the
Molecular Modeling
PDF document to lab with you, both for this experiment and for
Experiment 2. Find time during these two lab periods to build the molecules used in
Experiment 1, Part 2. Solubility Tests. Your TA will assist you, and you may work on it
with other students.

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