hash oil made with supercritical co2 extraction
- Thread starter heady blunts
- Start date
M
Mr. Mountain
Everything you need to know about making an "absolute" can be found on perfumery/essential oil websites.
BHO is a waxy "Concrete" full of lipids (this is why it's solid at room temp). These lipids are far less soluble in Ethanol (at a low temperature) than in a Hydrocarbon (such as butane)
They can be easily removed by re-dissolving the BHO in Ethanol (or 99% Iso) and placing the liquid in the freezer overnight. This will coagulate the lipids. Then I filter it off a few ounces at a time (with the filter rig in the fridge, to keep the alcohol cold during filtering.)
I leave the majority of the alcohol in the freezer during filtering for the same reason (to keep the waxes out of solution.)
After filtering I evaporate the solvent, usually on large pieces of plate glass under a fan or outside.
What is left is semi solid at best (usually a liquid) I use a pipette to suck it up and put it in vials for later use.
BHO is a waxy "Concrete" full of lipids (this is why it's solid at room temp). These lipids are far less soluble in Ethanol (at a low temperature) than in a Hydrocarbon (such as butane)
They can be easily removed by re-dissolving the BHO in Ethanol (or 99% Iso) and placing the liquid in the freezer overnight. This will coagulate the lipids. Then I filter it off a few ounces at a time (with the filter rig in the fridge, to keep the alcohol cold during filtering.)
I leave the majority of the alcohol in the freezer during filtering for the same reason (to keep the waxes out of solution.)
After filtering I evaporate the solvent, usually on large pieces of plate glass under a fan or outside.
What is left is semi solid at best (usually a liquid) I use a pipette to suck it up and put it in vials for later use.
Thanks Mr. M, but I think you misunderstood my question. I know that stuff.^^
What I wanted to know is why use the butane in the first place? Using a cold ethanol wash on your trim/bud in the first place leaves the fats/waxes behind, so you don't have to precipitate them out later. I assume the answer is that you get a higher yield using the butane, but I wanted to know how big of a difference, if it is worth the extra work. In my experience it is not, so I thought I must be missing something.
I know theoretically this is correct, but then why do people "clean up" their BHO with cold alcohol?
Greens are not precipitated from the frozen ethanol iirc.
Soxhlet gives the highest "yield", not butane.
The highest yield is obtained by simple ultrasonic extraction in a little chloroform and methanol. That is the most recommended method for quantitative analysis of the cannabinoid content of cannabis material.* (And apparently the terpenes: http://www.google.com/patents?id=ZJcbAAAAEBAJ)
The first fatality from exploding CO2 cylinders was Osmin ("the unfortunate M.") Hervy, Professor of Chemistry in the School of Pharmacy, Paris, explosion Dec. 30, 1840. The iron (2" thick) Thilorier cylinder of 3 liter capacity had been charged many times before and the process was routine. Just days after using the cylinder in front of 1200 students, the cylinder he was charging blew him through a closet door, broke one thigh and mangled the other, which was amputated the next day. He died 3 days after the explosion. The room was destroyed, but a witness survived.
*from Handbook of Forensic Drug Analysis:
A wide variety of extraction solvents and methods have been used to separate the cannabinoids and other compounds of interest from the plant material or the resins. They include soaking in petroleum ether (Barni Comparini and Centini, 1983; Stephanou et al., 1984), chloroform (Kanter et al., 1979; J.C. Turner and Mahlberg, 1984), or methanol (Björkman, 1982; Wheals and Smith, 1975; Nakahara and Sekine, 1985). Soxhlet extraction with cyclohexane has been used (Novotny et al., 1976). R.N. Smith and Vaughan (1976) used methanol–chloroform (9 : 1), as did Brenneisen (1984). Baker et al. (1980) also used methanol–chloroform (4 :1). Brenneisen and ElSohly (1988) compared various solvents and methods and concluded that methanol–chloroform (9 :1) gave the overall best extraction efficiency for the wide range of analytes in Cannabis. Sonication at room temperature of powdered sample with this solvent has become the method of choice for comparison studies with Cannabis.
Veress (1994) used Cannabis as an example for a method of optimizing extraction efficiency in supercritical fluid extraction (SCF) for quantification. An evaluation of the effect of particle size on the SCF extraction of Cannabis showed that selection of a given sieve fraction leads to erroneous conclusions about the sample as a whole (Eory et al., 2001a). SCF has been applied to the measurement of THC and THCA concentrations in plant material (Eory et al., 2001b).
Barni Comparini, I., and Centini, F. (1983). Forensic Sci. Int. 21, 129–137.
Stephanou, E., Lawi-Berger, C., and Kapetanidis, I. (1984). Pharm. Acta Helv. 59(8), 216–224.
Kanter, S.L., Musumeci, M.R., and Hollister, L.E. (1979). J. Chromatogr. 171, 504–508.
Turner, J.C., and Mahlberg, P.G. (1984). J. Chromatogr. 283, 165–171.
Björkman, S. (1982). J. Chromatogr. 237, 389–397.
Wheals, B.B., and Smith, R.N. (1975). J. Chromatogr. 105, 396–400.
Nakahara, Y., and Sekine, H. (1985). J. Anal. Toxicol. 9(3), 121–124.
Novotny, M., Lee, M.L., Low, C.E., and Raymond, A. (1976). Anal. Chem. 48(1), 24–29.
Smith, R.N., and Vaughan, C.G. (1976). J. Chromatogr. 129, 347–354.
Brenneisen, R. (1984). Pharm. Acta Helv. 59, 247–259.
Baker, P.B., Fowler, R., Bagon, K.R., and Gough, T.A. (1980). J. Anal. Toxicol. 4, 145–152.
Brenneisen, R., and ElSohly, M.A. (1988). J. Forensic Sci. 33(6), 1385–1404.
Veress, T. (1994). J. Chromatogr. A 668(2), 285–291.
Eory, L., Danos, B., and Veress, T. (2001a). Z. Zagadnien Nauk Sadowych 47, 322–327.
Eory, L., Szalay, V., and Veress, T. (2001b). Z. Zagadnien Nauk Sadosych 47, 328–332.
The first fatality from exploding CO2 cylinders was Osmin ("the unfortunate M.") Hervy, Professor of Chemistry in the School of Pharmacy, Paris, explosion Dec. 30, 1840. The iron (2" thick) Thilorier cylinder of 3 liter capacity had been charged many times before and the process was routine. Just days after using the cylinder in front of 1200 students, the cylinder he was charging blew him through a closet door, broke one thigh and mangled the other, which was amputated the next day. He died 3 days after the explosion. The room was destroyed, but a witness survived.
*from Handbook of Forensic Drug Analysis:
A wide variety of extraction solvents and methods have been used to separate the cannabinoids and other compounds of interest from the plant material or the resins. They include soaking in petroleum ether (Barni Comparini and Centini, 1983; Stephanou et al., 1984), chloroform (Kanter et al., 1979; J.C. Turner and Mahlberg, 1984), or methanol (Björkman, 1982; Wheals and Smith, 1975; Nakahara and Sekine, 1985). Soxhlet extraction with cyclohexane has been used (Novotny et al., 1976). R.N. Smith and Vaughan (1976) used methanol–chloroform (9 : 1), as did Brenneisen (1984). Baker et al. (1980) also used methanol–chloroform (4 :1). Brenneisen and ElSohly (1988) compared various solvents and methods and concluded that methanol–chloroform (9 :1) gave the overall best extraction efficiency for the wide range of analytes in Cannabis. Sonication at room temperature of powdered sample with this solvent has become the method of choice for comparison studies with Cannabis.
Veress (1994) used Cannabis as an example for a method of optimizing extraction efficiency in supercritical fluid extraction (SCF) for quantification. An evaluation of the effect of particle size on the SCF extraction of Cannabis showed that selection of a given sieve fraction leads to erroneous conclusions about the sample as a whole (Eory et al., 2001a). SCF has been applied to the measurement of THC and THCA concentrations in plant material (Eory et al., 2001b).
Barni Comparini, I., and Centini, F. (1983). Forensic Sci. Int. 21, 129–137.
Stephanou, E., Lawi-Berger, C., and Kapetanidis, I. (1984). Pharm. Acta Helv. 59(8), 216–224.
Kanter, S.L., Musumeci, M.R., and Hollister, L.E. (1979). J. Chromatogr. 171, 504–508.
Turner, J.C., and Mahlberg, P.G. (1984). J. Chromatogr. 283, 165–171.
Björkman, S. (1982). J. Chromatogr. 237, 389–397.
Wheals, B.B., and Smith, R.N. (1975). J. Chromatogr. 105, 396–400.
Nakahara, Y., and Sekine, H. (1985). J. Anal. Toxicol. 9(3), 121–124.
Novotny, M., Lee, M.L., Low, C.E., and Raymond, A. (1976). Anal. Chem. 48(1), 24–29.
Smith, R.N., and Vaughan, C.G. (1976). J. Chromatogr. 129, 347–354.
Brenneisen, R. (1984). Pharm. Acta Helv. 59, 247–259.
Baker, P.B., Fowler, R., Bagon, K.R., and Gough, T.A. (1980). J. Anal. Toxicol. 4, 145–152.
Brenneisen, R., and ElSohly, M.A. (1988). J. Forensic Sci. 33(6), 1385–1404.
Veress, T. (1994). J. Chromatogr. A 668(2), 285–291.
Eory, L., Danos, B., and Veress, T. (2001a). Z. Zagadnien Nauk Sadowych 47, 322–327.
Eory, L., Szalay, V., and Veress, T. (2001b). Z. Zagadnien Nauk Sadosych 47, 328–332.
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wow! this thread really bloomed in the last few days!
okay first off i'd like to disclaim the original post.
I DON'T MAKE OIL OF ANY KIND. just like to smoke it
when i posted this i had just gotten my prescription and had joined a collective that was selling "supercritical co2 hash oil."
now i'll use quotes, because although it was a decent hash oil, i have since learned more about the producer's character, and he has a bit of a swindler's reputation. after doing more research, i've decided this character is not capable of building a DIY extractor more complicated than a turkey baster BHO set up
so i'm almost 100% certain i got conned. my apologies for my shameful newb-ness.
on the other hand (barring the troll) mr. mountain, mofeta, lazyman, et al, have offered some very nice bits of information. thanks to you!
okay first off i'd like to disclaim the original post.
I DON'T MAKE OIL OF ANY KIND. just like to smoke it
when i posted this i had just gotten my prescription and had joined a collective that was selling "supercritical co2 hash oil."
now i'll use quotes, because although it was a decent hash oil, i have since learned more about the producer's character, and he has a bit of a swindler's reputation. after doing more research, i've decided this character is not capable of building a DIY extractor more complicated than a turkey baster BHO set up
so i'm almost 100% certain i got conned. my apologies for my shameful newb-ness.
on the other hand (barring the troll) mr. mountain, mofeta, lazyman, et al, have offered some very nice bits of information. thanks to you!
M
Mr. Mountain
To answer your question directly (sorry about that.) Yes, I do find it increases the yield. Also hash oil made in this manner is much more liquid than most quick wash I have made.
My quick wash usually comes out like little flakes of gold when you evap it on large pieces of plate glass. Yellow, brittle and shiny. But when it's placed in a vessel overnight it will turn into a solid (dark-ish amber) mass again.
I find absolutes (properly made) will almost never be solid, only viscus liquids and have a more "golden" color and generally taste better.
^^All of this is just my opinion of course, I'm sure many will disagree.
I smear it on papers, pipette it onto cigarettes (for concerts,) soak it back onto finished flowers and drip it onto just about everything!
Bottom line after 10 years of making BHO and quick wash, I have settled on this method. For now at least! I'm sure there is a better, higher yielding, cleaner procedure available.
Sadly I'm not an organic chemist!
(Those that are, feel free to chime in!)
Hope that answers your question, feel free to PM me.
Mr. M
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Hello from Southern CA and a borrowed computer!
Thanks brother mofetta for pointing out that I improperly used the word ambient temperature.
You are absolutely correct that liquid C02 is not at 75 psi when the temperature is 77F.
What I was how ever trying to communicate, is that you can extract using liquid C02, but it is not in a critical state until it reaches critical pressure and temperature.
I personally don't know that super critical state is required, but this thread is about super critical state and my intent in pointing out the pressures required, was to make it clear that it wouldn't be happening in a pressure cooker or a paint pot.
l looked at using liquid C02 and heating it up to obtain the pressure required. I designed a system to utilize that principle and it is posted here somewhere but I will post it again when I get back home to my own computer.
I used Schedule 160 316 SS pipe for my 4" X 24" pressure vessel, giving it greater than a 3X safety factor at burst.
I pre-pressurized the vessel to 150 psi, so that when I transferred the C02 from the Dewar, it didn't immediately freeze.
Back to vacation....... Hee, hee, hee...........
PS: I also included a back pressure regulator, so that anything above operating pressure was vented to atmosphere.
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Trichgnomes
Member
Interesting notes, Mr. Mountain. I too have dabbled in the realm of absolutes. I do find that properly made absolutes are incredibly smooth, but all of what I have considered to be properly purged came out glassy shatter, or maybe a bit tacky at best like fruit leather.
All of my results with absolutes have never been as flavorful as the original BHO it came from however. What is so amazing about butane as a solvent is its ability to extract the true essence of flavor from each strain.
I have had a very difficult time in both removing the ethanol while preserving the terpene content. I actually stopped making absolutes until I get a vacuum oven or different ethanol. Even when I am positive the alcohol is gone, there is sometimes a slight sweetness in the aftertaste that smells like the ethanol I have.
Theoretically, I should be able to remove it all without terpene degradation, but I have only be able to do one or the other.
I have been using Neutral Grape Spirits maybe I should switch to a different source of alcohol?
Anyways, I think I may start a new thread about flavor comparison of absolutes and concretes from the same starting material, as this is getting a bit off topic. Oiled out on some cheese concrete.. pics in the morning where they belong...
Ah, back home to the lair!
To put my input in perspective, I have never done Super Critical C02 extraction, but have designed and built other high pressure and cryogenic systems, so thought I would give it a try and kept it to a size that will fit in my home shop lathe, so that I might afford to build it.
I did some research on SCFE extraction and designed a front end system that uses liquid C02 to eliminate the pumps and refrigeration required and operates at 1500 psi.
I've attached a schematic showing how I thought one might achieve the super critical state using liquid C02 and heat.
The system uses a Dewar of liquid C02 with a dip tube, so that the gas head pressure can be drawn off as a gas, or it can be used to force liquid out the dip tube.
The process starts by pressurizing the 4" X 24" Schedule 160 SS pipe pressure vessel containing the plant material, so that when liquid is transferred, the whole thing doesn't turn into a block of dry ice.
The liquid is then heated using clamp on electric resistance pipe heaters heater, which drives up the pressure to super critical levels. Pressure above the 1500 psi operating pressure is vented off using a back pressure regulator, so that we maintain process pressure parameters, but prevent the vessel from over pressurizing and exploding at around 14,200 psi.
I chose stainless because of the loss of properties suffered by a carbon steel pressure vessels at cryogenic temperatures.
After the material has soaked for the prescribed period of time, the liquid is drained off into a secondary holding vessel, from which the C02 is bled off as a gas, leaving behind the oil.
I haven't finished the receiving vessel and bleed off design, as when I changed my computer from a 32 bit to a 64 bit program, my Auto Cad 2002 no longer works and they want $1900 for a Auto Cad 2012, that will work on a 64 bit program.
Given that I am now long since retired and can't justify the ~$2K just for play, I will pick up a cheap (~$200) computer for just running Auto Cad 2002 at 32 bits. Really sorry I already gave my old one away!
Now, having discussed the above, may I toss out a question?
Have any of ya'll with a SCFE unit, experimented with just using liquid C02 in a sub critical state, and what were the results?
Given that the meds that we seek are in the surface trichomes, vis a vis buried deep within the plant structure, is super critical state even necessary? Why do we need a super solvent?
As we previously discussed in this thread and for which the curves have been posted, C02 is liquid below the super critical point, so can we actually achieve an extraction at anywhere on the curve where the C02 is still in a liquid state?
To put my input in perspective, I have never done Super Critical C02 extraction, but have designed and built other high pressure and cryogenic systems, so thought I would give it a try and kept it to a size that will fit in my home shop lathe, so that I might afford to build it.
I did some research on SCFE extraction and designed a front end system that uses liquid C02 to eliminate the pumps and refrigeration required and operates at 1500 psi.
I've attached a schematic showing how I thought one might achieve the super critical state using liquid C02 and heat.
The system uses a Dewar of liquid C02 with a dip tube, so that the gas head pressure can be drawn off as a gas, or it can be used to force liquid out the dip tube.
The process starts by pressurizing the 4" X 24" Schedule 160 SS pipe pressure vessel containing the plant material, so that when liquid is transferred, the whole thing doesn't turn into a block of dry ice.
The liquid is then heated using clamp on electric resistance pipe heaters heater, which drives up the pressure to super critical levels. Pressure above the 1500 psi operating pressure is vented off using a back pressure regulator, so that we maintain process pressure parameters, but prevent the vessel from over pressurizing and exploding at around 14,200 psi.
I chose stainless because of the loss of properties suffered by a carbon steel pressure vessels at cryogenic temperatures.
After the material has soaked for the prescribed period of time, the liquid is drained off into a secondary holding vessel, from which the C02 is bled off as a gas, leaving behind the oil.
I haven't finished the receiving vessel and bleed off design, as when I changed my computer from a 32 bit to a 64 bit program, my Auto Cad 2002 no longer works and they want $1900 for a Auto Cad 2012, that will work on a 64 bit program.
Given that I am now long since retired and can't justify the ~$2K just for play, I will pick up a cheap (~$200) computer for just running Auto Cad 2002 at 32 bits. Really sorry I already gave my old one away!
Now, having discussed the above, may I toss out a question?
Have any of ya'll with a SCFE unit, experimented with just using liquid C02 in a sub critical state, and what were the results?
Given that the meds that we seek are in the surface trichomes, vis a vis buried deep within the plant structure, is super critical state even necessary? Why do we need a super solvent?
As we previously discussed in this thread and for which the curves have been posted, C02 is liquid below the super critical point, so can we actually achieve an extraction at anywhere on the curve where the C02 is still in a liquid state?
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Alcohol is highly polar and also extracts other undesirables, which the mostly non poplar butane avoids.
By using the two in sequence, you end up with the best of both worlds.
As a side note, I also wash my ISO and Methanol extracts with less agressive Ethanol, which drops out some of those undesirables.
Did this research include the oft-referenced, rarely read patents on the subject? They seem to be sound sources of information. Large flows of CO2 are prominent.
http://www.google.com/patents?id=kraGAAAAEBAJ
http://www.google.com/patents?id=1N2oAAAAEBAJ
Thanks GOJ! Good stuff, both of which highlight that C02 extraction actually works better sub critical and mixed with other solvents, but requires a lot of C02 flow, as you have just pointed out.
These folks are not soaking cannabis in liquid C02, but steadily pumping the liquid through the material for extended periods, to achieve best results.
I will check on cryopumps, but I am unaware of any cheap ones at this point.
Ohmmmmmmmmmmmmmmmmmmmmmm!!!!!!!!!!!!!!!!!!!!!!1
I think lazyman made the only real point regarding extraction off TCH using CO2 at its tripelphase all the vessel i see are so small that u cant run any materiale thu.
Like a tumbler can take kilos at a time and process alot off materiale.
One important point in hash making is that u concentrate so u start with alot off materiale and work u way to purity.
U could put u dry sift in a 30.000 dollar lab equipmet to get out some very pure stuff but if u just are going to smoke it that would be stupid one could just smoke to puffs more off u dry sift and get just as high.
But if u want to make some lab grade pure cannabinols then maby CO2 extraction is the way but i think the labs that do that stuff go another rute much more chemical using many solvents and steps.
I dont think u need to get to scientific about making u concentrate make some dry sift or waterworks and get a clean solvent and make some insane strong oil..
But wow this tread is lame and make me think how many in here really make hash.
Sorry but have fore along time missed oure good convos about hash, I learned alot from this subforum.
Like a tumbler can take kilos at a time and process alot off materiale.
One important point in hash making is that u concentrate so u start with alot off materiale and work u way to purity.
U could put u dry sift in a 30.000 dollar lab equipmet to get out some very pure stuff but if u just are going to smoke it that would be stupid one could just smoke to puffs more off u dry sift and get just as high.
But if u want to make some lab grade pure cannabinols then maby CO2 extraction is the way but i think the labs that do that stuff go another rute much more chemical using many solvents and steps.
I dont think u need to get to scientific about making u concentrate make some dry sift or waterworks and get a clean solvent and make some insane strong oil..
But wow this tread is lame and make me think how many in here really make hash.
Sorry but have fore along time missed oure good convos about hash, I learned alot from this subforum.
Bubbly Terps
Member
I'm confused, people say that the guy who got banned is some massive troll spewing false information, but his posts saying what was needed to make your own supercritical CO2 came three months before one of the detractors posted a link to someone using that very technology to make the first videotaped private supercritical CO2 experiments.
Also I find GO Joe's story about "The Unfortunate M" to be extremely misleading. Why do you provide false information in order to get people to believe you? M. was NOT his middle name, as you suggest, nor was his nickname "The Unfortunate". It was his first initial. There is NOTHING in the Paris explosion to impugn CO2 extraction. It was a CAST IRON vessel. He was filling it by POURING SULFURIC ACID onto BAKING SODA in another vessel, CREATING CO2 and filling a CAST IRON vessel with NO PRESSURE RELEASE SAFETY from a source that had no control on the rate of reaction. Why do you leave all of these things out? After the explosion the pressure safety burst disc was invented. This has NEVER happened again, and is where we get this safety device from. Don't quote a story that should ENCOURAGE people as if it should DISCOURAGE them.
Also I find GO Joe's story about "The Unfortunate M" to be extremely misleading. Why do you provide false information in order to get people to believe you? M. was NOT his middle name, as you suggest, nor was his nickname "The Unfortunate". It was his first initial. There is NOTHING in the Paris explosion to impugn CO2 extraction. It was a CAST IRON vessel. He was filling it by POURING SULFURIC ACID onto BAKING SODA in another vessel, CREATING CO2 and filling a CAST IRON vessel with NO PRESSURE RELEASE SAFETY from a source that had no control on the rate of reaction. Why do you leave all of these things out? After the explosion the pressure safety burst disc was invented. This has NEVER happened again, and is where we get this safety device from. Don't quote a story that should ENCOURAGE people as if it should DISCOURAGE them.
The troll that left?
"M." stands for Monsieur. The quote (there are similar quotes using the word unfortunate by older authors of chemistry encyclopedias) is by previously very well-known dead author/inorganic chemist J.W. Mellor:
http://www.lateralscience.co.uk/liquidgas/index.html
Not a single fucking one of my details are incorrect much less false; they're directly from and verified by the original literature written at the time. It is still unclear to me whether it was the generator or receiver that exploded.
To encourage recklessness would be asinine, and the story is an appropriate illustration of the dangers of the pressure involved.
Bubbly Terps
Member
You left out the fact that the CO2 was produced from a reaction left uncontrolled. You left out the fact that the vessel was made from brittle cast iron. You left out the fact that the incident is famous due to its necessitating the advent of the pressure release safety disc. Said advent makes your mention of this horror tale unnecessary except to discourage research. You then post the research you claim to deplore, in video form.
If I was going to post the tale of the Parisian discovery and harnessing of liquid CO2, I'd point to it as proof that proper procedure will result in safe extraction. Tolerances, stainless steel, pressure burst discs. I wouldn't omit facts about the event in an attempt to twist what happened toward my argument. BTW nice post edit months ago to hide the fact that you got chloroform and methanol confused. You sure know how to copy and paste, except for when you botch it. Don't try to deny it because I saw you.
Thank you for admitting that the M. stands for Monsieur and that as such your attempt to portray it as his middle initial is absurd. Your assignment of an arbitrary nickname to the person, along with your shallow attempt to paint Mellor as the assignitor, speaks much of your motives while communicating little in the way of fact.
If I was going to post the tale of the Parisian discovery and harnessing of liquid CO2, I'd point to it as proof that proper procedure will result in safe extraction. Tolerances, stainless steel, pressure burst discs. I wouldn't omit facts about the event in an attempt to twist what happened toward my argument. BTW nice post edit months ago to hide the fact that you got chloroform and methanol confused. You sure know how to copy and paste, except for when you botch it. Don't try to deny it because I saw you.
Thank you for admitting that the M. stands for Monsieur and that as such your attempt to portray it as his middle initial is absurd. Your assignment of an arbitrary nickname to the person, along with your shallow attempt to paint Mellor as the assignitor, speaks much of your motives while communicating little in the way of fact.
