SEPARATION TECHNIQUES

There are a number of laboratory operations that are found in the study of material purity.
Because most products are often found naturally in the form of mixtures, ways of separating their
components are important techniques in the laboratory. Common methods of separating mixtures
include:
Decantation. This is a process of separating the solid-liquid components of mixtures by settling the
heavy solid particles and gently pouring out the liquid without disturbing the solids at the bottom of the
container.
Filtration. This is the process of separating fine solids from liquids (filtrate) by using porous filter
(paper, cloth, sand). By allowing the liquid to pass through the filter, the solid particles are separated
as they remain in the filtering medium.
Extraction. The process involves the distribution of a solute in two immiscible solvents. A substance
previously dissolved in a given solvent may be 'extracted' or removed by shaking the solution with another
solvent where it is more soluble. The separatory funnel is commonly used in this process. It is designed
with a narrow base near the stopcock so that the interface between the immiscible layers is confined in
a small space for accurate separation.
Sublimation. This is a process in which a solid with high vapor pressure passes directly to the gaseous
state without passing through the liquid state. Gentle heating of a solid mixture containing a substance
that sublimes will cause its separation, as it is changed to the gaseous state while the other components
do not. Separation is completed by taking care that it does not mix with the other components again as
the vapor is cooled and changes back to solid.
Distillation. This is a process of separating liquid mixtures with components of varying degrees of
volatility or significant differences in boiling point. The solution is heated causing the evaporation of the
more volatile component; thus separating it as a vapor which is changed back to liquid by cooling
(condensation).
Chromatography. This is the process of separating the substances in a complex mixture by different
affinities to an adsorbent. The components of the mixture are separated as they move along the
adsorbent material at different rates.
Evaporation. This process practically reduces the volume of a solution. It is usually carried out using
an evaporating dish or porcelain dish. When evaporating to dryness, the dish must be removed from
the flame with a tong while there are still a few drops of the liquid left. The heat of the dish is sufficient
to complete the operation. The solid particle left in the dish is the residue.
Centrifugation. The process uses a device called centrifuge in which centrifugal force, produced by an
electric motor, speeds up the rate of settling of a precipitate of smaller size. This is usually used in
semimicro procedures in which insoluble particles containing the analyte is separated from its mother
liquor. Precipitation is involved where two chemical liquids reacted to form insoluble solid particles
called precipitate. The liquid portion separated in this process is called centrifugate.
In this activity, you are going to separate components of mixtures using different separation
methods.

Objectives
At the end of the activity, you should be able to
1. Perform different methods and techniques of separating components of mixtures;
2. Observe proper laboratory operations and techniques in performing the experiment; and
3. Identify substances the substances present in mixtures.
Materials
balance separatory funnel watch glass mixture sample
spatula (2) beakers, 250-mL/100-mL cork iodine crystals
centrifuge Erlenmeyer flask droppers (3) n-hexane
alcohol lamp graduated cylinder, 10-mL boiling chips acetone
wire gauze glass tubing, bent filter paper 0.05 M Pb(NO3)2
tripod test tube (2) Whatman paper 0.025 M K2CrO4
glass rod iron ring and stand marking pens (4) distilled water
funnel evaporating dish

Procedure

A. Separation of Components of a Mixture with Different Solubilities

1. Weigh about 3.00 g of the mixture prepared by the instructor in a previously weighed evaporating
dish. Observe the mixture.
2. Heat the evaporating dish containing the mixture IN THE HOOD until white fumes are no longer
visible. After heating for about 5 minutes, remove the flame and gently stir the mixture with a
glass rod.
3. Allow the evaporating dish to cool and weigh its content.
4. Add about 20 mL distilled water to the remaining mixture in the evaporating dish.

[Q1] What is the purpose of adding water to the mixture in this step?

5. Stir and filter. Collect the filtrate and observe the substance in the filter paper.

[Q2] Describe the substance collected in the filter paper. What substance remained in the filter
paper?

6. Evaporate the filtrate over a low flame using the same evaporating dish until the crystals are
formed. Observe.

[Q3] What substance was left in the filter paper after filtration?

7. Determine the weight of the crystals (residue) and the dish.

[Q4] What does the difference in weight between procedure A.3 and A.7 mean?
[Q5] Make a schematic diagram showing the separation of the components of mixture in procedure A

B. Separation of a Solute between Immiscible Solvents

1. Get a very small amount of iodine crystals with a spatula and add to 10.0 mL distilled water in a
beaker.

[Q5] Describe the solubility of iodine crystals in water.

2. Transfer the mixture into a separatory funnel with the stopcock closed. Add in 5.0 mL of n-
hexane into it. Observe where the n-hexane layer forms.

[Q6] How is the n-hexane layer identified?

 3. Cover the funnel; and carefully shake the resulting mixture to allow the iodine to reach partitioning
equilibrium between the two solvents. Observe what forms after shaking.

[Q7] In which solvent do iodine crystals readily dissolve? What observation proves this?

4. Uncover the separatory funnel containing the immiscible mixture. Turn the stopcock to release
the lower layer to another vessel and separate it from the upper layer.

C. Separation of Components of a Mixture with Different Volatilities

1. Prepare a solution of 20 mL water and 5 mL acetone in an Erlenmeyer flask.

[Q8] Define volatility.

2. Add two or more boiling chips to the solution to avoid bumping during heating.
3. Cover the Erlenmeyer flask with a cork with bent glass tubing inserted in it. The other end of the
glass tubing must be connected to an empty, dry test tube in side a beaker.
4. Fill the beaker about three quarters full with water carefully so that the test tube remains dry
inside.
5. Heat the solution in the flask with a small flame. Control the heat so that the substance that
volatilizes can condense into liquid as it reaches the test tube in the beaker.
6. Stop heating when about 1 mL of liquid is collected. Identify the liquid obtained by its odor.

[Q9] What substance is collected in the test tube?

D. Separation of Minute Components of a Mixture by Paper Chromatography

1. Place 10 mL of distilled water into a 250-mL beaker.

2. Cut 4 x 8 cm piece of Whatman paper to fit into the beaker lengthwise.
3. Using a pencil, draw a line across the paper one centimeter from the bottom of the paper.
4. Using four different colored marking pens (water-soluble), mark small spots along the line.
5. Suspend the paper with the stick/glass rod in the beaker. Be sure that the bottom edge is dipped
in the water but not the colored spot samples.
6. Cover the beaker with a watch glass and allow the solvent to travel three-fourths of the way up
the paper. Do not turn the beaker.
7. A good ink/dye sample will register two or more spots if complete separation is achieved.

E. Effective Separation of Precipitate from its Mother Liquor

1. Add 1.0 mL of 0.05 M Pb(NO3)2 to 1.0 mL of 0.025 M K2CrO4 in a small test tube. Observe.

[Q10] Describe what is formed when the two solutions are mixed.
[Q11] How does precipitation differ from the other separation processes encountered in this
experiment?

2. Centrifuge the mixture using a mechanical/electrical centrifuge.

3. Devise your own method to effectively separate the liquid from the precipitate.

[Q12] How will you separate the liquid from the precipitate effectively?
Please write your answers to the questions on a separate coupon bond.
Activity No. _____ SEPARATION TECHNIQUES
Name _____________________________________________________
_____________________________________________________
_____________________________________________________
_____________________________________________________
Date Started ____________________________
Date Finished ___________________________
Section ___________________________

DATA AND RESULTS

Sample Mixture Observation Method of Substances
Separation Separated
Used
A. Ammonium chloride Weight of mixture + evaporating dish
Sodium chloride Before heating ____________ g
Sand After 1st heating ____________ g
After 2nd heating____________ g

B. Iodine crystals
+ water

+ n-hexane

C. Water and acetone

D. Water and soluble ink

E. Precipitate with its

mother liquor
Pb(NO3)2 and
K2CrO4