DXM extraction issue (not answered in other threads)

[iamthetalker]

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!

 

[Solipsis]

What is your equipment available for separation? Can you decant only? Or do you have (makeshift) pipettes, turkey basters.... any of these sorts of things?

Foam like this is often a product of proteins, best thing to do with that usually is scoop it off. As an illustration: What my father made for his saltwater aquarium is a bubbler that bubbles air into a bottomless soda bottle. That creates a lot of scummy foam from the proteins. It rises up and comes out of the open top of the soda bottle ready to throw away. One solution you might have is to get creative and try to make even more foam, then throwing it away. It's possible that a little DXM will be in it but I'd think only traces.

At this stage it looks like it doesn't matter in what form (salt or freebase) the DXM is since it's all shitty to separate. But the pH should be so that most of the DXM is indeed protonated, it would be the hydrocitrate but in solution there simply isn't a salt formed yet. Have you checked the pH? Let's assume that you did that correctly. The DXM should be in the bottom layer, the aqueous (watery) layer if its protonated.

You need some way to suck out the bottom layer, like with a pipette. Many use a turkey baster. Personally Ive got lab gear (the way to go is a separatory funnel, but you need to put in a little effort to get one). So stick it in till the bottom and suck the watery layer out and put it in another container. Make sure none of the naphtha comes along. At the end you can add a little water, mix and repeat. Do that two times to get the last bit out. That is a lot better than trying meticulously to find a little drop with a turkey baster. It's a pain in the ass to evaporate water though.

Of course the lemon juice materials are impurities so you cannot weigh the resulting residu as if it was pure DXM. You have to calculate how much you started with and apply that to your end result weight.

Hopefully this info helps you?

Frankly, I don't understand the point of the lemon tek at least not doing it like this. I would rather extract and evaporate a naphtha layer and be 10 times happier than doing it with a watery layer.
What I would do is evaporate in the naphtha stage and yield freebase DXM, then measure a volume of water with a pinch of muriatic acid added, at least enough to dissolve all the freebase DXM. Then neutralize to pH 7 with lye and you've got a drinkable solution. If you MUST have powder or crystal for some reason, still do the same and evaporate it to yield DXM HCl.

Oh by the way I see that on dextroverse they use ziplok bags to create makeshift separatory funnels by pinching a tiny hole in the bottom...
So, I guess it can work, if you manage to get some foam scooped out, maybe add a little salt. Salt is sometimes used in chemistry to bind to random gunk as a sort of basic chelation, it might help with the foam. Of course expect your end product to have more mass and be extra salty.

 

[iamthetalker]

Thanks for the advice. I was working on this late, so I ended up leaving it to sit overnight and the foam eventually settled out. (The protein thing is new information, good to know.) 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? I am in fact using the ziploc method (though I also have a baster and pipettes). I would LOVE to have a true separatory funnel, but gotta save up for it at the moment.

Anyway, I went with the Agent Lemon process because I live in an apartment and was frankly concerned about dust and gunk getting in the dish if I left it on the balcony overnight to evaporate. This leaves us a usable product my lady and I can just down tonight. Next time I would use a true citric acid solution or something. I'm not going for crystals, at least not at this point. Maybe in the future.

 

[Solipsis]

Alright then fair enough. But my point still stands that lemon juice contains plant compounds that I wouldn't want. Micro pulp you might say, anyway I would find even vinegar superior because at least that is a pure compound (well, an aqueous solution / dilution to be precise). I guess if your layers settle you can just carry on as planned but to prevent such things in the future I'd try not to use truly organic materials (here meaning natural, not carbon-based).
Ideally I would use strong acids like muriatic acid, not citric acid. Vinegar is somewhere in the middle but surely good enough I guess.

Whatever you do, if you measure your liquid volumes you should always end up with a watery DXM solution of known concentration. No need to evaporate. Just calculate your dose as if it were syrup, only without the additives / other active ingredients.

Do you have any more questions?

 

[iamthetalker]

I didn't even think about the 5% white vinegar I have. Though I imagine a mixture with that wouldn't taste too hot, even mixed with something... Muriatic acid is diluted hydrochloric acid, isn't it? Is that safe to ingest? Granted HCl's what's in our stomachs, but it seems a little harsh on the esophagus.