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

SweetSue said:
I was thinking, it's cool, but a touch of THC potentiates the CBD to such an extent that it's crazy not to have any in there. Wouldn't take much at all, to my understanding. You and the lovely wife probably have enough THC already in your system to do the job, but I was considering those who choose not to use THC at all.

It's still wonderful that they're doing strain specific formulations.
Click to expand...

The plan is to combine the CBD and terpene concentrate, some not decarbed hi CBD strain extract (Thunderstruck) and some decarbed Thunderstruck extract. Then make caps with the mixture. Hopefully the THC will be low enough for her to tolerate. It should be rather healthy with the acids, two strains of terpenes, CBD and a touch of THC.

I never know
 
Kicknitup1 said:
So who has played with dissolving CCO into VG and or Pg? Not combining as well as I would think. Isn't that pretty much what would be in a cartridge?
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I know that some are dissolved in PEG, while others are directly extracted into MCT for vaping. Not sure if either of these helps you.

Cheers from the darkside
 
I had a great deal of trouble getting a proper constitution when mixing cco and vg. It would separate a bit overnight irrelevant of what I did. My solution was to dissolve the cco with a small amount of ethanol and combining that with the vg. No separation. I used it as a tincture or for caps and the little alcohol wasn't a problem. If you're planning on vaping it, however, you my want to heat your final mix at low temps for a short period to boil off the ethanol. Remember ethanol boils at 173 degrees.
 
Quick Update

Yesterday and todayI made two more runs. The first one sprang a leak, but it held some pressure so I continued the run and got a weight loss of 0.4g from 10g starting material. The second run went better. It was 10g and also had a 0.4g weight loss. There was just under 6psi after the decarb and cooling, which is inline with a full decarb, just guessing at the cannabinoid content and needing to remeasure the volume.

I decided to move the trip to the lab to tomorrow. I am going to get a quick test for thc, thca, cbd and cbda. If I have a near complete decarb on the second run, I will get terpene tests on the raw material and the decarbed batch.

I will be back tomorrow night but it will probably be late. I will have the cannabinoid tests to post tomorrow. the terpene tests will probably post Friday or Monday.

I never know

 
Expect the Unexpected
 Yes, CBDA is harder to decarb than THCA!
I knew there was a difference. I just had no idea how much.

The THC content is a lot higher than advertised. I think I can work with it by using the raw material and adding an amount of the decarbed material to equal a one percent addition of THC. Then, I can do a cold alcohol extraction. Once it is a concentrate I can make any strength of caps that I want.

I have a lot of time, temperature and pressure notes on these two runs. There are some things that are not matching the math. It is going to take me a while to sort out what is happening.

The good news it the lab is interested in what I/we are doing. This time they ask if they could keep some of the second run. I said, "Sure".

Without a near full decarb of CBDA to CBD, I decided to hold off on the terpene tests. I am going to put a Thunderstruck from another seed into flower or a CBD clone that I have some tests on her mother already.
I never know

This is from a run that developed an air leak at about 4psi. I decided to keep going with the run at some higher temperatures than I had planed. When I have the numbers compiled I will post them.


SteepHill-Thunderstruck_1st_Decarb-cannabinoids.jpg

Next Test Next Test Next Test Next Test
This is a run that I held the upper oil bath in 230-240f range. With an instant read meat probe, holding the tip on the chamber under the oil's surface, the reading dropped 3-4 degrees depending how near the top or bottom of the oil the probe was. There is a lot of heat lost from the metal that is not submerged.
SteepHill-Thunderstruck_2nd_Decarb-cannabinoids.jpg


 
Canyon said:
Expect the Unexpected
 Yes, CBDA is harder to decarb than THCA!
I knew there was a difference. I just had no idea how much.

The THC content is a lot higher than advertised. I think I can work with it by using the raw material and adding an amount of the decarbed material to equal a one percent addition of THC. Then, I can do a cold alcohol extraction. Once it is a concentrate I can make any strength of caps that I want.

I have a lot of time, temperature and pressure notes on these two runs. There are some things that are not matching the math. It is going to take me a while to sort out what is happening.

The good news it the lab is interested in what I/we are doing. This time they ask if they could keep some of the second run. I said, "Sure".

Without a near full decarb of CBDA to CBD, I decided to hold off on the terpene tests. I am going to put a Thunderstruck from another seed into flower or a CBD clone that I have some tests on her mother already.
I never know

This is from a run that developed an air leak at about 4psi. I decided to keep going with the run at some higher temperatures than I had planed. When I have the numbers compiled I will post them.


SteepHill-Thunderstruck_1st_Decarb-cannabinoids.jpg

Next Test Next Test Next Test Next Test
This is a run that I held the upper oil bath in 230-240f range. With an instant read meat probe, holding the tip on the chamber under the oil's surface, the reading dropped 3-4 degrees depending how near the top or bottom of the oil the probe was. There is a lot of heat lost from the metal that is not submerged.
SteepHill-Thunderstruck_2nd_Decarb-cannabinoids.jpg


Click to expand...
Hi Canyon,

I tried going back a few pages to see, but couldn't find anything: Could you briefly tell me how the extraction was done? I'm also curious about the lack of CBDA conversion...

Cheers from the darkside
 
GW,
If you go back until you start seeing pictures of a frying pan on an induction hot plate, you will be able to catch up on what we are doing. It is not that far back. The thread moves in spurts.

The extraction I referred to in the last post is something that I will be doing now that the decarb process is complete enough for my needs. It uses as cold as you can get Everclear to strip cannabinoids and terpenes form plant mater. The alcohol is then evaporated off. The idea is to not add heat after the sealed decarb. The CBDA conversion does not play by THCA rules.

One of the lab techs said that a client or maybe just someone he knows, was working with times of 6 hours. I did not quiz him further. In some environments, it is best to just listen. He acted more interested in what we were doing than the meeting he had to attend. He grows nice smoke from the cell phone pictures he had. He also grows in some kind of 35 gallon containers. That has my interest.

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

Canyon said:
GW,
If you go back until you start seeing pictures of a frying pan on an induction hot plate, you will be able to catch up on what we are doing. It is not that far back. The thread moves in spurts.

The extraction I referred to in the last post is something that I will be doing now that the decarb process is complete enough for my needs. It uses as cold as you can get Everclear to strip cannabinoids and terpenes form plant mater. The alcohol is then evaporated off. The idea is to not add heat after the sealed decarb. The CBDA conversion does not play by THCA rules.

One of the lab techs said that a client or maybe just someone he knows, was working with times of 6 hours. I did not quiz him further. In some environments, it is best to just listen. He acted more interested in what we were doing than the meeting he had to attend. He grows nice smoke from the cell phone pictures he had. He also grows in some kind of 35 gallon containers. That has my interest.

Best
Click to expand...
I found the setup and remember reading this this a short while back. I know in physics that heat and pressure can be interchanged for some things, but that in chemistry (not my strongest suit, by far) they can interfere. Is it possible that THCA gives up it's CO2 more easily than CBDA and that, with the pressure, there is a CO2 saturation point being reached?

Cheers from the darkside
 
about 10 years ago, a group of researchers from GW Pharmaceuticals from Great Britain applied for a U.S. patent for some fancy pancy extraction method. Buried deeply in the overly complex description of the methodology was there lab results of decarbing cbd and thc.

Therefore laboratory studies demonstrate the optimum conditions for the decarboxylation of:

Chemovar producing primarily CBD is 1 hour at 120° C. or 0.5 hour at 140° C.
Chemovar producing primarily THC to minimise CBN formation, is 1 to 2 hours at 105° C. or 1 hour at 120° C.
Thin layer chromatography reveals that virtually all of the THCA has disappeared after 4 hours at 105° C. and after 1 hour at 120° C. No THCA is visible at any time point when the herb is heated at 140° C. A small amount of residual staining at this retention value on THC and the presence at low levels of a peak coincident with THCA on HPLC analysis may indicate the presence of a minor cannabinoid rather than residual THCA

Looks like the sweet spot for both is going to be 120c for 1 hr according to their results. .
 
If you dissolved BHO into 151 Everclear..I know thats not ideal... but is the ethyl % high enough to dissolve it all? I know it's not as good for extracting raw mtls but I was hoping it would be good enough to just dissolve BHO.
 
Bucudinkydow said:
about 10 years ago, a group of researchers from GW Pharmaceuticals from Great Britain applied for a U.S. patent for some fancy pancy extraction method. Buried deeply in the overly complex description of the methodology was there lab results of decarbing cbd and thc.

Therefore laboratory studies demonstrate the optimum conditions for the decarboxylation of:

Chemovar producing primarily CBD is 1 hour at 120° C. or 0.5 hour at 140° C.
Chemovar producing primarily THC to minimise CBN formation, is 1 to 2 hours at 105° C. or 1 hour at 120° C.
Thin layer chromatography reveals that virtually all of the THCA has disappeared after 4 hours at 105° C. and after 1 hour at 120° C. No THCA is visible at any time point when the herb is heated at 140° C. A small amount of residual staining at this retention value on THC and the presence at low levels of a peak coincident with THCA on HPLC analysis may indicate the presence of a minor cannabinoid rather than residual THCA

Looks like the sweet spot for both is going to be 120c for 1 hr according to their results. .
Click to expand...

Bucudinkydow I remember reading that. I used it as a decarb go by also.
 
Re: Decoding The Holy Grail: Terpene & Cannabinoid Retention - Decarb to Extracti

greatwolf said:
I found the setup and remember reading this this a short while back. I know in physics that heat and pressure can be interchanged for some things, but that in chemistry (not my strongest suit, by far) they can interfere. Is it possible that THCA gives up it's CO2 more easily than CBDA and that, with the pressure, there is a CO2 saturation point being reached?

Cheers from the darkside
Click to expand...


I don't think that CO2 saturation is the problem. Once the CO2 is freed from the molecule, it is a gas. I don't think it can recombine with the cannabinoids to form the acids. Even so there should be equal or at least some THCA present if saturation or pressure is the cause.

THCA boils at 105c (221f).
CBDA and CBCA boil at 120c (248f).

All three have the same formula. THCA has slightly more molecular weight, with 358.4733g V 358.2144 for CBDA and CBCAg.

I don't know what part these differences have on decarb. It is just an observation.

Check my numbers, they are from old notes.

Best
 
Re: Decoding The Holy Grail: Terpene & Cannabinoid Retention - Decarb to Extracti

Canyon said:
I don't think that CO2 saturation is the problem. Once the CO2 is freed from the molecule, it is a gas. I don't think it can recombine with the cannabinoids to form the acids. Even so there should be equal or at least some THCA present if saturation or pressure is the cause.

THCA boils at 105c (221f).
CBDA and CBCA boil at 120c (248f).

All three have the same formula. THCA has slightly more molecular weight, with 358.4733g V 358.2144 for CBDA and CBCAg.

I don't know what part these differences have on decarb. It is just an observation.

Check my numbers, they are from old notes.

Best
Click to expand...
Gases, especially under pressure, do behave as liquids, if I remember correctly. I also remember that gases have saturation points in closed systems.

If THCA has a lower boiling point, then it could boil off first. But if this was the case, I wouldn't expect a perfect break - all of one converted and none of the other. That wouldn't make sense at all. There must be something else going on here and I wish I knew.

Back to the darkside
 
Re: Decoding The Holy Grail: Terpene & Cannabinoid Retention - Decarb to Extracti

greatwolf said:
Gases, especially under pressure, do behave as liquids, if I remember correctly. I also remember that gases have saturation points in closed systems.

If THCA has a lower boiling point, then it could boil off first. But if this was the case, I wouldn't expect a perfect break - all of one converted and none of the other. That wouldn't make sense at all. There must be something else going on here and I wish I knew.

Back to the darkside
Click to expand...
Just to be clear, most of the chemistry that I know was learned in the last three months and I am only on page 110.

The tests that I had run were "While you wait.". They are relatively cheap at about $40 and I wanted to decide about more tests while I was there. They clam plus or minus 1%. They also said that it may not read CBD or THC above 6% because it was tuned (for lack of a better word) for the acids. Obviously, it read the THC at 7.4 levels. I would tend to treat any non acids that were over 6% as close numbers but not necessarily within 1%. Also, the less than 2% on the THCA can too easily be thought of as none rather than it will not read below 2%

So, near complete decarb for thc and 18% for CBD. The temperatures that I was running were probably less than I thought because of heat loss of the iron that was exposed. I need to find a better oil bath setup.

I tracked most of what I could with both tests. I will try to get them posted after some grow room maintenance and trimming a smallish Nightmare Cookies plant.

I never know
 
Bucudinkydow said:
about 10 years ago, a group of researchers from GW Pharmaceuticals from Great Britain applied for a U.S. patent for some fancy pancy extraction method. Buried deeply in the overly complex description of the methodology was there lab results of decarbing cbd and thc.

Therefore laboratory studies demonstrate the optimum conditions for the decarboxylation of:

Chemovar producing primarily CBD is 1 hour at 120° C. or 0.5 hour at 140° C.
Chemovar producing primarily THC to minimise CBN formation, is 1 to 2 hours at 105° C. or 1 hour at 120° C.
Thin layer chromatography reveals that virtually all of the THCA has disappeared after 4 hours at 105° C. and after 1 hour at 120° C. No THCA is visible at any time point when the herb is heated at 140° C. A small amount of residual staining at this retention value on THC and the presence at low levels of a peak coincident with THCA on HPLC analysis may indicate the presence of a minor cannabinoid rather than residual THCA

Looks like the sweet spot for both is going to be 120c for 1 hr according to their results. .
Click to expand...


I had not seen this before.

Unless someone has more to add, I will use these numbers for future tests.

FYI the best guess sustained high temperatures are 235-140 for 60 minutes for test one. Test 2 was around 220-230 for 1hr and 40 minutes.

The Thunderstruck plant was only 40 grams and the last high cbd plant that I had in flower. There is not going to be any left after I make caps for another run and test. I am going to start another cbd plant tonight or early next week.

I will find some better oil containers and tweak whatever I can think of while we wait for plants to grow.

The plant that I am harvesting is a clone of the Nightmare Cookies plant that we started this thread with. I can run some tests with it if anyone thinks of something. We have raw tests on the mother. However, it has no CBD. I cannot justify buying dispensary cbd cannabis and the windshield time for this project when I have plants in flower.

Best


 
Canyon said:
I had not seen this before.

Unless someone has more to add, I will use these numbers for future tests.

FYI the best guess sustained high temperatures are 235-140 for 60 minutes for test one. Test 2 was around 220-230 for 1hr and 40 minutes.

The Thunderstruck plant was only 40 grams and the last high cbd plant that I had in flower. There is not going to be any left after I make caps for another run and test. I am going to start another cbd plant tonight or early next week.

I will find some better oil containers and tweak whatever I can think of while we wait for plants to grow.

The plant that I am harvesting is a clone of the Nightmare Cookies plant that we started this thread with. I can run some tests with it if anyone thinks of something. We have raw tests on the mother. However, it has no CBD. I cannot justify buying dispensary cbd cannabis and the windshield time for this project when I have plants in flower.

Best
Click to expand...
The problem may be relative boiling points and the pressure involved. Check my logic here please:

We know that at lower pressure, the boiling point is lower. And at higher pressure the boiling point is raised.

THCVA has a lower decarb point.

The CO2 released, as well as any water vapor from water in the material, raises the pressure as you measured.

Could this increased pressure raise the decarb point for CBDA beyond what you reached? This might explain what happened.

Back to the darkside
 
greatwolf said:
The problem may be relative boiling points and the pressure involved. Check my logic here please:

We know that at lower pressure, the boiling point is lower. And at higher pressure the boiling point is raised.

THCVA has a lower decarb point.

The CO2 released, as well as any water vapor from water in the material, raises the pressure as you measured.

Could this increased pressure raise the decarb point for CBDA beyond what you reached? This might explain what happened.

Back to the darkside
Click to expand...

I think the lack of CBD decarb in this experiment is mostly not enough time and too low of a temperature. There may be some difference between an open container and this experimental method, however I don't think is going to cause a large change in decarb time and temperature. I could be wrong.

I have time, temperature and pressure readings for the two runs along with more questions. There are numbers that don't match the math in ways that I cannot account for. I also have some computed volume, mass, temperature and pressure numbers to compare. I just need the time to type them up.

I am beginning to think it may be a good idea to do a run with the Nightmare plant and use the last free terpene test to find out if we are making progress with the terpene retention. The raw terpene test form her mother should be close enough to the clone for what we are doing.
 
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