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I.

EXPERIMENT TITLE

: Fractional Distillation

II.

EXPERIMENT DATE

: April 30th , 2015 at 7.30 p.m

III.

END OF THE EXPERIMENT

: April 30th , 2015 at 10.00p.m

IV.

EXPERIMENT PURPOSE

V.

Determine refractive index of distillate

Determine purify of distillate

BASIC THEORY
DISTILLATION
Distillation is process of heated liquid until its boiling point reached,
then flow the vapor into condenser and collected the condensed vapor as liquid
substance. The aim of distillation is to purify the liquid substance which is has
different boiling point. Fractional distillation is the separation of a mixture into its
component parts, or fractions, such as in separating chemical compounds by their
boiling point by heating them to a temperature at which one or more fraction of the
compound will vaporize. Simple distillation can be used to separate components of a
mixture that have a large difference in their boiling points. If two components have a
boiling point difference of less than 40-50oC, simple distillation will not be successful
at separating them. In this case, fractional distillation must be used. When two
compounds with relatively close boiling points are heated, the vapor above the liquid
will be composed of both components at the boiling point. Consider the simple
distillation of a mixture of 50:50 A and B, where A has a lower boiling point than B.
When the mixture begins to boil, the vapor will be richer in A, but still have a
significant proportion of B; lets say the vapor above the boiling liquid is 66:33 A:B.
This vapor would get cooled in the condenser and drip into the receiving flask. At the
end of the simple distillation the receiving flask has been enriched in A and the liquid
remaining in the still pot is enriched in B. To purify A you would take the liquid from
the receiving flask composed of 66:33 A:B, set up another simple distillation,
enriching to perhaps 80:20 A:B. After a series of these vaporization/condensation
cycles you would finally get pure A. Fractional distillation can be considered a series
of simple distillations but rather than having many condensers and receivers, the
evaporation/condensation cycles take place in a single distillation column. Distillation
columns are high surface area tubes that allow multiple vaporization/condensation
cycles to occur at once. The added surface area in the column can come from glass

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protrusions like in Vigreux columns, the ones we will be using, or from a packing
material such as glass beads or steel wool put in a hollow tube which is known as a
Hemple column. In fractional distillation, vapor rises up the column and condenses on
the packing, then re-evaporates, rises further up the column and condenses again. This
evaporation/condensation continues up the column and with each cycle the vapor
becomes more and more pure in the lower boiling component. In this way, fractional
distillation accomplishes in one apparatus what would require several simple
distillation setups. The more vaporization/condensation cycles that the mixture goes
through, the better the separation. Although more surface area in the column leads to
better separation, it also makes the distillation process slower. Additionally, surfaces
in the column will be covered with condensation, and liquid that sticks to the surfaces
will not be distilled. The liquid condensed on the surfaces in the column is known as
hold-up. When using fractional distillation chemists try to strike a balance between
the quality of the separation and the speed of the distillation. During fractional
distillation there is a temperature gradient over the length of the column. The boiling
point of a mixture varies with the composition of the mixture; the higher the
percentage of the low boiling component, the lower the boiling point will be. Thus as
the mixture travels up the column and becomes purer, the temperature of the column
decreases. When the distillate finally reaches the still head, the thermometer reading
begins to rise. The thermometer reads the boiling point of the vapor that is condensing
on it. (Boiling point and condensation point are the same temperature.) If the
thermometer reads at the boiling point of the lower boiling compound, the distilled
liquid is pure. When the temperature rises above the boiling point of the low boiling
compound that means more and more of the high boiling component is starting to
distill over. To ensure a temperature gradient over the column, the still pot should be
heated slowly. Most of the vapor from the boiling still pot should condense and drip
back down into the still pot, a process known as refluxing.
If one compound is much more volatile than the other, the compounds
can be separated in one evaporation step. Such a step is called simple distillation and
uses an apparatus that consists of only a pot, a distillation head, a condenser, an
adapter, and a receiver. When the boiling points of two compounds differ by less than
40 C, they cannot be separated efficiently by simple distillation. Fractional
distillation, a process that has the effect of many simple distillations, must be used. A

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fractional distillation apparatus includes a fractionating column or a Vigruex column


placed between the pot and the distilling head
At this experiment we use spirit which is has 85% composition of
methanol. Methanol has 64,70C and refraction index 1,3284.Because distillation is a
separated method based on difference of boiling point of component. There is two
step of distillation that is boiling process and condensed process. Boiling point of
substance was effect by interaction inter-ionic, van der waals, dipole-dipole
interaction, and hydrogen bonding. Pressure and vapor composition can be determined
if the pressure and vapor composition of the purify substance has been known, based
on the Raoult law.

METHANOL
Methanol is a colorless volatile liquid with a faintly sweet pungent odor
similar to ethyl alcohol. The substance is fully soluble in water. Vapors of methanol are
slightly heavier than air and may travel some distance to a source of ignition and flash
back. Accumulations of vapors in confined spaces such as buildings or sewers may
explode if ignited. There is potential for containers of liquid to rupture violently if
exposed to fire or excessive heat for sufficient time duration. Methanol is listed as a
Poison-Class B. It is harmful if swallowed or absorbed through the skin. Ingestion of
as little as one ounce can cause irreversible injury to the nervous system, blindness, or
death. It cannot be made nonpoisonous. Causes eye and respiratory system irritation

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and may cause skin irritation. Avoid liquid, mist, or vapor contact. Vapor inhalation or
liquid penetration of the skin can cause central nervous system depression.

Physical and Chemical Properties


Physical Form: ............................................Liquid
Color: ..........................................................Colorless
Odor: ...........................................................Faintly sweet pungent odor like ethyl
alcohol
Boiling Point:..............................................148o F at atmospheric pressure
Melting point:..............................................-144o F
pH:...............................................................7.2
Solubility:....................................................100%
Specific Gravity: .........................................0.792 (@ 68o F)
Vapor Density: ............................................1.11 (@ 60 o F)
Vapor Pressure:...........................................1.86 psia (@ 68 o F)
% Volatile by Volume: ...............................100
Molecular Weight: ......................................32.04
Density: .......................................................6.63 lb. per gallon (@ 60 o F)
Critical Temperature:..................................464o F
Critical Pressure:.........................................1142 psia

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VI.

TOOLS AND MATERIALS


A. Tools
Electric stove
Pipe
Test Tube
Refraction meter
Distillation Flask
Liquefier
Thermometer
B. Materials
100 mL spirit
Methanol 95%
Methanol 80%
Methanol 70%
Methanol 60%
Methanol 50%
Methanol 40%
Methanol 30%
Boiled stone

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VII.

FLOW CHART

100 mL spiritus
-Put into destilation flask
-Heat until 64,5oC
100 mL Destilate
-

-Measure
Calculate fraction index with refratometer
Compare with

Methanol

Methanol

Methanol

Methanol

Methanol

Methanol

Methanol

95%

80%

70%

60%

50%

40%

30%

- Calculate % purify of
distilate
% purify of destilate

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VIII.

DATA OF EXPERIMENT

No.

Data of Experiment
Before
After
Spiritus: light
Distillate :

Procedure

purple solution

100 mL spiritus

colorless

Methanol 95% :
-Put into destilation flask

Hypothesis/Reactions

Conclusion

Boiling point of

Purify of

methanol 64,5%

distillate
86,6774%

colorless solution

% average

Methanol 80% :

purify of

colorless solution

distillate

Methanol 70% :

86,6774%

-Heat until 64,5 C


10 mL Destilate
-Measure
Calculate fraction index with
refratometer
Compare with

1.

colorless solution
Methanol 60% :
colorless solution
Methanol 50% :

Meth

Meth

Meth

Meth

Meth

Meth

Meth

colorless solution

anol

anol

anol

anol

anol

anol

anol

Methanol 40% :

95%

80%

70%

60%

50%

40%

30%

colorless solution
Methanol 30% :

- Calculate % purify of distilate

colorless solution

% purify of destilate

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IX.

EXPLANATION
Distillation is a separation method based on difference of boiling point of
component or based on the rate or the easier vaporization of the substance as we
known as volatility compound, for example is methanol, hexane, chloroform, and
acetone. At this experiment, we want to determine refractive index of distillate and
determine percentage purify of distillate. So, first we filled 100 mL of spirit which is
has light purple color of solution into distillation flask, then we set the apparatus like
picture below, we heated and we added boiling stone at the distillation flask to make
the heat even on the solution, then we waited it to produce distillate. And distillate
that is produce methanol, because spirit was contained by methanol and water.
Methanol which is has boiling point 64,70C and water has 1000C, so methanol will
vapor first and condensed become condensed vapor or distillate. And it is the reason
why temperature of distillation should keep on 64-650C. At this step we know that the
atmosphere pressure is same with methanol pressure, so methanol will vapored and
water still on liquid phase at distillation flask because when the temperature shown
number 64,70C water was not vapored.

Fractional Distillation

Fractional Distillation Apparatus set on

Apparatus set on theory

experiment

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Spirit has purple light color

Spirit has purple light color

The methanol vapor will be condensed into condenser which is flowed with
water as cooler, then the methanol vapor will be methanol condensed vapor and
become at liquid phase then flowed into measuring glass.
While we waited for it, we determine the refractive index with refraction
meter. First we tested the methanol 95%, methanol 80%, methanol 70%, methanol
60%, methanol 50%, methanol 40%, and methanol 30%. From our group observation
we get Refractive index of
30% methanol: 1,33404
40% methanol: 1,34050
50% methanol: 1,34160
60% methanol: 1,34510
70% methanol: 1,34160
80% methanol: 1,34370
95% methanol: 1,34680
There was a fault at data refractive index of 60% methanol, it should be not
too great but is too great then it make the refractive index of 70% methanol until 80%
methanol was smaller than 60% methanol.

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At this experiment we take 3 test tube sample of distillate, each test tube filled
by 10 mL of distillate. The distillate has colorless solution and the odor was alcohol
characteristic.

The distillate has colorless

The distillate has colorless solution

solution
First distillate has difference refractive index with second distillate and third
distillate because at first distillate the temperature was smaller than second and third
distillate. It make the distillate that we got will be purifier at first distillate. We can
explain it with the difference boiling point of methanol and water that contained in
spirit. When the temperature was more increase or bigger than 650C or approach
1000C, the distillate that produce will be contain by water too, not just methanol. Then
after we take three sample of distillate we test it with refraction meter to know the
refractive index of the distillate. And the refractive index of sample distillate is:
First sample: 1,34475
Second sample: 1,34685
Third sample: 1,34365
And the average of refractive index sample is 1,34508, so we can compare the
distillate that we got in the range of 80% methanol and 95% methanol. We count the
% purify of distillate with the function below:

% purify of distillate =
(

Fractional Distillation

) (
(

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We got % purify of distillate was 86,6774.%, it mean that the distillate contain by
86,6774% methanol and the other substance 13.3226%. And based on the theory that
we got we know that the methanol which is contained on spirit was 85% methanol. It
was close with our experiment result. So, we can say that our experiment result was
right.

X.

DISCUSSION
There is no From this experiment that we have committed there are based on
the theory. And there are no errors in our experiments.

XI.

CONCLUSION
Based on the experiment that we got, we can conclude that:
a. The average refractive index of distillate is 1,34508
b. The purify of distillate that we got is 86,6774 % it was close with theory that
we got that is 85%.

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REFERENCES

Anonymous. 2001. Methanol-MSDS.pdf.


(online).(http://terranitrogencorporation/methanol-msds.pdf , accessed
May 17, 2015 at 7.52 a.m.)
Anonymous. 2007. MATERIAL SAFETY DATA SHEET-Brandspiritus 85%.pdf.
(online).(http://hbvchemicalien.nl , accessed May 17, 2015 at 8.15 a.m.)
Anonymous. 2008. Experiment 6 - Simple and Fractional
Distillation.pdf.(online).(http://chemistry.about.com/exp.6.1.pdf ,
accessed May, 9 2015 at 9.23 a.m.)
Anonymous. 2015. Fractional Distillation.pdf (online).
(http://www.nvcc.edu/stb/chm/45_fractdist.pdf, accessed May, 9 2015 at
7.18 a.m.)
TimPenyusun .2015. Panduan Praktikum Kimia Analitik II: DDPK. Surabaya:
Jurusan Kimia FMIPA Unesa
Underwood,A.L dan Day.R.A.Jr.2002. Analisis Kimia Kuantitatif Edisi Keenam.
Jakarta: Erlangga
Wright, B. F. 2001. Distillation of Alcohol and DeNaturing.pdf.(online).(http://www.distillationgroup.com/distillationofalco
holandde-naturing.pdf , accessed at May 9, 2015 at 7.13 a.m.)

Surabaya, May 18th, 2015

Mengetahui,
Dosen/Asisten/Pembimbing,

Praktikan,

(.)

()

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Attachment

Spirit with light purple

Methanol 30%, colorless

Methanol 40%, colorless

color of solution

solution

solution

Methanol 50%, colorless

Methanol 60%, colorless

Methanol 70%, colorless

solution

solution

solution

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Methanol 80%, colorless

Methanol 95%, colorless

solution

solution

Setting the apparatus of distillation

The temperature of
distillation was 64,50C

Distillate produce is

Three test tube which is filled with

colorless solution

distillate 10 mL

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CALCULATION
Given :
Refractor index of
30% methanol = 1,33404
40% methanol = 1,34050
50% methanol = 1,34160
60% methanol = 1,3451
70% methanol = 1,34160
80% methanol = 1,34370
95% methanol = 1,34680
Sample I = 1,34475
Sample II = 1,34685
Sample III

= 1,34365

Asked : % purify of distillate ?


Answer :
-

Average refractor index of sample

=
=
= 1,34508

Botton Limit = 80% methanol

Upper Limit = 95% methanol

% purify of distillate =
(

=
=

) (
(

) (
(

)
)

+80%

=
= 6,6774 + 80%
= 86,6774 %

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