EXPERIMENT 2

PURIFICATION AND MELTING POINT DETERMINATION

Name: Lamela, Pauline Anne; Talaman, Kyla Julienne; Tumacole Erick John Date: February10, 2020
Group number: 2 Section: 2

1. Recrystallization of Naphthalene

a. Selection of a solvent for recrystallization

DESCRIPTION OF MIXTURES
Appearance of
SOLVENT
at room crystals
during heating on cooling
temperature
Insoluble, the
Precipitate formed
solute settled at White, smaller
H2O soluble at the bottom of
the bottom of the crystal formation
the test tube
test tube

Insoluble, the
Precipitate formed
solute settled at White, larger
95% ethanol soluble at the bottom of
the bottom of the crystal formation
the test tube
test tube

Appropriate solvent: Ethanol

1. What is a crystal and what is meant by recrystallization?

A crystal is a substance in which the constituent atoms, molecules, or ions are packed in a regularly
ordered, repeating three-dimensional pattern. Most crystals are solids.

2. What must be considered in choosing a solvent for recrystallization?

High temperature coefficient, dissolves impurities readily or not at all, does not react with the solute
nonflammable, inexpensive and volatile

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 b. Observations on recrystallization of naphthalene

SAMPLE OBSERVATIONS

Mixtures of crude sample The solute settled at the bottom of the test tube. The solute can be
and solvent observed through the solvent.

a. Filtrate Colorless; some crystal formations were observed

b. Residue Few wet solids were seen on the fluted filter paper
Hot filtration

a. Filtrate Colorless with faint odor

Vacuum
filtration

b. Residue Wet, coarse textured

Air dried crystals White crystal, fine texture, strong odor

3. Compute for the %recovery of naphthalene after recrystallization.

Crude sample Recrystallized sample

Mass of container + sample (g) 40.6671 g 41.2559 g

Mass of container (g) 38.5959 g 40.2983 g

Mass of sample (g) 2.0712 g (A) 0.9576 g (B)

% recovery (B/A x 100) : 46.23%

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4. In recrystallization, the goal is to obtain a purified material with maximum recovery? What are the
effects of the operations below on purity and recovery? Explain briefly.

a) In the solution step, an unnecessarily large volume of solvent is used.

Effect on purity: The purity is not affected.

Effect on recovery: Lower recovery because a large amount of the compound should still be
dissolved in the solution with an unnecessary large volume of solvent.

b) The crystals obtained are washed with cold solvent.

Effect on purity: Higher Purity because the cold solvent removes the impurities from the surface.

Effect on recovery: _____________________________________________________________

c) The crystals referred to in (b) are washed with hot solvent.

Effect on purity: The purity is not affected.

Effect on recovery: Lower recovery because crystals collected would be dissolved

5. Why must hot filtration step be carried out quickly? Why is a fluted filter paper used rather than an
ordinary filter paper cone?

_____________________________________________________________________________

_____________________________________________________________________________

_____________________________________________________________________________.

2. Sublimation of Benzoic Acid

Mass of the benzoic acid sample (g) 0.1192 (A)

Mass of the filter paper (g) 0.6722 g

Mass of the filter paper and the sublimate (g)

Mass of the sublimate (g) (B)

% recovery (B/A x 100) : _______________

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6. What is a sublimate and what is meant by sublimation? How does sublimation and recrystallization
free a substance from impurities?

Sublimate is a chemical product obtained by sublimation. Filtration leaves behind insoluble impurities that
are dissolved in an appropriate solvent in a minimum of near boiling. Cooling without interruption
decreases the solubility of the compound as well as the solubility of impurities. This leads to a saturated
solution that crystallizes excluding the said impurities from the lattice that formed.

3. Sublimation of Caffeine

Mass of crude caffeine (g) 0.0980 g (A)

Mass of the watch glass (g) 38.5957 g

Mass of the watch glass and the sublimate (g) 38.6499 g

Mass of the sublimate (g) 0.0542 g (B)

% recovery (B/A x 100) : 55.31%

4. Melting Point Determination

Temp. When Temp. When Melting point Melting point

Sample melting starts melting complete range range (°C)
(°C) (°C) (°C) (Literature value)

79-81°C
Napthalene crystals

72-74 °C
Crude naphthalene

122°C
Benzoic acid
sublimate

123°C
Crude benzoic acid

178-237 °C
Caffeine sublimate

178°C
Crude caffeine

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7. Before packing into a capillary tube, a solid substance has to be powdered. Why is this done on a
watch glass rather than on a piece of filter paper?

It is done in a watch glass rather than a piece of filter paper because filter paper is usually a poor
material on which to powder a solid sample before introducing it into a capillary melting-point tube
because small particles of paper may end up in the tube along with the sample.

8. Describe the errors which may cause an observed melting point range of a PURE sample to be:

a) higher than the correct melting point

_____________________________________________________________________________

b) broad in range

Too much sample can result in a melting point range that is too wide. This is because extra heat is
required to completely melt the sample. Generally 3-4 mm in the bottom of a capillary tube works
well.
9. What is melting point? Why can it be used as an index of purity?

Melting point is a temperature at which solid and liquid forms of a substance exist in equilibrium.
A substance with higher impurities result to lower melting points than the pure compound.

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