EXPERIMENT 1

SUBSTANCE SEPARATION AND PURIFICATION

I.Purpose

Students have knowledge about the technique of separating and refining one or several substances
from the mixture.

Students know some basic properties of matter / substances through physical and chemical properties.

II. Basic Theory

In chemical practicums, often various substances must be separated into its constituent
substances. The purity of a substance can be determined by measuring some of its physical properties.
Physical properties are characteristics of substances that can be observed and measured without
changing their chemical composition, including: melting point, solubility, boiling point, vapor
pressure, density, and others.

The process of separating substances from the mixture can be done in several ways. The
separation method can be classified into:

1. Separation of solid from liquid.

2. Separation of solids from solids.

Separation of solid from liquid, can be done by:

a. For solids which cannot dissolve in liquid.
(1). Decantation
(2). Filtration

b. Forsolids which dissolve in liquid:

(1). Evaporation.

(2). Crystallization.

(3). Distortion.

Separation of solids from solids can be done by:

a. Dissolving and filtering, for example: separation of table salt (soluble in water) from sand
(insoluble in water)
b. Multi-level crystallization
c. Sublimation

Another method of separation can be done by:

a. Extraction
b. Chromatography

III. Tools and Materials

- 4 beakers - CuSO4.5H2O
 - 1 funnel - table salt
- 1cup vaporizer - yod or camphor
- 1 50 mL measuring cup - chalk
- 1 burner - sand
- 1watch glass - filter paper

IV. Work Procedures

1. Decantation
Put ± 1 tablespoon of sand into a beaker containing 80 mL of water, then stir. Take a few
moments. Observe what happened, record your observations! then slowly pour the top
solution with the aid of a stirring rod.
2. Filtration
Put ± 1 tablespoon of chalk powder into a beaker filled with water, then stir. Prepare a funnel
and filter paper, do the filtering. Compare the color of the liquid before and after filtering.

3. Recrystallization
Dissolve 5 grams of copper sulfate, CuSO4. 5 H2O, into 25 mL of water. Filter if needed and
evaporate so that the volume is ± 10 mL (the solution becomes saturated). Chill and leave it
somewhere so it is not disturbed (without shake).

4. Filtration and crystallization

Mix ± 1 spoon of sand and 1 tablespoon of salt until homogeneous, put in a beaker. Add 50
mL of water until all the salt dissolves. Heat this mixture, then strain. Solids are left in the
funnel, washed two until three times with ± 5 mL of water. Put together the filter water and
washing water, then steam in the evaporation cup. If the water is low, heating is stopped and
let the water evaporate on its own.
 5. Sublimation
Add 2 tablespoons (spatula) of iodine crystals or dirty camphor powder (littered with sand)
into the evaporation cup. Cover the evaporation cup with a watch glass filled with water. Heat
it slowly until a solid is formed on the watch glass base. After cooling, collect the crystals.
Compare the substances formed with the original substances.
6. Extraction
Insert a small iodine crystal into a test tube containing 5 mL of water, shake and pay attention
to the color of the solution. Take 1 mL of CCI4 (carbon tetrachloride), or CHCI3
(chloroform), pay attention to the color, then put it in an iodine solution. Shake by hitting the
bottom of the tube on the palm of your hand, observe what happens. Compare this separation
method with Soxhlet extraction (demonstrated by assistant or supervisor).

V. Observation and Calculation Sheet

No Experiment Observation Result

Distillation

Distillation is used to purify liquid, which is based on differences in the boiling point of liquids. In
this process the liquid turns into steam. This vapor is a pure substance. Then this steam is cooled in
the condenser. In this cooling, steam condenses into pure liquid called distillate.

Distillation can be used to obtain pure solvents from solutions containing solutes. For example, the
distillation of tea water to obtain pure water.

1. Tools and substances

Tools :
- 1 set of distillation apparatus (distillation flask, Liebig condenser / cooler, adapter, alon,
distillator reservoir, thermometer–10-100ºC, asbestos and gauze asbestos, incinerator, stative
and clamp, rubber hose).

Materials :

- Tea water / dirty water / ink water, boiling stones

2. Work Procedures :
1. Install the tool as shown!

2. Fill distillation flask with tea water / dirty water / ink water. Add two boiling stones.
3. Flow water through a cooler / condenser.
4. Heat the distilled flask until the water boils.
5. Observe the temperature rise on the thermometer.
6. Read the boiling point of the distillate.
3. Observation Result
1. Differences between distillate and liquid before distilled
NO. Fluid Before Distillation distillate

2. Distillate boiling point………ºC

4. Questions and Discussions

1. Why is the flow of water in the condenser made in the opposite direction to the distillate
flow?

2. Explain the principle of water purification by distillation?

 Chromatography

Introduction

Chromatography is a way to separate and identify mixtures. There are several types of
chromatography, including: paper chromatography, typhoid chromatography and column
chromatography. Paper chromatography, using paper chromatography as a stationary phase (buffer).
One of the uses of paper chromatography is the constituents separation of an ink.

Tools and Substances

- Chromatographic paper
- Beaker
- Stick
- Blue, red, green ink (water soluble type).

Work Procedures

1. Prepare a filter paper size of 6 x 10 cm (as shown).

2. Make a line with a pencil ± 1 cm from the bottom end of chromatographic paper (if there is
nothing can be replaced with filter paper).
3. Make a dot with a certain color ink in the middle of the line.
4. Make a dot with other color ink on the left and to the right of the green dot at a distance of 2
cm. Let the ink dots dry.
5. Roll the paper so that it forms a cylinder.
6. Place the paper in a beaker containing 1 cm of water, so that the tip of the paper is immersed
in water (keep the ink dots immersed / submerged in water).
7. Let the water spread to the top of the paper. Observe what happened!
8. If the water has crept closer to the top edge of the paper, remove the paper. Put a limit on the
water propagation.
9. Pay attention to dye stains in ink. Let the filter paper dry.
 10. Measure the distance between the water level and the distance of each dye stain, from the
pencil line at the bottom end of the paper.
11. Measure the price of the ratio of the two distances, (Rf) = distance of stain / distance of water.
12. Make chromatograms from unknown ink points, for example a mixture of two kinds of ink.
Observation Sheet

Observation

Ink type : …………………..

Ink Color Stain Color Stain Distance / Water Distance ( Rf )

1.

2.

3.

4.

1.

2.

3.

4.

1.

2.

3.

4.

Questions

1. Are there different dyes from the same ink ?

………………………………………………………………….
How can this be known?

2. Are the unknown inks made from the same two inks?

VII. Conclusion

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VIII. References
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Singaraja, 12 September 2019

Supporting lecturer, Students,

(Dr. I Nyoman Suardana, M.Si) (IPutu Adi Payana Putra)

NIP. 196611231993031001 NIM. 1913071015