Name: Year/Course:

Subject/Section: Instructor:
Date performed:
Experiment no:
Experiment title:

I. Objectives:
1. Purify a sample of crude benzoic acid using recrystallization and sublimation
2. Determine the melting point of the purified benzoic acid crystals and
evaluate its purity based on the melting point’s temperature range
3. Understand the process behind recrystallization, sublimation, and melting
point determination

II. Materials and Apparatus

Reagents:
Crude benzoic acid
Charcoal

Equipment/Apparatus:
250 mL Erlenmeyer flask Oil bath
100 mL graduated cylinder Pasteur pipette
Capillary tubes Stirring rod
Filter papers Vials
Hot plate Watch glass
Ice bath

III. Diagrams/Figures for special set-ups

Figure 1: Filtration of hot solution

Recrystallization of benzoic acid https://blog.gregwilson.co.uk/recrystallization-of-benzoic-acid-lab-
report/?showimg_qne=recrystallization+of+benzoic+acid+lab+report.gif (accessed 19 September 2020)
 Figure 2: Experimental set-up of melting point determination
Boiling point apparatus (adapted from Feiser & Williamson) http://organicchem.org/oc2web/lab/exp/ban/bppro.html (accessed 19 September 2020)

IV. Outline/Schematic Diagram of Procedure

A. Recrystallization

After removing the flask

Prepare 0.25 g of crude Pour 20 mL of distilled Stir the solution while from the hotplate, add a
benzoic acid in a 250 mL water and boil for 1-2 boiling. Do not let the pinch of charcoal to the
Erlenmeyer flask (Flask A) minutes sample dry solution while gently
stirring

Prepare another 250 mL

Let the filtrate come down Using a fluted filter paper, Erlenmeyer flask (Flask B)
Boil the solution once again
to room temperature by filter the hot solution into containing 3 mL of hot
to prepare for the filtration
itself Flask B water. Set Flask B on a hot
plate to maintain its heat

Collect the recrystallized

benzoic acid and wash with Transfer the crystals to a
Cool the filtrate by setting it Place the crystals on a filter
a small amount of cold vial and record its weight
in an ice bath paper for it to dry
water to remove mother and percent recovery
liquor
 B. Sublimation

Place a filter paper covering

Prepare 0.10 g of crude
benzoic acid in a 50 mL
beaker
Dip only about 1/3 of the
the beaker's mouth and Place the water bath on a
beaker in a water bath,
place a rubber band around hot plate and heat for
making sure that the fiter
the beaker to hold the filter about 100℃
paper does not become wet
in place

Continue to heat until

Record its weight and
percent recovery
needle-like crystals
Transfer the sublimate in a Remove the filter paper
accumulate on the filter
vial carefully
paper and the sides of the
beaker

C. Melting point determination

Place the dry benzoic Press firmly the open

acid crystals on a
watch glass and
gently crush them
using a spatula
Fill the capillary tube Insert the
end of the capillary Prepare 25 mL of oil
with the sample until thermometer
tube against the placed inside a 50 mL
it is filled up to 2-4 through a cork to
heap of the beaker
mm height hold it in place
pulverized sample

Using a thin strip of

Record the
Once the sample has
temperature once a
become completely
drop of liquid is
liquid, record the
observed from the
temperature reading
capillary tube
Switch to a low
temperature setting,
allowing the
temperature to rise
about 3℃ per minute
Heat the oil bath to a
rubber tubing, attach
great extent until the
the capillary tube
temperature reaches
with the sample near
10-15℃ below the
the tip of the
known melting point
thermometer

V. Waste Disposal
• The sample of benzoic acid that has not recrystallized should be
recovered and then dried. Formed crystals should be placed in a vial and
surrendered to the instructor
• Dispose the used oil in the proper disposal container labeled “Used Oil”
• Dispose the used capillary tubes in the proper disposal container labeled
“Broken Glassware”

VI. Any interesting things you’ve learned in this pre-lab that you didn’t know
before? Share it with me!

Almost everything in this prelab module is new to me because we didn’t do a lot of

experiments like this during high school. Unfortunately, even in college, I wouldn’t be able to
perform this because of the online class set-up. It’s embarrassing to admit that I wasn’t aware
of recrystallization as a separation method in chemistry. I think I only heard the term once
or twice during a chemistry lecture class back in 2016 but it wasn’t really explained in detail
so I didn’t really know how it worked. I didn’t bother to understand it further because I
thought it was too complicated, so being able to comprehend this pre-lab was a surprise
because the idea of recrystallization was just really easy to understand especially when one
already knows basic chemistry concepts. What’s another interesting thing for me in this
experiment is how we can use filter paper to “trap” the crystals because I’ve never really
thought about using filter paper that way. This might only seem like a small discovery from
a college student but I’m glad knowing and understanding the process behind accumulating
the benzoic acid crystals.