A student placed about 1 cm of freshly recrystallized loosely packed solid into a melting-point capillary tube. The student noted that the solid melted 30 degrees lower than expected and the solid seemed to jump/separate in the tube as the temperature increased in the melting point apparatus. When the student measured the melting point the following day with less solid that was more tightly packed, the melting point was at the literature value. Explain what all went wrong with the student's first sample

Principles of Instrumental Analysis
7th Edition
ISBN:9781305577213
Author:Douglas A. Skoog, F. James Holler, Stanley R. Crouch
Publisher:Douglas A. Skoog, F. James Holler, Stanley R. Crouch
Chapter31: Thermal Methods
Section: Chapter Questions
Problem 31.5QAP
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A student placed about 1 cm of freshly recrystallized loosely packed solid into a melting-point capillary tube. The student noted that the solid melted 30 degrees lower than expected and the solid seemed to jump/separate in the tube as the temperature increased in the melting point apparatus. When the student measured the melting point the following day with less solid that was more tightly packed, the melting point was at the literature value. Explain what all went wrong with the student's first sample

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