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Topic: Recrystallization - Trial and Error?  (Read 3910 times)

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Offline ovenmits

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Recrystallization - Trial and Error?
« on: July 31, 2010, 01:51:15 AM »
I'm creating a macrocycle coordination complex that appears to be soluble in water.  I'm sure there are other salts forming in solution that are also soluble in water.  Due to my lack of experience with purification of inorganic compounds, how would i go about 'recrystalizing?'

 Is it as simple as drying down the products, dissolving them in various solvents, analyzing them by some means (NMR, MS, ect), and just collecting that sample? Or is there a less involved way to do this?

Thank you very much for your input


Offline ovenmits

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Re: Recrystallization - Trial and Error?
« Reply #1 on: July 31, 2010, 02:03:16 AM »
I've also wondered this...

When forming a complex with a symmetric chelator, say cyclam, with a metal, does the polarity of the molecule increase or decrease, relative to the polarity of the individual chelator?

Figured i'd get these two questions out of the way off the bat since i just found this site :]

Offline MasterLardo

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Re: Recrystallization - Trial and Error?
« Reply #2 on: August 07, 2010, 12:52:35 AM »
In your case, it seems like your complex would be the least soluble substance in water, seeing as how your byproducts are all salts. In that case you could try saturating your product mixture in water and then cooling it down (without freezing it), and wait and see if anything recrystallizes or precipitates.

Do you know what other solvents your complex is soluble in? If not, you could try doing successive washes of your product mixture, starting with the least polar. Generally the order is hexanes, ether, toluene, and THF. The goal is to have your complex appear in one of the less polar solvent solutions and have all the salts be in the more polar solvent solutions.


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