meltpnts.

doc

MELTING POINTS
(Zubrick, 12, 86 - 102)
The melting point of a solid is a physical property of great importance in characterizing it.
In many cases it is more useful than a boiling point or other physical property because of its
sensitivity to the presence of impurities. Even a small percent of impurity depresses the melting
point of a solid to an easily observable extent;-- several degrees or more. In addition, a most
convincing proof of the identity of two samples is obtained by a mixed (mixture) melting point. If
the two are identical, no change is observed in the melting point on mixing them. If they are
different, one acts as an impurity on the other, and the melting point of the mixture is altered.
Melting points are routinely taken throughout the laboratory portion of this course, and skill
in performing this operation will be of value to you.
thermometer is supported in a thermometer
PROCEDURE

holder (Z. p.101) so that the thread can be

read for that portion of the thermometer that
is of interest to you.
Your instructor will demonstrate the
proper technique for preparing the sample
and introducing the sample into the capillary
melting point tube (Z. Fig 12.1, p. 88).
A rubber band, or a ring cut from a piece
of burner hose may be used to fasten the
capillary so that the sample is alongside the
thermometer bulb (Z Fig 12.10;. p. 100)
NOTE: When the sample is immersed in the
oil bath, the rubber ring must not come in
contact with the oil.
Your primary objective is to determin-

OIL BATH METHOD

Melting-point oil-baths are located on the

ing the melting RANGE of a sample: ie. to

superstructures of the lab benches. Each is

observe the temperature at which the materi-

a DRY 100 or 150 mL beaker about half-

al (1) BEGINS to melt, and (2) is COM-

filled with clear mineral oil.

The stirrer is

PLETELY melted.

fashioned from 12 gauge copper wire.

BE RECORDED!!

BOTH VALUES MUST

CONTINUOUS STIRRING IS ESSENTIAL!!

Light your burner and adjust the
flame (Z. p. 128 - 9).
To conduct a melting point, a 260 o C

When passing through the melting range,

the temperature of the oil bath must be

raised

If the melting point is unknown, one

sample may be used to get a rough idea of

V-E-R-Y, V-E-R-Y S-L-O-W-L-Y -- about 1

to 2 degrees per minute.

the melting point by heating relatively rapidly.

The usual

A second sample can then be used for a

procedure is to raise the temperature rapidly

more careful determination after the bath

to within about 15 - 20 degrees of the ex-

has

pected melting point, -- then ADJUST THE

BELOW the approximate melting point.

FLAME to slow down the rate to about 1 to 2

degrees per minute.

DO NOT REMOVE

THE FLAME!!

cooled

down to 15-20

de grees

CAUTION!! Always be prepared in case

the oil bath should break while hot.

This

means standing back from the bath and

keeping your hands from underneath the
bath.

NEVER TRY TO COOL A HOT OIL BATH OR THERMOMETER

BY IMMERSING THEM IN COLD WATER!!

MEL-TEMP METHOD
In many laboratories, the Mel-Temp apparatus
is replacing the oil-bath and Thiele-tube methods.
Consult the Zubrick pages (p 90 f) for procedures
for using the Mel-Temp apparatus.
Since time is required for the apparatus to cool
between trials, it may be necessary for two or
three to use the Mel-Temp together.
apparatus

is

able

to

accommodate

The
three

capillaries at once.

COMPLETE YOUR LABORATORY REPORT

FORM AND TURN IT IN
BEFORE YOU LEAVE TODAY!!

01 meltpnts LR.doc

LABORATORY REPORT
Melting Points and Mixed Melting Points
NAME:

Section:

___

Date:_________________

NAME(S) of your partners:______________________________________________________

Melting Points (ranges) of the PURE compounds

Compound Name

M.p.[range] (Obs)

M.p.(lit)

a
b
Melting Points (ranges) of the Mixtures of (a) and (b)
25:75

50:50

75:25

Identification of the Unknown

Melting point (range) of the pure unknown
Melting point (range) of the unknown mixed with a
Melting point (range) of the unknown mixed with b
The Unknown substance is:
(CHECK one of the following options)----->

is a

is b

is neither a nor b

1. Why should the sample be finely powdered and tightly packed when a capillary melting
point determination is to be made?

2. What effect would using too much sample have upon the m.p.?

3. What effect would heating too rapidly have upon the m.p.?

4. Usually is it not wise to use the same sample for a second m.p. determination once it has been
melted. Upon re-melting the second m.p. may be substantially higher or lower. WHY?