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Ryan Jacob C.

Agdon

Group No. 1

BSE 21

December 5, 2014

Experiment No. 2
ISOLATION AND CHARACTERIZATION OF EUGENOL FROM CLOVES

SCHEMATIC DIAGRAM:
Part I. Steam Distillation of Clove Oil
Weigh 5.00 g of round cloves on a
watch glass and transfer them
quantitatively into 250 ml distilling flask.
+ 75 ml distilled water
+ few boiling chips
Swirl gently to mix
Assemble the steam distillation set-up
(see figure 1)
Turn-on the water supply and heat source
Record the temperature at the point you start
to collect the initial distillate
Adjust the heat to prevent rapid
boiling and foaming of mixture
Figure 1. Steam distillation set-up
(http://lowkerindo.com/job/how-toperform-simple-distillation-in-thechemistry-lab/)

Collect a total of 50 ml of distillate


Record the temperature for
every 5.0 ml of collected liquid
Construct a distillation curve with
the gathered data

-Turn off the heat and water source


-Dispose the residue properly
-Disassemble the set-up once it is cool enough for handling

Part II. Active Solvent Extraction and Characterization


Transfer the distillate into a 250 ml Erlenmeyer Flask
+ 3. 0 g NaCl
Swirl to
Cool the content of the flask in an ice bath

Transfer the content into a 250 ml seperatory funnel


+ 25.0 ml hexane
Stopper then shake for 5 minutes
-Place the seperatory funnel through an iron
ring.
-Allow two layers to separate
Drain the aqueous layer to the
Flush with copious amount of water
+ 25. 0 ml of NaOH
Shake for 5 minutes
-Place the seperatory funnel through an iron
ring
-Allow two layers to separate
Drained the aqueous at the bottom into the
cleaned and dried to a 250 ml Erlenmeyer flask
Discard the organic layer
properly to an organic waste jar
Cool the aqueous extraction in an ice
bath
-Acidify the solution with enough 6.00 M HCl
Use R litmus paper (PH of the solution)

Continuation. See next page

Return the acidified extract into the cleared and


dried original seperatory funnel
+ 25.0 ml hexane
Stopper then shake for 5 minutes

Continuation.

-Place the seperatory funnel through an iron


ring
-Allow two layers to separate

Drain the aqueous at the bottom into the


cleaned and dried to a 250 ml Erlenmeyer flask
Leave the organic layer
inside
Discard the aqueous layer into an acid waste jar
Transfer the remaining hexane extract into 250 ml
Erlenmeyer flask
+ Small amount of anhydrous sodium sulphate
+ Swirl
Filter the hexane extract into a clean and dried
250 ml Erlenmeyer flask (to sodium sulphate)

Place about 10 drops of extract into two separate test tubes

+ 1.0 ml 1% FeCl3

+ 1.0 ml of Bayers Reagent

Observe the ensuing reactions

Remove the organic solvent in the remaining extract using a rotary


evaporator with the water bath temperature at 40

and rotary

speed of 90 rpm (Ask for the help of your facilitator)


Determine the weight of the obtained eugenol

Calculate the percent yield

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