View Full Version : Purifying Heroin - HELP!!
jaydon
02-27-2006, 06:12 AM
The following text was kindly taken from the Heroin User's Handbook:
Removing Particulate Matter
The use of cotton for filtration when heroin is cooked before being used is a small attempt at purifying the heroin ingested. But a much better job can be done with a little hydrochloric acid (HCl). Place about a gram of heroin in a small glass container (a test tube is best, but any glassware that will allow mixing will work). Add a couple of drops of 28% hydrochloric acid and allow it to react for a couple of minutes. Next, add 5 ml of distilled water and mix vigorously so that everything dissolves that can.
At this point in the process, the heroin is in solution. The non-soluble material in the container is garbage that you do not wish to ingest. Let the solution sit so that the particulate matter settles to the bottom and then pipette out the solution, leaving the particulate matter behind. The simplest kind of pipette is an eye-dropper. If a pipette is not available, it is possible to pour the solution out of one container into another, being careful not to allow any of the particulate matter to be transferred.
Removing Soluble Impurities
Add ammonium hydroxide to the solution, one drop at a time. This will cause a white precipitate to form. Continue adding the ammonium until you are certain that there is no more precipitate being formed. The solution is then gently mixed to assure that the ammonium is evenly distributed. At this point, the solution will have a milky look.
The solution is then added to about 100 ml of ethyl ether-a chemical with which great care must be taken, since it is quite combustible. This new solution is then vigorously mixed and left to sit. This will cause the water to settle at the bottom of the container; it is removed with a pipette and then discarded.
A mixture of 5 mL of HCl and 5 mL distilled water is created and added to the ethyl ether mixture. This is stirred vigorously for several minutes. Afterwards, a water layer will form at the bottom of the container. You then pipette this out and into a small container such as a petri dish.
Deacidification
Slowly add baking soda to the solution in the petri dish. This will cause the solution to bubble. When the bubbling stops, this process is finished. The resulting solution is then air-dried, which yields pure heroin and table salt (NaCl). The salt is harmless and may be ingested along with the heroin.
Anyway, my question is does anyone know of any substitutes to ethyl ether in this process or any easier purification techniques? Cheers!
bogumil
02-27-2006, 07:08 AM
You can substitute it with chloroform.
Thats the easiest method I think. Make sure to dilute the ammonia. 1 drop on 200 drops water.
mmnyc9
02-27-2006, 09:06 AM
Just curious what would 1 gram of street H yield? I know it depends on the purity and so forth I have heard what is on the street is anywhere from 2 to 50 percent pure. I have know idea besides a taste test what is true. All those chemicals, not something one can go into the local Rite Aid and get. I really should have paid more attention in School having no idea about basic Chemistry.
stvip
02-27-2006, 10:59 AM
Both chloroform and (di)ethyl ether are highly flammable, as well as being volatile anaesthetics. Chloroform is a carcinogen and degrades into phosgene (WWI poison gas). Ethyl ether tends to form an explosive peroxide.
Here is my suggested alternative for cleaning (not purifying):
1. Salt formation: place in warm water/ethanol, acidify with a clean acid (citric acid or acetic acid, preferably) until everything dissolves.
2. Filter insolubles. Save filtrate.
3. Precipitation of base: with a premixed basic solution (sodium hydroxide or calcium hydroxide in water), adjust the pH to about 8.5. Allow the alkaloids to settle on the bottom of the container.
4. Carefully remove the supernatant (preferably by pipetting).
5. Add more basified water and repeat 4. until supernatant is clear.
6. For smoking - evaproate and leave as is. For oral, rectal or intranasal use - acidify again.
Possible variations: after the second step, evaporate the solution, and perform an NP wash. Activated charcoal could also be useful.
This is all in febrile, demented theory, of course.
flashbit3206
03-02-2006, 02:59 AM
detroit diesel seems to be yielding 30-60% pure if you have a strong connect and buying 8 balls or it at a time... if you are just buying packs expect to only get 15-20% pure... but it differs with everyone... everyone cuts it and it varies so widely from different street hustlers...
there seems to be a TON of fentanyl going around detroit right now being sold as heroin... you can tell that it is fentanyl because it tastes very different then heroin, and smells different... pluuuss the high lasts about 30-60 minutes which is an extremely short duration compared to IV'd heroin.. its even shorted then insufflated heroin which usually lasts 2 hours for me..
fentanyl also has a short half life, so after 3 weeks of using everyday you can feel withdrawls starting to set in at about 8-12 hours, like bowel movements etc...
fentanyl is heroin, like crack is to cocaine... did i say that right??? fentanyl is short lasting and has you coming back for more very quickly... it just sucks in my opinion..
ok im rambling.... ill stop now.. i just sniffed a few lines of some brown about 5 minutes ago, and the onset always gets me to chatting...
bogumil
03-02-2006, 08:51 PM
I have a few questions about the below:
- Why do you use ethanol in your theory? Wouldnt water be enough, or has the ethanol some advantages?
- Couldnt one basify best with diluted ammonia? SWIM did it and he can say that it gives beautiful whit precipitate (see pic).
The pippeting idea is good because when you pick it up with an NP it usually pulls over some dirt and you never end up with white product.
Both chloroform and (di)ethyl ether are highly flammable, as well as being volatile anaesthetics. Chloroform is a carcinogen and degrades into phosgene (WWI poison gas). Ethyl ether tends to form an explosive peroxide.
Here is my suggested alternative for cleaning (not purifying):
1. Salt formation: place in warm water/ethanol, acidify with a clean acid (citric acid or acetic acid, preferably) until everything dissolves.
2. Filter insolubles. Save filtrate.
3. Precipitation of base: with a premixed basic solution (sodium hydroxide or calcium hydroxide in water), adjust the pH to about 8.5. Allow the alkaloids to settle on the bottom of the container.
4. Carefully remove the supernatant (preferably by pipetting).
5. Add more basified water and repeat 4. until supernatant is clear.
6. For smoking - evaproate and leave as is. For oral, rectal or intranasal use - acidify again.
Possible variations: after the second step, evaporate the solution, and perform an NP wash. Activated charcoal could also be useful.
This is all in febrile, demented theory, of course.
pic
http://i35.photobucket.com/albums/d166/poppyjohnny/testtube1.jpg
SomniGod
03-02-2006, 09:19 PM
MMMmmmmmmm.......
the stuff dreams are made of.....
~S~
bogumil
03-02-2006, 10:17 PM
Isnt it beautifully white? I wish it would always look like this in the end. Most of the times it looks white when it precipitates but gets brownish once you dried it. There are always some impurities left ...
But this, where SWIM took the pics, stayed as white I think.
And I tell you it so few. Maybe 1/3 to 1/10 of the amount SWIM started with ...
stvip
03-03-2006, 12:46 PM
I have a few questions about the below:
- Why do you use ethanol in your theory? Wouldnt water be enough, or has the ethanol some advantages?
- Couldnt one basify best with diluted ammonia? SWIM did it and he can say that it gives beautiful whit precipitate (see pic).
The pippeting idea is good because when you pick it up with an NP it usually pulls over some dirt and you never end up with white product.
Ethanol is useful for those who wish to perform an NP wash after step 2 (which is probably most helpful for those starting with "black tar"), for the simple reason that it evaporates faster.
Ammonium hydroxide would work, though I don't see why it would be best. The problem is that of purity - househould ammonia should not be used. Likewise, hardware store hydrochloric acid should not be used (it is contaminated with arsenic and heavy metals, perhaps even some old lace), which is why citric, tartaric or acetic acid, which are readily available at food-grade purity, are recommended (they also have limited acidity in solution). Sodium hydroxide is produced from seawater and is usually reasonably pure (though I have never researched the exact nature of commonly impurities). Substitutes should, of course, work. Remember - the idea of the theoretical protocol is to allow people who cannot obtain chloroform or ethyl ether, or who correctly believe they should not handle such dangerous chemicals (flammable, anaesthetic, carcinogenic, and with a tendency to degrade into even more dangerous substances), to nevertheless be able to clean their dose (though I get the feeling some people here are thinking "mmm... cancer! They might give me some morphine or fentanyl at the terminal stages!").
As for "NP" - that is somewhat misleading, since morphine (and apparently its diacetylated derivative) is not sufficiently soluble in most NP solvents (hence the need for chloroform or ether specifically in a standard acid-base extraction). Interestingly, and possibly useful, I've found that oleic acid is a good solvent for morphine base - the utility of this should be explored.
Isnt it beautifully white? I wish it would always look like this in the end. Most of the times it looks white when it precipitates but gets brownish once you dried it. There are always some impurities left ...
After base is precipitated, wash it more than once. Afterwards, activated charcoal and recrystallization(s) should allow further purification. Then you'll have to throw your Stranglers records away.
When I say this is theoretical - I mean it. I have never procured heroin (or any other street drug), and have thus certainly never verified this works.
bogumil
03-03-2006, 03:50 PM
Ok, I see what you mean ...
You said, diamorph is almost as insoluble in Nps as morphine ... I always thought that heroin reacts much more like the other opioids than morphine and that one because of this has to choose a pH a little highe than 9.1 for the NP wash ...
Lets imagine, someone had access to chloro and ether. He performed two cleanings:
1. With ammonia, HCl and ether
- saltforming with HCl
-wash with ether
- neutralizing to 7 with ammonia
- picking up with ether
-evaporating and then neutralizing with water and Na2CO3
2. With ammonia and chloroform
- saltforming with HCl
- filtering
- adjusting to 9.1 with ammonia
- shaking with chloroform
-drying
He had the following problem:
In process 1 with the ammonia, the stuff looks very white in the beginning, when it precipitates out but then become more and more brown.
He wonders if pH 7 isnt too low? Would 9 - 10 be better? Can he use 9.1 just like with morphine or has it to be higher, like with codeine and so on?
In process 2 he isnt sure if 9.1 is the right pH, as the other procedure calls for adding base until precipitat forms and that is always at 7.
- So, is the precipitate at pH 7 (when HCl was used for salt-forming) is it diamorphine-base?
- would it be better to make the pH 9.1 + for the NP wash?
mmnyc9
03-03-2006, 07:23 PM
I remember Tango and Cash in New York a while back it was pure fentanyl. A bunch of people OD on it. I have heard fentanyl is supposed to be easy to make it's called Bathtub fentanyl Is this true?
stvip
03-05-2006, 07:45 AM
You said, diamorph is almost as insoluble in Nps as morphine
Not quite - I said "apparently". Neither the Merck Index nor Clarke's Analysis provide solubility information for diamorphine base in other NP solvents. You're German - why don't you dig up Bayer's original patent and other documents and share your findings?
I always thought that heroin reacts much more like the other opioids than morphine and that one because of this has to choose a pH a little highe than 9.1 for the NP wash ...
The pKa of diamorphine hydrochloride is 7.6, so I think 8.6 or slightly higher should be a good place to be.
Your two protocols do not make much sense. In the first - why wash with ether? (unless you mean petroleum ether). Why neutralize to pH 7 specifically (you'll be making salty water)? What do you mean by "neutralizing with water and Na2CO3"? (what is there to neutralize?) In the second - what do you mean by "shaking with chloroform" and drying?
For further purification, use activated charcoal (never heard of using magneisum oxide as a substitute, nor do I see any reason for that) after the last step and recrystallize (for morphine, forming the bitartarate salt and recrystallizing in ethanol should work very well - not sure about diamorphine).
bogumil
03-05-2006, 03:58 PM
Your two protocols do not make much sense. In the first - why wash with ether? (unless you mean petroleum ether). Why neutralize to pH 7 specifically (you'll be making salty water)? What do you mean by "neutralizing with water and Na2CO3"? (what is there to neutralize?) In the second - what do you mean by "shaking with chloroform" and drying?
The two procedures are both from heroinhelper.com.
From what I know the first wash is there to get rid of some impurities, which are soluble in Ether (Diethyl) at pH <4.
I think the first step is there to get rid of insoluble cuts, the second to get rid of the stuff soluble in ether at <4, the third just picks it up form the ether again. so its just an A/B I think.
I have been thinking the same if at 7 maybe only junk and salt precipitate out ... You too think, that below 9 not much heroin will be precipitating, or go into an NP, or?
The second procedure is more or less the same ... salt forming .. leaving insolubles behind, as well as stuff that prefers the aqueous ...
But Id be really glad if you could add some info ... BTW I have been digging for the diamorph - patents for months now. Ill definately post the info once I have it.
So you think that the stuff that precipitates out at 7 isnt diamorph but other junk? Then one could filter the precipitate and then raise the pH to 8.6 + and shake it with chloroform...
Maybe you want to read the original procedures from heroinheloer. Would be really great if you could help me with some of the stuff ...
http://www.heroinhelper.com
stvip
03-05-2006, 04:22 PM
Yes, but I think you would be better doing the NP wash with petroleum ether (or hexane, paraffin, whatever). Especially if you're starting from "black tar".
Anyway, my proposed procedure is explicitly meant to deviate from that posted in Heroin Helper (and Erowid), because I believe enabling the purification of street drugs is of the utmost importance to the community, yet using ethyl ether or chloroform is a rather questionable venue for harm reduction. Nevertheless:
The second procedure seems ok, except "shaking with chloroform and drying" is nonsensical - the idea is to allow the two layers to separate within the container (sufficient time should be given), then separate the layers between containers, and allow the chloroform to evaporate (and discard the aqueous portion). Perhaps that is what you meant to write. The other point is the 9.1 pH - should be ok, but remember that that figure relates to separating morphine from other opium alkaloids. Now then, after the chloroform has completely evaporated, you can form a salt in a solution, heat it with activated charcoal and filter the charcoal out. Then you can attempt to recrystallize. Note that the end product, while being relatively free from non-alkaloidal impurities, might still be a mixture of alkaloids. Also note this is all uselss if you're not using pure chemicals for the extraction.
As for what you're seeing precipitating out en masse at pH 7 - I don't know. Maybe salt formation was not complete?
Have I already mentioned that this is all theoretical? Good.
If you can't find the patents online, you could always walk to a local patent office and ask a clerk to help you - there could be plenty of legitimate reasons for your interest (he may also teach you the theory of opioid relativity, which is: travelling at the speed of light is fun)
By the way, I found this typo - heroinheloer somewhat amusing.
bogumil
03-05-2006, 05:07 PM
...
The second procedure seems ok, except "shaking with chloroform and drying" is nonsensical - the idea is to allow the two layers to separate within the container (sufficient time should be given), then separate the layers between containers, and allow the chloroform to evaporate (and discard the aqueous portion). Perhaps that is what you meant to write. The other point is the 9.1 pH - should be ok, but remember that that figure relates to separating morphine from other opium alkaloids. Now then, after the chloroform has completely evaporated, you can form a salt in a solution, heat it with activated charcoal and filter the charcoal out. Then you can attempt to recrystallize. Note that the end product, while being relatively free from non-alkaloidal impurities, might still be a mixture of alkaloids. Also note this is all uselss if you're not using pure chemicals for the extraction.
As for what you're seeing precipitating out en masse at pH 7 - I don't know. Maybe salt formation was not complete?
Have I already mentioned that this is all theoretical? Good.
If you can't find the patents online, you could always walk to a local patent office and ask a clerk to help you - there could be plenty of legitimate reasons for your interest (he may also teach you the theory of opioid relativity, which is: travelling at the speed of light is fun)
By the way, I found this typo - somewhat amusing.
Lol. Thanks man. Yes, thats what I meant, seperating and then driyng. SWIM will see what he finds in his experiments ...
JunkYardSaint
03-05-2006, 06:05 PM
This may be a stupid question, but I've not heard or seen this done before - for one thing I've never found the need to - but now a days I need to do something to make the tar here a little easier on SWIM's system, - so my question is, can SWIM follow these directions to purify or at least purify to a degree what we all know and love as "Mexican Mud"? I suppose I can find these items that would be best to use online at some sort of science website/store....but is this procedure the same one SWIM could use on tar? ... Thanks for your input.
bogumil
03-06-2006, 03:14 PM
I dont know which chemicals you can get ... For a good procedure wait for stvip to reply since he has a way better knowledge of chemistry. I can tell you what SWIM did and what will help you for sure to make it a little cleaner.
If you start with tar, you might want to get the wors junk out first ...
1. Put your tar in a vessel and pour 5x its weight water on it. For 1 gram that would be 5ml water for example. MAybe a little more, but I wouldnt add more than 8x the amount by weight.
2. The tar wont dissolve at this point because H and other opies dont dissolve that good in just water.
3. Because of that you will have to add an acid, which forms salts from the opies, called "salt-forming". Almost every acid will work. Preferred are citric (by far the healthiest), hydrochloric (HCl), sulfuric, acetic acid. I personally like HCl the most because you can easily make table salt from it with carbonates in case you added too much. So you add HCl, about 1 drop per ml. This is much HCl, but that beter than not enough acid ...
4. After you added it, you let it rest for a good amount of time and you do anything to get the tar as small as possible, like swirling, cutting (maybe even before you put it into the water), heating slightly (but not above 60C) and so on.
5. After, lets say 1 hour, maybe less, maybe more, depends on how easily it dissolves you go on. At this point the heroin and codeine and whatever there is in it opiatewise will have dissolved in the water and will be present in its salt form. Thats the reason why it dissolves: Salts dissolve very easily in water.
So you now filter it. Choose something with bigger pores firs, like coffee filters for example. Make sure to use small vessels and small filter papers and so on because this makes it way easier.
After the first filtration you can suck it up into a syringe and filter it through a millipore filter. This will make the solution wonderful clear and help you get rid of lots of junk. SWIM used millipores on H in solution and he can tell you it is great.
6. Now you can just add some base until the pH is 5 to 6.5. This pH makes sure the product gets along with your body pH well. So you add the base. Best is Na2CO3 because it forms table salt with any excess HCl and table salt is healthy, can even be injected, as long as it is solution. LOL. You can use NAOH instead or ammonia. I would use Na2CO3.
7. When the pH is adjusted you just put it in a flat vessel in the oven at 50C, place a fan in front of it and 3o minutes later it is dry. If not just let it stand a little onger. It might be oily, then you will have to wait another day so that you can chop it.
Thats about it. Easy, nothing hazardous is used (as long as you handle the HCl and the other things with care.
If you want it better and cleaner, you can do the following. But this now is something you shoud wait for more replies. SWIM did it ut he didnt have the best success, so better wait if there are improvements possible. Ok.
8. You dissolve the dried salt in water now. 5x the amount of the salt by weight again. Do this in a test tube which you can close with either your thumb or a rubber thing. If it doesnt dissolve 100%, add 1 or 2 drops of HCl. If then not everything has dissolved, filter it again.
9. Add 1/3 the volume NP. USe ether, toulene, chloroform or any of the NP that stvip mentioned.Shake it toughly for 2 minutes. Discard the NP or collect it in another (brown or in another way UV-resistant) vessel for later use. Repeat this 2 times.
10. Adjust the pH to 8.6 - 10, maybe starting with 8.6 and then going up with the pH until you reach 10. Shake it with chloroform or another NP like in step 9. First shaking pH 8.6, second shaking at pH 9.1, third shaking at pH 9.6 and the last at pH 10 for example. Chloro and ether are supposed to be the best for h, but they are also some of the most dangerous NPs. Keep the NP and collect it.
11. Then dry it. Thats it. Chop it and snort it, shoot it, whatever you want to do. But always make sure you filtered it well before shooting. USe a millipore for this. And for every product that you did produce yourself, snort some first to see, how it is. Dont shoot it before you know the effect.
stvip
03-07-2006, 05:55 AM
This may be a stupid question, but I've not heard or seen this done before
Err, the entire thread is devoted to answering that very question.
Bogumil: there are all kinds inaccuracies in your procedure, the majority of which I believe I've already addressed. For the success of the procedure, however, it is critical that you do not use chloroform for defatting (step 9 in your procedure), since it dissolves diamorphine HCl (as well as the base). In step 10, the base extraction, you most probably cannot use any NP solvent, but rather would have to rely on ethyl ether or chloroform (which is the whole point of why I suggested an alternative that does not require base extraction). Step 11: once again you have a base - most uses require resalting. For further purification reread my posts.
Nobody should be using in any manner an unpurified street drug.
bogumil
03-07-2006, 03:33 PM
Bogumil: there are all kinds inaccuracies in your procedure, the majority of which I believe I've already addressed.
Wisely, already assuming, that this might be the case, I wrote the following in the post above:
If you want it better and cleaner, you can do the following. But this now is something you shoud wait for more replies. SWIM did it ut he didnt have the best success, so better wait if there are improvements possible. Ok.
@JunkYardSaint: Just to take the confusion away: The steps 1 - 7 are proven to work and are a rather healthy and good way to clean your stuff. But make sure to check the pH and do not go below 3 and above 10 as this would pretty fast make MAM from the H.
The steps 8 - 11 need to be improved the way stpvip mentioned: Especially dont use chloroform if you want the H to stay in the aqueous. Basically what is done in these is that the heroin is first dissolved in the water, then with an NP junk is washed out. Then the H-solution is made a pH that makes it easily go into the NP (somewhere around 8.6 - 12 we found out ... maybe someone will somewhen find the heroin data). It is then shaken with NP and the NP seperated fro the aqueous and dried. So its: making salt (low pH) ... shaking with NP (at low pH) ... making pH x to make heroin almost insoluble in the water ... shaking with NP again ... pipetting /decanting NP off and drying it. The correct solvents and pHs are in the posts above. I havent put a 100% procedure together yet and am experimenting a bit here and there ... (says SWIM).
But I think for tar, to have a powder is already a nice improvement. So go from 1 - 7 and youll be happy.
BTW: I found in a doc about heroin that "the hydrolisis rate for heroin is markedly increased at extremes of pH (e.g. < pH3 and >pH 10) and as a result such routine tasks as liquid-liquid extractions need to be performed carefully." http://www.unodc.org/pdf/publications/report_st-nar-35.pdf
kramorph
03-15-2006, 08:13 AM
Cant DCM (dichloromethane) be used in place of chloroform +/or ether? Although Ive never even seen enough to even think about cleaning it, even if I did obtain a large enough amount to make it worthwhile, I'd be frightened I'd lose it somewhere in solution, or acidently pour it away. So I suppose I will stick to my tried and true method, use a piece if cigarette filter, or cotton wool.Or if you are concientious a pill filter. Always a good idea to filter it coz there is nothing worse than a blocked syringe lol.
electros[h]ockpatient
03-16-2006, 06:50 PM
who correctly believe they should not handle such dangerous chemicals (flammable, anaesthetic, carcinogenic, and with a tendency to degrade into even more dangerous substances), to nevertheless be able to clean their dose (though I get the feeling some people here are thinking "mmm... cancer! They might give me some morphine or fentanyl at the terminal stages!").
i have little formal (or otherwise learned) knowledge to follow your seemingly "chemist" approach to cleansing street dope, but i found that little quip hilarious :D
stvip
03-18-2006, 07:15 PM
The steps 1 - 7 are proven to work and are a rather healthy and good way to clean your stuff.
Steps 1-7 are nothing but a filtration, that leaves you with a product that is neither clean nor healthy, but merely not ridiculously contamined with insoluble particles.
Cant DCM (dichloromethane) be used in place of chloroform +/or ether?
Possibly, but probably not.
Although Ive never even seen enough to even think about cleaning it, even if I did obtain a large enough amount to make it worthwhile, I'd be frightened I'd lose it somewhere in solution, or acidently pour it away
These types of procedures should be well suited to small (even per-dose) amounts.
Always a good idea to filter it coz there is nothing worse than a blocked syringe lol.
How about a blocked blood vessel? Say, one that feeds your brain. That could really ruin your day. It's really hard shooting up without a brain, that's why you seldom see lettuces with needles, or a disc-player wielding a syringe (though I did once see a carrot using a needle, long story).
Opiyum
03-18-2006, 07:33 PM
Yeah I wish I paid attention more in chemistry class...I guess I should say I wish I enrolled for the chemistry class I never took.
And were the fuck are all these chemistry wiz Dope fiends coming from anyway I've never met a junky with this kind of intellect. My theory is the smart ones were all meth cooks because of all the dopers I've met only two talked like you guys and they were both cooks.
In an unrelated topic I got an 1180 on my SAT's....suck an egg
This is all very impressive and such, but what IS heroin? A molecule that looks mostly like morphine I 'spose. Is it water soluble as are opiates in poppy heads?
bogumil
04-04-2006, 07:41 PM
Look, what I found:
DETAILED ANALYSIS:
Separations based on chloroform extraction from HCl solution. The following method was originally devised chiefly as a means of separating diacetyl-morphine as such from quinine (without hydrolyzing the former to morphine). However, its utility goes far beyond this separation.
A.
Put a weighed quantity of the sample, estimated to yield not over 0.2 gramme diacetylmorphine (generally 1 to 5 grammes of the usual adulterated and diluted sample), into a separatory funnel.
Treat with 5 to 15 cc cold diluted HCl (10% by volume of concentrated HCl). The larger amount is used when it is necessary to take 5 to 10 grammes of the sample because of an extremely low content of diacetylmorphine. Some undissolved lactose can be disregarded.
In a second separatory, put 2 to 2.5 cc cold diluted HCl; in a third separatory, 25 cc water plus 0.5 cc concentrated NH 4OH solution; in a fourth separatory, 25 cc water.
Extract 5 times, with 30 to 20 cc chloroform each time. Filter through cotton in the stem of the separatory into the second separatory.
Shake each extract in turn with the wash HCl solution in the second separatory and filter into the third separatory. Also shake each with the ammo-niacal solution and filter into the fourth separatory. Also shake each extract with the wash water, and finally filter into a weighed glass dish or beaker.
Finally, shake the wash HCl in separatory #2 with an additional 20 cc chloroform, and take this extract along to separatory #4, withdrawing all the chloroform from #3 and finally from #4, and filtering into the weighed dish or beaker.
Evaporate the chloroformic extracts. The residue is primarily diacetylmorphine; it frequently also contains acetylcodeine, and may also contain papaverine, methadone, or caffeine. (See E.)
B. (8) Barbiturates, if present, will be in the ammoniacal solution. They may be separated by acidifying and extracting with chloroform.
C. (9) If the determination of quinine is the prime consideration at this stage, it is only necessary to combine the HCl solutions, make alkaline with NaOH, and extract the quinine with chloroform. The aqueous solution can then be reacidified, made ammoniacal, and any morphine present extracted with 3:1 chloroform-isopropanol. Such morphine is actually the morphine equivalent of the monoacetyl-morphine and morphine of the original sample. Codeine, if present as such in the original sample, would be mostly left with the quinine, and extracted with it, but this very seldom occurs, as apparently the codeine is practically all acetylated in most samples. Procaine, if present, is left in the HCl solution by the extractions under A. It can be determined by method 8, below.
D. (10) For poorly acetylated samples, combine the HCl solutions after the extraction given under A, but instead of making alkaline with NaOH as in C, neutralize the acid gradually with NH 4OH while cooling, and make slightly ammoniacal. Then extract with CCl 4. This will extract the monoacetyl-morphine, leaving the morphine in the aqueous layer. The morphine can then be extracted with 3:1 chloroform-isopropanol. Quinine, if present, will come out with the monoacetylmorphine, and after weighing or titrating the residue the quinine can be extracted from alkali solution, and the monoacetylmorphine (or morphine, if it has become hydrolyzed) extracted from ammoniacal solution with chloroform-isopropanol, titrated, and the titration calculated as monoacetylmorphine. Procaine, if present, would also come out in the CCl 4 in this step.
E. (11)In order to determine the various alkaloids in the residue from the chloroform extracts of procedure A, the hydrolysis method is used. When the sample has evidently been made from an impure morphine, the papaverine and codeine are of interest (the latter comes from acetylcodeine reconverted to codeine by hydrolysis), and they are separated from the morphine by shaking out the solution, after making it alkaline, with CCl 4. Methadone, if present, is separated from the morphine resulting from the hydrolysis in the same way. No detailed studies have yet been made on its separation from codeine and papaverine.
(12) In the case of codeine and papaverine, the alkaloids are recovered from the CCl 4 by shaking with dilute H 2SO 4 solution. Papaverine is then shaken out of the dilute H 2SO 4 solution with chloroform. The chloroform extracts are washed with dilute ammonia solution and water, and evaporated. The H 2SO 4 solution is then made alkaline and extracted for codeine.
(13) Usually, it is sufficient to determine the diacetylmorphine by difference, by merely subtracting the weights found for papaverine and codeine from the weight of residue found at step (7). The aqueous solution of step (12) can be reacidified, and shaken with CHCl 3 to remove any caffeine that may still be present (after acid hydrolysis). (To determine caffeine, however, it is better to process the original sample as in procedure 4 or 5.) The aqueous solution can then be made ammoniacal and extracted with 3: 1 chloroform-isopropanol to recover the morphine, from which the original diacetylmorphine can be calculated.
http://www.harmreduction.org/index.html?research/heroin_info.html
sebastian869
01-24-2007, 10:33 PM
Both chloroform and (di)ethyl ether are highly flammable, as well as being volatile anaesthetics. Chloroform is a carcinogen and degrades into phosgene (WWI poison gas). Ethyl ether tends to form an explosive peroxide.
Here is my suggested alternative for cleaning (not purifying):
1. Salt formation: place in warm water/ethanol, acidify with a clean acid (citric acid or acetic acid, preferably) until everything dissolves.
2. Filter insolubles. Save filtrate.
3. Precipitation of base: with a premixed basic solution (sodium hydroxide or calcium hydroxide in water), adjust the pH to about 8.5. Allow the alkaloids to settle on the bottom of the container.
4. Carefully remove the supernatant (preferably by pipetting).
5. Add more basified water and repeat 4. until supernatant is clear.
6. For smoking - evaproate and leave as is. For oral, rectal or intranasal use - acidify again.
Possible variations: after the second step, evaporate the solution, and perform an NP wash. Activated charcoal could also be useful.
This is all in febrile, demented theory, of course.
Is this the "paper" you were going to post on the other thread? For converting morphine to H?
OxyContinuously
01-25-2007, 10:06 AM
I won't address some of the guesses and speculation that is apparent in this thread; I'll just offer my suggestion that *works* and is fact, not inference.
Here's a very simple procedure that shoud work. (Don't get me wrong; what I mean is that the theory is sound, but I have not personally done it)
You'll need a moderately strong acid (not sulfuric, or nitric no no no these are wrong for the final product that must be soluble and usable by the body as far as absorption is concerned.; try maybe muriatic (hydrochloric) or a strong citric acid) remember, the form of H good for snorting, or injecting if that's your thing should be a hydrochloride salt, but your body will accept a citrate; in other words, it will work just as well. The only thing is that if you are not in a lab setting, you may have trouble getting conc. citric acid, so HCl in the form of "muriatic" acid can be found at Joe Shmoe Hardware and works just fine.
you will need, unfortunately, an ether, or chloroform or something similar. I say unfortunate, cause these compounds are flammable and can hurt/burn you pretty badly. You could obtain the ether from diesel starting fluids.
you will need a strong base. Clear ammonia probably is the easiest to come by, although NaOH *could* work too.
basically, first combine the acid, and the dope; add a sprinkle of water, then basify with the ammonia but do it right: in other words try to use a dropper (a pipette is best but do what you can), yada yada
if you did it right, some solids'll form, but now is when u need the ether (or the chloroform) and dissolve the solution in the ether or chloroform; give it a bit to let the water separate from the solution, the use your trusty dropper to get rid of the water
pretty much done. wash this ether/dope mixture with water and some of the HCl i mentioned before. then please separate the ether from the solution.
youll have a liquid so put it in a dish or somehting and add calcium carbonate, or baking soda or something like that (when i say something like that i dont mean anything--all im saying is that you can use a couple diff. carbonates, whatever you can get easily. baking soda is probably the easiest, so use baking soda)
mix with the solution in the dish you have separated from the ether, etc. wait till the reaction stops, and let it evaporate.
ta da!! dope.
note: if you use hydrochloric acid, your end result will be heroin hydrochloride, if you used citric acid, you'll have heroin citrate, get it?
I purposely didnt put down maesurements and all that. This is the theory, and if you are skilled enough to do it, you'll know exactly how much of each to use. if anyone seriously gets stuck or anything, PM me and I'll be happy to guide you.
take care guys
oxy
stvip
01-25-2007, 11:45 AM
The procedure above is the exact same one found at HH and posted at the start of this thread, albeit written less clearly. A few notes to keep people safe: Citric acid is widely available in pure form meant for human consumption at various grocery shops. Tartaric acid is another good alternative. Talk about "concentrated citric acid" and supposed trouble finding it is rubbish, it is available in pure crystal (solid) form. You cannot use any muriatic acid from a hardware store - muriatic acid meant for industrial use (cleaning pipes and the like) is often contaminated with arsenic and heavy metals. Be careful. As for sulfuric acid, I see no particular reason why it wouldn't be a suitable substitute (in fact, in the US, Avinza and MS-Contin, for example, are morphine sulfate). Talk about "the body accepting" this or that salt is nonsense. Another possible acid to use which is easily available in pure form is acetic acid (though at least in the case of morphine, the salt isn't very stable). Some combinations of base/acid/solvent may be problematic, however. For example, what is suggested above - using hydrochloric acid and chloroform is wrong, because diamorphine hcl is soluble in chloroform, and hence would be lost when the chloroform is discarded.
sebastian869
01-25-2007, 10:44 PM
I won't address some of the guesses and speculation that is apparent in this thread; I'll just offer my suggestion that *works* and is fact, not inference.
Here's a very simple procedure that shoud work. (Don't get me wrong; what I mean is that the theory is sound, but I have not personally done it)
You'll need a moderately strong acid (not sulfuric, or nitric no no no these are wrong for the final product that must be soluble and usable by the body as far as absorption is concerned.; try maybe muriatic (hydrochloric) or a strong citric acid) remember, the form of H good for snorting, or injecting if that's your thing should be a hydrochloride salt, but your body will accept a citrate; in other words, it will work just as well. The only thing is that if you are not in a lab setting, you may have trouble getting conc. citric acid, so HCl in the form of "muriatic" acid can be found at Joe Shmoe Hardware and works just fine.
you will need, unfortunately, an ether, or chloroform or something similar. I say unfortunate, cause these compounds are flammable and can hurt/burn you pretty badly. You could obtain the ether from diesel starting fluids.
you will need a strong base. Clear ammonia probably is the easiest to come by, although NaOH *could* work too.
basically, first combine the acid, and the dope; add a sprinkle of water, then basify with the ammonia but do it right: in other words try to use a dropper (a pipette is best but do what you can), yada yada
if you did it right, some solids'll form, but now is when u need the ether (or the chloroform) and dissolve the solution in the ether or chloroform; give it a bit to let the water separate from the solution, the use your trusty dropper to get rid of the water
pretty much done. wash this ether/dope mixture with water and some of the HCl i mentioned before. then please separate the ether from the solution.
youll have a liquid so put it in a dish or somehting and add calcium carbonate, or baking soda or something like that (when i say something like that i dont mean anything--all im saying is that you can use a couple diff. carbonates, whatever you can get easily. baking soda is probably the easiest, so use baking soda)
mix with the solution in the dish you have separated from the ether, etc. wait till the reaction stops, and let it evaporate.
ta da!! dope.
note: if you use hydrochloric acid, your end result will be heroin hydrochloride, if you used citric acid, you'll have heroin citrate, get it?
I purposely didnt put down maesurements and all that. This is the theory, and if you are skilled enough to do it, you'll know exactly how much of each to use. if anyone seriously gets stuck or anything, PM me and I'll be happy to guide you.
take care guys
oxy
Oxy I was just wondering, why would you not give directions for converting morphine sulfate to diamorphine, yet you're willing to give these?
Since I agree with you that novices should not do the procedure, dont you think if you gave clear and comprehensive directions you could actually help some one who will try the procedure from getting hurt? Especially since you said that the direction currently available on the net are not complete.
Also, are there substitute chems that are able to be used for the process that are safer that AA for example?
Thanks
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