Experiment #4

Sublimation
Purification Technique (For Solids)
- Purify from non-volatile impurities

- When other purification techniques are not feasible

How does Sublimation happen?
- Some solid substances have significant vapor pressure at
temperatures < M.P.( non polar and highly symmetrical structures)

1. non-polar substances
Lower dipole moment  lower attraction between molecules 
easier for surface molecules to escape from neighbors

2. Highly symmetrical molecules  higher M.P.  many surface

molecules can attain sufficient energy to vaporize before M.P.
temperature is reached

naphthalene
Examples
- Iodine chamber
Visualization of colorless compounds in TLC (thin layer chromatography)
- Solid air fresheners
- Dry ice to transport frozen goods
- “Freeze-Drying”: Lyophilization
sublimation of water under mild conditions (under reduced pressure)
useful for biological samples, instant coffee, etc.
What to perform in the lab:
Experiment:

- Place 50 mg of the “unknown” in the filter flask

- Finely powdered and spread out evenly on the bottom of the flask

- Position the tip of the tube ~38 mm above the bottom of the flask
The tip should not touch the sample being sublimed!
Experiment Cont…

- Add ice/water to the tube after setting up the apparatus. Why????

- Heat carefully until sublimation starts
Maintain temperature until sublimation is complete
- Sublimate may be seen on the cooler upper parts of the flask
A loose cone of Al foil can be used to direct heat toward this region
.
- Cool, then
- remove ice-water with a pipette (don’t dismantle the apparatus yet)
- add tap water with a pipette. Why????
- Remove tube with and scrape the sublimate.
- Weigh the product and determine % recovery
Pre-Lab Questions:

Q.1. From your experience and knowledge of the process of sublimation, cite some
examples of substances that sublime.
Q.2. How might freeze- dried food be prepared?

Post-Lab Questions:
Q.1. Why does the centrifuge tube need to be filled with ice when
performing a sublimation?