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no bubbles in distillation of phenylacetone under vacuum
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Topic: no bubbles in distillation of phenylacetone under vacuum (Read 3658 times)
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shak22
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no bubbles in distillation of phenylacetone under vacuum
«
on:
December 03, 2012, 03:06:54 AM »
hello,
i have no bubbles in distillation of phenylacetone under vacuum, the heat is about 100c, and the vacuum pump produce around 20 torr.
is that normal? please help me.
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discodermolide
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Re: no bubbles in distillation of phenylacetone under vacuum
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Reply #1 on:
December 03, 2012, 03:11:13 AM »
You mean 1-phenylpropan-2-one? If so it has a BPt. of 214-216°C at normal pressure.
So in your case I would get a better vacuum. Check everything for leaks, 100°C seems a bit high for the bath temp.
But in your case go for a better vacuum first.
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shak22
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Re: no bubbles in distillation of hello, phenylacetone under vacuum
«
Reply #2 on:
December 03, 2012, 03:15:54 AM »
i have a vacuum pump with a vacuum gauge that state that my vacuum is at 20 torr, the temp that phenylacetone should evaporate under such vacuum is around 110-120c.
any other segestion?
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shak22
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Re: no bubbles in distillation of phenylacetone under vacuum
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Reply #3 on:
December 03, 2012, 03:20:04 AM »
in addition,
i have done this at a higher temp and the matirial just went throw the condencer.. as a liquid..
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discodermolide
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Re: no bubbles in distillation of phenylacetone under vacuum
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Reply #4 on:
December 03, 2012, 03:22:23 AM »
To be sure you did put 1-phenylpropan-2-one into the distillation apparatus?
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shak22
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Re: no bubbles in distillation of phenylacetone under vacuum
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Reply #5 on:
December 03, 2012, 03:23:05 AM »
yes
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shak22
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Re: no bubbles in distillation of phenylacetone under vacuum
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Reply #6 on:
December 03, 2012, 03:23:41 AM »
it's basiclly a mixter..
somthing should be boiled...
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discodermolide
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Re: no bubbles in distillation of phenylacetone under vacuum
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Reply #7 on:
December 03, 2012, 03:32:21 AM »
I take it the mixter = mixture?
I would dismantle the distillation apparatus and start again. Make sure all the joints are gas tight.
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shak22
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Re: no bubbles in distillation of phenylacetone under vacuum
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Reply #8 on:
December 03, 2012, 03:36:28 AM »
yes a mixture.
it's the third time i'm trying this...
any segestion?
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shak22
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Re: no bubbles in distillation of phenylacetone under vacuum
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Reply #9 on:
December 03, 2012, 03:38:41 AM »
and i put silicone grease all over the joints..
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discodermolide
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Re: no bubbles in distillation of phenylacetone under vacuum
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Reply #10 on:
December 03, 2012, 03:39:44 AM »
I take it that suggestion = suggestion.
What else is in the mixture?
My suggestion again: I would dismantle the distillation apparatus and start again. Make sure all the joints are gas tight.
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shak22
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Re: no bubbles in distillation of phenylacetone under vacuum
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Reply #11 on:
December 03, 2012, 03:45:28 AM »
some toleune and water - very little because i have disttiled them at normal disttilation
i realy can't figure this out.. i shold create some bubbles right?
thank you by the way!
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discodermolide
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Re: no bubbles in distillation of phenylacetone under vacuum
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Reply #12 on:
December 03, 2012, 04:55:02 AM »
As I said, re-build the distillation apparatus and get a better vacuum.
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no bubbles in distillation of phenylacetone under vacuum