Practical issue with limonene tek

[AMPAR]

I don't come to the site very often so this has probably been discussed at some point and all I need is someone to point me in the right direction hopefully.

I'm using limonene for an extraction and I've noticed that the extract, free base, whatever the proper term is, is floating right next to the lye layer. This is problem for me since my intention is to use a baster to remove the limonene rather than a separatory funnel. I think I have one but finding it could be problem and last time I got pretty twitchy trying to use it. A baster is more my speed.

Are there any tricks I should know for avoiding getting lye in my peanut butter? Yes, be careful. The problem there is that the suction from the baster is very likely to penetrate into the next layer unless I'm extremely careful.

So should I take some lye with the limonene and try to mix in another food grade solvent and THEN do the separation? In that case overshooting from one solvent layer to the other wouldn't be a problem, assuming that the extract has a preference for solvents. That's really the only other thing I can think of other than the sep funnel.

Thanks for any help.

 

[DreaMTripper]

I'm not sure you've used enough Limo as the freebase is very soluble in limo so it's either an emulsion and or oils from the plant or the limo is supersaturated.

 

[AMPAR]

That's the thing. There is a very thick layer of limonene and the extract is in a very thin layer right near the boundary. Initially I thought the same thing so I added more but all it did was make the limonene layer thicker.

 

[downwardsfromzero]

That is surely a layer of emulsion!

A full description of what you have done and the materials you have used will aid the diagnostic.

Strongly basic or salt saturated aqueous solutions, isopropanol and limonene form three phases when mixed (four if the salt starts precipitating). Was any IPA involved?

 

[AMPAR]

I'm reluctant to say precisely what I'm doing. Call me paranoid I suppose. But I guess hypothetically let's assume it's a popular unnamed root bark.

I think I understand what an emulsion is but I'm not sure I got the rest of that and what is IPA?

 

[downwardsfromzero]

I'm reluctant to say precisely what I'm doing. Call me paranoid I suppose. But I guess hypothetically let's assume it's a popular unnamed root bark.

I think I understand what an emulsion is but I'm not sure I got the rest of that and what is IPA?

IPA = isopropyl alcohol.

An emulsion = like mayonnaise, margarine or well-shaken salad dressing.

You can tell us how you processed your unnamed root bark, I'm sure your oak root skin cream is perfectly legal

"Hopefully all the unwanted alkaloids will have migrated into the limonene, leaving the emulsion layer safe for use as a skin cream." Aw, come on this is silly. If you're that paranoid, why are you posting here?

e.g.: Tea made with [bark] plus acid [citric? vinegar? lemon juice?] Citric acid tends to cause emulsions.

Base added [lye/caustic soda/sodium hydroxide? presumably.]

Limonene added [rolled/stirred/shaken/more or less vigorously] vigourous shaking tends to cause emulsions.

Layer between limonene and base soup resembles [mayonnaise/mucus/blood/spaghetti/etc.]?

What could be simpler?

Questions about emulsions have been asked before. There are a variety of ways of breaking emulsions such as adding salt, heating in a hot water bath, vacuum filtration or applying vibration. Similar experiences to yours can surely be found by searching around the forum.

Limonene can be a bit of a pain sometimes...

 

[AMPAR]

Thanks for the information. I appreciate it. No IPA by the way.

The tek I was following I believe was designed for mhrb and skipped the tea/acid part so maybe that's the problem. Although I don't see why it would be.

I'm worried about overshooting and getting lye because I was sloppy and didn't use a good hydroxide source. I figured since all of the impurities were water soluble it wouldn't be an issue but now it is.

So if I manage to extract the emulsion, can I go to the fumaric acid step or should I just try to resupply and start over?

 

[downwardsfromzero]

Thanks for the information. I appreciate it. No IPA by the way.

The tek I was following I believe was designed for mhrb

So you adapted Jorkest's method by using - I'm guessing - ACRB? Jorkest suggests this tek can be used for other plant material and I see no intrinsic problem with this.

skipped the tea/acid part so maybe that's the problem. Although I don't see why it would be.

The tea part is the basic mimosa sludge that gets extracted by the limonene, the acid part is where the crude product gets extracted from the limonene. Are you sure you've understood the instructions?

I'm worried about overshooting and getting lye

Now, this has left me struggling to understand what you mean. If you didn't use lye (which is the same as sodium hydroxide), what did you use? This is the reason you were asked to describe exactly what you did in the first place.

because I was sloppy and didn't use a good hydroxide source.

What did you use? Ammonia? Tri-rubidium phosphate?

I figured since all of the impurities were water soluble it wouldn't be an issue but now it is.

Are you sure you've understood the instructions? Anyhow, how big is the emulsion layer relative to the limonene layer? It's quite commonplace for a thin layer of emulsion to remain with limonene. Also, did you read the bit that says:

add a few more grams of lye right into the jug. This should break any emulsions.

or is that a problem because you don't have any lye?

It sounds like this thread would help you a bit.

So if I manage to extract the emulsion, can I go to the fumaric acid step or should I just try to resupply and start over?

If your emulsion is only a thin layer, then it shouldn't be a problem. Anyhow, it's the top layer - the limonene - that you want (it should be slightly yellowish by now) so it would be best to stop fretting about the emulsion and get on with the fumaric acid business.

If you still think the emulsion layer is a problem perhaps you could post a photo of your extraction.

As you still haven't said what materials you've used (other than limonene) and what procedure you actually followed it's hard to suggest anything else!

 

[AMPAR]

I used standard drano but I have some pure sodium hydroxide.

I'm going to re-read the tek and try a few things like adding some more NaOH and then come back.

I probably won't be any more forthcoming about my objectives but I appreciate all of the help so far. I know I'm making things more difficult but thank you for hanging with me.

I might be a few days but I'll try to get back to this.

 

[downwardsfromzero]

(Hope you caught the edits, for some reason my typing reverted to a previous version and I had to fix it.)

 

[downwardsfromzero]

I'm not bothered about your objectives, but make sure your Drano doesn't contain anything except >98% sodium hydroxide, i.e. no aluminium powder and no sodium nitrate.

Bear in mind that emulsions are exacerbated by fine particulates!

 

[Jagube]

Can one use ammonia as base in this tek?

Also, I have a drain cleaner that (according to the stated ingredients, not the detailed sheet) is 10% sodium hydroxide and 90% sodium carbonate. Can this be used?