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Experiment 4.freezing Point of An Unknown Sample 2

Experiment

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42 views8 pages

Experiment 4.freezing Point of An Unknown Sample 2

Experiment

Uploaded by

nevaeh.chand2005
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Experiment 4.

Freezing Point on an Unknown Sample

Table of Contents
Experiment 4. Freezing Point on an Unknown Sample.......................................................1
Goal..................................................................................................................................1
Introduction......................................................................................................................1
Procedure.........................................................................................................................5
Laboratory Report 4. Freezing Point on an Unknown Sample............................................6
Data..................................................................................................................................6
Post lab questions............................................................................................................8

Goal
 To learn about three physical states of matter and their properties
 To gain proficiency in constructing a graph and plotting data points.
 To find freezing point of an unknown organic compound from the cooling curve.

Introduction
Every Matter has certain mass and occupies a certain volume. The three physical states
of matter are solid, liquid, and gas. Matter exists in one of these physical states
depending upon its chemical identity, temperature and pressure. Certain obvious
differences among three states of matter are volume, shape, density, compressibility
(volume change due to pressure change), and thermal expansion (volume change due to
temperature change).

The solid and liquid states have many similarities, whereas the gaseous state is
markedly different as shown in the table below:

Property  Solid state Liquid state Gas state


Volume definite definite indefinite
Shape definite indefinite indefinite
Density high high, normally very low
lower than solids
Compressibility small small, normally large
Property  Solid state Liquid state Gas state
more than solids
Thermal expansion very small small moderate
(0.01% per oC) (0.01% per oC) (0.3% per oC)
Energy potential energy >> kinetic energy  potential energy <<
kinetic energy potential energy kinetic energy

A change of state is a process in which a chemical is transformed from physical state to


another physical state. An exothermic change of state is a change of state that releases
heat energy and is accompanied by temperature increase. For example, freezing (liquid 
solid), condensation (gas  liquid) and deposition (gas  solid) are exothermic changes.
An endothermic change of state is a change of state that requires absorption (input) of
heat energy and is accompanied by temperature decrease. For example, melting (solid 
liquid), evaporation (liquid  gas), and sublimation (solid  gas) are exothermic changes.
Identifying an unknown compound is a tedious task which requires measurements of
several physical and chemical properties of the compound. Some important physical
properties that are often utilized by chemists in identifying an organic compound are
color, odor, physical state, melting point, boiling point, density, refractive index, infrared
spectrum, nuclear magnetic spectrum and ultraviolet spectrum. Physical constants are
numerical values measured under standard conditions (temperature, pressure, etc.), which
can be found in CRC Handbook.

Crystalline solids are composed of atoms, ions, or molecules in a highly ordered


geometric pattern (crystal lattice). The atoms, ions or molecules are held in their positions
by electrostatic, dipole and/or London forces. When a pure crystalline solid is heated, the
atoms, ions or molecules vibrate more and more rapidly until at a definite temperature the
thermal mot ion of the particles becomes great enough to overcome the forces of
attraction. Then the atoms, ions or molecules enter a more random and mobile state, the
liquid state. Then melting (solid  liquid) transition occurs.. This temperature is referred
to as the melting point. The freezing point and the melting point of a substance have the
same value, theoretically. Useful information as to the compound's identity and its
purity can often be obtained from its melting point. A solid is said to melt sharply if the
melting point range is 0.5 - 1.0 deg. C. A pure solid will generally melt sharply because
the forces of attraction between its particles are the same. However, the presence of a
foreign particle in a crystal lattice interrupts its uniform structure and the forces of
attraction are weakened. An impure solid melts at a lower temperature and over a wider
range.
Suppose two compounds X and Y have identical melting point of 135 oC each. One can
easily determine whether or not X and Y are the same or two different compounds by
mixing a small amount of X with Y (or vice versa) and finding the melting point of the
mixture (mixture melting point). If X and Y are the same compounds, the mixture
melting point will be 135 oC. If X and Y are two different compounds the mixture
melting point will be much lower than 135 oC and will not be melt sharply.

In this experiment, first you will melt an unknown organic solid in a hot water bath and
then allow the liquid to air cool. During the cooling process, you will record the
temperature every 30 seconds and the reappearance of solid will take place. The data will
then be plotted on a graph paper (titled and well labeled). The plot will show the time
along the horizontal axis {x-axis} and the temperature on the vertical axis {y-axis).
Each point will be circled and a smooth cooling curve connecting or passing through
maximum points will be drawn. An extrapolation of the flat portion of the curve to the
vertical axis will give the value of the freezing point as shown below:
The freezing point thus found can be used to identify you unknown sample by
comparison.
Compound mp or fp (oC)
Benzophenone 49-51
Steric acid 69-70
Vanillin 80-81
Naphthalene 80-82
1-Naphthol 95-96

Paradichlorobenzene 54-56
Biphenyl 69-71
Palmitic Acid 61-64
Procedure
1. Students may work in pairs. No flames are allowed in this experiment. Only
electrical hot plates will be used. Do not touch hot beakers or test tubes. There is
no chemical waste in this experiment. After you finish your work, replace the
test-tube containing the chemical, thermometer, and the copper-wire.

Review the figure given below carefully:

2. Each pair needs only one set up. Set up 400-mL beaker containing about 300
mL water on top an electrical hot plate. Obtain a big test tube containing the
unknown organic solid, a thermometer, and a copper wire stirrer. Clamp this test
tube and immerse in water. Now, start heating. Do not boil the water. After the
entire solid has melted, shut-off the electrical hot plate and unplug the electrical
hot plate. Now, carefully raise the test tube out of the hot water. Begin recording
the temperature every thirty seconds for ten minutes. It is necessary to stir the
liquid using the copper wire stirrer every 10 seconds or so. You will notice that
the temperature readings will drop as the time passes by and the liquid inside the
test tube will turn into a solid. In some cases it may take more than 10 minutes.

3. Plot the temperature vs. time data on the graph paper provided.

4. Replace the test tube.


Laboratory Report 4. Freezing Point on an Unknown Sample

Last Name_____________________________, first name________________


Date of Experiment___________ Instructor’s Initials_______

Data
Your Unknown Sample Number:__________________

Time (min) Temperature (oC) Physical state (solid, liquid or both)


0.0
0.5
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
5.5
6.0
6.5
7.0
7.5
8.0
8.5
9.0
9.5
10.0
Cooling Curve for Unknown #__________ Freezing Point from this graph =________oC

[Y- axis: temperature (1 oC/box), X-axis: time (30 sec/box)].


Last Name__________________________, first_________________date____________

Post lab questions


Show all your work and use proper units and significant figures!

1. What are the applications of finding the melting point of an organic compound?

2. What is the effect of impurity on the melting point value?

3. The freezing point of ethyl alcohol is -117 oC. Express this in oF and K units.

4. Give the names of three exothermic and three endothermic processes.

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