Curious DXM extraction issue

iamthetalker

This may belong here, or in Psychedelic Drugs, but I have an issue with my current DXM extraction.

I decided to combine the “single-step” A/B that uses NaOH with the Agent Lemon process, since I already had NaOH lying around from another particular extraction. The two processes are really the same, they just use a different basic solution, and the Agent Lemon extraction adds another step.

Anyway, what I did was add an amount of NaOH solution to the syrup as per the single-phase A/B, mixed it up, added an amount of naptha, shook for ~5 minutes, let it separate, drained off the syrup+water layer and decanted the organic naptha layer into another jar. Here I went into the Agent Lemon process; instead of evaporating the naptha overnight (or with a hair dryer), I added an equivalent amount of concentrated lemon juice. It was not pure lemon juice, and had preservatives in it, but that’s what the tek on Dextroverse uses anyway so I figured it wouldn’t be an issue. Again, I shook it up for ~5 minutes to make sure the layers mixed and the freebase DXM would convert to its…citrate? salt, then let it sit to separate.

My problem is, it’s not separating, at least not very well. There are two separate layers, but the top (naptha) layer is very small, and on top of that is a thick (~1in.) layer of froth/bubbles that won’t dissipate. Any idea how I can get that to dissipate/redisolve? (Do I even need to bother?)

All help welcome. Thanks!
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iamthetalker

Here’s a mediocre picture of the mixture. You can see the “3” layers.

http://i55.tinypic.com/2s8h7pl.jpg

amapola

Yeah probably because of all the crap in the lemon juice giving strength to the bubbles’ exterior. Usually they would slowly sink back down into the liquid but there is naptha blocking their path. A simple straight forward acid would have been better.

As for what to do now hmmm I dunno. What about freeze distillation. Toss it in the freezer for a couple hours then (still in the freezer) strain the ice out with a chilled coffee filter?

Simpler might be to try pour in some water breaking up the bubbles or scoop the bubbles up add to water and then pour back in.

iamthetalker

As you say, they actually are sinking back in, albeit VERY slowly. It’s gone from an inch to maybe a third of an inch. I’m considering just letting it sit longer (overnight?) to finish separating.

It sounds like the bubbles are lemon stuff and/or good stuff, is that right? If so, I’m glad I didn’t just decant as-is. Patience pays! If the waiting game doesn’t work, however, I like the sound of the freeze distillation. I know from my experience with DMT extractions (er, reading about them *cough*) that the naptha won’t freeze so if the lemon juice does it should be the perfect way to separate the layers, though I’m a little concerned about the jar cracking or something when the lemon juice freezes.

Actually…if it worked out that way, wouldn’t I end up with: layer of frozen lemon bubbles (top), liquid naptha (middle), frozen juice (bottom)? Then how do I get the naptha outta there? 😕

Scooping the bubbles would be difficult at best; it’s a large jar, and my spoons are small. 😡

Thanks for the ideas! Next time I’ll pick up some citric acid. I just decided to go with what I had tonight.

amapola

As you say, they actually are sinking back in, albeit VERY slowly. It’s gone from an inch to maybe a third of an inch. I’m considering just letting it sit longer (overnight?) to finish separating.
Super! Definitely just leave it then.

It sounds like the bubbles are lemon stuff and/or good stuff, is that right?
Bubbles are probably lemon juice. It’s mostly air of course but the foam was multiple times the volume of your liquid so worthwhile to not discard.

Actually…if it worked out that way, wouldn’t I end up with: layer of frozen lemon bubbles (top), liquid naptha (middle), frozen juice (bottom)? Then how do I get the naptha outta there?
Yeah but you could crunch it all up with a chilled fork or something once frozen and just pour the liquid off or use a chilled filter to collect the solid ice crystals.

iamthetalker

Ah, gotcha. I’ll do that if need be, but most of the bubbles are gone now so I’ll come back to it in the morning (or afternoon as the case may be XD). Thanks for the help!

iamthetalker

Now there are two distinct layers, though neither of them is clear like I would expect the naptha to be. Looks like maybe the naptha pulled something out of the lemon juice. Either way, I should still be able to decant the bottom layer and have what I want, neh?