Making pure Delta9-THC oil

canndo

Well-Known Member
No, this is Dr. Atomic's Hash multiplier, named that because they actually thought they were preforming alchemy. The "alchemy" was really just taking not so active cannabinoids and turning them into the most active cannabinoid possible. Just read the first post, this is all in the first post.

But that is what the iso- thing was supposed to do as well. I read the piece, frankly Fin, it is too rudamentary for me, I like to know the mechanics or the chemsitry of things a bit more thorougly, I am not faulting you at all here - we must always decide upon our audience, sometimes explainations don't work for everyone.


and.... I dont know about the bong thing - what does acetone and petrolium ether do to an acrylic bong?
 

canndo

Well-Known Member
You're really grasping at straws :lol: You would use a glass bong dipshit :dunce:
Wait a minute Fin, I am on your side here, but lots of folks might use acrylic unthinkingly and I am not even sure that acrylic won't withstand those solvents.


All I want to know is why it works as touted, I don't doubt that it may well work, I went back and re-read it and it looks like your first wash would take out most of the waxes and such. What does each step do chemicaly is all I am wondering. I see that you have been beaten up here, I'm not one of them - k?
 

Finshaggy

Well-Known Member
Wait a minute Fin, I am on your side here, but lots of folks might use acrylic unthinkingly and I am not even sure that acrylic won't withstand those solvents.


All I want to know is why it works as touted, I don't doubt that it may well work, I went back and re-read it and it looks like your first wash would take out most of the waxes and such. What does each step do chemicaly is all I am wondering. I see that you have been beaten up here, I'm not one of them - k?
I'm actually going to have to rewrite it, I missed a step. Let me pull up the old book and get everything.
 

Finshaggy

Well-Known Member
Initial Extraction ~~~~~~~~~~~~~~~~~~ In a previous version of this file, I recommended ethyl alcohol as the menstruum (solvent) for the initial extraction. However, after further reading and experimentation, I now recommend acetone instead of alcohol. THC's solubility in acetone is, it would seem, much greater than with any other solvent (except for petroleum ether, which we use in stage 2 to purify this first-stage oil). The reason? Alcohols are too water soluble for the best possible purity, and too many other non-psychoactive materials remain in the finished oil. In the interest of brevity, and to save wear and tear on your obedient typist's fingers, it's your own responsibility when reading the following to substitute "acetone" wherever you see "alcohol" used. Fill a large pot with water, and heat to boiling. Place in the water a glass jar filled with loosely packed, cleaned female flowers of cannabis. (Male flowers and even leaves may be used, but only if there is no other alternative.) Add sufficient solvent to completely cover cannabis. Solvent may be any alcohol of 95% or greater purity (i.e., rubbing alcohol works), but ethyl alcohol is best, as it is non-toxic and will not harm you if you "screw up". My personal recommendation is either 99.99% laboratory alcohol, or, since this is damn difficult to acquire, Everclear 190 proof grain alcohol. 151 proof rum isn't the greatest, but if the others are too hard to acquire, this may be your only option. MAKE SURE THAT THE SMALL GLASS JAR IS HELD IN PLACE SOMEHOW! Otherwise, when enough of the solvent boils away, the jar will be light enough that the water pressure will tip it over, and then you will be extremely unhappy (and possibly unlucky enough to witness a gigantic ball of flame lighting up your kitchen, and maybe even yourself). A set of rubber lab grips attached to a heavy base works nicely. Place a watchglass over the top of the jar so that the alcohol will be constantly recirculated instead of boiling off, and keep water at a gentle boil for three to four hours. Let everything cool, and strain all liquid thoroughly from the plant fibers. Place fibers in a cast iron skillet. Ignite the alcohol to burn it off, and while you continue with the extraction of the essence, keep a very low flame under the ashes of the fibers for one hour, stirring them occasionally. If you have an assistant, it's best to have them stir the ashes while you keep working with the essence. To remove the alcohol, you need an accurate thermometer. Set up the system the same way as before, but this time, do not cover the jar. Place thermometer in jar and heat the essence to 220F. Keep a small mirror held over the jar. When the mirror stops fogging up -- i.e., no more steam -- enough of the water has boiled away. IMMEDIATELY turn off the heat and remove the jar from the hot water (don't forget to wear gloves!). This is crude extract, and can contain anywhere from 10 to 50 percent THC. It's perfectly all right to use this oil any way you like. But you can do better.
 

Finshaggy

Well-Known Member
Purification Stage ~~~~~~~~~~~~~~~~~~ To further extract and purify the essence, petroleum ether must be used as the solvent. USE ONLY ELECTRIC HEAT WITH A QUICK SHUTOFF SWITCH, AND DON'T LET OPEN FLAME ANYWHERE NEAR YOU! Petroleum ether is one of the most explosively flammable things in existence, so treat it accordingly -- keep any ether in extremely well-sealing containers and store only in appropriate locations which will not have sparks, flamers, or heat. This article formerly recommended freezing ether, but one problem with this suggestion is that most freezers have a circulating fan that could cause a small spark. Even at normal freezer temperatures, ether is still quite volatile and can leak slowly from many containers. [Edited by Erowid: Feb 26, 2002] Dissolve the crude extract from the previous step in 5 times its own weight of ether, amd add to this volume an equal volume of water. Both the water and the ether must be as cold as possible. Close the holding container TIGHTLY, and gently shake up and down. Uncap to relieve pressure buildup, re-cap, and repeat until you're sick of it. Set it down somewhere cool and safe, where it won't get knocked or vibrated, and let it settle into layers. This will take about a half hour. (The bottom layer consists of alcohol, water, tars, and minor resins. The next layer up is the emulsion layer, and the top layer is the ether extract which is holding the THC in suspension.) Now you need to blow the bottom two layers into another container, which is easy to do if you set up the first container as a bong. Attach a tube to where the bowl would normally go and hang the other end in the sink. Very gently, blow into the tube where you would normally inhale. MAKE SURE THE BOTTOM END OF THE TUBE THAT EXTENDS DOWN INTO THE CONTAINER IS *ALL* THE WAY DOWN TO THE BOTTOM! Otherwise, you will blow all the good stuff into the sink, and you will be very unhappy. Just watch the water level, and don't blow too hard. Don't try to get every last drop; just get as much as you can without getting too close to the ether-THC layer. If you like, add more ether and water and repeat this stage. When it's purified enough for your taste, cook the ether extract in the double boiler at 104F to evaporate the ether, again making sure to hold the extract jar in place. This being the next step up from crude, I guess you'd call this resulting sticky stuff "forty-weight", or something like that. And, as before, it's perfectly fine to stop here. Read on for the gory details on the final stage...because you know you can do better.
 

Finshaggy

Well-Known Member
Isomerization ~~~~~~~~~~~~~ This stage rotates all the existing lesser cannabinoids and cannabinols into THC, and all the existing THC into the most active isomer, delta-9-THC. This step involves the use of sulfuric acid, so I shouldn't have to remind you to wear long rubber gloves, don't inhale its fumes, DON'T TREAT IT CASUALLY BECAUSE IT CAN EAT HOLES IN LOTS OF THINGS, INCLUDING YOU. Dissolve the extract in 10 times its own weight in ether. SLOWLY, add one drop of sulfuric acid for each gram of extract, stirring with a glass rod. Heat as in the initial extraction, with the jar covered by a watchglass. Cook two hours, stirring occasionally, and allow to cool. Mix the solution with an equal volume of cold water and one-half its volume of cold ether, and repeat the shaking and separation steps. Take extract and slowly add the calcined ash from the first extraction. Stir it all in, and run the solution through filter paper to strain the ash sediment out. Check for any remaining acid by adding a small pinch of sodium bicarbonate (baking soda). If the solution fizzes, keep adding bicarb very slowly until fizzing stops. Add fresh water and ether, shake and separate. Cook at 104F until the ether is evaporated. Voila! You now have essence of cannabis, which can contain anywhere from 85 to 99 percent THC
 

Finshaggy

Well-Known Member
I will do the procedure myself eventually and once I have done that I will be able to explain it better, and will have documentation that people can follow.
 

Finshaggy

Well-Known Member
Initial Extraction ~~~~~~~~~~~~~~~~~~ In a previous version of this file, I recommended ethyl alcohol as the menstruum (solvent) for the initial extraction. However, after further reading and experimentation, I now recommend acetone instead of alcohol. THC's solubility in acetone is, it would seem, much greater than with any other solvent (except for petroleum ether, which we use in stage 2 to purify this first-stage oil). The reason? Alcohols are too water soluble for the best possible purity, and too many other non-psychoactive materials remain in the finished oil. In the interest of brevity, and to save wear and tear on your obedient typist's fingers, it's your own responsibility when reading the following to substitute "acetone" wherever you see "alcohol" used. Fill a large pot with water, and heat to boiling. Place in the water a glass jar filled with loosely packed, cleaned female flowers of cannabis. (Male flowers and even leaves may be used, but only if there is no other alternative.) Add sufficient solvent to completely cover cannabis. Solvent may be any alcohol of 95% or greater purity (i.e., rubbing alcohol works), but ethyl alcohol is best, as it is non-toxic and will not harm you if you "screw up". My personal recommendation is either 99.99% laboratory alcohol, or, since this is damn difficult to acquire, Everclear 190 proof grain alcohol. 151 proof rum isn't the greatest, but if the others are too hard to acquire, this may be your only option. MAKE SURE THAT THE SMALL GLASS JAR IS HELD IN PLACE SOMEHOW! Otherwise, when enough of the solvent boils away, the jar will be light enough that the water pressure will tip it over, and then you will be extremely unhappy (and possibly unlucky enough to witness a gigantic ball of flame lighting up your kitchen, and maybe even yourself). A set of rubber lab grips attached to a heavy base works nicely. Place a watchglass over the top of the jar so that the alcohol will be constantly recirculated instead of boiling off, and keep water at a gentle boil for three to four hours. Let everything cool, and strain all liquid thoroughly from the plant fibers. Place fibers in a cast iron skillet. Ignite the alcohol to burn it off, and while you continue with the extraction of the essence, keep a very low flame under the ashes of the fibers for one hour, stirring them occasionally. If you have an assistant, it's best to have them stir the ashes while you keep working with the essence. To remove the alcohol, you need an accurate thermometer. Set up the system the same way as before, but this time, do not cover the jar. Place thermometer in jar and heat the essence to 220F. Keep a small mirror held over the jar. When the mirror stops fogging up -- i.e., no more steam -- enough of the water has boiled away. IMMEDIATELY turn off the heat and remove the jar from the hot water (don't forget to wear gloves!). This is crude extract, and can contain anywhere from 10 to 50 percent THC. It's perfectly all right to use this oil any way you like. But you can do better.
This part basically says to do a regular extraction with acetone (I have a video of one on YouTube if you need help) . And to keep the plant material which you extracted from and burn it to ash in a pan. The acetone extraction should be a black colored oil/tar, and the ashes should be left separate.
 

Finshaggy

Well-Known Member
Purification Stage ~~~~~~~~~~~~~~~~~~ To further extract and purify the essence, petroleum ether must be used as the solvent. USE ONLY ELECTRIC HEAT WITH A QUICK SHUTOFF SWITCH, AND DON'T LET OPEN FLAME ANYWHERE NEAR YOU! Petroleum ether is one of the most explosively flammable things in existence, so treat it accordingly -- keep any ether in extremely well-sealing containers and store only in appropriate locations which will not have sparks, flamers, or heat. This article formerly recommended freezing ether, but one problem with this suggestion is that most freezers have a circulating fan that could cause a small spark. Even at normal freezer temperatures, ether is still quite volatile and can leak slowly from many containers. [Edited by Erowid: Feb 26, 2002] Dissolve the crude extract from the previous step in 5 times its own weight of ether, amd add to this volume an equal volume of water. Both the water and the ether must be as cold as possible. Close the holding container TIGHTLY, and gently shake up and down. Uncap to relieve pressure buildup, re-cap, and repeat until you're sick of it. Set it down somewhere cool and safe, where it won't get knocked or vibrated, and let it settle into layers. This will take about a half hour. (The bottom layer consists of alcohol, water, tars, and minor resins. The next layer up is the emulsion layer, and the top layer is the ether extract which is holding the THC in suspension.) Now you need to blow the bottom two layers into another container, which is easy to do if you set up the first container as a bong. Attach a tube to where the bowl would normally go and hang the other end in the sink. Very gently, blow into the tube where you would normally inhale. MAKE SURE THE BOTTOM END OF THE TUBE THAT EXTENDS DOWN INTO THE CONTAINER IS *ALL* THE WAY DOWN TO THE BOTTOM! Otherwise, you will blow all the good stuff into the sink, and you will be very unhappy. Just watch the water level, and don't blow too hard. Don't try to get every last drop; just get as much as you can without getting too close to the ether-THC layer. If you like, add more ether and water and repeat this stage. When it's purified enough for your taste, cook the ether extract in the double boiler at 104F to evaporate the ether, again making sure to hold the extract jar in place. This being the next step up from crude, I guess you'd call this resulting sticky stuff "forty-weight", or something like that. And, as before, it's perfectly fine to stop here. Read on for the gory details on the final stage...because you know you can do better.
This part says to take that acetone extraction and put it into Petroleum Ether/Naptha, and it will dissolve. Then mix that that with water. The water should take the bad stuff (Oils and everything that Canndo was talking about), while the Ether grabs all the alkaloids/cannabinoids. This is where you would use a bong like I said.
 

Finshaggy

Well-Known Member
Isomerization ~~~~~~~~~~~~~ This stage rotates all the existing lesser cannabinoids and cannabinols into THC, and all the existing THC into the most active isomer, delta-9-THC. This step involves the use of sulfuric acid, so I shouldn't have to remind you to wear long rubber gloves, don't inhale its fumes, DON'T TREAT IT CASUALLY BECAUSE IT CAN EAT HOLES IN LOTS OF THINGS, INCLUDING YOU. Dissolve the extract in 10 times its own weight in ether. SLOWLY, add one drop of sulfuric acid for each gram of extract, stirring with a glass rod. Heat as in the initial extraction, with the jar covered by a watchglass. Cook two hours, stirring occasionally, and allow to cool. Mix the solution with an equal volume of cold water and one-half its volume of cold ether, and repeat the shaking and separation steps. Take extract and slowly add the calcined ash from the first extraction. Stir it all in, and run the solution through filter paper to strain the ash sediment out. Check for any remaining acid by adding a small pinch of sodium bicarbonate (baking soda). If the solution fizzes, keep adding bicarb very slowly until fizzing stops. Add fresh water and ether, shake and separate. Cook at 104F until the ether is evaporated. Voila! You now have essence of cannabis, which can contain anywhere from 85 to 99 percent THC
And this one says to use Sulphuric acid (sorry for my mistake when trying to rehearse from memory, I accidentally said Acetic Acid before) to turn all Cannabinoids into THC and THC into Delta-9-THC, so this is where the real "magic" happens.
 

canndo

Well-Known Member
I was right - it is isomerization:

Direct isomerization

Sometimes if pot is totally rank and crappy, or you're dealing with a bunch of roaches, trimmings, or some other inferior source of THC it is desirable to go well beyond what a simple volatile solvent or super critical fluid extraction can do. You want to convert all those free available cannibidiols into more potent THC analogs and cannabinols.

This technique also will render a fully decarboxylized end product, as well as destroying many terpenes and aromatics which can improve or destroy a product depending on the original quality. It is important to understand this is not a full conversion to ƒ´9-THC, but to THC analogs and more active cannibidiols, and is included in this discussion more as an educational exercise. Basic isomerization takes place with a quick reflux of your cannabinoids in the presence of any H+ source (acid).

1. Treat your stuff as if it were a volatile solvent or critical fluid extraction.
2. With the remaining resin, dissolve it in a non-polar solvent. Be sure to use one that separates easily from water such as naphia or white gas.
3. Treat this mixture with sulphuric or hydrochloric acid until a pH around 1-2 is reached (approximately one drop of concentrated acid per gram of extract).
4. Place this in a reflux apparatus and cook it for about an hour. In case you¡¦re not familiar this is basically just Pyrex breaker with a large looped tube plugged into the top. This will cause the solution inside to be exposed to elevated pressures as well as temperatures, as well as preserving all of the original contents. Simply simply boiling the mixture in a small strong covered vessel can mimic it.
5. Wash what¡¦s left with water, keep the oil layer.
6. Neutralize your mix (bring it to pH 7.0) with a little Sodium Hydroxide solution (pH 9.0) or baking soda then rewash it with water. Save the oil layer again.
7. Allow your oil to evaporate and you should be left with a sticky amber liquid that contains almost pure THC.

I would recommend an extraction for a starting point, since if you start clean your product can only get much better. Once you¡¦ve obtained nearly pure THC, converting it to an acetate is supposed to produce more psychedelic like effects.




 

Finshaggy

Well-Known Member
I was right - it is isomerization:

Direct isomerization

Sometimes if pot is totally rank and crappy, or you're dealing with a bunch of roaches, trimmings, or some other inferior source of THC it is desirable to go well beyond what a simple volatile solvent or super critical fluid extraction can do. You want to convert all those free available cannibidiols into more potent THC analogs and cannabinols.

This technique also will render a fully decarboxylized end product, as well as destroying many terpenes and aromatics which can improve or destroy a product depending on the original quality. It is important to understand this is not a full conversion to ƒ´9-THC, but to THC analogs and more active cannibidiols, and is included in this discussion more as an educational exercise. Basic isomerization takes place with a quick reflux of your cannabinoids in the presence of any H+ source (acid).

1. Treat your stuff as if it were a volatile solvent or critical fluid extraction.
2. With the remaining resin, dissolve it in a non-polar solvent. Be sure to use one that separates easily from water such as naphia or white gas.
3. Treat this mixture with sulphuric or hydrochloric acid until a pH around 1-2 is reached (approximately one drop of concentrated acid per gram of extract).
4. Place this in a reflux apparatus and cook it for about an hour. In case you¡¦re not familiar this is basically just Pyrex breaker with a large looped tube plugged into the top. This will cause the solution inside to be exposed to elevated pressures as well as temperatures, as well as preserving all of the original contents. Simply simply boiling the mixture in a small strong covered vessel can mimic it.
5. Wash what¡¦s left with water, keep the oil layer.
6. Neutralize your mix (bring it to pH 7.0) with a little Sodium Hydroxide solution (pH 9.0) or baking soda then rewash it with water. Save the oil layer again.
7. Allow your oil to evaporate and you should be left with a sticky amber liquid that contains almost pure THC.

I would recommend an extraction for a starting point, since if you start clean your product can only get much better. Once you¡¦ve obtained nearly pure THC, converting it to an acetate is supposed to produce more psychedelic like effects.




Yeah it's isomerization, but you were talking about something with isopropyl and a reflux something before. And that whole reflux step in yours is unnecessary. I believe that the reason you save the plant material and the ash is actually used somehow with the sulfuric acid. I'm pretty sure that's why it tells you to keep it. This was something ANYONE could do in the 60's. This wasn't something that you had to set any kind of lab equipment up for, and I know a reflux thingy isn't as simple as it really seems. I thought it would be easy when I was looking into muscimol, and it's precursor. And it's not just as simple as "evaporate and drip" even though that's what it looks like.
 

qwizoking

Well-Known Member
I know this is kinda old but I recently isomerized and acetalyzed some of my hash oil...googled it and found you...not sure what yall were talking about with ash and stuff I didn't feel like reading.. Anyway I use a crockpot to reflux also tried lecithen Wich works too.

Anyway how did you like it ?
 

qwizoking

Well-Known Member
Oh wow lol read a Few pages ...well if anyone has done this and actually knows chemistry I want to hear.....I thought my product was amazing if a but racy. But I did it on some mex brick weed do was very pleased
 
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