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FASA not really precipating out from Xylene! Options
 
Hupecat
#1 Posted : 10/24/2012 12:03:08 AM
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hi.. i did some pulls with Xylene in naphta-used sludged..
Then i Fasad it and left it oveer 48 hours untouched..
but there is still lots of precipate floating in my Xylene-Solution..
How can i siphon the xylene now, without pulling all the fumarate salts out again..
see pix





It just doesnt really precipate..
Any ideas??

 

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Hupecat
#2 Posted : 10/24/2012 6:46:42 PM
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so, this is what i ended up after pulling Xylene out from precipate and dried it i the oven..
You can still see soe Fumarate needles.
Does it look ok, as a Jungle Fumarate??
hasnt bee washed yet, just took out of the oven.

will scrape the glass and try to wash it somehow( which chemical should be taken for that..??)
i want to get it to Freebase-Jugle later.

it was 3 FASA pulls frm a naphta used Slurry with 180 gr MHRB in it..



 
Infundibulum
#3 Posted : 10/26/2012 10:50:18 PM

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Hupecat wrote:
will scrape the glass and try to wash it somehow( which chemical should be taken for that..??)
i want to get it to Freebase-Jugle later

After scraping it out, you can use dihydrogen monoxide to dissolve and recover the fumarates.





Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
Hupecat
#4 Posted : 11/4/2012 10:46:58 AM
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Infundibulum wrote:
Hupecat wrote:
will scrape the glass and try to wash it somehow( which chemical should be taken for that..??)
i want to get it to Freebase-Jugle later

After scraping it out, you can use dihydrogen monoxide to dissolve and recover the fumarates.






Yeah, thx,,
but can you exolain me why this Xylene just stays milky, without showing any precipitation, after 48 h undisturebed??
 
endlessness
#5 Posted : 11/4/2012 11:59:09 AM

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In my experience, it seems FASA/FASI not precipitating is a result of either or a mix of the following possibilities:

1- Water, from condensation or traces in the container or chemicals used, sinks to the bottom and traps at least part of the fumarates in a darker gooey layer (potentially not visible till you pour the solvent off slowly)

2- Some might have precipitated but you dont see with the cloudy container.

3- Solvent not concentrated enough with alkaloids

4- Too much impurities in solvent might affect crystallization, hold alkaloids in solution and make it slower or just not precipitate at all

5- Sometimes it just takes longer, leave for a week or more.


As infundibulum said, you can always wash with water to recover alkaloids plus excess fumaric acid and some other potential impurities, which you can proceed to purify in any number of ways.
 
Hupecat
#6 Posted : 11/4/2012 1:23:08 PM
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Well, i thought about theSodium Carbonate thing, and decided to add a bit of water with SC, which helped quite a lot... will post later..

THx
 
endlessness
#7 Posted : 11/4/2012 1:37:40 PM

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"Helped a lot"? How?

With what did you mix the sodium carb exactly?

If you add sodium carbonate you are raising the pH and making the alkaloids turn into freebase again, and they will move again to the xylene. Sounds like a possible mess
 
wearepeople
#8 Posted : 6/13/2013 1:53:12 AM

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endlessness wrote:
In my experience, it seems FASA/FASI not precipitating is a result of either or a mix of the following possibilities:

1- Water, from condensation or traces in the container or chemicals used, sinks to the bottom and traps at least part of the fumarates in a darker gooey layer (potentially not visible till you pour the solvent off slowly)

2- Some might have precipitated but you dont see with the cloudy container.

3- Solvent not concentrated enough with alkaloids

4- Too much impurities in solvent might affect crystallization, hold alkaloids in solution and make it slower or just not precipitate at all

5- Sometimes it just takes longer, leave for a week or more.



I'm working on an experimental species (5-MEO) and I'm having trouble. It definitely clouded when I added FASA, so thats a good sign. I did 3 pulls of 100 mL for a total of 300 mL of Xylene.

I believe I have a mix of problems 1 and 3.

(Problem 1, because I stuck the jar in the freezer and during a moment of impatience I opened it, then quickly realized that was not a good idea, condensation wise. Problem 3, is pure speculation. The species has no numbers)

How would I troubleshoot this? Is #5 the only way?
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The Day Tripper
#9 Posted : 6/13/2013 6:49:49 PM

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If you accidentally get h2o in your fasa container, i would put it uncapped in a larger airtight container with a wide mouth on a DEHYDRATED epsom salt bed to dry.

Ideally, a pyrex dish, and a large flat seal-able container would work best for surface area reasons, but thats for another day. Non electronic/heat vacuum sealable bags, mgso4 in a permable mesh enclosure (like silica packets), underneath the pyrex dish. That would dry the hydrated solvent real good one would think. Just be careful with electronic, heat, or even mechanical mechanisms in your vac pump. A spark/ignition source can come from anywhere.

put a few oz's of dried epsom salts down, and then place the vessel with your fasa & acetone/fasa & limo/or fasa and xylene in, only sealing the outer jar. Since you want the very dry air to make contact with the hydrated binary solvent with fasa/x np or acetone. Leave it in a dry, dark, and not cold, but not hot place.

Seal the top and leave it overnight, make sure its AIRTIGHT. Remove the inner vessel, cap immediately in a airtight container, and freeze it if its acetone/fasa. IDK if i would do that with limo or xylene, as that might crash out all the fumaric acid too.

You could always bring the inner vessel without breaking the outer vessel seal before bringing it back to room temp (should do anyway to prevent condensation from warmer air/cold liquid), and the excess fumaric acid would dissolve again.

I've never frozen fasa, so i couldn't really say though.
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GreenDMT
#10 Posted : 7/31/2018 1:40:54 PM

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endlessness wrote:
In my experience, it seems FASA/FASI not precipitating is a result of either or a mix of the following possibilities:

1- Water, from condensation or traces in the container or chemicals used, sinks to the bottom and traps at least part of the fumarates in a darker gooey layer (potentially not visible till you pour the solvent off slowly)



As infundibulum said, you can always wash with water to recover alkaloids plus excess fumaric acid and some other potential impurities, which you can proceed to purify in any number of ways.


I think that happened to my friend he now waiting for crystalization but n the bottom is some goo kind of oil. what can he do to recover fumarates or whatsoever, just mix with wate? ther is also FASA in toluene solution, this could migrate to water, he don't know a rout to recover.
 
endlessness
#11 Posted : 7/31/2018 10:31:53 PM

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You can separate the goo and spread it in a dish to dry, then clean up by re-basing and re-fasa, or wash with cold dry acetone, or a number of different ways. As always, dont throw anything away until you're completely finished and happy with final yield, because if something goes wrong or yield is small, you can always go back and recover your alkaloids from some previous step.
 
 
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