DMT-Nexus member
Posts: 167 Joined: 06-Dec-2015 Last visit: 08-Apr-2019
|
So i'm doing FASA on xylene and backwash the acetone back in to the new clean water but i added a little vinegar because i thought it might assist some of the oils or other alkaloids back in to the clean water so I can have purer recycled xyxlene.
Now, when i dip my finger in the xyxlene and it evaps i can smell vinegar even though its only xylene. Also it is still yellow and not see through (slightly cloudy). Any problems re-using this?
I put that xylene back in the extraction vessel and the xyelene clouded up again which makes me think that there is still some FASA in the xylene even tho i backwashed with water? I then mixed the extraction vessel and separated the xylene and what do you know? No alkaloids present...
So why could acetic acid causing my xylene to keep FASA in it? Or why isn't the acetone mixing with the water on backwash?
|
|
|
|
|
DMT-Nexus member
Posts: 385 Joined: 20-Mar-2016 Last visit: 26-Sep-2024
|
Try cleaning your xylene, first with acidic water, then with basic water (ie sodium carbonate dissolved in water) and finally, remove excess water using anhydrous epsom salts (baked dry in oven) then filtering.
|
|
|
DMT-Nexus member
Posts: 167 Joined: 06-Dec-2015 Last visit: 08-Apr-2019
|
ijahdan wrote:Try cleaning your xylene, first with acidic water, then with basic water (ie sodium carbonate dissolved in water) and finally, remove excess water using anhydrous epsom salts (baked dry in oven) then filtering. All of that just to recycle my xylene? should the acetone really be this hard to get out of the xylene?
|
|
|
❤️🔥
Posts: 3648 Joined: 11-Mar-2017 Last visit: 14-Nov-2024 Location: 🌎
|
n0thing wrote:ijahdan wrote:Try cleaning your xylene, first with acidic water, then with basic water (ie sodium carbonate dissolved in water) and finally, remove excess water using anhydrous epsom salts (baked dry in oven) then filtering. All of that just to recycle my xylene? should the acetone really be this hard to get out of the xylene? Yes, as I understand it, acetone partions about 50/50 in the xylene and water layers. So each time you wash xylene it with fresh water you only remove about half of the actone. After 7+ washes you should be close to 99% purity (roughly). See attached for a discussion on the toluene/acetone/water system. Cheers.
|
|
|
DMT-Nexus member
Posts: 385 Joined: 20-Mar-2016 Last visit: 26-Sep-2024
|
Thats interesting about the 50/50 thing. I washed my last batch of post FASA xylene about three times till I couldnt smell acetone. Maybe Ill do another few washes then to be on the safe side. Epsom salts turned it crystal clear but the yellow colour remains. Plant oils?
|
|
|
❤️🔥
Posts: 3648 Joined: 11-Mar-2017 Last visit: 14-Nov-2024 Location: 🌎
|
ijahdan wrote:Thats interesting about the 50/50 thing. I washed my last batch of post FASA xylene about three times till I couldnt smell acetone. Maybe Ill do another few washes then to be on the safe side. Epsom salts turned it crystal clear but the yellow colour remains. Plant oils? Well it's a rough estimate so take it with a grain of salt, best info I could find was with toluene. There must be some ternary system data for xylene/acetone/water somewhere. Yes plant ouils can surely make it yellow. As argued before that should not be an issue and some folks extract with vegetable oil itself.
|
|
|
❤️🔥
Posts: 3648 Joined: 11-Mar-2017 Last visit: 14-Nov-2024 Location: 🌎
|
ijahdan wrote:Thats interesting about the 50/50 thing. I washed my last batch of post FASA xylene about three times till I couldnt smell acetone. Maybe Ill do another few washes then to be on the safe side. Epsom salts turned it crystal clear but the yellow colour remains. Plant oils? Well it's a rough estimate so take it with a grain of salt, best info I could find was with toluene. There should be some ternary system data for xylene/acetone/water somewhere. Yes plant oils can make it yellow. As argued before that should not be an issue and some folks extract with vegetable oil itself.
|
|
|
DMT-Nexus member
Posts: 167 Joined: 06-Dec-2015 Last visit: 08-Apr-2019
|
|
|
|
DMT-Nexus member
Posts: 167 Joined: 06-Dec-2015 Last visit: 08-Apr-2019
|
After many attempts, the acetone doesn't seem to want to move back in to the polar solution. I have a 1/4-1/2 ratio of polar/nonpolar with no effect even on multiple washes. So instead what i was thinking of doing is doing an acid wash with vinegar and keeping the vinegar to see if it has any dmt-acetate in it. But the problem was that the xylene smelled like vinegar so I will have to evap both to see what is what.
I wonder if I just left the xylene out in the open for a week whether the acetone would evaporate off and just leave fumaric acid at the bottom? Would this not be the best way to reuse xylene?
|