Separating Immiscible through the process of Steam Distillation

Abstract: Used the process of Steam distillation to practice and observe the technique of
distilling insoluble liquids in relation to vapor pressure and boiling points.

Introduction: Steam distillation is a certain type of distillation and which is certain liquid is
passed through a boiling flask that have immiscible properties. Immiscible means that the liquid
separate and do not dissolve within each other. Substances that are distilled in steam
distillation are sometimes temperature sensitive and the process offers away for substances to
be purified with out contamination. Steam distillation also has the advantage of selectivity as it
allows for immiscible substances to be precisely distilled or separated. Immiscible substances
are not dissolvable to each other and therefore are not diluted into each other. This explains
why the vapor pressure exerted by the substances remain the same as the temperature below
the range of the two original boiling points. When the exerted pressure equals the external
pressure substance begin to boil. Steam distillation results in a more accurate separation and
purer liquid.

Materials
250 mL 3 opening round bottom flask
6 mm glass tubing
Trap
5 mm rubber tubing
Clamp
125-Erlenmeyer flask
200 mL flask
Hearing mantle
Bent adapter
Magnetic stirrer
Stopper
Thermometer adapter
Seperatory funnel
Distillation adapter
Condenser
Vacuum adapter
Graduated cylinder

Procedure

Citral, a fragrant terpene aldehyde made up of two isoprene units, is the main component of the steam-
volatile fraction of lemongrass oil and is used in a commercial synthesis of vitamin A.
1. anAlternative Steam Distillation Setup: If a steam line is not available, the steam distillation
setup use a different one.

2. A 250-mL 3 opening boiling flask containing the mixture to be distilled is equipped with a boiling
chip and heat on a heating mantle.

3. Equip the boiling flask with a distillation adapter to which is attached a thermometer adapter
and a separatory funnel, which serves to add water to the boiling flask during the distillation.

4. A condenser is attached to the thermometer adapter and is equipped with a vacuum adapter,
which is attached to the receiving flask.

5. The receiving flask can be cooled by placing it in an ice-water bath. Make sure you securely
clamp the distillation flask and condenser.

6. Make sure to use a rubber band or a Keck clip to hold the vacuum adapter on the end of the
condenser.

7. Steam Distillation: Using a graduated cylinder, measure out 5 mL of lemongrass oil (not lemon
oil) into a 250-mL 3 opening boiling flask.

8. Rinse the remaining contents of the graduated cylinder into the flask with a small amount of t-
butyl methyl ether.

9. Add 50 mL of water, make the connections as in Figure 6.4, heat the flask under a sand bath that
is on top of a clamped ring stand, and pass in the steam.

10. To start the steam distillation, heat the flask containing the mixture on Sandbath to prevent
water from condensing in the flask to the point where water and product splash over into the
receiver.

11. Then turn on the steam valve, being sure that the screw clamp on the bottom of the trap is
open.

12. Slowly close the clamp and allow steam to pass into the flask. Try to adjust the rate of steam
addition and the rate of heating so that the water level in the flask remains constant

13. Because, Unlike ordinary distillations, steam distillations are usually run as fast as possible, with
proper care to avoid splashing of material into the receiver and the escape of uncondensed
steam.

14. Distill as rapidly as the cooling facilities allow and continue until droplets of oil no longer appear
at the tip of the condenser (about 250 mL of distillate).

Observation: When temperature reached 100 C, the distillation still continued and the
temperature no longer increased
 15. Extraction: Pour 50 mL of t-butyl methyl ether into a 125-mL seperatory funnel, cool the
distillate if necessary, and pour a part of it into the funnel.

16. Shake gently back and forth, let the layers separate, discard the lower layer, add another
portion of distillate, and repeat.

17. When the last portion of distillate has been added, rinse the flask with a small amount of t-butyl
methyl ether to recover adhering citral. Use the techniques described in Chapter 7 for drying,
filtering, and evaporating the t-butyl methyl ether.

18. Take the tare of a 1-g tincture bottle, transfer the citral to it with a Pasteur pipette, and
determine the weight and the yield from the lemongrass oil.

19. Label the bottle and store (in the dark) for later testing for the presence of double bonds
(alkenes) and the aldehyde group (see Chapters 18 and 36).

Cleaning Up. The aqueous layer can be flushed down the drain. Any t-butyl methyl ether goes in the
organic solvents waste container. Allow t-butyl methyl ether to evaporate from the calcium chloride
pellets in the hood and then place the calcium chloride in the nonhazardous solid waste container.
However, be aware of the regulations in your area, as they may not allow evaporation of small amounts
of organic solvents in a hood. If this is the case, special containers should be available for the disposal of
these wet solids.

Conclusion: The experiment really exemplified how immiscible mixtures could be seperatory
and what happens to the molecule through macroscale experiment. When the mixture began to
distill it was observed that the resulting product showed how the water molecules carried the
lemongrass oil along with it. The experiment was successful in that it the separation of the water
and the lemongrass oil was accomplish. The challenges in this experiment were marking sure
there were no leaks in the apparatus system and removing the water from the resulting material
in the funnel. These challenges may have lead to a lesser amount of recovered material.