Decoding The Holy Grail: Terpene & Cannabinoid Retention: Decarb to Extraction

Rider509 said:
The vapor pressure of EtOH at 121C is 49.5psi. The offset pressure would be 34.5psi. I see no reason why a Ball canning jar wouldn't remain intact at that internal pressure. Time to break out the pump and rig up a test.

edit: I'm going to install a Schrader valve in the lid, enclose the 1 gallon jar in a bag to capture the shrapnel, and test to failure. Any guesses how much pressure it'll take and whether the lid or glass fails first?
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OOOOH!! This sounds like fun!
 
Rider509 said:
The vapor pressure of EtOH at 121C is 49.5psi. The offset pressure would be 34.5psi. I see no reason why a Ball canning jar wouldn't remain intact at that internal pressure. Time to break out the pump and rig up a test.

edit: I'm going to install a Schrader valve in the lid, enclose the 1 gallon jar in a bag to capture the shrapnel, and test to failure. Any guesses how much pressure it'll take and whether the lid or glass fails first?
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Jar by far. 30 PSI.
After that try a half pint. I suspect that the half pints with the decorative diamond design would hold up best and also act a lot like a fragmentation grenade.

Are you conducting these medical experiments outside?

I never know, you know
 
Canyon said:
How are you getting your offset pressure numbers?
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I took the vapor pressure number derived from the Clausius-Clapeyron equation for EtOH at 121C and subtracted the known steam vapor pressure of 15psi at 121C. That yields the effective pressure inside the vessel.

Canyon said:
Jar by far. 30 PSI.
After that try a half pint. I suspect that the half pints with the decorative diamond design would hold up best and also act a lot like a fragmentation grenade.

Are you conducting these medical experiments outside?

I never know, you know
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I'm thinking you're likely very close. I'm going to try to blow up a Ball jar in the morning. I'll have to use a quart jar though because the gallon jars have plastic lids and are full of flowers. And yes, if it ever progresses to full-on autoclave testing it'll be outside in a very explosion-proof location.
 
Canyon said:
If you are not in a rush, I could could get you some rough temp and pressures for Everclear in a few days.
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I'm using 200 proof which simplifies the math. No partial pressures to figure out, right?
 
Sounds like fun and something useful to know. If you knew the max pressure, then you could calculate what pressure a decarb would generate and adjust the amount of cannabis to stay under a "safe" pressure for flowers and nondecarbed dried concentrates.

What effect would 121C have on the fail pressure?
 
BCDD's use of a sealed jar flower decarb is really interesting and something I'll def give a try. But if I can decarb a liquid concentrate in a sealed system that would make things so easy and emit no tell-tale smells. I don't think the processing temp will play a role in failure since the canning jar seals are designed to withstand high temps.
 
FWIW Prior to my closed decarb venture, I attempted to find some specs on what granny's ol' mason jars could withstand. I never could find any info on pressurization but there are random tests done by the manufacturer at 15psi for vacuum.

I remember a discussion on a home brewers forum concerning mason jars. Most experienced decarbonation due to leaking lids. I feel this is going to be the weak link. My question would be will the lid leak fast enough to serve as a safety valve? Of course, I'm not sure if an autoclave full of vaporized ethanol is going to be a safer alternative to an exploding jar?!?

Anxious to hear the results. Good luck and don't forget to duck!
 
After reading a doctoral dissertation written in 1953 by JM Teague, the Chief Quality & Research Engineer of the Quality & Specifications Department of Owens-Illinois Glass Co., Toledo, Ohio, I'm no longer concerned that the glass will fail under the expected pressures. The lid, however, is a different story. I have two lids to test. The standard canning lid and a heavy stainless one-piece lid with a heavy silicone seal. If either will hold 50psi the next test will be in one of the spare autoclaves. Testing won't happen until tomorrow though because I'm going to work early to put the new clave in service. That Tuttnauer is a $5000 unit that cost me $15 to fix. They lost the reservoir drain plug! LOL. That clave is only two years old with less than 2000 cycles. Gotta love a dental practice with more money than sense, and good friends that look out for you. It's been spore tested and is ready to rock. Woo Hoo!!!
 
Bucudinkydow said:
Of course, I'm not sure if an autoclave full of vaporized ethanol is going to be a safer alternative to an exploding jar?!?

Anxious to hear the results. Good luck and don't forget to duck!
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I'll def post up photos if anything newsworthy happens! LOL. But a heated chamber full of pressurized ethanol vapor is exactly how a chemi-clave works. A steam-clave doesn't have the condensing coils for spent solvent recovery but since it'll be outside during testing even a catastrophic failure venting to atmosphere won't pose a health hazard.

edit: I'd bet a lung-full of vaporized 200 proof ethanol would get your attention. haha
 
Problem solved. No exploding glass jars, though. Sorry.
reactor_vessel.jpg

reactor_vessel.jpg

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Testing with just EtOH won't produce the same reaction as a cannabis tincture. When the THC-a is heated the carboxyl bond is broken and H2O and CO2 are produced. Someone with a better recollection of inorganic chemistry than I possess could calculate/estimate the volume of CO2 produced and the resultant pressures. I'm taking the safe route because I don't want my first batch to be spattered all over the inside of the autoclave with sticky glass shards.

edit: I kinda fudged with the photo. :cool:
 
Scientific did some heavy duty calculations on this somewhere back in this thread. Hurt my head to try to follow that. There was some question if the added pressure impeded the the ability of the co2 molecule to be off gassed. I don't think the question was resolved.

You've got some pretty cool toys. Looking forward to your finding.
 
Bucudinkydow said:
Scientific did some heavy duty calculations on this somewhere back in this thread. Hurt my head to try to follow that. There was some question if the added pressure impeded the the ability of the co2 molecule to be off gassed. I don't think the question was resolved.

You've got some pretty cool toys. Looking forward to your finding.
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Another factor to consider. Damn. I had wondered if the reaction might be reversed under pressure, recarboxylation in a sense, but after some quick and dirty research that doesn't appear likely. My gut feeling is that the bonds will be broken and the CO2 will stay in solution until the pressure is released. Carbonated tincture maybe? LOL, I have no idea. I do know that after the reaction I'll supercool the reaction vessel before opening it to hopefully avoid the warm champagne response, then allow the CO2 to offgas naturally.

I know that once a bond is broken, say H2O into H and O, you can't just mix the gases to create water again. There has to be a catalyst.

"Damn it Jim! I'm a doctor, not a chemist!"
 
The oil I extracted with the dry ice in the alcohol had a lot of CO2 in the alcohol. It effervesced vigorously for a while when I pored it into a baking dish. The temperature change would be from Circa -50 to +50f.

In water CO2 will/can form H2CO3(aq), carbonic acid. I am not sure what is happening in alcohol.

From 5 pages before the currant spot in my chemistry book.

"CO2(g) +H2O(l)>>>>>>H2OCO3(aq)

The gas CO2 is not highly soluble in water, so if the amount of H2CO3 formed in this reaction is in excess of the amount that would be present in a saturated solution of CO2, the H2CO3 will decompose, and CO2 will bubble out (effervesce) of the solution until all the excess CO2 has been emitted."

I never know
 
Rider509 said:
Problem solved. No exploding glass jars, though. Sorry.
reactor_vessel.jpg

reactor_vessel.jpg

  • Media owner Rider509
  • Date added

Testing with just EtOH won't produce the same reaction as a cannabis tincture. When the THC-a is heated the carboxyl bond is broken and H2O and CO2 are produced. Someone with a better recollection of inorganic chemistry than I possess could calculate/estimate the volume of CO2 produced and the resultant pressures. I'm taking the safe route because I don't want my first batch to be spattered all over the inside of the autoclave with sticky glass shards.

edit: I kinda fudged with the photo. :cool:
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The decarboxilated CO2 will be 12% of the weight of the acids in your concentration. CO2 weighs 44.01g/mol.
Just solve for P Here
 
Canyon said:
The decarboxilated CO2 will be 12% of the weight of the acids in your concentration. CO2 weighs 44.01g/mol.
Just solve for P Here
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So I just have to do a chemical assay to determine how many total moles of the analyte are bonded to the THC-a molecules in a given sample. So easy a cave dude could do it. o_O

edit: Ha! That's what you just did! I crunched the numbers and when I saw 44 I went, "DOH!" LOL
 
Rider509 said:
So I just have to do a chemical assay to determine how many total moles of the analyte are bonded to the THC-a molecules in a given sample. So easy a cave dude could do it. o_O
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Or, you could weigh the starting material, guess at the cannabinoid content, multiply by 12% and allow for extraction loss. Then divide by 44.01to get the number of moles. It should be close.
 
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