EXPERIMENT

Melting Points
LABORATORY REPORT

Report Prepared By: Katelin McGory

Lab Partners (Group #2): Bryanna, Lane, Debbie
Instructor: Shabree Knick
CHM 211 LAB, SECTION 002
Date of Experiment: January 19, 2012

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PURPOSE:

Students will gain an understanding of melting point analysis and be able to use it as a

method of identifying an unknown compound. The technique of melting point determination will
be explored and students will be able to apply this technique to analyze the purity of an unknown
compound. Through the measurement of mixed melting points, students will be able to verify the
identity of this unknown compound.

PROCEDURE:

Students determined the purity and identity of an unknown compound using the

technique of melting point determination and measurement of mixed melting points. The
following materials were used throughout Experiment 1; 5 one-open-end capillary tubes, 1 MELTEMP apparatus, 3 mortar and pestles, and 1 piece of long tubing. The one-open-end capillary
tubes were used to hold both the known and unknown substances being melted, the MEL-TEMP
apparatus was used to heat, at a specific rate, and measure the melting points of both the known
and unknown compounds, the mortar and pestle were used to finely grind all compounds, and the
tubing was used to pack the substance into the capillary tubes. The following chemicals were
used in Experiment 1: unknown compound (compound from vial #12), benzophenone, maleic
anhydride, and palmitic acid.

Students began Experiment 1 by choosing an unknown solid compound from a provided

selection of unknown substances. The following figure shows all possible unknown compounds,
their structures, and their handbook melting points.

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Possible unknown compounds and their melting points:

Figure 1: Knick, S. from Ivett, G.; Warner, K. Laboratory Manual TTC for CHM 211. Department of Physical Sciences. 2011, 13-16.

The unknown compound that was selected to be used throughout the experiment was taken from
vial #12. After obtaining a small sample of the unknown compound, students finely ground
enough of this compound to fill two of the one-open-end capillary tubes to a height of
approximately 1 mm. Students then packed the compound into the capillary tubes by rapping the
closed ends of the tubes on the lab table and by dropping the tubes down piping. Using the
MEL-TEMP apparatus, the unknown compounds melting point range was experimentally
determined. A quick trial run in which the rheostat was set to 8.5 C per minute was completed to
provide a fast estimation of the unknown compounds melting point as well as to quickly
increase temperature. Students allowed the MEL-TEMP apparatus to cool to approximately
15 C below the quick melting point and then completed a slow run in which the temperature
increased at a rate of 2.5 C per minute. The slow run provided an accurate or true melting point

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(range) for the unknown compound. This was due to the fact that the slow heating used allowed
equilibration between the thermometer and the sample. Students then selected three known
compounds, all having handbook melting point temperatures similar to the unknown compounds
experimental melting point, from the compounds shown in Figure 1. Students repeated the
process used above to finely grind the known compounds in order to prepare three different
mixtures containing 1:1 proportions of the unknown compound and one of the known
compounds. Three capillary tubes were filled and packed in the same manner as above. Mixed
melting points for the three mixtures, measured using the MEL-TEMP apparatus, were then
performed in an attempt to identify the unknown compound. If no melting point depression
occurred, the mixture was pure and the unknown compound was identified. If melting point
depression occurred the mixture was impure and contained more than one compound.

DATA:
Table 1: Unknown compound vial # and observations.
UNKNOWN COMPOUND VIAL #

PHYSICAL OBSERVATIONS OF
UNKNOWN COMPOUND

12

white, powdery, solid substance

Table 2: Unknown compounds experimentally determined melting point. A fast heating

provided a rough melting point and a slow heating established the compounds true range.
HEATING SPEED

HEATING RATE
DEGREE(C ) INCREASE PER MINUTE

UNKNOWN COMPOUND
MELTING POINT (mp) C

Fast Heating

8.5 C / minute

48.0 C

Slow Heating

2.5 C / minute

60.9 - 63.1 C

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Table 3: Three known compounds selected based on how similar their handbook melting points
were to the unknown compounds experimentally determined melting point.
SELECTED KNOWN COMPOUNDS

HANDBOOK MELTING POINT (mp) C

benzophenone

48 - 49 C

maleic anhydride

54 - 56 C

palmitic acid

61 - 64 C

Table 4: The composition of the three mixed melting point mixtures, the heating rate (C per
minute) used to reach the melting point for each of these three mixtures, and the experimentally
determined mixed melting points (ranges).
MIXTURE
#

MIXED MELTING POINT

MIXTURE
COMPOSITION
Vial #12 UNKNOWN COMPOUND +
SELECTED KNOWN COMPOUND
(1:1 proportions)

HEATING
RATE
DEGREE (C)
INCREASE
PER MINUTE

MIXED
MELTING
POINT
(mp) C

OBSERVATIONS:
mp DEPRESSION
or IDENTICAL mp

unknown compound +
benzophenone

2.5 C /
minute

43.8 - 54.4
C

DEPRESSION

unknown compound + maleic

anhydride

2.5 C /
minute

51.6 - 60.3
C

DEPRESSION

unknown compound + palmitic

acid

2.5 C /
minute

61.4 - 63.2
C

IDENTICAL
(approximately)

NOTE: If melting point depression occurred during a the mixed melting point, meaning that the mp

temperature was lower than the unknown compounds experimentally determined melting point,

DEPRESSION was recorded in observations. If the mixed melting point was identical

(approximately) to the unknown compounds experimentally determined melting point,

IDENTICAL was recorded in observations.

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RESULTS:
Sample Calculation:

RANGE (of a set of data) = HIGHEST VALUE - LOWEST VALUE

Example: Unknown compounds melting point range = 63.1 C - 60.9 C = 2.2 C

Table 5: The unknown compounds melting point range and the assessment of the unknown
compounds purity based on this sharp melting point range.
mp RANGE

PURITY OF UNKNOWN COMPOUND

For the unknown compounds measured melting point.

2.2 C

PURE

Table 6: The melting point range for each mixed melting point mixture and the estimated
identity of the vial #12 unknown compound.
MIXTURE #

mp RANGE

IDENTITY (estimation)
of UNKNOWN COMPOUND

For the 3 measured mixed

melting points.
1

10.6 C

NOT benzophenone

8.7 C

NOT maleic anhydride

1.8 C

palmitic acid

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CONCLUSION:

Students met the objective of Experiment 1 by accurately using the technique of melting

point determination to analyze vial #12 unknown compounds purity and by performing mixed
melting points to identify this unknown compound. Recorded data produced accurate results,
thus allowing students to draw conclusions in regard to the unknown compounds purity and
identity. Using the MEL-TEMP apparatus, students determined the purity of the vial #12
unknown compound by performing a fast estimation run and then a slow run. First, a fast heating
rate of 8.5 C per minute was used to estimate the unknown compounds melting point as 48 C.
Second, a slow heating rate of 2.5 C per minute was then used to accurately measure the
unknown compounds true melting point (range). The slow heating rate ensured accurate
measurement because it allowed equilibration between the thermometer and unknown compound
being heated. Students found the melting point (range) of the unknown compound to be 60.9 63.1 C and concluded that the vial #12 unknown compound was a pure substance. This
conclusion was made because the range was sharp, 2.2 C, a characteristic of pure compounds.
Organic compounds that are highly pure will melt at the published melting point range. This
range is sharp, usually 1- 2 C. Compounds that are impure exhibit melting point depression and
therefore melt below the published melting point temperature. Impure compounds also melt over
a broadened, large temperature range. Because palmitic acids published melting point range is
61 - 64 C, the vial #12 unknown compounds identity was estimated to be that of palmitic acid.
Taking into account typical calibration errors present in laboratory thermometers, the unknown
compounds melting point range of 60.9 - 63.1 C was approximately identical to palmitic acids
published melting point range of 61 - 64 C. This identification was verified by performing
mixed melting points with the following three known compounds: benzophenone, maleic

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anhydride, and palmitic acid. Melting point is a colligative property, meaning the more
contaminant added to a pure substance the more the melting point of this pure substance will be
depressed or lowered. Therefore, when melting point depression occurred, the known compound
being used was eliminated from the could be identity of the unknown compound. Mixture 1 (a
1:1 proportion of vial #12 unknown compound and benzophenone) and mixture 2 (a 1:1
proportion of vial #12 unknown compound and maleic anhydride) both had depressed melting
points. Benzophenone and maleic anhydride were then both eliminated from the possible
identities of the unknown compound. Melting point depression did not occur in mixture 3 ( a 1:1
proportion of palmitic acid and vial #12 unknown compound). Mixture 3s melting point (range)
was 61.4 - 63.2 C, while vial #12 unknown compounds experimental melting point (range) was
60.9 - 63.1 C. Melting began in the unknown compound at a temperature of 60.9 C and in
mixture 3 at a temperature of 61.4 C. Therefore, mixture 3 began melting at a temperature
0.5 C higher than the unknown compounds experimentally determined beginning melting
point temperature. Melting ceased in the unknown compound at a temperature of 63.1 C and in
mixture 3 at a temperature of 63.1 C. Therefore, mixture 3 ceased melting at a temperature
0.1 C higher than the unknown compound. Because students did not know the calibration of the
thermometer in the MEL-TEMP apparatus or that of the device itself, slight temperature
variances of 1 -2 C were be attributed to device error. Excluding the slight temperature
variances stated above, vial #12 unknown compounds experimental melting point range and
mixture 3s melting point range were identical. Students concluded that mixture 3 was pure and
entirely composed of palmitic acid. This conclusion verified the identity of vial #12 unknown
compound as pure palmitic acid. All in all, students met the objectives of Experiment 1 and
produced accurate results.

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References
Ivett, G.; Warner, K. Laboratory Manual TTC for CHM 211. Department of Physical Sciences.
2011, 13-19.

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