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Question about acid-base extraction with Hydrochloric acid and Dimethyl Ether

RedHat

Bluelighter
Joined
Jan 2, 2015
Messages
91
I had a question regarding purifying Heroin #3 via acid-base extraction using Hydrochloric acid (aka: Muriatic acid) and Dimethyl Ether. Though there are quite a few articles on the web covering this process (using HCl and Ether, as opposed to Sodium Hydroxide and Chloroform), the one I'm referring to in this post is the How to Purify Heroin to Nearly USP article on drugsandbadideas.com.


The question I have is in regards to the pH levels. Though there are a lot of articles covering this process, not a single one of them include details about the pH level (or even mention pH testing at all). The only article that does include such details is one of the two heroin purification articles on Heroin Helper, Purifying Street Heroin Again.
I realize that even though the two articles use different chemicals with a slightly different process, they both use a form of acid-base extraction to yield a higher quality of heroin. But Im not certain this means one could simply use the pH levels detailed in the latter article and apply them to the process in the former. And even if I was wrong, and one could do that, I'm not confident that it's as simple as "copy & paste". Primarily because the article on Heroin Helper starts out using a base (Sodium Hydroxide), where as the article on drugsandbadideas.com starts off using
Hydrochloric Acid.



Thanks in advance.
 
Dimethyl ether is gaseous at room temperature, BP below -20, not hugely below, but at the very least your going to need efficient cooling, either a dry ice-acetone bath for convenience, or chaining progressively more efficient freezing mixtures, it does have one thing going for it-it doesn't tend to peroxidize, and also, its quick to strip, but unless you are tooled up to handle it, to keep it cold then it'll boil and evaporate right in front of your eyes. Diethyl ether would be more tractable, although, if you intend to store it, make sure that you test it regularly for peroxidation, and if you produce your own via either williamson synthesis or using sulfuric acid to dehydrate ethanol, then some BHT (butylated hydroxytoluene) or BHA (butylated hydroxyanisole) should be added, only a little is needed, to help inhibit peroxide formation.

Many ethers, diethyl ether included, have a nasty tendency to forming a corresponding hydroperoxide, itself reportedly deflagrating rather than detonating, but this then reacts further to form the alkylidene peroxide, and these are nasty customers, shock-sensitive, friction-sensitive, and on occasion, in seriously peroxidized ether, just going off for the hell of it. It'd be wise to do a little reading about how to handle and store ethers safely, and maybe a few nightmare scenarios to familiarize yourself with both best practice in general use, and how things go wrong, when they go wrong and what can happen when the shit hits the fan, or, if something does go tits up peroxide-wise and you end up with a fridge blown through the ceiling...(not trying to scare you off, its just one that sticks in my mind, not personal experience, but goes to show, a bottle of badly peroxidized ether is a bomb waiting to happen, and one thing to keep in mind, is if EVER a bottle develops any visible crusting around the top, don't even touch it, call the bomb squad. At least, if you prefer a potential bollocking to getting blown to pieces. )

That said, ethers can be reasonably, safely and responsibly used by people without formal chemistry training. Just look up the various methods of inhibiting peroxidation, and be aware that peroxide test strips can be made by soaking potato starch or starch spray into paper, along with a solution of potassium or sodium iodide. A sample of ether should be regularly tested, a few drops onto such a strip, and the oxidizing nature of peroxides lends itself to liberating iodine, if present, which then undergoes the characteristic blue-black colour change. The more deep the colour, the worse peroxidation is, if it is a problem in a given sample, the ether should be treated to destroy the peroxide. Storage over something like one of the more reactive alkaline earth metals, calcium would be a good choice IMO due to its non-pyrophoric nature, as granules/chips would suffice although there are a few ways of doing it.

Personally, I like to 'top off' bottles of peroxidation-prone solvents like diethyl ether, THF, diisopropyl ether etc. with argon, and ideally sparge the lot whenever I get it to drive off any dissolved oxygen, and fill container headspace with inert gas. Be mindful if you were to find lithium the only available highly reactive metal (Na is frequently used) that if you were to take it out of batteries, there can be be other components in there which are oxidizing, such as MnO2 in Li metal batteries, that wouldn't make ideal additions (its cheap as pellets on ebay, clean, or in somewhat thin strips for example, which have a rapid (in air) but quite controllable, 'tame' alkali metal, if you've never handled sodium, potassium before, Li doesn't have nearly the tendency towards pyrophoric behaviour, especially in thin or small amounts, which can easily oxidize before having the change to burst into flames.

Sodium on the other hand, its a bit more lively (especially when chucked into water, yes, yes, I know, but find me a hobby chemist who hasn't had fun with Na in water), and K has teeth, so IMO Li makes the ideal candidate, as does Ca, in that they are less likely to bite the less experienced chemist in the ass, especially when you take into account the flammability and volatility of ether (another thing to take into account, is any stirrer or heating method used needs to have sparkless motors, or at least, a copper mesh attached to the air intakes to serve as a fire arrester. Some switches can spark when the pole is flipped, and with volatile solvents around, it never pays to think 'oh it won't happen'

Because as they say, 'shit happens'. Bad days in the lab happen, I've had a few myself, and all one can do is take the appropriate precautions.

If your using ether for availability reasons, can I reccomend dichloromethane instead? it, and chloroform, are excellent solvents for morphinan opioids, in their freebase forms. Aqueous ammonia makes a good base, not too harsh and not overly prone to cleaving esters such as heroin, which are a somewhat labile functional group, sensitive to excessively acidic or basic conditions.

DCM is preferable, of the two, IMO, due to its lower boiling point, and being more convenient to strip. Its nonflammable, but something important to remember about halogenated solvents is NEVER allow them to end up being pyrolyzed, such as by smoking, as they don't tend to catch fire, but if they are forcibly passed through sufficient heat to decompose them, phosgene is a common byproduct. And if phosgene scares the living crap out of you, whilst ether shouldn't, phosgene should.
 
Regarding crystallizing things in general, I find it is often a very useful technique, to prepare solutions of gaseous acids such as HCl, by dripping concentrated aqueous HCl into concentrated sulfuric acid (bog cleaner grade is fine for this, its not carried over into the product, the H2SO4, that is), the conc. H2SO4 acts as a dehydrating agent, binding the water in the HCl and releasing gaseous HCl, which can be gassed into various solvents to prepare solutions which can be titrated to a known concentration, and added dropwise, using PH measurement where the solvent permits, using a digital meter for accuracy, or if not, then with moistened PH paper, and if all else is lacking, watching turbidity evolution and its cessation as solvent with a known concentration is added dropwise, and be aware that if its based with NH3, and the NH3 not removed, then ammonium chloride would be left behind. Its not particularly toxic, but can follow through with organic solvents and the H freebase ought to be washed with ice cold H2O, keeping the washings to exclude any mistakes until you are sure you have got it where you want it to be (a general principle, if you've ever find your workup went to pot and your baby out with the bathwater, so to speak, you'll understand how shitty it is to lose something due to a mistake you could have prevented)
 
Many ethers, diethyl ether included, have a nasty tendency to forming a corresponding hydroperoxide, itself reportedly deflagrating rather than detonating, but this then reacts further to form the alkylidene peroxide, and these are nasty customers, shock-sensitive, friction-sensitive, and on occasion, in seriously peroxidized ether, just going off for the hell of it. It'd be wise to do a little reading about how to handle and store ethers safely, and maybe a few nightmare scenarios to familiarize yourself with both best practice in general use, and how things go wrong, when they go wrong and what can happen when the shit hits the fan, or, if something does go tits up peroxide-wise and you end up with a fridge blown through the ceiling...(not trying to scare you off, its just one that sticks in my mind, not personal experience, but goes to show, a bottle of badly peroxidized ether is a bomb waiting to happen, and one thing to keep in mind, is if EVER a bottle develops any visible crusting around the top, don't even touch it, call the bomb squad. At least, if you prefer a potential bollocking to getting blown to pieces. )
Holy Jesus. Good to know, thanks for that.. Maybe I should go with Chloroform instead.

Personally, I like to 'top off' bottles of peroxidation-prone solvents like diethyl ether, THF, diisopropyl ether etc. with argon, and ideally sparge the lot whenever I get it to drive off any dissolved oxygen, and fill container headspace with inert gas. Be mindful if you were to find lithium the only available highly reactive metal (Na is frequently used) that if you were to take it out of batteries, there can be be other components in there which are oxidizing, such as MnO2 in Li metal batteries, that wouldn't make ideal additions (its cheap as pellets on ebay, clean, or in somewhat thin strips for example, which have a rapid (in air) but quite controllable, 'tame' alkali metal, if you've never handled sodium, potassium before, Li doesn't have nearly the tendency towards pyrophoric behaviour, especially in thin or small amounts, which can easily oxidize before having the change to burst into flames.
Also very useful information. Thank you.

If your using ether for availability reasons, can I reccomend dichloromethane instead? it, and chloroform, are excellent solvents for morphinan opioids, in their freebase forms. Aqueous ammonia makes a good base, not too harsh and not overly prone to cleaving esters such as heroin, which are a somewhat labile functional group, sensitive to excessively acidic or basic conditions.
I'll definitely try dichloromethane then, thank you for that suggestion.

And I had another question... I tried this purification process and ran into a problem when I added Ammonium Hydroxide to it, the "white precipitate" ended up turning into a mostly solid substance...

Here are the steps I went through. Also, I wasn't purifying a full gram of H, but mearly .25 of a gram, just to test the process out so I wouldn't waste much if I failed (which I'm glad I did, because it seems like I did fail).


  1. Weighed out exactly .25g of #3 heroin and poured it into a test tube (a centrifugal test tube to be specific. The kind with the narrow bottom).
  2. Added 28% hydrochloric acid to the test tube, drop by drop, just until all of the Heroin powder was damp.
  3. Allowed this to react for roughly 2 minutes (maybe longer).
  4. Added 1.25ml of distilled water to the test tube containing the heroin and HCl.
  5. Put the test tube lid on and gently shook and swirled the mixture around.
  6. Placed the centrifugal test tube into a centrifuge and ran the centrifuge for a couple minutes.
    • While the centrifuge was going, I prepared a setup for vacuum filtration by placing a 3ml Buchner funnel on top of a 50ml filtering flask (with a vacuum adapter sidearm), and placed a sufficiently sized filter paper inside the Buchner funnel (filter paper was .22 um pore size)
  7. Using a pipette, I extracted the liquid from the test tube and slowly dropped it into the 3ml Buchner funnel, which slowly filtered down into the filtering flask
  8. Using a pipette again, I extracted the liquid from the filtering flask and moved it into another test tube.
    • Note: At this point, the liquid is a very clear brown liquid with no solid particles floating around inside it.
  9. Added Ammonium Hydroxide to the test tube 1 drop at a time. And the white precipitate started to form on the top layer, but when I swirled it around a bit, it became evident that it was a semi-solid substance. Trying to stir it around with a glass rod just confirmed this. It was very thick, almost like a really hard caramel substance that gets stuck on your teeth >_<

Any idea why this may have happened?

P.S. I meant to add a picture of the test tube with the Ammonium hydroxide precipitation but forgot to take a picture. I will post that later, but if someone knows whatsup with this, please share.
 
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The semisolid is your heroin base with water mixed in.

You be well served to get an organic solvent like chloroform and mix with your mixture than separate the chloroform layer, dry it with Epsom salt then evaporate the chloroform.

Also you shouldnt have added concentrated acid to your heroin. You should diluted the acid
 
You should also be checking the pH as you add acid or base and make sure you get 2 ph units beyond whatever the pka of the ammonium or freebase version of the heroin is that you are trying to convert during dropwise addition
 
Yeah, 28% HCl is too strong for this, you stand the risk of getting some ester hydrolysis back to morphine, 6-MAM and 3-MAM, the ester linkage is a pretty labile functional group, sensitive to either excesses of acid or of too strong base.

And even though MSDS sheets can be pretty hair-raising even for very safe things, are often exaggerated, it is worth at least looking them over, and you should familiarize yourself with anything you intend to use. Because that way, you end up learning things like the peroxidation of ethers the easy way rather than the hard way. Which at best involves it shredding glassware, potentially blowing out windows in a room, at worst, gets someone killed if they happen to be present as a shrapnel-magnet and get caught in an explosion in a glass vessel full of flammable solvent and minced by flying glass, assuming its not in sufficient volume to just take your head off altogether. alkylidene peroxides are known for their being highly brisant contact-explosives, and only a few mg are sufficient to destroy a flask if it were to go off.

Better to find out where the potential pitfalls of the shrapnel bomb variety lie before you walk in on one. Stuff that goes 'boom', the ones that want to melt your face off, carry hideous toxicity, react nastily with water, or are pyrophoric, kinda better to know about those kinds of chemicals BEFORE you encounter any of them, that way one is much more likely to live to a ripe old age with the full compliment of limbs, eyes, internal organs and genitalia. And just for fun, there are a few that fit in several, or potentially even most or all of the above categories.

Know your reagents is obvious, but solvents are just as importent to handle safely. The likes of THF, diisopropyl ether for example, peroxidize especially rapidly, beginning within 10 minutes IIRC when actually out and exposed to air, and concentrating them if they contain peroxide whilst removing solvent, concentrates the peroxide in a reduced volume, and makes it more liable to explode. Which for the likes of isopropylidene peroxide, isn't really saying much, but then again, MORE probable explosion in ether peroxides, is pretty rotten odds given they are as sensitive as a nancy-boy paedo bent pig in a prison shower=D

If there was ever a super-sensitive, violently explosive bastardly little nightmare of a chemical with a determined desire to blow your head off, its ether peroxides.

You reminded me though, I've been meaning to grab myself some really small capacity fritted Buchner funnels myself. Just got paid today too, I know what my first treat this week is going to be. A new set of microscale and small prep-scale fritted Buchner funnels. Could use a few spare mercury thermometers too. Oh and some fresh packs of PH buffer solution calibration mixtures for calibrating my electronic PH pen and dissolved salts meter. Might grab myself some more LAH and SOCl2 come to think of it since I'm getting paid extra too. Think I'll do me a little shopping for a few...errm...household sundries=D

Also, before using epsom salt as a dessicant, just make sure it has been freshly baked out in the oven, until it turns white, opaque and easily powdered. Store in airtight container, and ideally, when using a portion if its been a while, bake it again, with the oven door propped open, on a high heat (NOT when solvents are around), the epsom salts, once washed with dry solvent to collect any adhering product, can be recycled by baking the bejeezis out of them until they are opaque white, you need the anhydrous MgSO4 not the hydrated form, which is epsom salts, but epsom salt is easily and repeatably dehydrated by heat.
 
The semisolid is your heroin base with water mixed in.
Is it really? Why did it turn so damn hard? All of the articles I've read that use this technique with these precursors say that it should be "milky" and able to be mixed with the solution. This was far from that. I poured out the liquid and with the semi-solid remaining, I tried to mix it and I had to use some force to peel it off the sides of the test tube. It wasnt just "kinda" sticky, its just shy of rock hard.

And trust me, in this semi-solid, theres no water. Theres water under it when it gets formed, but the semi-solid is not a liquid by any stretch of the imagination.

You be well served to get an organic solvent like chloroform and mix with your mixture than separate the chloroform layer, dry it with Epsom salt then evaporate the chloroform.

Also you shouldnt have added concentrated acid to your heroin. You should diluted the acid

Im confused as to why this 28% is too concentrated, yet the three articles Im using as a reference (here, here and here) all use 28%, and others on these forums have said it worked. The first step is literally adding 28% HCl to the Heroin 8(

You should also be checking the pH as you add acid or base and make sure you get 2 ph units beyond whatever the pka of the ammonium or freebase version of the heroin is that you are trying to convert during dropwise addition
I would love to verify that the pH levels are where they should be, but unfortunately im kind of a novice, and none of these fucking articles even mention the pH levels. When I get more familiar with this, I plan on posting a tutorial with extreme detail, pictures, pH levels, what you'll see if you do it right, as well as if you do it wrong, etc. These shitty purification articles are just like "Mix this in with this. Then move on".. No detail whatsoever :!


Yeah, 28% HCl is too strong for this, you stand the risk of getting some ester hydrolysis back to morphine, 6-MAM and 3-MAM, the ester linkage is a pretty labile functional group, sensitive to either excesses of acid or of too strong base.
28% HCl is too strong? All three of the articles I'm reading (here, here and here) say that thats the correct concentration to be using.

And even though MSDS sheets can be pretty hair-raising even for very safe things, are often exaggerated, it is worth at least looking them over, and you should familiarize yourself with anything you intend to use. Because that way, you end up learning things like the peroxidation of ethers the easy way rather than the hard way. Which at best involves it shredding glassware, potentially blowing out windows in a room, at worst, gets someone killed if they happen to be present as a shrapnel-magnet and get caught in an explosion in a glass vessel full of flammable solvent and minced by flying glass, assuming its not in sufficient volume to just take your head off altogether. alkylidene peroxides are known for their being highly brisant contact-explosives, and only a few mg are sufficient to destroy a flask if it were to go off.
You're doing an amazing job at making me super paranoid :p lol. And I actually have the MSDS sheets printed out for all the chemicals involved, I just haven't read every one of them in detail yet. But I will for sure... Starting with Ether, lol.

You reminded me though, I've been meaning to grab myself some really small capacity fritted Buchner funnels myself. Just got paid today too, I know what my first treat this week is going to be. A new set of microscale and small prep-scale fritted Buchner funnels. Could use a few spare mercury thermometers too. Oh and some fresh packs of PH buffer solution calibration mixtures for calibrating my electronic PH pen and dissolved salts meter. Might grab myself some more LAH and SOCl2 come to think of it since I'm getting paid extra too. Think I'll do me a little shopping for a few...errm...household sundries
I have a 3ml, 35ml and 100ml Buchner funnels. I haven't used them too much other than just experimenting with stuff, and this acid-base extraction, but they're definitely a good buy. I find that I do have to manually cut the filter paper to fit the 3ml funnel though (doesn't look like anyone sells them in that size)

@Limpet_Chicken - You've provided lots of detail about what solvents I should use and how to store and treat the chemicals involved, which I greatly appreciate, but do you have any input on why the white precipitate that was created after adding ammonia damn near was rock hard? I can't even find a way to get some of this off the side of the test tube (I'll use some HCl on it, but its stuck on there... I mean its damn near part of the test tube now)

Thanks for taking the time to reply guys!

Update: Ill perhaps try the whole process again, and take pictures of every step this time. Then maybe upload them here (after stripping all EXIF data ;-) )
 
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You might want to consider washing your #3 with ice water before starting the whole process as it's probably only 25-40% H, you might be turning some of the cutting agents into something rock hard.

Also when I precipitate Morphine (which is always a fine, fluffy powder) I have much better results using Whatman Grade 1575 resin hardened filter paper, it's >2um and smooth so precipitates nearly slide off compared to untreated high ash content paper, it's a tad bit pricey though. I like the .22um as a final step but in a triple layer Omicron syringe filter.
These extremely strong filter papers have a high wet strength due to the addition of a small quantity of chemically stable resin. Normal qualitative applications will not introduce any significant impurities into the filtrate
 
You might want to consider washing your #3 with ice water before starting the whole process as it's probably only 25-40% H, you might be turning some of the cutting agents into something rock hard.

Also when I precipitate Morphine (which is always a fine, fluffy powder) I have much better results using Whatman Grade 1575 resin hardened filter paper, it's >2um and smooth so precipitates nearly slide off compared to untreated high ash content paper, it's a tad bit pricey though. I like the .22um as a final step but in a triple layer Omicron syringe filter.

Silly question, How exactly does one "wash" #3 heroin with cold water?

You might be right about the purity of the H. I have some of the Heroin Purity Test Kits, ill use one tomorrow to see if itll give me an idea of the purity (Its not exactly definitive, but its better than nothing). And not that a picture of it helps, but heres what im working with (so you can see its not some crappy black tar H):


And here are some pictures of the flask and test tube with the precipitated substance stuck to them:

Those were taken after I tried to mix it around after dropping some ammonia into it. It just stuck to the sides as you can see.

So what change do you suggest I make for the next attempt? (Keep in mind im only testing the process with .25g)
 
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Mix with ice cold water, then separate with your Buchner funnel, if you notice some crap in the catch flask then rinse a little more over it. You might pull out cuts like diphenhydramine, as that's used in the southeast states a lot.

I'm curious about that purity test, hopefully you get coffee colored results.
 
Mix with ice cold water, then separate with your Buchner funnel, if you notice some crap in the catch flask then rinse a little more over it. You might pull out cuts like diphenhydramine, as that's used in the southeast states a lot.
I didn't get this from within the states. Got it from the Netherlands.
So the heroin that I would continue with is what gets caught on the filter paper, correct? (seems obvious, but im just trying to be 100% certain about everything here)

I'm curious how ice cold water would make the heroin filter differently? And what pore size would you suggest? Right now I have .22 um and 11 um.

I'm curious about that purity test, hopefully you get coffee colored results.
Alright, ill post pictures of the results tomorrow.
 
The cold water will pull out any water soluble cuts before you begin the salting, diphenhydramine is just one example of a benign cut, but could possibly be what's rocking up in the end?

So the antihistamines or whatever will run through but the #3 should stay behind and probably only lose a small percentage of weight if it's decent stuff, coming from the Netherlands hopefully it is.

The .22 is cool for tiny samples but will slow things up for the larger ones. I've used 20 micron grade 1 paper before and lost only maybe 5% of a large sample, the morphine freebase was very fine and fluffy when dry. Sparkled nicely in the light.

Did you run the purity test yet? Was it light tea or dark coffee?

Just out of curiosity, why are you going back to a base in the end?
 
Just curious because this seems like a McGyver type purification, going from base to salt (and harshly with nothing but 28%HCl at first) to base to salt. It would appear that you have the ability to use Methylene chloride and do a proper A/B extraction and separation with a separatory funnel. With .22um filtering on top of that you should be golden.

The laid out purification just seems a bit rough and wasteful:
step 17: Using the eye dropper or pipette, remove this clear layer and deposit it into the petri dish. The remaining substance in the beaker contains heroin base can be saved for future projects, or disposed of.

..while you seem quite capable of something more refined.
 
Could be ammonium chloride thats formed the hard bits? as for why the specific hardness, can't say, but once you verify if it is or isn't the product of course, if its not, then the ammonium chloride, if you've any stuck to stuff, can be cleaned off using caustic alkali (sodium hydroxide solution, which will liberate ammonia gas, and leave table salt behind. The NaCl will wash off easily enough. And at the scale your working on, the amount of ammonia liberated isn't going to be dangerous, smell a bit 'ew' maybe (I hate the smell of NH3, although anhydrous ammonia is the worst of course) and a kitchen with an open door and if you have it, extractor fan will do fine to get rid of it.

With ammonium salts, strong base causes them to liberate ammonia gas, the principle being that with the salt of a weaker base, a strong base will displace the weaker base from its salting counterion, forming the corresponding salt of the strong base, and displacing the weaker one, ammonia, as NH3 gas. So NaOH solution, once you verify that the hard stuff is or isn't as suggested, H base, which probably isn't likely to be rock hard, if you are certain its ammonium chloride, sodium hydroxide solution will work nicely to remove it. I use ammonium salts often, for generating NH3 gas, by addition of NaOH or KOH to the salt in dry form, followed by addition of water, dropwise from a pressure-equalized addition funnel, and this reaction works nicely for removing solid NH3 salts.

Sometimes salty residues can get caked on pretty damn hard once they dry out, I've had it happen plenty times with NaOH and KOH, as they turn to carbonate, in neglected electrolyte baths in electrolytic cells running on hydroxide for Na or K, or NaK production (the NaOH-KOH system depresses the melting point compared to either alone, although the result is NaK alloy, when refining alkali metals via electrolytic means, a liquid metal alloy, which is VIOLENTLY reactive, much more so than potassium is.)

And some old electrolytes, well, lets say I use disposable cans in my heating bath now, that I can just get rid of rather than re-use, once of course, the requisite modifications are made to them for inert atmosphere conditions, especially with the eutectic KOH-NaOH mixture once it fuses, after the electrolysis is as done as you are taking it at the time, the residues get bloody rock hard. Although I prefer using a magnesium powder-Na or K hydroxide mixture like thermite now, and after smashing up the resultant slag, after ignition in a closed crucible so the alkali metal vapor can't boil off, boiling the powdered slag under 1,4-dioxane, its a lot less fiddly and touchy compared to electrolytic methods, and works rather nicely, with the dioxane coming from antifreeze concentrate (ethylene glycol) and bog cleaner grade conc. sulfuric acid. Again disposable tin can stills, rather than my glassware, for distilling the dioxane, as a lot of tarry polymeric glorp gets produced too, but otherwise, it works nicely for DIY alkali metal production :)
 
The cold water will pull out any water soluble cuts before you begin the salting, diphenhydramine is just one example of a benign cut, but could possibly be what's rocking up in the end?


So the antihistamines or whatever will run through but the #3 should stay behind and probably only lose a small percentage of weight if it's decent stuff, coming from the Netherlands hopefully it is.


The .22 is cool for tiny samples but will slow things up for the larger ones. I've used 20 micron grade 1 paper before and lost only maybe 5% of a large sample, the morphine freebase was very fine and fluffy when dry. Sparkled nicely in the light.

Ok. Ill give this a try. I understand why this should work now.. Because Heroin #3 isnt water soluble... (Duh, not sure why that didn't occur to me... /facepalm).


These are the proper steps, verify if you can please :)

  1. Select a small portion of Heroin #3 to be washed, taking note of the weight of this sample.
  2. Submerge the Heroin in ice cold water (the heroin should be suspended in the cold water, as its not water soluble)
  3. Run the entire mix through a vacuum filtration using .22 um pore size filter paper
  4. Dispose of the liquid in the filter flask and let the filter paper dry (with the heroin base still on it)
  5. Once the filter paper and heroin are dry, remove as much of the heroin as possible
  6. Weigh the remaining heroin, comparing the weight with the original weight (to get an idea of how much was removed)
As far as the temperature of the water, just out of curiosity, why does it have to be ice cold? If heroin #3 isn't water soluble, why is the temperature of the water significant at all? (Not questioning your suggestion. Just want to understand it completely)

---------


Did you run the purity test yet? Was it light tea or dark coffee?
I did test it, and it looks to me like its 2.5 or 3 stars. But I'm a little skeptical about this test, because I tested some shit-grade black tar heroin from my area, and it was only slightly lower quality, but trying both samples out, its obvious to me that the tar is much lower quality.


And to be honest, I didn't ever intend to use these tests as an absolute indication of the purity of the heroin sample anyways. What I planned on doing was:

  1. Test some Heroin #3
  2. Purify that same heroin using the acid-base extraction to yield diacetylmorphine hydrochloride
  3. Test the diacetylmorphine hydrochloride using the same Heroin purity test
  4. Compare the before and after tests to one another to judge how effective the extraction process was (or rather how effective I was at using it)
Thus using the tests as an indication of the purification process, rather than as an indication of the original heroin purity level.

---------


Just out of curiosity, why are you going back to a base in the end?

Im not? The three articles I linked to (here, here and here) all claim to yield diacetylmorphine hydrochloride (fluffy white powder heroin). Unfortunately these articles don't have shit for detail, they don't even say what type of heroin they start out with in the beginning, if its Heroin #3 or #4, or something else.


---------


Just curious because this seems like a McGyver type purification, going from base to salt (and harshly with nothing but 28%HCl at first) to base to salt. <moved sentence to next quote response>


The laid out purification just seems a bit rough and wasteful:
step 17: Using the eye dropper or pipette, remove this clear layer and deposit it into the petri dish. The remaining substance in the beaker contains heroin base can be saved for future projects, or disposed of
..while you seem quite capable of something more refined.


From what I understand, the 28% HCl is used to remove any particulate matter, then the ammonium hydroxide and ether is used to remove any soluble impurities.


--------

It would appear that you have the ability to use Methylene chloride and do a proper A/B extraction and separation with a separatory funnel. With .22um filtering on top of that you should be golden.
Well Dichloromethane is just the solvent though, right? You still need an acid to do the extraction.
Would you maybe send me a rough outline of the steps for the specific A/B process you're suggesting? I plan on getting this whole process down as well as possible, testing multiple processes, using different acids and solvents, etc, then posting an in-depth article on how to do it properly, which would include:


  1. SAFETY FIRST - I'll include details on:
    1. The proper precautions to take
    2. Adequate safety gear (goggles, gloves, etc)
    3. How to properly handle and store each chemical, as well as how to neutralize any that may spill
    4. How to handle the situation if any chemicals get spilled on those involved
  2. How to test the original Heroin sample (verifying its heroin and not some ripped off product, and how to tell if its cut with fentanyl (which would be deadly if it was))
  3. Various options for the glassware (EG: suggesting one utilize a separatory funnel, but if not, just use a pipette or eye dropper)
  4. What chemicals to use (the concentrations, specific quantities, etc etc)
  5. How to keep an eye on the pH throughout the entire process
  6. Pictures of every single step (actually multiple pictures for every step)
  7. What to expect after each step, and how one can tell if it was done improperly
  8. How to test the resulting yield
Which I would be more than happy to post on this site, if the mods would be cool with it. If not, then thats totally fine too. But I'll give credit wherever its due (unless otherwise instructed).

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Could be ammonium chloride thats formed the hard bits? as for why the specific hardness, can't say, but once you verify if it is or isn't the product of course, if its not, then the ammonium chloride, if you've any stuck to stuff, can be cleaned off using caustic alkali (sodium hydroxide solution, which will liberate ammonia gas, and leave table salt behind. The NaCl will wash off easily enough. And at the scale your working on, the amount of ammonia liberated isn't going to be dangerous, smell a bit 'ew' maybe (I hate the smell of NH3, although anhydrous ammonia is the worst of course) and a kitchen with an open door and if you have it, extractor fan will do fine to get rid of it.


I actually just purchased a bottle of sodium hydroxide solution online, but in my chemistry naivety I forgot to look at the concentration, and when it arrived, I immediately noticed that its like 98.3% water or something >_< So ill return that and go to the local chemical supply store (I try to get everything there, but they're only open 9:30a to 5p on weekdays, which is a pain in the ass because thats when I work). What concentration of sodium hydroxide would you suggest I purchase?


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With ammonium salts, strong base causes them to liberate ammonia gas, the principle being that with the salt of a weaker base, a strong base will displace the weaker base from its salting counterion, forming the corresponding salt of the strong base, and displacing the weaker one, ammonia, as NH3 gas. So NaOH solution, once you verify that the hard stuff is or isn't as suggested, H base, which probably isn't likely to be rock hard, if you are certain its ammonium chloride, sodium hydroxide solution will work nicely to remove it. I use ammonium salts often, for generating NH3 gas, by addition of NaOH or KOH to the salt in dry form, followed by addition of water, dropwise from a pressure-equalized addition funnel, and this reaction works nicely for removing solid NH3 salts.

Ok, so just to reiterate what you're suggesting: I need to verify if the substance that forms when I drop ammonium hydroxide into the filtered heroin/HCl mix is either Heroin base or ammonium chloride, which can be done by introducing a strong base (such as sodium hydroxide solution). If this interaction releases NH3 gas, then it's ammonium chloride, if it doesn't, then its heroin base. is that correct?

It'll be a few days before I can get to the local chemical store to get some NaOH solution (maybe as late as Friday). Perhaps I could maybe test it with the Mecke test kit to see if it has any opiates in it, but even if its ammonium chloride (as opposed to heroin base), I would think theres still a very small amount of H base in it as well, which would probably turn the Mecke test positive and lead me down the wrong path.



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And by the way, Limpet_Chicken, LucidSDreamr, and Jekyl Anhydride, thanks thus far for your input. I don't usually get too many replies when I post to forums, so I was fully expecting this to be a ghost thread. So I appreciate you guys taking the time out of your day to help me out, seriously. :)
 
And you guys were asking about the purity test - Heres a couple pictures. It was hard to judge because the color of the solution would look quite a bit lighter or darker based on how one was looking at it or holding it. But this looks like a 3 star result to me (taking it with a grain of salt, since the black tar wasn't that much lighter in color, but was complete shit)



And Jekyl Anhydride, For the cold water wash, it sound like what you're talking about is similar to the CWE technique, (which I've seen on these forums a few times as well). That wiki article says:
Opiates are much more soluble in cold water than acetaminophen
Now obviously the substance I'm dealing with isn't acetaminophen, but do you know if H #3 is more or less soluble in cold water than opiates in other forms? Because the CWE articles Im reading says the cuts are soluble in warm water while opiates are soluble in cold water (which means with cold water, the opiates pass through the filter), but you're saying thats the opposite with H #3?
 
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Hmm, I was hoping the purity test would have yielded better results but the BTH result sounds a little discouraging. Guess you'll have to judge it the old fashion way.

Yes H #3 is not water soluble but no need taking a chance of stripping anything good off of it with warm or even room temp water, which is why I suggest very cold distilled H2O. The CWE procedure is for Opioids in salted form, such as bitartrates, sulfates & HCl's, freebase does not apply.

Still I think it's worthwhile since this is about purification as hopefully you can get your H down to fairly pure diacetyl and monoacetyl morphine. I'm at work right now but I'll jump into this a little later and see if we can't lay down something worthwhile and see this come to fruition.
 
Hmm, I was hoping the purity test would have yielded better results but the BTH result sounds a little discouraging. Guess you'll have to judge it the old fashion way.
Yeah. Another thing about it is the only other results I have to compare them against is the results from other tests I've ran. (One from a local BTH dealer, and 3 from 3 different dealers all from the Netherlands). The 3 from the Netherlands were very similar. If there was someone that was able to successfully purify H and test it, then post the results, I would have something to compare them against. It'll speak volumes if the results after purification still aren't 4 or 5 stars.


Yes H #3 is not water soluble but no need taking a chance of stripping anything good off of it with warm or even room temp water, which is why I suggest very cold distilled H2O. The CWE procedure is for Opioids in salted form, such as bitartrates, sulfates & HCl's, freebase does not apply.
Still I think it's worthwhile since this is about purification as hopefully you can get your H down to fairly pure diacetyl and monoacetyl morphine.
Got it. Well I'll try it out then.


I'm at work right now but I'll jump into this a little later and see if we can't lay down something worthwhile and see this come to fruition.
Thanks a ton! Looking forward to it. I'm at work as well (Perhaps I should have worked from home today, hah).

Also, if either of you know what concentration sodium hydroxide solution I should look for, that may be helpful. The only alternative A/B extraction document of heroin I've been able to find is this one, which uses sodium hydroxide and chloroform, and also even includes some details about the pH levels.

Also, if you go to Google, and search for type:pdf "Lab 1: Separation of an Unknown Mixture", then click the first result (I cant hyperlink to it, it just redirects and if I hyperlink to that it throws a 401), what do you think of that document? Looks pertinent
 
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