A/B Extraction Basics?

[Hunter66]

I'm trying to learn how to do A/B extractions properly, starting out with a simple DXM agent lemon extraction. One thing that I always come across is that tutorials will list specific chemicals for the base, nonpolar solvent, and acid. In my specific instance, most places have recommended using ammonia for the base, naptha for the nonpolar, and then citric acid for the acid.

Is there any reason why I would need specifically to use ammonia? I understand the basic theory of AB extractions, but not the more intermediate stuff. I have, for example, a can of 100% lye. It's rooto brand, and is in very small spheres. Is there any reason why I couldn't use that instead? Some places say that lye is not pure sodium hydroxide, but if that's the case, then could I use a different base such as baking soda? Another thing that confused me, is that why can't I transform the salt into freebase, let it settle out, wash it in something polar (water?) and then let it dry before turning it back into a salt? Then I would not even need to use a solvent.

Also, almost everywhere says to use a non-polar like naptha. Why could I not just use, say, olive oil, for example? Or any other non-polar substance?
Is it because these are not good solvents, perhaps? That seems like the obvious answer, but I don't want to rely on guesses.

Assuming that is the case, why can I not use something like low-odor mineral spirits (easier for me to get ahold of) that leave a residue? Assuming I cannot remove all of the mineral spirits (I obviously don't wanna be drinking those), then I cannot simple evaporate it off without leaving a residue on the salt. However, could I not simply wash the salt in something polar such as vegetable oil to remove the residue? I don't mind drinking a little bit of vegetable oil floating on top of my DXM salt solution, but I do mind drinking mineral spirits residue.

TLDR: I would like to have AB extractions explained a bit better to me so that I can understand some of the AB drug extraction conventions and if they really need to be done that way.

[Von Bass]

You could use a base like NaOH yeah, but you'd be wise to make up a known conc solution (i.e. 2M or whatever) and use that, rather than adding it solid. Pure NaOH can seriously sodomise more intricate structures.

If you're using naphtha, ensure that you do a spot test to make sure it evaporates cleanly. You technically could use something like olive oil, although in some cases, a small amount of polarity is good for pulling certain molecules (hence why something like DCM is often used). Sadly olive oil is difficult to get stuff to dissolve into, and harder to then get it out - can you imagine evaporating olive oil, or filtering out a crashed solid?

When starting out, its best to work exactly as a tech says, really is the best method for learning. I would recommend using a clean evaporating NP and either ammonia or 2M NaOH. A base like baking soda, sodium hydrogen carbonate, often isn't strong enough to push your target molecule around.

[AC&C]

I'm trying to learn how to do A/B extractions properly, starting out with a simple DXM agent lemon extraction. One thing that I always come across is that tutorials will list specific chemicals for the base, nonpolar solvent, and acid. In my specific instance, most places have recommended using ammonia for the base, naptha for the nonpolar, and then citric acid for the acid.

My understanding is the Agent lemon extraction method uses materials that are easier to obtain in lieu of more effective, yet more difficult to obtain, materials. (Easy and hard being relative to the target demographic.) Specific chemicals are called for because this is a recipe approach to chemistry that attempts to minimize errors by chemistry inept individuals.

In my opinion, starting with a tutorial and learning the theory behind it is very helpful in learning the general principles it uses. I think it's a good approach to improving your chemistry knowledge.

Is there any reason why I would need specifically to use ammonia? I understand the basic theory of AB extractions, but not the more intermediate stuff. I have, for example, a can of 100% lye. It's rooto brand, and is in very small spheres. Is there any reason why I couldn't use that instead? Some places say that lye is not pure sodium hydroxide, but if that's the case, then could I use a different base such as baking soda? Another thing that confused me, is that why can't I transform the salt into freebase, let it settle out, wash it in something polar (water?) and then let it dry before turning it back into a salt? Then I would not even need to use a solvent.

As DXM HBr is a weakly acidic organic acid (pKa 8.5) you ideally want a strong base such as NaOH to convert it to the freebase. Ammonia works, but not as well as sodium hydroxide, as ammonia is a weak base.

You need a solvent to prevent the freebase from being washed away. I don't know what you have in mind, but I doubt it will work. A solvent is called for because it will keep the freebase in that layer while water soluble impurities are washed away in the aqueous layer.

Also, almost everywhere says to use a non-polar like naptha. Why could I not just use, say, olive oil, for example? Or any other non-polar substance?
Is it because these are not good solvents, perhaps? That seems like the obvious answer, but I don't want to rely on guesses.

In terms of the solvent, I'd say that naptha is called for because it is readily available, but any nonpolar solvent would probably suffice. As far as using olive or vegetable oil, I have no idea.

Here's some information from the Merck index that might come in handy.

Derivative Type: d-Form hydrobromide
CAS Registry Number: 125-69-9
Additional Names: Dextromethorphan hydrobromide; demorphan hydrobromide
Manufacturers' Codes: Ro-1-5470/5
Trademarks: Benylin (Warner-Lambert); Canfodion (Gentili); Cosylan (Parke-Davis); Hihustan (Maruko)
Literature References: HPLC-MS/MS determn of free base in urine: M. L. Constanzer et al., J. Chromatogr. B 816, 297 (2005).
Properties: Occurs as the monohydrate, crystals, mp 122-124°. [α]D20 +27.6° (c = 1.5 in water). Approx soly in water: 1.5% at 25°, 5% at 50°, 25% at 85°. Soly (w/w): 25% in 95% ethanol at room temp, 10% in glycerol. Sol in propylene glycol, chloroform. Practically insol in ether. pH of a 1% aq soln: 5.2-6.5. Long range stability of aq solns obtained by adjusting pH within 4-5.6. Reacts with alkalies forming the free base which is practically insol in water.

[dedraic]

M
In my opinion, starting with a tutorial and learning the theory behind it is very helpful in learning the general principles it uses. I think it's a good approach to improving your chemistry knowledge.

This


In terms of the solvent, I'd say that naptha is called for because it is readily available, but any nonpolar solvent would probably suffice. As far as using olive or vegetable oil, I have no idea.


I can confirm this works, at least with Salvia spathacea, T. pachnoi, and Lactua sp. It also gakked the end product horribly with the T. pachnoi, leading to a ridiculously excessive amount of clean-up to get anything approaching a pure alkaloidal salt.

Emphasis on the ridiculous. Likely because I'm a lot less willing to give up a quarter of my alkaloids working with mescaline, than some random sage that I found to be psychoactive after smoking and my favorite non-cannabinoid sleep-aid.

[Hunter66]

So if I were to mix, say, 1 tablespoon of lye into a third of a cup of water and use that, it shouldn't damage the DXM? According to this lab instruction I read, that should be roughly equivalent to a 2M, mixture, based on the density of lye instead of using grams (I have no scale yet). I could then replace the ammonia in the tutorial with that, and I could get some zippo fluid to use as naptha, as the only other mineral spirits I have do not evaporate cleanly. This should work as normal?

Also, the questions for olive/vegetable oil were for possible future extractions, and because if I could find other nonpolars, I did not know if there was some specific reason I needed to use naptha. If I were to extract into oil, I could just drink the oil, or maybe even cook with it.

Also, I was asking if you could simply freebase the DXM and then wash it with water because I was under the impression that the DXM would not wash away. Do you think a significant portion of it would go with the water? That would explain needing to use a solvent.

Also, I did start with a tutorial, several actually, lol. I can run the experiment, but that won't teach me anything except give me practice and experience. Although these are useful, which is why I intend to start off doing a small and fairly simple DXM extraction, they still aren't really teaching me much chemisty besides what I've already read. I hope to learn more by questioning parts of the tutorial here as to how they work and such.

Thanks Von, AC&C, and dedraic so far, you've all been helpful :bluecool:

[stateofhack]

I could just drink the oil, or maybe even cook with it.


wut

[Hunter66]

If all of the *insert whatever drug here* has been transformed to freebase and dissolved into the vegetable/olive oil, then I could just drink the oil to get the effect, or cook it into pancakes or something.

[AC&C]

Also, I was asking if you could simply freebase the DXM and then wash it with water because I was under the impression that the DXM would not wash away. Do you think a significant portion of it would go with the water? That would explain needing to use a solvent.

The problem I see with that is being able to keep the freebase physically in place. Like, if you were to have a beaker with DXM settled at the bottom with water on top, and you wanted to pour out the water while keeping the DXM at the bottom... you'd either pour out some product or have impurities and water mixed in with it. While the freebase would remain insoluble it would still be "mixed in" (in a sense) with impurities. The advantage of using a solvent is that it will have the DXM in it, while keeping it completely separated from any water-soluble impurities.

Also, the questions for olive/vegetable oil were for possible future extractions, and because if I could find other nonpolars, I did not know if there was some specific reason I needed to use naptha. If I were to extract into oil, I could just drink the oil, or maybe even cook with it.

Sounds like someone's going to be eating dissociative pancakes.

:bluecool:

YYYYYEEEEEEEEEEAAAAAAAAAAAAAAHHHHHHHHH

[dedraic]

The problem I see with that is being able to keep the freebase physically in place.

In my search for ghetto chemistry, I've found pushing a cotton ball into the end of a funnel, pouring in the basic solution with the precipitate, then running an acidified solution through afterward(into something else, of course) works remarkably well. Not perfect of course, but it does the trick well enough. It might need to be repeated(resulting in more loss of product, I'm sure) though.

[Hunter66]

The problem I see with that is being able to keep the freebase physically in place. Like, if you were to have a beaker with DXM settled at the bottom with water on top, and you wanted to pour out the water while keeping the DXM at the bottom... you'd either pour out some product or have impurities and water mixed in with it. While the freebase would remain insoluble it would still be "mixed in" (in a sense) with impurities. The advantage of using a solvent is that it will have the DXM in it, while keeping it completely separated from any water-soluble impurities.


Ah, that would make sense then. Thank you


Sounds like someone's going to be eating dissociative pancakes.

Indeed ;)

In my search for ghetto chemistry, I've found pushing a cotton ball into the end of a funnel, pouring in the basic solution with the precipitate, then running an acidified solution through afterward(into something else, of course) works remarkably well. Not perfect of course, but it does the trick well enough. It might need to be repeated(resulting in more loss of product, I'm sure) though.
Hmm, I might need to try this.

I'll probably end up buying/obtaining multiple bottles of cough syrup, and then I can mess around with various methods/formulas/etc.

[Frequency]

In my search for ghetto chemistry, I've found pushing a cotton ball into the end of a funnel, pouring in the basic solution with the precipitate, then running an acidified solution through afterward(into something else, of course) works remarkably well. Not perfect of course, but it does the trick well enough. It might need to be repeated(resulting in more loss of product, I'm sure) though.

Best advice in the thread. Get a buchner funnel and an air pump if you can penny up.

[Hunter66]

I tried the extraction with roughly 2M NaOH solution and water washer mineral spirits. All I yielded was a small amount of yellow oil, however the expected yield was only about 100mg because I was using half of a small bottle of 10mg DXM/5 ml syrup, so I don't really know if it worked or not. Next time I'm going to try to do the extraction with more cough syrup and using ammonia. I haven't decided which solvent to use yet, however I'm leaning towards ethyl acetate. It smells pleasant, evaporates really quickly, is very poorly soluble in water, and doesn't cause brain damage like naptha. I could also use something like hexane, but I have access to as much ethyl acetate as I want at 28 bucks per liter, or $77.20 for 4 liters. It's also environmental grade; it's 99.5+% pure, leaves approximately 5ppm evaporation residue, and has been filtered through a submicron filter. Thoughts?

[Von Bass]

Assuming that it is a suitable NP solvent for a DXM extraction (i.e., the damn stuff is soluble in it at freebase), I haven't checked at all, that's the perfect choice!

I don't recommend consuming your yellow oil, mineral spirits can be fucked for having all types of shit added to them.

[Hunter66]

Assuming that it is a suitable NP solvent for a DXM extraction (i.e., the damn stuff is soluble in it at freebase), I haven't checked at all, that's the perfect choice!

I don't recommend consuming your yellow oil, mineral spirits can be fucked for having all types of shit added to them.

Yea I already threw it away. lol

[Tick Tock]

It looks like you've already got a better solvent than naphtha but I'll still throw this out there: DO NOT use lighter fluid. Use VM&P Naphtha, it is much cleaner.

I've done DXM A/Bs with ammonia, and I felt like I lost a lot of product, so I think the NaOH would be better. Did you get any DXM freebase crystal precipitation when you used lye? (Answer this if nothing else, I'm interested.) You won't get any freebase precipitation with ammonia, basically just a huge volume of nasty red liquid. I know you've read the teks, but just in case you don't know, remember to use clear ammonia that doesn't produce suds when you shake the bottle. Janitor's strength ammonia might work even better if you can find it. I haven't tried it yet with NaOH, so if you try both NaOH and ammonia let us know which base yielded more final product.

Since you're so new to the process, I suggest you only salt your final product out with lemon juice/citric acid. 100% food safe, so excess won't kill you. Don't bother consuming anything that isn't in the citric acid form right now, and never bother consuming freebase DXM. Even if olive oil worked as a NP solvent, you need to have your DXM in salt form to really feel anything. Making food with oil that has DXM freebase dissolved in it will get you little or no effects. Unless you're mixing some lemon juice in with your pancakes, skip that idea.

[Hunter66]

Okay. I didn't get any precipitate using lye. All I got was some yellow oil, however, there was only about 100 mg of DXM in the cough syrup I was using anyway, and it was expired. Next time I was going to use ammonia and DCM, however I could also use the lye on a separate bottle and see if it makes any difference.

And I was planning on evaporating all of the solvent leaving me with freebase crystals, and then mixing those with pure citric acid. Either that, or mixing the acid in first, so it precipitates out, then evaporating the solvent. I have to wait for my paycheck to order some DCM, but when I do I'll try it.

Also, the DCM I'm planning on using is stabilized with amylene. Since it has a fairly low boiling point (38.5 degrees Celsius), I don't think it will be very hard to remove completely along with the DCM.

[Tick Tock]

Okay. I didn't get any precipitate using lye. All I got was some yellow oil, however, there was only about 100 mg of DXM in the cough syrup I was using anyway, and it was expired. Next time I was going to use ammonia and DCM, however I could also use the lye on a separate bottle and see if it makes any difference.

And I was planning on evaporating all of the solvent leaving me with freebase crystals, and then mixing those with pure citric acid. Either that, or mixing the acid in first, so it precipitates out, then evaporating the solvent. I have to wait for my paycheck to order some DCM, but when I do I'll try it.

If you could use the lye again that would be great. I always wondered whether ammonia or NaOH was the better base for DXM extraction, but I don't have any glassware to mix up the NaOH right now so I haven't gotten around to trying it. Report back though, I'm hella interested.

Also, you don't have to evaporate your nonpolar solvent. When you mix your citric acid with your nonpolar solvent containing freebase DXM, the DXM is converted to DXM citrate. The DXM citrate is then insoluble in the nonpolar solvent and precipitates out. There's no need for evaporation of NP solvent because you don't need DXM in the pure free base form. One way or the other, your free base has to get dissolved in the nonpolar layer. One way or the other, you have to convert it to the salt form. Make it easier on yourself and just convert it to the salt form from the entire nonpolar layer. You will get the same DXM salt, regardless of whether you pull from the NP solvent or evaporate it off. Evaporating will be wasted effort.

After you do this, you still not need evaporate. You will be left with two layers: one in which the newly extracted goodies are soluble and one in which they are not. Drain off the polar layer (with your DXM salt), this contains the goodies. Then drain off the nonpolar solvent, it's trash now. You don't have to evaporate it, if you let the two liquid layers separate they will not mix with each other, just like oil and vinegar. I don't know how you've been doing it so far, but a separatory funnel offers a huge advantage over any other method I know. If you don't have a separatory funnel, use a plastic bag (maybe not with the lye though!) You can use the sep funnel to do both of the separations in the dual-phase extraction.

Also, I'm not quite sure if you can use anhydrous citric acid in this process. Based on the variety of A/B teks I've read, I'm under the impression that citric acid should always be in solution. However, I don't know what the reasoning would be behind this, can anyone explain?

Do you plan on consuming the end product? If you're just doing this for yourself, you can extract with lemon juice and boil it down to a very tiny lemon juice shot. This is much easier to down than a whole bottle of syrup. It still tastes nasty, but it's over much quicker. If you aspire for a pure powder, I'm not sure. Even if you can react with anhydrous citric acid, that's going to be a fucking sour ass hit of DXM when it hits your tongue. Maybe you can gel cap it; wish I could tell you more. Gassing with HCl will yield a pure powder, but I think you might need to try a few more extractions before you graduate to that.

What tek are you using? http://www.dextroverse.org/extractions.html
^A great tek with lots of pictures and it explains how to do everything very nicely. Apologies if you've already come across it, but if not, hope it helps. I guarantee if you follow that tek to the letter you will end up with a tiny, yet powerful shot of DXM citrate. You can even try gel capping it the way they do in the tek, but I never tried that.

[21st Century 1776er]

OP, check my post in the following thread for some relevant descriptions...

http://zoklet.net/bbs/showthread.php?t=39125

see post # 32

good luck...

[Hunter66]

Stuff here


Yea, I've read that one. I was going to buy anhydrous citric acid in powder form. Then I could simply mix it into a little bit of water and mix the DXM into it, then that could be evaporated into a powder and put in gel caps, or possibly dissolved into PEG and put into gel caps. I have to wait for my paycheck to buy the supplies, but once I get it I can try a couple of different methods and report back.

[Rizzo in a box]

Awesome thread is awesome.

I love people who know how to ask questions properly.

+1

<3

[missingno]

Also, almost everywhere says to use a non-polar like naptha. Why could I not just use, say, olive oil, for example? Or any other non-polar substance?
Is it because these are not good solvents, perhaps? That seems like the obvious answer, but I don't want to rely on guesses.



ether, xylene, toluene, chloroform, DCM, MEK, etc.

*if using methanol for a mineral spirit, DONT DRINK ANY or you may risk blindiness, especially if one consumed atleast 15mls of it*

[Fractals]

ether, xylene, toluene, chloroform, DCM, MEK, etc.

*if using methanol for a mineral spirit, DONT DRINK ANY or you may risk blindiness, especially if one consumed atleast 15mls of it*

You shouldn't really drink any of the solvents you listed, except ether, provided it's diethyl and not petroleum. Even then, you should be huffing it...

[BungHole]

MMM ether....

[missingno]

now ive just wondered if OTC ether from starting fluid cans are sufficiant enough for the NP solvent to get remove whateverfreebasesubstance from the a/b extraction...afterwards evaporation and then recrystalization if desired..

[Fractals]

now ive just wondered if OTC ether from starting fluid cans are sufficiant enough for the NP solvent to get remove whateverfreebasesubstance from the a/b extraction...afterwards evaporation and then recrystalization if desired..

It depends on what is in your starting fluid other than ether, as long as it's just mixed with other NPs that won't react with your alkaloids. It's always a good idea to do extra recrystallizations and washes if using OTC's like this, though.