A.

Tiltle Of Experiment
The title of this experiment is “Mixture Separation”

B. Objective Of Experiment
The objective of this experiment s to know the layer of separating mixture
by filtration, by crystallitation, by chromatography, by sublimation. And by
distillation.

C. Literature Review
The separation of chemical mixtures into their constituents has been
practiced, as an art, for millennia. Early civilizations developed techniques to (1)
extract metals from ores, perfumes from flowers, dyes from plants, and potash
from the ashes of burnt plants, (2) evaporate sea water to obtain salt, (3) refine
rock asphalt, and (4) distill liquors (Seader.2006:3).
The separation of mixtures, including enrichment, concentration,
purification, refining and isolation are of extreme importance to chemists and
chemical engineers. Separation technology has been practiced for millennia in the
food, material processing, chemical and petrochemical industry. In the food,
material processing and petrochemical industry most processes do not involve a
reaction step but are merely used for the recovery and purification of products
from natural resources. Examples are oil refining (Fig. 1.1), metal recovery from
ores and the isolation and purification of sugar from sugar beats or sugar cane
schematically (Han.2013:1).
The phrase ‘filtration and separation’ contains a certain amount of
redundancy. The safe separation of iron particles in engine oil away from sensitive
parts can be achieved using a filter, but equally using a simple magnetic device,
other physical fields, such as gravity, can equally deliver a form of separation.
Separation need not require filtration, but, for our purposes, filtration actually
implies separation (Sparks.2016:4)
In solution crystallization, the mixture, which includes a solvent, is cooled
and/or the solvent is evaporated to cause crystallization. In melt crystallization,
two or more soluble species, in the absence of a solvent, are separated by partial
freezing. A particularly versatile melt crystallization technique is zone melting or
refining, which relies on selective distribution of impurity solutes between a liquid
and a solid phase to achieve a separation. Many metals are refined by this
technique, which, in its simplest form, involves moving a molten zone slowly
through an ingot by moving the heater or drawing the ingot past the heater. The
manufacture of single. crystals has been a vital development in the semiconductor
industry in recent years (Seader.2006:13)
Supersaturated solutions are not very stable. In time, some of the solute
will come out of a supersaturated solution as crystals. Crystallization is the
process in which dissolved solute comes out of solution and forms crystals. Note
that both precipitation and crystallization describe the separation of excess solid
substance from a supersaturated solution. However, solids formed by the two
processes differ in appearance. We normally think of precipitates as being made
up of small particles, whereas crystals may be large and well formed
(Chang.2010.514).
Chromatography is a physico-chemical method of separation of
components within mixtures, liquid or gaseous, in the same vein as distillation,
crystallization, or the fractionated extraction. The applications of this procedure
are therefore numerous since many of heterogeneous mixtures, or those in solid
form, can be dissolved by a suitable solvent (which becomes, of course, a
supplementary component of the mixture) (Roessac.2007:3).
Thin layer chromatography for the purpose of qualitative analysis of
gunpowder samples is a reliable method and largely depends on the expertise of
individuals and from the interpretations of the results. Results of qualitative thin
layer chromatography analysis provides very good guidance in purpose of life
prediction of gunpowders. Thin layer chromatography method can be
economically employed for routine use because the consumption of mobile phase
is low and, hence, there are scarcely any disposal problems. Thin layer
chromatography method does not require the use of machines or special devices, it
is fully portable and easy to handle and considerably cheaper than most
commercial methods (Namir.2019).
In Ion-exchange chromatography, retention is based on the attraction
between solute ions and charged sites bound to the stationary phase. Ions of the
same charge are excluded. This form of chromatography is widely used in
purifying water, Ligand-exchange chromatography, Ion-exchange
chromatography of proteins, High-pH anion-exchange chromatography of
carbohydrates and oligosaccharides, etc (Ghanjaoui.2020).
Sublimation is the transfer of a substance from the solid to the gaseous
state without formation of an intermediate liquid phase, usually at a relatively high
vacuum. Major applications have been in the removal of a volatile component
from an essentially nonvolatile one. Examples are separation of sulfur from
impurities, purification of benzoic acid, and freeze-drying of food
(Seader.2006:3).
Sublimation is the transfer of a species from the solid to the gaseous state
without formation of an intermediate liquid phase. Examples are separation of
sulfur from impurities, purification of benzoic acid, and freeze-drying of foods. A
common application of sublimation is the use of dry ice as a refrigerant for storing
ice cream, vegetables, and other perishables (Seader.2011:11).
Sublimation is the process in which molecules go directly from the solid
into the vapor phase. Deposition is the reverse process, that is, molecules make
the transition from vapor to solid directly. Naphthalene, which is the substance
used to make mothballs, has a fairly high (equilibrium) vapor pressure for a solid
(1 mmHg at 53°C); thus, its pungent vapor quickly permeates an enclosed space.
Iodine also sublimes. Above room temperature, the violet color of iodine vapor is
easily visible in a closed container. Because molecules are more tightly held in a
solid, the vapor pressure of a solid is generally much less than that of the
corresponding liquid. Molar heat of sublimation (∆𝐻𝑠𝑢𝑏 ) of a substance is the
energy (usually in kilojoules) required to sublime 1 mole of a solid
(Chang.2010.497).
 In sublimation, a solid vaporizes into a gas phase without passing through
a liquid state. At low pressure both sublimation and desublimation are governed
by the solid vapor pressure of the solute. Sublimation of the solid takes place
when the partial pressure of the solute in the gas phase is less than the vapor
pressure of the solid at the system temperature (Seader.2006:146).
Distillation is basically a process of separating a mixture into two or more
products, by exploiting the differences in the volatile capabilities of the
components in the mixture. In other words, distillation is a method of separating a
solution using heat as a separating agent. This process is carried out in a tray
column or a packing column, so that a better separation work can occur
(Arwized.2017).
In distillation (fractionation), a feed mixture of two or more components is
separated into two or more products, including, and often limited to, an overhead
distillate and a bottoms, whose compositions differ from that of the feed. Most
often, the feed is a liquid or a vapor-liquid mixture. The bottoms product is almost
always a liquid, but the distillate may be a liquid or a vapor or both
(Seader.2006:252).
Distillation is a method of separating mixtures based on differences in the
level of volatility (ease of a substance to evaporate) at a certain temperature and
pressure. Distillation is a physical process and there is no chemical reaction during
the process. In distillation, the mixture of substances is boiled so that it
evaporates, and this vapor is then cooled back into liquid form. The substance
with the lower boiling point will evaporate first. This method includes a chemical
unit operation of the mass transfer type. The application of this process is based
on the theory that in a solution. Each component will evaporate at its boiling point
(ethanol boiling point 78°C) (Batutah.2017).
The separation requires that (1) a second phase be formed so that both
liquid and vapor phases are present and can contact each other on each stage
within a separation column, (2) the components have different volatilities so that
they will partition between the two phases to different extents, and (3) the two
phases can be separated by gravity or other mechanical means. Distillation differs
from absorption and stripping in that the second fluid phase is usually created by
thermal means (vaporization and condensation) rather than by the introduction of
a second phase that may contain an additional component or components not
present in the feed mixture (Seader.2006:252).

D. Apparatus and Chemicals

1. Apparatus
a. Beaker 250 ml (1 Piece)
b. Beaker 100 ml (1 Piece)
c. Beaker 1000 ml (1 Piece)
d. Measuring Cup (1 Piece)
e. Strirring Rod (1 Piece)
f. Spaula (1 Piece)
g. Erlenmayer Pumpkin (3 Pieces)
h. Stopwatch (1 Piece)
i. Mortar (1 Piece)
j. Pastle (1 Piece)
k. Distillation Apparatus (1 Piece)
l. Spray Bottle (4 Pieces)
m. Funel (2 Pieces)
n. Vaparizer Cup (2 Pieces)
o. Three Feet and Kasa (3 Pieces)
p. Spirit Burner (3 Pieces)
q. Scissors (1 Piece)
r. Watch Glass (1 Piece)
s. Ruler (1 Piece)
t. Digital Glass (3 Pieces)
u. Stick (1 Piece)
2. Chemicals
a. Clean Stand
b. Filter Paper
c. Three Color Marker
d. Sodium Chloride (Nacl)
e. Stove (C10H16O)
f. Alcohol 70% (C2H5OH)
g. Aquades
h. Ice Cubes
i. Stick
j. Tissue
k. Match

E. Work Procedures
1. The mixture separation by filtration
a. The mass of the cup was weighed
b. 20 grams of sands were weighed, then placed in a beaker and 100 ml
c. A piece of filter paper was taken, folded four parts like a cone and then placed
on a funnel
d. A mixture of sand and water was filtered
e. Observation was record
2. The mixture separation by crystallization
a. The mass of the cup was weighed
b. 8 grams of table salt were weiged, then dissolved in 25 ml of water in a beaker
c. The solution was transferred to an evaporation cup whose mass is known, the
solution was boiled until it is reduced (thickened)
d. The solution was cooled to crystallize
e. The evaporation cup and salts crystals in it were weighed
f. The obtained crystals mass was calculated
3. Separation of mixture by chromatography
a. Filter paper of taken wit a size of 5x15 cm
b. 3 different colors of ink were sported at a distance of 1 cm from the edge of the
paper
c. The beaker glass was filled with 250 cm of distilled water
d. Filter paper by rolling the end of the paper with a stick hanging and the and of
the paper dipped in a beaker containing water try not to touch the water that
was been smeared on the filter paper.
4. Separation of mixture by sublimation
a. The mass of the cup was weighed
b. The camphor was weighed as much as 20 grams
c. The sands was weighed as much as 20 grams
d. Crushed camphor and sands was mixed into beaker
e. Watch glass was placed on top of the beaker
f. Heated until it evaporate
g. Observation result was recorded
5. Separation of mixture by distillation
a. Distillation apparatus was assembled
b. 20 ml alcohol and aquades were put in the same ration, into a distillation flask
c. The distillation flask was closed and the thermometer was attached to he
stopper of he flask
d. Water and conclenser in the condenser and drips on the erlenmayer flask to a
boil, keep doing it until there is a substance that evaporates and condenser in
the condenser and drips on the erlenmayer flask
e. The temperature was recorded when the first drop of liquid occurs in the
erlenmayer flask
f. Boiling was carried out until the temperature on the thermometer showl a
constant value
g. The temperature was recorded when the first drop of liquid in the distillation
flask occurs
h. If there is an increase in temperature, remove the erlenmayer flask and the
volume was recorded of liquid that is accomudated
i. Erlenmayer flask was replaced to accomudated he remaining liquid in
distillation flask
F. Observation Result
1. Table of observatiom
a. Mixture separation by filtration

No Treatment Result

1. 100 ml aquades Clear

2. 100 ml aquades + 20 gr sand Nessy

3. 100 ml aquades + 20 gr sand + filtering Clear but not as clear as

before
b. Mixture separation by crystallization

No Treatment Result

1. 8 gr table salt 8 gr

2. 8 gr table salt + 25 ml aquades Dissolved

3. Heat 8 gr table salt 9,17 gr

c. Mixture separation by chromatography
𝑇he distance traveled by the compound
RF =
𝑇he distance traveled by the solvent
1) Green
1,9
RF yellow = = 0,19
10
0,4
RF blue = = 0,04
10

2) Red
1,4
RF pink = = 0,14
10
0,4
RF yellow = = 0,04
10

3) Brown
1,3
RF pink = = 0,13
10
 0,8
RF yellow = = 0,08
10

d. Mixture separation by sublimation

No Treatment Result

1. 20 gr camphor 20 gr

2. 20 gr sand 20 gr

3. 20 gr camphor + 20 gr sand 20 gr camphor and 20 gr sand

mixture

4. Camphor + sand + heated + closed the Camphor evaporated upward

watch glass filled icu cube and have crystal
e. Mixture separation by distillation
Temperature Volume when
Solution Treatment First drop Constant temperature change
20 ml aquades + Solution
83°c 83°c 18 ml
20 ml alcohol 70% being
heated
2. Data analysis
Mixture separation by chromatography
𝑇he distance traveled by the compound
RF =
𝑇he distance traveled by the solvent
a. Green
1,9
RF yellow = = 0,19
10
0,4
RF blue = = 0,04
10

b. Red
1,4
RF pink = = 0,14
10
0,4
RF yellow = = 0,04
10

c. Brown
 1,3
RF pink = = 0,13
10
0,8
RF yellow = = 0,08
10

G. Discussion
Chemical separation of mixtures of its constituents has been practiced as
an art, for thousands of years early civilizations developed techniques to (1)extract
metals from perfume seeds from flower dyes from plants and potassium from
burnt plant ashes (2)evaporating seawater to obtain salt (3) smoothing asphalt
stone (4) filtering liquor (Seader2006:3). The results of our experiments are as
follows,
1. Filtration
Filtration is a separation method for separating solids from liquids by
using a filter, sand and water can be separated through this process the sand will
be retained on the filter paper and the water will pass through the filter paper. The
basic principle in this method is the difference in particle size between the solvent
and the solute. The working principle of this method is filtering.
The tools and materials used are a scale to determine the mass of the
material, a beaker as a place to dissolve a mixture of sand and water, a spatula to
stir the ingredients, filter paper as a filter between sand and water through the
paper pores, a funnel serves as a place to store filter paper for separate the mixed
solids and liquids and an Erlenmeyer flask as a container for filtration. The
material used is sand as a solid which will later be dissolved and water as a liquid
which will become a solvent.
From the results of experiments carried out, it can be proven that sand and
water can be separated through the filtration method even though the water results
are not completely clear, the water produced is as much as 60 ml, this is in
accordance with the theory of Agusdin’s (2020) that filtration will hold solids that
have larger particle size and filter pores and will continue the solvent, the
filtration process carried out is the material that must be made in the form of a
solution or in liquid form and then filtered. The filtered result is called the filtrate
and what is left is called the residue.
2. Crystallization
Crystallization is a separation method by crystallizing the mixed
components by heating and then cooling, this method can separate salt from water
to produce crystals. The basic principle in this method is the solubility of the
material in a solvent and the difference in freezing point. The working principle is
a state of supersaturation, mixed substances will form crystals.
The tools and materials in this experiment are a beaker as a container for
dissolving salt and water, a scale to determine the mass after and before
conducting the experiment, a petri dish as a container for storing salt and water, a
stirrer rod that functions to stir the two mixtures. The gauze serves as a wire
holder and the gauze acts as a buffer when heated, the spritus to heat the solution.
While the material is a solid salt to be dissolved and water as a liquid to dissolve
it.
based on the results of the experiments carried out, the salt and water were
dissolved and then heated until boiling and thickened, then cooled to obtain
crystals, the crystals obtained were whiter and shinier than salt, this was due to
evaporation of the water and the salt coagulated to form crystals. The results of
this experiment are in accordance with the theorythat crystallization separation is
carried out to separate solids from solution by evaporating the solvent, the solids
in a supersaturated state will form crystals (Ayuningtyas. 2011).
3. Chromatography
Chromatography is a method of separating mixtures based on differences
in the speed of propagation of solvents in layers of certain substances. The basic
principle of this experiment is the speed of propagation between the stationary
phase and the mobile phase, while the working principle is the solubility in the
solvent, the absorption power by the adsorbent, and the valatility (evaporation
power).
The tools and materials used are 1000 ml beaker as a container to separate
the mixture, markers with three different colors, namely green, red, and brown,
sticks for hooking chromatographic paper so that they do not get immersed in
water. While the material is chromatographic paper as a place to put 3 color
markers and water serves to dip the end of the paper .
Based on this experiment, three markers ink with different colors are
applied and the end of the paper is dipped until the water absorbs into the paper,
and then green ink produces yellow RF = 0.19 cm and blue RF = 0.04 cm, red ink
produces pink RF = 0.14 cm and Yellow RF = 0.04 cm, brown ink produces pink
RF = 0.13 cm and yellow RF = 0.8 cm.
4. Sublimation
Sublimation is a method of separating mixtures by evaporating solids
without going through the liquid phase first so that impurities that do not
sublimate will be left behind. The basic principle in this experiment is a mixture
consisting of a substance that sublimes and a substance that does not sublimate,
while the working principle is to separate substances that easily sublimate with a
sublimator so that they become gas or vapor.
The tools and materials used are a scale to measure the mass of substances,
a beaker as a container to accommodate materials, an evaporation cup to separate
the substances that make up the solution, a spatula to stir the solution, three legs
and gauze as a wire holder and gauze as a buffer, a Bunsen burner. as a tool for
heating substances, as well as a watch glass to close the beaker when the
evaporation process occurs. While the materials used are camphor or lime as a
substance that will sublimate, sand as a solid that does not sublimate and ice cubes
to cool the two substances.
Based on the results of this experiment, 20 grams of camphor and 20
grams of sand were heated by placing a watch glass on top of a beaker and placing
ice cubes, then it was observed that there was sublimation of the camphor and it
stuck to the watch glass and formed shiny white crystals. This is in accordance
with the theory that sublimation is a change in the state of matter from solid to gas
and vice versa (Agusdin.2020). If the particles that make up solids are given an
increase in temperature, the particles will sublimate into a gas.
5. Distillation
 Distillation is a method of separating mixtures of liquids that have
different boiling points by heating a non-volatile solid solution dissolved in a
liquid in a flask. The basic principle of this method is different boiling points and
the working principle is to separate two solutions with different boiling points.
The tools and materials used are distillation equipment as a tool to carry
out the separation process between alcohol and distilled water, a distillation flask
as a container for a mixture of substances, a thermometer as a temperature
measuring device, tripod and gauze as a wire holder and gauze as a buffer, a
Spiritus burner to heat the solution , the condenser as a place for steam, a cooling
bath as a container to cool the solution and a heating bath to heat the solution. The
materials used in this practicum are alcohol 70% as a liquid and aquades as a
mixed liquid.
Based on this experiment, it was found that the alcohol will evaporate first,
this steam is the distillation and goes to the condenser and then cooled in the
evaporation bath. Obtained a temperature of 83 at the time of the first drop, and 95
constant temperature. After that, the volume of the substance that has been heated
is 18 ml. This is in accordance with Agusdin's (2020) theory that the result of the
distillation process can be a two-component binary liquid consisting of only a
liquid phase or a mixture of steam and liquid.

H. Conclusion
Based on this experment that have been carried out. We can conclude that
are several ways of Separation mixtures, are filtration, crystallization,
chromatography, sublimation, distillation. Substance such as sand can be
converted into liquids by the filtration. Salt can be separated by cristallization. Ink
can be separated by Chromatography. Camphor and sand can be separated by
sublumaton Water and alcohol can be separated by distillation.

I. Suggestion
1. For Laboratory, Laboratory used is clean. Some of apparatus and chemicals
have been provided by the Laboratory.
2. For Assistant, Assistant is very friendly, and kind teach us well so we can
understand more, correct and help us in this practicum.
3. For Apparantice, Provide complete apparatus and chemicals, understand well
the work procedure in this unit, and study the lots of references about this unit.
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