Prelab Questions Experiment 1
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Avery O’Brien
CHEM 341-76
PRELAB QUESTIONS EXPERIMENT 1 (2.5 points each)
1.
How will the melting point change if the solid sample is impure versus being pure? In
other words, what differences would you expect to see in the melting point for an
impure and a pure compound?
If the solid sample is impure, it will have a lower melting point and a broader range of melting
points than a pure sample of that compound. A pure compound will have a higher melting point
and a narrower range.
2.
When checking the melting point of your impure sample, what temperature should you
set as the starting temperature (the SET temperature) and what should the ramp rate
be? For example, if the sample is believed to melt at 70°C, at what temperature should
you begin to heat the sample? The ramp rate is how fast the sample is heated per
minute. Remember, for your impure sample, you simply want to identify possible
compounds based on a rough estimate of the melting point.
If a sample was believed to melt at 70°C, I would begin to heat the sample within a 20° range,
probably around 55°. I would use a ramp rate of 5-10°C/min initially and then decrease to 1-
2°C/min to try to get more data and provide a better idea of a range of melting points.
3.
Describe the characteristics of a good mixed solvent system for doing a recrystallization.
A good mixed solvent system for doing a recrystallization occurs after all other potential solvents
have been tested and failed. A good example of a of a mixed solvent system uses tiny amounts
of hot ethanol and water to dissolve remaining solids. The crystals can then be separated,
cooled and dried.
4.
Based on the melting point of your impure solid, you look at the given samples and
believe you have compound A. Compound A is recrystallized using a mixed solvent
system of ethanol and water. You add 1 ml of hot ethanol to your sample and it doesn’t
completely dissolve. You continue to add hot ethanol but there isn’t any change. Some
solid remains. What should you do next?
If adding hot ethanol still leaves remaining solid, the next step would be to add hot water to the
solution. This should help force the remaining solid to dissolve because water and ethanol are
miscible and will mix. Then let it cool and pure product should crystalize.
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