Steam Distillation

The purpose of this experiment is to demonstrate the ability to distill an organic liquid at a
temperature considerably below that of the boiling point of the pure liquid.
Procedure
Construct a steam distillation apparatus as set up in the lab.
Add your pulp and water to the distillation pot UNTIL HALF FULL.
Heat the mixture to a boil.
Note: Attempt to control the rate of heatin so that excessi!e foamin does not occur.
At the first drop of distillate, record temperature and volume of distillate collected. epeat this
every four m!, until "# m! of distillate has been collected.
"top the distillation. The distillate should ha!e two layers. The top layer should be oil and
the bottom one should be a#ueous. Transfer the distillate to a separatory funnel and allow the
mixture to stand for $ % &' minutes to allow complete separation. ("ee Fiure abo!e).
*rain off the a#ueous layer.
+ut the oranic li#uid (probably about , mL) in a clean- dry test tube and add a few ranules
of anhydrous calcium chloride.
$easure the volume of the organic liquid %now dry&.
Draw a Temperature vs 'olume graph of your lab data in your lab report.
Test for unsaturation (multiple bonds between two carbon atoms).
a) +lace one drop of cyclohexane in a depression of a white spot plate and add /0n12
dropwise until a red%brown color persists for 3' seconds.
b) +lace one drop of your distilled oil in another depression of a white spot plate- and add
/0n12 dropwise until a purple color persists- or until you ha!e added ten (&') more
drops to it than you added to the cyclohexane.
c) 4ecord.
. the number of drops used for cyclohexane
. the number of drops for your oil- and whether or not a purple
color was reached
Turn in your product in an appropriately labeled narrow mouth bottle.
((((((((((((((((((((((((((((((((((((((((((((((
Disposal of Spent Orange Peel
Construct a filtration apparatus as set up in the lab.
+lace the piece of cheese cloth pro!ided into your 5uchner funnel.
*raw a !acuum on the funnel.
+our the contents of your $'' mL round%bottom flas6 into the cheese cloth- and allow the
li#uid to drain into the filter flas6.
1nce the li#uid has been suctioned from the orane peel- discontinue !acuum and throw the
cheese cloth into the trash.
7777777777777777777777777777777777777777777777
)he *#+ Su,-##*
!ab Data Sheet
Title. "team *istillation
Name.
*ate.
!ab Data
Appearance of the liquid
% circle the appropriate description%s& &
Colorless color cloudy clear
other comments
8olume of Li#uid Used. mL.
Temp. at which first drops enter the recei!in !essel.
o
C
8olume9Temp *ata
'ol
%m!&
2 : &, &; ,' ,2 ,: 3, 3; 2' 22 2: $, $;
Temp
(
o
C)
8olume of total distillate 4eco!ered. mL.
8olume of oranic compound reco!ered. mL.
. the number of drops of /0n12 used for cyclohexane
. the number of drops for your oil- and whether or not a purple color was reached
(<9N)
)he *#+ Su,-##*
!ab eport
Title. Steam Distillation
Name.
*ate.
4esults.(*raw Temp. !s 8olume =raph)
*e C
&3'
&,'
&&'
&''
>'
:'
?'
;'
$'
2'
3'
8olume (mL)
Con!ert the !olumes of water and compound to moles utili@in
the information pro!ided
Constituent 0olecular Aeiht (m) *ensity (9mL)
Aater &: &.''
Citral &$,.,2 '.:::
moles oranic component 7
In addition to the information as6ed for in the procedure- calculate the percent reco!ery in mL9l''m
of startin material. Assume that the rind of six oranes weihs :'.' m.
Conclusion