CHEM 203 LAB RECORD #5

Instructor’s initials before ___________after____________

Name: Charles Okorom Date: 10 - 15- 2007

Phase- I

Title: Steam Distillation

Purpose of Experiment
This experiment is to separate a mixture of two miscible liquids (liquids that mix in all
proportions) with different boiling points.

Pertinent Equations:
pt = pA + pB (immiscible liquid)
Tp = NAPA + NBPB (miscible)
Apparatus setup for simple distillation

Given Substance: BP: Mixed BP:

Oil of Cloves (15g)/water(250ml) 250oC / 100oC 98oC
Toluene/water 110oC / 100oC 85oC
Nonane/water 150oC / 100oC 95oC

Procedures

1
 Clamped a 500 ml 3-neck flask at a slight angle, with inlet for steam in one neck and
distilling head in the center. This is to avoid splashing.
 Add 15g of Oil of cloves in 3-neck flask containing 250ml of distilled water. make sure to
also place boiling stones in the flask to avoid bumping.
 Use rubber tubing with clamp to seal off the top of the distilling head.
 Steam is delivered from a separate distilling flask;
 A separatory funnel and a two-hole rubber stopper with glass tubing could be use as a
trap to remove excess condensate.
 Keep the rubber tubing from the trap to flask short, to minimize condensation.
 Properly seal the joint between the distilling head and the water condenser, if possible,
use one of the plastic joint clips or adjust the clamps to be sure that the joint surfaces are
press together and not pulled apart.
 Connect the water input to the lower opening in the jacket and the exit hose to the upper
opening.
 Although a heating mantle may be used it is probably best to use a flame with this
method.
 Note that the rate of distillation may be limited by the cooling capacity of the condenser.
 Adjust heating of the flask to maintain an approximately constant level in the flask.
 If liquid begins to back up in the tube, immediately open the system by loosening the
stopper on the separatory funnel.
 Use a 500ml Erlenmeyer flask as the receiver.
 Collect the distillate until no more oil can be seen in the fresh distillate.
 Discontinue distilling before the distilling flask becomes empty; leave 4-5ml solution in
the distilling flask.
 Approximately 125ml of distillate should be collected and stored for phase II

2
Phase II

Extraction

Purpose: To separate oil from water using methylene chloride.

Procedure:
 Assembly the apparatus for extraction

 Use a separatory funnel to extract the distillate by adding 3 separate 35ml portions of
methylene chloride.
 Shake and vent separatory funnel until no significant amount of gas is left in funnel.
 When the lower layer methylene chloride and upper water layers are separated skillfully
drain the lower methylene chloride into an Erlenmeyer flask.
 A reasonable amount of Magnesium sulfate anhydrous should be added to extracted
methylene chloride, to eliminate any water present by forming a milky cake at bottom of
flask.

Phase III

3
Concentration

Purpose: Removal of solvent (methylene chloride) using a rotary evaporator.

Procedure:

 First get magnesium sulfate out by filtration and let it dry out.
 Evaporate the combined methylene chloride layers on a rotovap or water bath.
 Stop procedure when bubbles are no longer present in rotary flask.
 Transfer the clove oil using a Pasteur pipette to a weighed vial and reweigh.
Conclusion/Comments:
Calculate the yield of the oil based on the weight of the original plant material used.

Weight of vial with oil = 31.22g

Weight of empty vial = 27.92g
Weight of oil recovered = 3.30g
Weight of original plant = 15.0g

% yield = weight of oil(g) × 100%

15.0g

% yield = 3.30g × 100% = 22%

15.0g

Comments: Plant material from clove could really be distilled extracted and concentrated
using a Rotary Evaporator to obtain a good yield of clove oil.