Laboratory Techniques in Organic Chemistry
Laboratory Techniques in Organic Chemistry
4th Edition
ISBN: 9781464134227
Author: Jerry R. Mohrig, David Alberg, Gretchen Hofmeister, Paul F. Schatz, Christina Noring Hammond
Publisher: W. H. Freeman
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Chapter 14, Problem 4Q
Interpretation Introduction

Interpretation:

The reason to seal the capillary tube from the open end for the melting point determination for a compound that sublimes should be stated.

Concept introduction:

For a crystalline substance, the temperature at which the substance changes from solid phase to liquid phase is referred to as melting point. Melting point is directly associated with the presence of intermolecular forces like hydrogen bonding, dipole-dipole interactions. High molecular symmetry, large surface area, polarity is related to high melting temperature.

A pure compound melt at a narrow range and compounds with impurities have broad melting temperature. Melting points are obtained by filling the organic compound into the capillary tube with one sealed end.

Sublimation is a process where a gaseous phase is obtained directly from the solid phase.

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What effect does the presence of impurity have on the melting point?
4. When performing a melting point on a solid compound using a melting point apparatus, two melting point determinations were made. One sample, which was 1 mm in height in the capillary, possessed a melting point of 200.0-200.5°C. The other sample was 25 mm in height. What would you expect the approximate melting point to be for this sample, assuming identical heating rates of 1°/min? (Hint: heat is applied from the bottom of the sample) (Give an actual numerical approximation!) 5. For the same solid compound as the question above, if the 1 mm sample was heated at 60° per minute on a melting point apparatus, what would you expect for an approximate melting point? (note that at this heating rate, the sample will melt rather quickly, but again give an actual numerical approximation)
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Laboratory Techniques in Organic Chemistry

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