For the upcoming experiment we are given an unknown which is composed of 2 compo

Question

For the upcoming experiment we are given an unknown which is composed of 2 components and have to seperate them, then purify them. Mine was a liquid with a small amount of solid on the bottom. First I took the liquid portion out and did "Simple Distillation." I was left with liquid which was distilled, and solid in the distillation flask. My solid looked contaminated.

1) Is my liquid purified through simple distillation? Or do I need to purify it more?

2) Is the solid in the distillation flask the same as the small amount found in the original bottle?

3) How should I purify the solid?

4) Any other steps that I'm missing?

Thank you

Explanation / Answer

I will answer each question to the best of my understanding of what you are doing given the information.

Question 1

Your liquid would be purified through distillation. You should, however, check, in case you need to distill it further. If it's a liquid, you ought to be able to check the purity through gas chromatography. If it is the only component in the chromatogram, then the liquid ought to be pure.

Question 2

It's hard to say if the solid in the distillation flask is the same as what's in the original bottle. Most likely yes because the solid might be somewhat soluble in the liquid. When you distill the liquid, some of that solid can precipitate out. You could check by analyzing an IR NMR, or melting point of the solid depending on what instrumentation is available to you.

Question 3

The solid could likely be purified by recrystallization. You'll have to find a good solvent mixture. You want the solid to be insoluble in the cold solvent, but soluble when in hot solvent. There are other criteria as well--the solid shouldn't react with the solvent, for instance. Generally, recrystallization is a good way to purify solids. Column chromatography would be another option.

Question 4

I don't think you're missing any other steps. I would only suggest making sure your solid is completely dry when you try to purify it. Don't want any other compounds laying around. You can check the purity of your solid by taking its melting point or acquiring an NMR spectrum.

Let me know if you've any questions!

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