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Sep. funnel help

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shr00m

Rising Star
So if one where to want to incorporate a seperatory funnel how would they factor in the volume of liguid being larger than that of which the funnel can hold? Would someone just do multiple seperations? Or is there a way to reduce the volume? Also with a seperatory funnel filtration of the bark is a must, right? Also when putting the liquid into the funnel wiuld you run a risk of making a large emulsion layer? Also any one have a supplier of glassware in the US that they suggest?
thanks,
Steve
 
Well reducing the volume would work just try to minimilize (fuck i cant spell that word) heat. Definatly filter the bark before adding to the funnel otherwise its going to plug it up in a way thats not easy to unplug. You can also do multiple separations with small volumes etc. Its really up to you. When pouring the two phases together (organic and aqeuous) do it slow and when you shake and mix the two do it slow and gently, thats how you avoid the tough emulsions. If you get really bad emulsions time will resolve them (sometimes its way too much time) so you can just pour more (at the right pH) water or more organic solvent to break them up after collecting the nicely separated layers. is this mystery person doing acid base?
 
The sep funnel would be useful during a defatting stage (where you mix a non-polar solvent like naptha with an acidic aqueous crude solution which contains organic material + spice), and also during the final extraction of basic solution into non-polar solvent. Doing extractions in a sep funnel, you want to shake fairly vigorously to get a decent yield. Occasionally, you get emulsions. These can be cleared up by adding a bit of saturated brine (saturate some water with table salt). Briny solutions dont form emulsions as easily. A final brine wash on your non-polar solvent that contains the free base spice is also a great way to improve crystallization quality and yield, as it removes dissolved water from the solvent.
 
rbwoodward said:
The sep funnel would be useful during a defatting stage (where you mix a non-polar solvent like naptha with an acidic aqueous crude solution which contains organic material + spice), and also during the final extraction of basic solution into non-polar solvent. Doing extractions in a sep funnel, you want to shake fairly vigorously to get a decent yield. Occasionally, you get emulsions. These can be cleared up by adding a bit of saturated brine (saturate some water with table salt). Briny solutions dont form emulsions as easily. A final brine wash on your non-polar solvent that contains the free base spice is also a great way to improve crystallization quality and yield, as it removes dissolved water from the solvent.

I'll second that.

In a dream, a friend's cat found salt to be a great emulsion buster: a bit cheaper than lye, less suspicion arousing to buy, and doesn't alter pH.

Is table salt OK? Or should one just use the non-iodized stuff?
 
non iodized would be best - im pretty sure that Kosher salt from the store is non-iodized. The main reason being that Iodine could potentially invoke various reactions. I doubt there is anything with DMT that iodine would do, but with various alkaloids in the mix, who really knows. Might as well go kosher right? :)
 
Ive never used NaOH to disrupt emulsions. In fact, with certain solvents, high levels of NaOH might actually help emulsions to form. The emulsions seen when performing a separation such as the ones we might be discussing are usually caused by the solvent and molecule having affinities with the aqueous layer. Its sort of like a confusion, where the solvent and molecule cant decide where to go. By putting NaCl into the water layer, it makes the osmotic pressure favor the water (that is dissolved in the np solvent) to move from the np solvent back into the aqueous layer. This is also why it is a good idea to do a final "drying wash" of your freebase (which is dissolved in whatever np solvent) with a saturated brine solution. It gets all the water out, helping crystallization and purity.
 
Can't think of a good way to reduce the volume. Evaporation would take forever, and I don't think you want the freebase hanging around in the solution that long. Plus pH would increase as the volume decreased.

Applying heat would be risky. The DMT is in freebase form so has low melting and boiling points.
 
Attention All Shipping said:
karma1485 said:
or why not use a Siphon 😉

Isn't that just an aquarium siphon - won't the naphta degrade it and carry bits of plastic/polyethylene/whatever into your spice?
I've thought of using a siphon but haven't seen any affordable ones that look like standing up to naphta, et al.

It's a petrol/gas syphon isn't it? well, looks just like one I saw in the car parts section of a shop the other day... If you buy it from the car shop it should be fine.
 
Much easier just to pour your mixture of polar and non-polar solvent into a tall glass container, like a jar, and use a turkey baster or some other such device just to remove the aq layer from the bottom. Just expunge the air, put the baster in the bottom, suck in the water, take the baster out and repeat...

I do this sometimes on a much smaller scale using a vial, and a pasteur pipette prior to taking a crude nmr etc.
 
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