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EXPERIMENT 2: Recrystallization and Melting Point
EXPERIMENT 2: Recrystallization and Melting Point
Recrystallization (or Crystallization) is a technique used to purify solids. This procedure relies on the
fact that solubility increases as temperature increases (you can dissolve more sugar in hot water than in cold
water). As a hot, saturated solution cools, it becomes supersaturated and the solute precipitates (crystallizes)
out. In a recrystallization procedure, an impure (crude) solid is dissolved in a hot solvent. As this solution
is cooled, the pure product crystallizes out and the impurities stay dissolved.
7) Analyze product
• let crystals dry thoroughly (ideally, this means overnight at room temperature or under vacuum)
• record mass (how much of your original solid did you recover? % recovery?)
• record melting point range (did you succeed in PURIFYING your solid?)
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EXPERIMENT 2: Recrystallization and Melting Point
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EXPERIMENT 2: Recrystallization and Melting Point
Recrystallization: Using a hot plate, dissolve approximately 1.0 g of impure benzoic acid in 30 – 35 mL of
hot water (water at or near its b.p.) in a 125 mL Erlenmeyer flask. If there is a residual amount of material
that does not dissolve upon adding a small amount of additional solvent (H2O), do not continue to add more
solvent; it is important to use a MINIMUM amount of solvent in a recrystallization. This material is
probably insoluble in the hot solvent and will be separated from the hot solution by gravity filtration. If
there is any such insoluble solid residue, gravity filter this hot solution through a fluted filter paper using the
apparatus shown in your laboratory textbook. Since the glass funnel you have used is much cooler than the
hot solution, cooling of the solution will occur, resulting in some crystallization of the benzoic acid in the
stem of the funnel and in the filter paper. Preheating the funnel by running a SMALL AMOUNT of hot
solvent (H2O) through the funnel will reduce the loss due to this crystallization. To further reduce the
amount of loss of material, do not fill the funnel with solution but rather add small portions of the hot
solution so a minimum amount of solution is in the funnel at once.
Allow the gravity-filtered hot solution to gradually cool to room temperature. As this occurs, much of the
benzoic acid will crystallize from the solvent. When the cooled solution is at or near room temperature,
cool it further in an ice-water bath. Collect the resulting crystals by vacuum filtration, using a water
aspirator and the apparatus shown in your laboratory textbook. Transfer the crystals from the filter paper to
a tared watch glass (note weight on Data sheet) and let dry thoroughly before weighing. Never weigh filter
paper along with the crystals; the filter paper will be wet. Determine the amount of benzoic acid recovered
and, based upon the initial amount you started with, determine the percent recovery.
Melting Point: Determine the melting point ranges of the impure benzoic acid and the crystallized benzoic
acid (after it is dry). Be sure to grind each sample well before introducing it into the melting point tube (you
may use a glass rod and a watch glass). Scoop a small amount of the powder into the opening of the melting
point tube and gently tap the tube on the benchtop to move the sample down to the bottom (dropping the
melting point tube through a long glass tube can also help you pack the sample). If you do not have at least
1 mm of sample, scoop another small portion and repeat. If the column of sample is over 3 mm, discard the
melting point tube and start again. Insert the packed melting point tubes into a melting point apparatus.
SLOWLY heat the sample (~ 1 ˚C per minute) and record the temperature at the very first sign of melting.
Continue to watch the sample and when the sample has melted completely, record the temperature again.
EVERY MELTING POINT IS REPORTED AS A RANGE.
Waste disposal: Please discard your purified benzoic acid into the container in the hood labeled: Benzoic
Acid - Student Prep. Melting point tubes should be placed in the glass waste container.
Your complete report for this experiment should include the data page, answers to the following
questions, and a conclusion (1 page maximum. Discuss your results – yield and mp. Consider: Did
the recrystallization work? How can you tell? How could you have improved your yield?). These
pages must be stapled.
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EXPERIMENT 2: Recrystallization and Melting Point
Instructor:
impure
pure
literature value
(cite source)
Your complete report for this experiment should include the data page, answers to the following
questions, and a conclusion (1 page maximum. Discuss your results – yield and mp. Consider: Did
the recrystallization work? How can you tell? How could you have improved your yield?). These
pages must be stapled.
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EXPERIMENT 2: Recrystallization and Melting Point
Questions
Attach answers to these questions on a separate sheet along with Experiment 2 Report.
1. What are the important solubility characteristics for a solvent for crystallization of an organic solid
which is contaminated with a small amount of impurity? Remember you want to separate the desired
solid from the contaminating impurities.
2. There are many opportunities during a recrystallization to lose crystals. How could you improve your
percent recovery? Explain.
5 Why do you need to heat the sample SLOWLY to record its melting point? Give at least two reasons.
6. How can a sample’s melting point indicate the presence of an organic impurity?
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