Introduction, & Questions on D-Limonene + Lye

[teckner]

So this isn't my first account here. I had an account with <50 posts a few months ago, but the username was something unrelated to me in any way, and I wasn't able to remember it now that my interest in spice has been rekindled. This account, of course, is also something completely unrelated to me in any way, but I've written down the credentials this time.

Anyway, about me. I saw the "banned TED talk" nearly a year ago. I thought it was brilliant, and I really appreciated the point of view about the western world needing spiritual medicine. I looked more into spice, and read Shulgin's perspective on it as well as other reports, and thought it sounded amazing. I got 200g of acacia root bark, and attempted to do an A/B extraction on 50g, and failed miserably. A few weeks later, I used another 50g and did an STB extraction using bestine as the solvent, and it worked!

Except that I probably ended up with a grand total of 5-20mg of product, but thought it was more like a gram, so I kept trying to use it and get virtually no results. Life went on and I ended up putting the last 100g of bark away. Recently, I've been drawn to the spice again for whatever strange cosmic reason. I attempted to buy some more bestine, and found out that it no longer is sold ANYWHERE in my area.

So I went out and got some D-Limonene, and decided to re-use the lye I got (the container was a ridiculous size), and combined the first part of this tek and the end part of this tek, but I didn't bother to read the part of the Q21Q21's tek that said "THIS TEK WILL NOT WORK WITH LYE, IT IS ONLY MADE FOR LIME."

I went all the way up to the part where you mix the vinegar with the D-Limonene (after mixing the solvent and the lye root bark solution for quite a while) and separated the solvent from the milky solution at the bottom, and attempted to heat it in a spoon as according to Q21Q21. I tested the blackish(?) substance that resulted on the spoon, and it didn't seem to react with my reagent test. Any suggestions anyone? And of course, leave a message if this isn't clear enough, I've spent the entire day on this extraction and I'm quite tired.

 

[The Day Tripper]

IF all else fails, take your basic sludge, and dry it with annhydrous epsom salts, and patience. No heat.

Pull with an alcohol to evaporate to an oil. If it there is water in whatever alcohol you use its ok, just try and get the driest one you can find. Isopropyl, acetone, ethanol, etc. Be safe and informed though when working with dry alcohols, very flammable.

Pull from the oil with a NP like naptha or bestine if you want to freeze x. Pull with limonene if you want to salt out with fasa, fasi, or fasw. Research if you don't understand those acronyms.

The point being, is to reduce the extraction mass to a small an amount as possible, so things are easier. You dont need the bark, lye or lime. Just the freebase oil you will get when its dried and pulled with a solvent.

Evaporate that, and freeze precipitate, or choose another way to the pure freebase. There are many ways, just take a look at the wiki, and step back and consider your options carefully.

 

[Randomness]

You could try growing water xtals.

Endlessness did a tek with showing how to do it. It's in the wiki under freebase conversions try this with some of the vinegar you salted with. Might be able to help you work out if you have pulled the spice from the lye soup.

Are you sure it's the right kind of bark? The previous fails don't seem to sound promising.

I personally like the max ion tek I think it is one of the best to get started with.

 

[teckner]

These are the jars that contain various stages of liquid. The two dark jars on the far right contain lye, bark, water, and small amounts of D-Limonene. The second jar from the left contains vinegar, D-Limonene, and (hopefully) some alkaloids. The jar on the far left I believe contained exclusively D-Limonene and water that was hot when poured in.

The Day Tripper:
Which jars should I dry out? I assume you meant the lye/bark mixtures, should I also allow the solvent/vinegar/alkaloid jar to evaporate? How about the solvent/water jar?
I have some "100% Acetone Nail Polish Remover" lying around, but the ingredients are listed as Acetone, and Denatonium Benzoate. Is this nail polish remover any good, or should I try to find something purer/distill this? I will also be going the FASI/FASA/FASW route, so I'm going to have to wait for the Fumaric acid to get here. It looks like it might be available in pill form, but it's much more expensive than buying it in powdered form. Unless I order bestine or naphtha online, which I don't want to do for security reasons, my only options are acetone, isopropyl alcohol, and limonene.

Regardless, thank you for all of your help! I've stayed away from even reading about Fumaric Acid techniques, and now I feel dumb for wasting time.

Randomness:
I'll read up on the water crystals, thanks a ton. The first fail was completely my fault for reading directions incorrectly and assuming I knew more chemistry than I really did. The second fail was very much the fault of me literally spilling a large portion (OVER HALF) of the bestine, and using a STB tek off of another site that was reported to have very low yields. That isn't to say that my bark isn't a dud, I have absolutely no idea unless I salvage this situation and get some decent yields, but I have no idea if it is bad because of my previous failures.

Thanks all for reading!

 

[teckner]

Update: I did a test on my D-Limonene. The packaging said it was pure, but apparently there was something else in it as when I tested the last mL or two, it went cloudy when being mixed with either vinegar OR water. An oil floats to the surface, the pure Limonene I presume.

I'm working towards doing a FASA extraction, but I fear that my acetone's other ingredient will do what the secret ingredient (probably a surfactant) in the limonene will do, anyone know if Nail Polish Remover with denatonium benzoate is unusable?

 

[benzyme]

denatonium benzoate is a salt, nothing more.
and as such, it is aqueous soluble.

limonene is an interesting solvent, because it has a chiral carbon, but so does DCM. strongly basic solutions may alter their conformations, but it won't alter their efficacies.

 

[teckner]

So I could mix water with the Acetone, and then dry with epsom salts?

Also, are you telling me that despite the appearance of the Limonene mixed with either the water or the vinegar, it's still good?

 

[downwardsfromzero]

Apologies in advance for any pedantry (but this can be important in pharmacology).

[...] Pull with an alcohol to evaporate to an oil. If it there is water in whatever alcohol you use its ok, just try and get the driest one you can find. Isopropyl, acetone [emphasis added], ethanol, etc. [...]

Acetone + lye = gunk. Also, it's not an alcohol.

[...] the ingredients are listed as Acetone, and Denatonium Benzoate. Is this nail polish remover any good, or should I try to find something purer/distill this? [emphasis added] [...]

If you are competent with distillation and have the right equipment, by all means distill your acetone. Its low (56degC) boiling point make this quite simple, but also make it quite a serious flammability hazard, however.

[...]
limonene is an interesting solvent, because it has a chiral carbon, but so does DCM. [emphasis added] [...]

DCM does not have a chiral carbon. It's not even prochiral.

 

[downwardsfromzero]

teckner, I just looked at your photo's. What colour was your limonene when fresh from its container? Pure limonene is a clear, colourless liquid. If it came out orange - which it looks as though it did - you have purchased mechanically pressed orange peel oil, which is largely limonene but contains a whole host of other stuff (hence its orange colour). Some of these additional compounds will form cloudy precipitates if boiling water is poured into the oil. Some will also form intractable gunk if mixed with alkalis (e.g., lye).

If you like playing with lab gear, you can steam distil orange peel oil to separate more nearly pure limonene and leave virtually all of the gunk-producing stuff behind.

 

[teckner]

When fresh, it was a bright orange oil that smelled strongly of orange peels. I recently acquired a separatory funnel, and the contents of the jars that had limonene have separated into a layer of gunk, a layer of what is probably vinegar, and a layer of the orange coloured oil. Give me a bit, I'll post more pictures.