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Highly enriched solvent, question.

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Northerner

Northerner

Rising Star
So as an experiment I ran almost half a kilo of phyllodes a/b-stb hybrid style, pulled with 2L of solvent and reduced to 350ml.

That 350ml of solvent I backsalted with 500ml of water.... The dmt actually flocculated when I based it. :p

Then I pulled again with another litre or so of fresh solvent and evapped it down a bit before sending to the freezer.

After I took it out from under the fan the solvent had chilled quite cool through endothermic reaction and in the bottom of the tray the DMT looked like a small amount of milk under the solvent.

Is this normal, (in the given parameters) or have I accidentally pulled some base somehow? This separated milk like substance concerns me as I haven't seen it before. Just highly concentrated DMT or base contamination?
 
pics?

hard to tell from your description but if you are concerned try decanting the clean layer from the milky and then proceeding with the clean and setting the milky aside for later work
 
It's already in the freezer, this happened late last night and I really didn't have any more power to do anything about it.

It wasn't a tremendous amount of milky liquid, looked like maybe 8-10 drops, but quite viscous and wanting to stay as a whole when the tray was tilted.

The other thing that just occurred to me is that is could be water droplets that have precipitated during the fanning and run down into the solvent, but aren't acidic enough to salt the DMT. Any thoughts on this?
 
Northerner said:
Is this normal, (in the given parameters) or have I accidentally pulled some base somehow? This separated milk like substance concerns me as I haven't seen it before. Just highly concentrated DMT or base contamination?
Click to expand...

I see it every time. It happens when I keep solvent under fan for too long and stuff starts crashing out since the solvent is chilled by the fan. I take it as a mark of full saturation.

However, after turning off the fan, the milky substance slowly redissolves. Sometimes the solvent stays milky but it's more homogeneous (the substance doesn't dissolve but spreads through the volume).

I observe chilled solvent getting "milky" with naphtha, heptane and DCM. Not sure about the chemistry/physics behind this. Possibly precipitates dragging some fat droplets and other stuff...
 
Thanks blue.magic. :)

I never bothered with fanning my solvent before, just go for an extended deep freeze and then recycle it.

Will see some crystals briefly chez northerer tonight I think, before the humidity gobbles them.
 
I'm having the same thing
I am doing a small extraction on 25g ACRB and i reused old naphtha. After pulling the solvent turned milky as it cooled to room temp(a small film formed which i discarded) and then i put it in a heat bath to evap some then i had to leave it for 8hrs at room temp before i put it in the freezer for 40 hours and i got that thick white milk stuck at the bottom
I'm planning to redissolve that in a minimal amount of vinegar, base and pull with new naphtha then freeze precipitate.
 

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When you look in the top of the jar Sakka is the white pooling and runny like milk? Or is it blobby like fat?
 
Apparently it's not sticky as i imagined, i just poured it and most of it poured with the naphtha so "runny" and there was some blobs
Guess i have to do a mini ab
 
dmusicaltrancistor said:
ya i have seen that i think it may be fats or something it will dry to a goo which is fine but i think you are looking for crystals
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Yeah goo is good but half of it or more got poured with the naphtha so i have to save that
Here's a pic of what was left in the jar
 

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Rapid cooling of the solvent will result in small crystals. Try a slower cooling process. Insulate your recrystallisation vessel - perhaps in a suitable box - to slow the cooling, and put it in the fridge before it goes in the freezer.
 
Crystals are a dry month anomaly here. :lol:

When I got the tray out of the freezer there was a LOT more of the white milk, except it was now frozen. I have no doubt it is condensation caused by the endothermic reaction. As it defrosted I saw the water melting away and the crystals inside surrendering to the elements and melting in due course.

Ended up with a dish full of clear goo.
 

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So i got 300mg 😁 50/50 crystals/goo, 1.2% which is lower that what i get usually with same bark 1.7%, i guess that was bcz i became impatient and a bit desperate and did just 2 pulls and discarded everything :?:

I agree that the white milk is condensation

My note for another time, never freeze precipitate reused naphtha alwas backsalt it :)
 
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