CHE 216 : LAB 1A NOTES (Week 1)

A. Background: Microscale Synthesis

1. Reaction: Chemical Hazards. These are summarized the lab
writeup. To minimize spillage and contact with concentrated nitric acid,
it will be dispensed using a 1-mL syringe. This will be performed by the
instructor.
2. Microscale Recrystallization (pp. 231-232, Mohrig)
a. Used for < 300 mg solid.
b. general procedure and apparatus
Place sample in reaction tube and add appropriate amount of
solvent (RT); heat tube in boiling water bath until solid completely
dissolves. Stir with glass rod.
Cool slowly to RT (~ 5 minutes).
Chill in ice-water bath (~ 5 minutes).
Quantitatively transfer to suction apparatus (using cold solvent)
and aspirate for ~ 5 minutes; use of plastic Hirsch funnel (w/ frit)
and 25-mL filter flask (Fig 15.5b). Important: Use of vacuum trap
to prevent water / organic vapors from entering vacuum line (Fig
15.4).
Air-dry in small vial covered with thin tissue (to reduce loss from
sublimation). Secure tissue with rubber band.
B. Procedure: Tips / Modifications
The glass reaction tube must be washed and placed back in the
fume hood at the end of todays experiment.

 Use a 100-mL beaker for the hot water bath. Fill ~half with water.
Set the hotplate to 300 to heat the water to boiling faster. To
prevent violent boiling, place a wood boiling stick inside beaker.
Use glass stirring rod when stirring the cooling reaction mixture.
When weighing a solid, crease the weighing paper beforehand.
This will make it easier to transfer the solid to the receiving vessel
and minimize spillage. It will also help minimize spillage and
contamination of the electric balance.
For the initial recrystallization step, add RT ethanol (1-2 mL) to the
crude solid and heat in a hot water bath (set at 160) until the solid
has completely dissolved before adding distilled water to render
cloudiness.
Chill the mixture in the ice-water bath (1/2 crushed ice + water)
for 5 minutes.
Secure the piece of paper towel around the vial using a small
rubber band.
Cleanup / Waste Disposal
Go over your fume hood floor with a damp pare towel before use.
Do likewise after you are through for the day. Paper towels
disposed in chemical paper waste receptacles.
Excess ethanol measured, record on waste slip and disposed in
hazardous waste container inside rear fume hood.
Pasteur pipettes disposed in waste glass receptacle.
Total neutralized recrystallization filtrate and aqueous rinse
volumes recorded on waste slip and disposed down sink.

Lab Notebook

Procedure outline (numbered or bulleted)

Pre-lab notes
Data: mass of benzoin, empty vial
Calculation: theoretical yield of benzil