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Procedure for conversion of salts to free base form. Example images - #4 heroin to high purity free base crystals. : Opiates | Torhoo darknet markets

The pictures I attached at the end are from a conversion of #4 heroin into high purity free base crystals, but this is a very versatile procedure. It's suitable for converting a wide variety of salts into their base form. This includes synthetic compounds like fent/fentalogues.

Usually the base form of a drug is more suitable for smoking/vaporization due to having a lower melting point. Sometimes the hydrochloride salt will be unsuitable for vaporization because it undergoes decomposition before it vaporizes (such as with cocaine hydrochloride).

This can also be used for purification purposes. For example, if I had taken the free base crystals I obtained and converted them to their hydrochloride form, I would have obtained high purity diacetylmorphine hydrochloride (#4 heroin). While the conversion of base to hydrochloride salt is outside the scope of this procedure, two methods are to bubble hydrochloric acid vapor through an organic solution of the base, causing it to precipitate out (commonly known as "gassing" in methamphetamine production), or to add a solution of HCl directly to the free base and evaporate off the solvent, commonly done in labs by using ether with HCl dissolved in it.

(If you substitute the base for ammonium hydroxide solution, and the solvent for diethyl ether you will get the method often known for obtaining free base cocaine, although I've used the exact method outline below without any modification and it worked fine.)

Materials required/recommended:

Syringes, you'll probably want at least 3.5mL ones. Luer-lock recommended but optional
Syringe filters (I used .22um PES w/ luer lock)
Test tubes with rubber stoppers or separatory funnel
Erlynmeyer flask
Evaporating dish (use something with a relatively large surface area, like a glass dish, or a glass tray)
Eyedroppers for drawing things up, adding reagents and solvents, and transferring things around
**glass pipettes with hand pumps are not required but are recommended for any home chemistry because of how useful they are. Look up serological pipettes on ebay or amazon and there's a commonly used 3 pack of hand pumps with blue, green, and red hand for 2ml, 10ml, 25ml capacity (you can find these individually too but it's like $15 for all three on amazon). Make sure you get glass pipettes though, not the plastic/polystyrene ones. I like to use the glass 10ml pipettes with the 2mL hand pump, because it gives you a lot of play with the wheel and lets you draw things up without accidentally sucking up too much.**
Sodium carbonate or another suitable base (baking soda usually works too)
Sodium sulfate (desiccant)
Sodium chloride NON-IODIZED (needed if you have an emulsion issue)
DISTILLED water
Naptha, or other appropriate organic solvent. (Ethyl acetate works pretty well too as general purpose extracting solvent)
Acetone isn't required here but it's good to have around for any home chemist for cleaning glassware and stuff.

READ THROUGH ALL OF THESE INSTRUCTIONS FIRST BEFORE YOU START

1.) First dissolve your sample in DISTILLED water, stir until no more will dissolve. You may want to warm the distilled water in the microwave first, this will help the sample dissolve faster. Don't use a crazy amount of water, you just want there to be enough to dissolve everything, and for there to be a nice aqueous layer when we get to the liquid-liquid extraction (LLE) part.

2.) Filter this through a syringe filer. I used a Polyethersulfone (PES) syringe filter with .22 micrometer pore sizing and a luer-lock inlet. Use a syringe and push your solution through the filter, once you've pushed everything through, follow this up by pushing a little bit of distilled water through, to wash out any product that might be trapped in the filter. If you're processing a large amount you might end up going through a few syringe filters since the filter will eventually get clogged up with debris, but they're cheap. You should end up with an aqueous solution that is completely translucent and free of suspended particulate matter.

3.) This is where the instructions are going to diverge a little bit depending on how much liquid you're working with. If you can fit everything into a test tube, or multiple test tubes, then that's what I recommend. To make things as easy as possible, you generally don't want to have your aqueous layer occupy more than around 1/3 of the height of the test tube. If you have a seperatory funnel then you can obviously use that, since this is what separatory funnels are made for. If you're trying to do this with a larger amount then you'll want to buy a separatory funnel (you can get one fairly cheap off of ebay).

4.) You'll want to have a solution of concentrated base set aside. Dissolve a large amount of your base in DISTILLED water. If you add too much and no more will dissolve you can either add a little more water or just give the solids time to settle to the bottom. I used sodium carbonate (you can find this at walmart in the soaps and detergent aisle in a yellow box that says WASHING SODA on it, you can also make this by taking a tray with some aluminum foil, putting baking soda on it, preheating the oven to 220F/104C and then heating for 30 minutes. Sodium carbonate decomposes into CO2, H2O, and sodium carbonate at 176F/80C)

5.) Add your concentrated base solution to your aqueous product solution drop by drop, immediately you will see everything turn cloudy and a bit of precipitate will start clinging to the sides. This is the product converting from the polar, water soluble salt form to the more nonpolar free base. Swirl slightly after each drop. Once you can add a drop and not observe any reaction then that means all of the product has been converted from it's hydrochloride salt form to it's free base form.

6.) Add a bit of your organic, nonpolar solvent. (I used naptha here, but I've done this with all kinds of solvents. Ethyl acetate is a good extracting solvent too) Enough to where there's a clear layer above the aqueous layer. With the exception of halogenated solvents like chloroform and dichloromethane, organic solvents have a lower density than water, and will always be the top layer. Cover the top of your test tube with a rubber stopper and shake (or you can be dumb and use your finger, as long as you don't tell anyone). This will cause the organic layer to build up vapor pressure, so be mindful of this keep your finger on the stopper so it doesn't fly off. Then carefully lift the stopper to vent and release the pressure. Let the mixture sit until everything separates out into two distinct layers.

**If you are having issues getting everything to separate, and it looks like there are a bunch of little bubbles then you have an emulsion problem. This can happen more often with certain solvents, but you can generally induce a separation by adding concentrated brine solution (dissolve sodium chloride in distilled water until saturated) and shaking.**

7.) Using an eyedropper or a pipette, carefully draw off the top/organic layer and transfer this to a clean, dry container. A good choice is an appropriately sized erlynmeyer flask. Be careful not to draw up any of the aqueous layer!

8.) Repeat steps 6 and 7 at least two more times. Each of these extractions of the aqueous layer with the nonpolar solvent is also colloquially referred to as a "pull". You generally want to do at least 3 pulls to make sure you get all the product out, I'll commonly do 4 just to be sure, with the 3rd and 4th pulls using less organic solvent.

9.) ***THIS IS A VERY IMPORTANT STEP, AND ONE THAT MOST PEOPLE LEAVE OUT IF THEY WRITE UP A PROCEDURE LIKE THIS. THIS STEP IS THE DIFFERENCE BETWEEN ENDING UP WITH GOOEY OIL VS CRYSTALS*** You should have all the extract layers pooled together in a vessel, like the aforementioned erlynmeyer flask. This organic solvent actually still has water in it, and it will interfere with the evaporation step that's coming up. We're going to use a desiccant to pull all the water out of solution and "dry" the organic layer. Take some sodium sulfate and add it to the flask, swirl it around and observe that it's clumping up as it absorbs water from the solution. When you can add sodium sulfate and see that it's not clumping up at all then you should be good, although there's not really any harm in adding excess sodium sulfate.

10.) In order to let the sodium sulfate work you can let it sit for around 5 minutes or so. Afterwards, you're going to carefully decant off the dry organic solution into whatever you want to evaporate it from. A good choice would be a large glass dish or tray. Some of our product-containing organic solution is trapped in the sodium sulfate still, so we want to rinse it off once or twice with whatever solvent you've been using. Add a little bit to the sodium sulfate, swirl it around, and then decant it off. Do this two or three times total depending on how much sodium sulfate you used.

11.) Now we get to the final step, you're going to evaporate the organic solution using a fan or a blowdryer or if you're patient and want some nice crystals you can just store it somewhere and let it evaporate on its own. If you're using a fan or blowdryer be careful as the solution starts to fully evaporate and you're going to get a solid. Don't blow that shit all over the place.

PICTURES:

Aqueous solution after syringe filtration:
http://uoxqi4lrfqztugili7zzgygibs4xstehf5hohtkpyqcoyryweypzkwid.onion/?img=371640032901.jpg

Aqueous solution after addition of base:
http://uoxqi4lrfqztugili7zzgygibs4xstehf5hohtkpyqcoyryweypzkwid.onion/?img=451640032927.jpg

Free base diacetylmorphine (heroin) crystals:
http://uoxqi4lrfqztugili7zzgygibs4xstehf5hohtkpyqcoyryweypzkwid.onion/?img=421640032956.jpg

Free base after scraping and collecting crystals:
http://uoxqi4lrfqztugili7zzgygibs4xstehf5hohtkpyqcoyryweypzkwid.onion/?img=281640032985.jpg

/u/plkqcs

2 points

3 years ago

Up vote. Thank you for some real content

/u/SolidSnake1982

2 points

3 years ago

Mods, this should be stickied. Seriously, imagine picking up some fent free dope from like MC, and just making it PERFECT. Those crystals are gorgeous.

/u/Haven_Shill_XHV

1 points

3 years ago

Yea this is awesome. Thank you.

/u/csanova

1 points

3 years ago

Badass contribution. Thank you! and GOTDAMN that is some beautiful looking powder. Well done.

/u/johnshade

1 points

2 years ago

This is a legendary post, /u/socat2me. It's exactly what I've been looking for. I've been reading every such guide I can find (three or four so far), and they all diverge at different points, making it hard for a novice like myself to discern the best way to proceed. Also, thanks for the great photos; they're the first I've seen documenting the process, and are EXTREMELY helpful in demonstrating what to expect. And goddamn is right: those are some glorious crystals. Do the salt crystals look similar? My intention is to arrive at a more refined salt.

A few (well really many) questions.

Is the syringe filtration superior to gravity filtration with lab filters and funnel? I've acquired #1 lab filters (10u, I think, considered the "standard" filter) and glass funnels, but I suppose a syringe does expedite the process. I've seen .22u filters mentioned in a few places for this and other procedures--does the smaller filter size result in a meaningfully better product? I've also just recently read that PES and certain other synthetic filters are more hydrophobic, allowing for more complete filtration. So much to learn and to acquire, but I insist on doing it right.

I know the pump pipettes provide enhanced control, but I have traditional glass pipettes with the rubber bubbles. If not as sophisticated, these should be satisfactory, no?

At steps 4 and 5, with regard to the basic solution, the guides I've read prescribe using ammonia. Is there benefit to using washing soda to make your own basic solution?

At step 6 for the organic solvent you describe using naphtha and mention ethyl acetate as another option. One guide I've read recommends ether while the others say chloroform, which they say is a more attractive option due to the dangers of ether. Are all of these fairly equally suitable?

Is it possible to dry the organic solvent before performing the extraction, or else to acquire an anhydrous solvent in the first place?

Finally, when converting the base to the salt, one is supposed to add approx. 5mL distilled water and 5mL HCl 28% to the approx. 100mL organic solvent that you've been using (although a few sources say the HCl should be more diluted than 28%) and perform an extraction, retaining the *aqueaous* layer and evaporating it. But that contradicts the description above of retaining the solvent and evaporating it. Where should the product be at that point? In the organic solvent or in the aqueous layer? Once it's been converted to its salt it should be highly soluble in water, but is it yet more soluble in the organic solvent?

Thanks again for such an amazing post, and I'm sorry about all the questions.

/u/socat2me 📢

1 points

2 years ago

Hey, took me a while to write a response up! I'm glad you found the post helpful! I'll try to answer all your questions and point you in the right direction:

First, just to help in guiding you if you decide to look up any other reference materials this reaction is an acid/base reaction with an extraction. Specifically, the type of separation used in the extraction is referred to as a liquid-liquid extraction/separation aka LLE.

Regarding the syringe filtration: I always use it when possible because of how easy and efficient it is. The only problem is that compared to gravity filtration or filtration with something like a buchner funnel the filter has a much lower capacity for the amount of solids it can remove before it gets jammed up all full of solids. Because of this it's most suitable for situations where there isn't too much suspended solid that need to be removed, or for when you're just working on a small scale reaction.

This is just a personal preference that I've developed, but I tend to avoid gravity and even vacuum filtration unless it's absolutely necessary (at large enough scale buchner filtration becomes hard to avoid), mainly I just find it to be a bit of a pain in the ass, it always seems to increase the amount of solvent that needs to be involved and even with vacuum filtration sometimes some solids get into the filtrate.

In the guide I perform what is essentially a microscale extraction (for scaling up, the main difference--aside from the amounts of solvent and materials--would be instead of the use of a seperatory funnel instead of the test tube and pipette to remove the organic layer) so the syringe filtration works perfectly.

The 22 micron filter size is actually for working with sterile media, because it's small enough that it can filter out viruses, so it's not really necessary for this application, but it's what I had available and it certainly gives a clean solution! For scaled up reactions where there's too much for a syringe filter, sometimes what I'll do is drop a bit of dense cotton into the solution, specifically like what you see with safety swabs (look up johnson's safety swabs), and then I'll draw the solution up through the cotton using a pipette.

As far as the pipette pumps vs the bulb ones you're good with those, it might take a little bit of practice to get the hang of how much force to apply to the bulb but those are totally fine to use. In terms of utility the pumps are super useful though, I would recommend upgrading to them at some point if you find yourself using pipettes on a regular basis.

The base you use isn't super important as long as it's strong enough to drive the acid/base equilibria, the most common choices are Ammonia (in the form of ammonium hydroxide), Hydroxide salts like potassium and sodium hydroxide, and carbonate salts like sodium carbonate and sodium bicarbonate (bicarbonate may not be strong enough for some reactions though). Sodium carbonate is one of my favorite bases for doing extractions with, it's strong enough for almost all acid base reactions, it's extremely cheap, fairly non-toxic compared to others, and the conjugate base isn't a very good nucleophile, so it isn't likely to produce any side products if there are impurities.

The extracting solvent can be anything that dissolves your product and isn't miscible with water, however the other factors to consider are how does it interact with water (does it absorb a lot? how hard is it to dry with desiccants?) and how easy is it to evaporate.

Chloroform and Dichloromethane are good choices, but they're pretty polar and may extract more than just your product (note: they're halogenated so they're heavier than water thus the organic layer ends up on the bottom at a liquid-liquid interface) dichloromethane also evaporates so quickly I've actually found that it can draw water into the solution because the endothermic evaporation cools the vessel and solution so much that water starts condensing into it. The other thing I haven't mentioned about chloroform, is that it's just not something you'll be able to get your hands on unless you have a chemical purchasing account.

Ethyl acetate is good but the problem is it's a fairly wet solvent, with about 25mg/ml of water in it even before it's shaken up with water. I recently read a japanese paper where they found that sodium sulfate doesn't work to dry ethyl acetate at all either, although adding equal parts hexane does. I've been experimenting with a mixture of ethyl acetate and naptha to try and address the moisture content of the ethyl acetate with some success****

Diethyl Ether is a great solvent for alkaloids and would be ideal here. It isn't too wet, evaporates easily, and it can also be dried easily but the downsides are it's quite expensive, it's a watched chemical (you'd have to buy a lot to raise eyebrows, but no reason to work with it if you don't need to), and it's extremely flammable. It can also form peroxides that spontaneously decompose and explode if stored incorrectly for long periods of time. Naptha is a bit more nonpolar than an ideal solvent in this case, but it still manages the extraction. It's also cheap, readily available, has a low moisture content, and isn't too bad when it comes to evaporation. You just need to watch the brand, anything other than VM&P/Kleanstrip may have additives in it, don't substitute camp fuel like some say to do. Do an evaporation test by putting some in a dish and making sure it evaporates cleanly (always good to do with any new solvents you get if you aren't sure of the brand/quality).

It's not possible to dry the organic solvent first in this case only because we're going to be shaking it up with water, so we have to dry it at the end regardless, otherwise it is common practice to dry solvents before their use in reactions. Especially for moisture sensitive reactions.

So for this post I isolated the base crystals, so I ended up with the organic layer since the base is nonpolar. Salts are ionic compounds so they are very polar, and will always end up with their highest concentration being in the aqueous layer (for alkaloid salts it's safe to assume >99% is in the water/aqueous layer).

Usually when I'm doing these acid/base reactions my goal is just to end up with the base because my preferred ROA for opiates is vaporization with a bubble. If you want to end up with the salt you'd add one last step of either gassing the base-containing organic solution with HCl gas (this is just theoretically, I don't really advise this if you aren't experienced), or alternatively adding a little bit of concentrated HCl or shaking the organic layer with a solution of 5-10% HCl solution. This will convert it back to the salt and move it into the aqueous layer which you would remove and set aside for evaporation. Granted, this will take a while since it's water you're evaporating. I'd put it in as big a glass baking tray as possible and pop it in the oven at around 220F if you want to evaporate it quickly and get the product. Do note that this won't give you crystals (good crystals always require slow formation) but it will make sure all the HCl evaporates away and most importantly the purity should be the same as it would be if you spent the agonizingly long time it would take waiting for all the water to evaporate just from diffusion into room temperature air, which is what would essentially be required to grow crystals from the aqueous solution (unless you do a follow up recrystallization on the product from the tray but at that point you're just losing product for the sake of aesthetic).

****Since I originally wrote this I have found that (so far) the best solution to drying ethyl acetate with sodium sulfate is to wait until you would normally dry it with the desiccant at the end of the process, but first add a volume of naptha equal to 60% of the volume of ethyl acetate that was used. The solution will get all cloudy from the water precipitating out. At this point add 300mg of sodium sulfate for every mL of ethyl acetate that was used (it's a lot!), then swirl it for 5 minutes and let it sit for another 10. The solution should be clear and contain much less water.

Finally, here's two good resources to reference for acid/base reactions and extractions (clearnet links) I highly recommend checking them out they have pictures and steps:
⚠️Resource 1⚠️
⚠️Resource 2⚠️

/u/johnshade

1 points

2 years ago

Wow, this is amazing. I'm so grateful for your extremely detailed and informative response. I now have such a better understanding not just of the process but of the principles underlying it. Unfortunately, I must apologize again for another long reply and yet more questions; but I hope they're fewer in number and more focused now. And at least this exchange adds to the base of knowledge.

I've been watching a bunch of acid-base liquid-liquid extractions on YT for the last week. I watched one video and since then I've been recommended dozens more. Thanks to the algorithm, I've also watched demonstrations of recrystallization and now column chromotography, among other primers on good lab technique.

I think I am going to use syringe filtration. I was unaware of it until reading your post, and after thinking about it--I don't have the means for vacuum filtration anyway--it seems like the superior method. You don't have to wait for gravity, and you can potentially push solutions through a finer filter and obtain a purer result. Anticipating the issue with clogging that you mention, I was planning to perform filtrations in sequence with increasingly finer wheel filters. Would that create any problems?

I've found glass syringes up to 100mL, with luer-lock tips, on eBay for cheap. In fact, I've been assembling all of my setup of beakers, tubes, cylinders, Erlenmayers, funnel, stand, and rings on eBay for a bargain. Same with a quality scale (though I'd like a true analytical balance), I also found the set of pump pipettes you mention. At first I could only find uL pipettes.

One of the main reasons I was confused about how to proceed was the conflicting, or at least different, information in the various guides I've been reading. (All sources with links are below; you're probably familiar with some of them.) These methods variously neglect to cite quantities, concentrations, pH, etc., or fail to specify whether they're starting with HCl salts or base. Consequently they begin differently--for example the first Heroin Helper method begins by acidifying while the second basifies--and all seem to recommend different solvents. I suppose--though I'm not certain--that the authors simply assumed that they were starting with either #3 or #4, respectively, but omitted to mention that fact, making for confusion among less chemically savvy readers.

As one begins the process of dissolving the reactant, your method provides the helpful suggestion to use enough water to create a discernible aqueous layer for the extraction stage. I actually just found a source that specifies that 1g of hydrochloride salts is soluble in 2mL water, so it certainly doesn't require much. The separatory funnels are available in a wide range of volumes, so there's some potential for variability in water volume used. I think I will only need a small funnel--100mL at most, and probably smaller?

As a matter of curiosity, does it matter whether you start with tar or powder? (I know this question threatens to open an entirely different can of worms about what, precisely, #3 and #4 are, and how to identify them, because there's a great deal of confusion about that question, and distinguishing gray from brown can be difficult. But it's too much to address here.)

I like what you say about sodium carbonate. It seems like a gentler base than lye, and it's easy to source, although ammonia is also easy to acquire.

As for the organic solvent--this is where things vary a lot, from ether to chloroform to ethyl acetate to the naphtha that you use. Most websites say they will only sell ether and chloroform to schools or businesses, but I think I found a couple sources that sell them regardless. I did recently read about the dangers of peroxidation. In fact, the Bluelight source below contains a clearly knowledgable and thorough description of the serious problems it poses.

I actually already have VM&P naphtha, which I've often used in the past for wood finishing. I know that it's less volatile than ketone and alcohol solvents, and I remember adding it to finishes to retard their drying so as to extend their working time. Does adding naphtha to ethyl acetate work better because it pushes the water out of solution with the EA, thereby making it easer for the sodium sulfate to absorb it?

I also recently read about gassing organic solvents, but that process is beyond me, so I will be adding HCl solution dropwise to the freebase-containing organic solution. I'm glad you specified 5-10%. The aforementioned sources mostly suggest using the 32% as it comes off the shelf. But the Bluelight thread warns that using too low a pH could break certain labile ester bonds. I will therefore titrate the acid appropriately. For example, if I have 100mL of 32% HCl, then to get roughly 15% HCl I would add about 70mL of water?

Out of curiosity, instead of adding water and HCl, is there another polar solvent, like methanol or ethanol, that would wash the alkaloid salt crystals out of the nonpolar solvent, and that would evaporate faster than water? Referring again to the same source on solubilitiy, 1g HCl is soluble in 11mL alcohol. So it would be a question of what evaporates faster--a smaller quantity of water or a larger quantity of alcohol.

Like the previous extraction, should the acidification and attendant extraction also be performed three or four times, to make sure all the target alkaloids have been converted and pulled out of the nonpolar solvent? The drawback of repetition is, of course, more water (or potentially alcohol) to evaporate.

I have been reading and thinking about recrystallization as well, though mainly with regard to cocaine washes. The crystals look awesome, but I think I'll hold off until I have some confidence in the acid-base extractions. You mention losing product thereby, but is there not a process of sequential recrystallizations to ensure you're drawing everything, or just about, out of solution? (By the way what are your thoughts on ether vs. acetone for washing?)

Thanks so much again. This has been so helpful. I can now begin to see clearly where before I was surrounded by a fog.

Sources

Erowid, "Heroin purification to nearly USP," https://www.erowid.org/chemicals/heroin/heroin_info5.shtml

"Heroin Helper," https://heroinhelper.com/pdf/heroin-helper.pdf

Reddit, "Purifying Street Heroin," https://www.reddit.com/r/drugsmart/comments/1utdnh/purifying_street_heroin/"

Bluelight, https://bluelight.org/xf/threads/question-about-acid-base-extraction-with-hydrochloric-acid-and-dimethyl-ether.847577/#post-14372167

/u/phatbagz P

1 points

2 years ago

Have you used the tech in OP to make #4 into a freebase and then given smoking it a try? If so, how was it? I've gathered that you seem to be interested in this more for purification purposes but I was curious if you'd tried smoking the product produced from the steps in OP.

/u/johnshade

1 points

2 years ago

Not yet. I'm not particularly keen on the smoking ROA, because I understand it's probably the most wasteful, and I also want an ROA that is more socially practicable--although I'm not averse to trying it at least once.

I also haven't yet performed the procedure. I'm still getting a few things together, but as soon as I hear back from /u/socat2me about a couple of my questions and have everything prepared I'm going to give it a go, and I'll report the results.

I am mainly interested in the purification aspect, just because it seems that if you have the means, using a purer product is always better, in part because I think it would be valuable for refining cheaper (though still possibly quite potent) tar from all the vegetal and other junk present into a powder, and simply because it's the kind of project that appeals to me.

/u/phatbagz P

1 points

2 years ago

Wow, I didn't think of using tar as the material for this tech. I wonder if it would produce what most call "gunpowder" the nice powder tar that will still tar up when you breathe on it. But is usually much more potent and always preferable to me in most cases compared to the tar that comes hard and sticky from the get.

Definitely lmk. Interested to see what your results will be.

/u/TwelveAngelz

1 points

2 years ago

well. ill. be. fkd...!
Something thats a real AND original post!

Thankyou, ive been in the game a long time and now must learn all this. Lovely. lol. (Na really, thanks)

/u/Yak50Tree

1 points

2 years ago

What turns gear into being able to run on foil and give it that turtle image look when you heat it up? That part has been fucking me.