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Fractionating Still: Hempel Bead Column on a Round Flask with Liebig Condenser (Gattermann, 1901)
The classic laboratory set-up for splitting a mixture of liquids by boiling point. A round flask is topped by a Hempel column, a tube packed with glass beads, with a side outlet near the top and a thermometer in a cork above it. The higher-boiling vapour condenses on the beads and runs back, so the vapour reaching the outlet is richer in the lower-boiling part; a Liebig condenser turns it to liquid in the receiver. One pass through it separates better than repeated distillations from a plain flask.
Result: a fractionating still for laboratory distillations at atmospheric pressure.
Source: L. Gattermann, The Practical Methods of Organic Chemistry (2nd American ed., 1901), pp. 16-24. Unknown: column and bead sizes. Picture: the book's Figs. 14-15.
Katamtaman
Unknown
Mga Tagubilin
1
1
Make the Hempel column
Make the Hempel column
Take a wide glass tube with a side outlet tube near its top and fill it with glass beads; the beads act like sieves, holding back the higher-boiling part. Fit it to a round, short-necked flask with a bored cork (or have it fused onto the bulb); flasks with the same neck width can share one cork. Choose a flask the charge will fill about two-thirds. Not given: sizes. Ours: a glass tube for the column body.
Mga materyales para sa hakbang na ito:
Tubong salamin1 column
Mga kuwintas na salamin1 packing
Prasko na bilog ang ilalim1 piraso
Mga tapon na kortsa2 pirasoMga kailangang kasangkapan:
Pambutas ng kortsa2
2
Set the thermometer and condenser
Set the thermometer and condenser
Pass the thermometer through a cork (not rubber) in the top of the column so its bulb sits level with the outlet, never down in the liquid. For liquids boiling up to 100° join the outlet to a Liebig condenser with a cork (long for very low boilers, short for high); from 100-200° cool the receiver with running water; above that a wide glass tube 50 cm long on the outlet is enough. If the vapour attacks cork, push the outlet far into the condenser instead. Clamp the apparatus above the outlet, never below it, or the hot glass may crack.
Mga materyales para sa hakbang na ito:
Termometrong Panlaboratoryo1 piraso
Kondenser na pinalalamig ng tubig1 piraso
Prasko ng Erlenmeyer2 receiversMga kailangang kasangkapan:
Tuntungang may baras (pang-laboratoryo)Pambutas ng kortsa3
3
Fractionate
Fractionate
Add a few bits of glass or platinum wire against bumping. Heat on the water-bath for liquids boiling up to about 80°, otherwise over a small free flame moved slowly to and fro under the flask, never above the liquid level, so the distillate falls into the receiver steadily in drops. With the Hempel column stop heating now and then so the liquid held in the beads can run back. Collect the first runnings, the main fraction at a steady temperature, and the last runnings in separate receivers; for a mixture, collect fractions over set ranges and distil them again.
Mga kailangang kasangkapan:
Bunsen burnerTuntungang may baras (pang-laboratoryo)Mga Materyales
7- 1 columnPlaceholder
- 1 packingPlaceholder
- 1 pirasoPlaceholder
- 2 pirasoPlaceholder
- 1 pirasoPlaceholder
- Placeholder
- 2 receiversPlaceholder
Mga Kinakailangang Kasangkapan
3- Placeholder
- Placeholder
- Placeholder
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