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Author: Subject: first dean stark.
arkoma
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[*] posted on 18-12-2020 at 16:29
first dean stark.


Getting a trip phasic liquid in my receiver. Water, "dirty toluene"?, Clean top later?

IMG_20201218_155931_979.jpg - 391kB

IMG_20201218_182637_928.jpg - 399kB

Top picture my makeshift setup. Clausen just in their to give me more reach.

[Edited on 12-19-2020 by arkoma]




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j_sum1
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[*] posted on 18-12-2020 at 17:27


That's one hell of a way to use a Claisen adapter.
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arkoma
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[*] posted on 18-12-2020 at 18:14


it works!! I've gotten pretty creative with my kit over the years.




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karlos³
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[*] posted on 18-12-2020 at 21:57


Agreed, thats pretty creative and looks really adventurous.
But hey as long as it works?

Did you write "its not a meth lab" on the whiteboard in the background? :D
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arkoma
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[*] posted on 18-12-2020 at 23:39


Very astute observation! It's not a meth lab. Any "meth cooks" I ever knew were working with coffeepots, duct tape, garden hose and kitty litter.

They certainly don't have a Corning PC-351!

This Dean-Stark all of a sudden makes sense to me now of how its yanks the water, after sitting here and watching it. Running Dougs Lab procedure for p-toluenesulphonic acid. another 45 minutes of reflux.....hopefully. Still getting some water coming over.




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RustyShackleford
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[*] posted on 19-12-2020 at 11:10


I used the setup here on the right for the same reaction. It worked and quite well, but it was some hassle getting the temperature right so it was nicely flowing through the side arm and not bubbling and stuff.

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[*] posted on 19-12-2020 at 12:07


Well, I've got a yield. Working up now.



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[*] posted on 25-12-2020 at 11:53


Damn, that's genius! lol. I was tempted to buy a DS apparatus, but I think your setup may suffice for my setup, haha.

Quote: Originally posted by j_sum1  
That's one hell of a way to use a Claisen adapter.

I didn't even notice that was there, lol. I thought it was just a short straight glass piece. But it looks closed off.
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Fyndium
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[*] posted on 27-12-2020 at 06:41


Well, that trap at least has decent volume for larger extractions.

It's funny how one can build up pretty much any kind of apparatus imaginable with all the glass parts there are. :D
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