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

hazebluez said:
Hi Canyon:thanks: ,
Im new to these forums, & though I'm not new to cultivation & edibles, concentrates are a whole new ball game for me!and I'm really trying to find the most efficient way to produce ending product. Throughout my research, i wanted to try something similar to this which was:
1)Decarb - THCA or CBDA or it is also possible in conjunction w/ 1 decarbed & non decarbed
2) Then follow using Extraction of cannabis plant material with supercritical CO2+
3) +2% w/w ethanol (everclear)
(which results in significant recovery of cannabinoid frm raw material)
4) Winterization (everclear)
5)Filtration
6)Evaporation
I have pressure&temp timings too,but I was looking at your Decard to Extraction process using Co2, ever clear and am fascinated! I am wondering if you wouldn't mind sharing a few more detailed tips as you went about the process? Materials needed? Temp/timing used?
I would really appreciate it.

If not, keep up the good work! :goodjob:
Thanks,Hazel:Namaste:
Click to expand...

Welcome to 420 and the thread Bluez!

I documented the extraction process in three posts Page 73 #1093, #1095 and the post you quoted on page 74 #1096.

Super critical and sub critical for that mater are very high pressure commercial setups that start around 60 thousand. There are people working with home built equipment. It is too scary for me.

My goal was to bring the alcohol temperature down to a-50 -60f range. You would have thought I would have checked the alcohol temp before I added it to the buds. I did not even think about it. It was cold enough that the CO2 boiling slowed to bubbles.

I also think that having the alcohol and dry ice in the soak cycles help with agitation and striping the oils. It is not pulling out any clorophyll that I can see.


The cocktail I made is mostly CBDA and THCA with small amounts of CBD and THC. As a concentrate, licking your fingers produces a slow burn that last. Diluted into a carrier oil would probably lessen it to something you could bake with.

I will be happy to answer any questions that I can.

All though,
I never know
 
Bucudinkydow said:
Thanx CCOiler. I think terpene additives are going to be a huge wave of the near future and perhaps a dedicated thread may be something of interest to enough members to make it worthwhile exploring.
Click to expand...

Every time I drop samples off at SH I grab the latest issue of "Terpenes & Testing". Jan Feb issue has an article discussing "botanically derived terpenes" from a commercial side. It maintains that branded blends will become the norm. It also maintains "If we rely only on native terpenens there simply aren't enough raw materials in the marketplace to standardize a specific cannabis essential oil".

New Thread?
What about including Terpenes and Isolates into this thread and inviting those with input to share? It would be nice to have fresh voices. And, the thread is overlapping into that area already.

I never know



 
"Alrite, so we have THC is soluble at 20.2 mg THC / ml alcohol (70%)"

Got that off mj.com. It cited a patent with a broken link. Can't verify. That sounds really low. Anybody have info on this?

While you are thinking...so if that's true, when you evaporate to strengthen tintures, is that as far as you can go? 20mg/ml? Just because a patent says so.... I would think it would be dozens of times higher in solubility.
 
Oldbear said:
Could someone do a wee test and share what happens?

one tiny drop of terpenes in some edible oil with no thc/cbd at all - Id really like to know what happens with that dose.
Click to expand...

Be happy to oblige, oldbear, but it's going to be late next week before I get back home to my supplies. My plans are to do a mix with some MCT oil to supplement some caps I already have prepared. I'll try a little of the mix by itself and give you a report.

Thanx for the photo upload directions. I'm gonna give it a try shortly.

BCDD
 
Kicknitup1 said:
"Alrite, so we have THC is soluble at 20.2 mg THC / ml alcohol (70%)"

Got that off mj.com. It cited a patent with a broken link. Can't verify. That sounds really low. Anybody have info on this?

While you are thinking...so if that's true, when you evaporate to strengthen tintures, is that as far as you can go? 20mg/ml? Just because a patent says so.... I would think it would be dozens of times higher in solubility.
Click to expand...

Thanx kickn, this is info I've been trying to ferret out for a while for extraction purposes. I generally use 3 ounces to 7 grams of material and have been curious how close I've been coming to a saturation point of the ethanol. Using the WAG system I've been estimating the 7 grams probably contains maybe 1 gram of total cannabinoids, but as canyon says "who knows".

Never been able to do a successful partial reduction because of my humidity problems so I don't know where that would lead to.
,
 
Kicknitup1 said:
"Alrite, so we have THC is soluble at 20.2 mg THC / ml alcohol (70%)"

Got that off mj.com. It cited a patent with a broken link. Can't verify. That sounds really low. Anybody have info on this?

While you are thinking...so if that's true, when you evaporate to strengthen tintures, is that as far as you can go? 20mg/ml? Just because a patent says so.... I would think it would be dozens of times higher in solubility.
Click to expand...

It sounds low to me.

Take the dry ice extraction for example. There was around 700ml of 190 proof and 5 grams of cannabinoids in the dish to start. As the alcohol evaporated the oil stayed in solution. There was no separation happening. Near the end there was a small amount of water that separated out and mostly stayed together rather than forming drops around the dish. It may be that how much can be dissolved is not the same as how much will stay in suspension.
 
Bucudinkydow said:
Thanx kickn, this is info I've been trying to ferret out for a while for extraction purposes. I generally use 3 ounces to 7 grams of material and have been curious how close I've been coming to a saturation point of the ethanol. Using the WAG system I've been estimating the 7 grams probably contains maybe 1 gram of total cannabinoids, but as canyon says "who knows".

Never been able to do a successful partial reduction because of my humidity problems so I don't know where that would lead to.
,
Click to expand...

I came up with 1.4g of THC and a concentration of 1.2% or 12ml/g. That is less than the 2% referenced above and above the bottle I used for two washes which would be a 0.94% concentration for the combined washes. I had about 75% extraction. I am convinced that longer washes will improve extraction with little degrade in quality. I will probably try Three 30 minute or one hour soaks with a good bit of stirring.
 
Kicknitup1 said:
There was a period where I was trying to reclaim more coconut oil from the dreggs by adding 10:1 water to the mix. I would squeeze out all I could and then add the hot water to try to float out all the additional oil trapped in the dreggs. Well, that works but I was making the nastiest tasting oil one could imagine. I mean awful. I wish there was a better way to get the chlorophyll, etc out of the Coconut oil. Even making edibles from CCO tastes pretty bad, hence the experimenting with alcohol...that and for gummys. So, we need a method of winterizing coconut oil.
Click to expand...

kickn, as promised, not what you expected; it's not new, it's old. Just combined some known techniques and you might like results. reposted from my journal:

Today I made 33 daytime caps. [Actually, I made 47, but managed to crush 14 in assembly; some are salvageable, in fact, under the influence of one now, so if more rambling or run-on than usual blame that, I think.]

I'd cut these buds on Tuesday and let them hang for 1 day, then placed them in the dehydrator to completely dry them out for this experiment (making a more tasteless, stronger oil than the I used in the nighttime caps, which I'm currently taking 2 at night, about an hour apart). Using a can with a metal hash screen, that was frozen along with the dried buds and a quarter, I shook this over a mirror to produce kief. I repeated this 3 more times, refreezing each time (the last didn't produce much, which is why I stopped at that point).

Here are close-ups I tried to take of the kief:

20180201_101216.jpg


20180201_102517.jpg


I assumed that I only collected about half of active material, which is why I only used 2 oz. of MCT oil this time. [I added the leftover material to the trim from the buds I've been collecting and will use it for pain cream.] I processed it in the instant pot for 115 minutes, same as last week. But I only filtered it through the coffee filter since there was little material and the resulting oil was much lighter in color and nearly flavorless. [Success kickn!!! :yahoo:]

The smooshed cap I had hadn't leaked yet, so I had that dose, plus some tastes off spoons, etc, and caught a slight buzz. Far more importantly, a 5 spasm was stopped (not masked, but stopped) within an hour. So success and success, so to speak. I'll try to add comparison photos of daytime/nighttime caps later, probably tomorrow. And on that note

Back to the darkside
 
Thank you Greatwolf. I was considering the same thing for the next run. I'm pretty sure using only keif will eliminate almost all of the taste problems. I am also going to eliminate grinding up the buds going forward. I suspect most of my woes come from that step. After I figured out that a dusting of PAM in the spice grinder would prevent loss of trichomes I thought I was home free.

Remember that the goal here was to try to get ALL the goodies without damage. I wanted every chance to get them all so by exposing every bit to the solvent was step one. I do not regret doing it that way for the sake of the experiments. But for actual use......ugg. Then I learned that ALL the THC is on the outside. So, that's different. Then the trick becomes getting all the trichs without all that grinding. Freezing & dry ice appear to be the best home style for that task. Skunk Pfarm looks at it with a 100x scope to see if he got them all.

Even with all that exposure, remember at Canyons- we still left 20% behind. I was seriously disappointed in that...and more than a little surprised. But, it answered a host of potency mysteries. It also explained why I thought our weed here was far worse than it was. -it's still on the low side of acceptable, even when you find the best you can. REMEMBER: I was testing the oil with the tcheck and working backwards to determine the potency of the weed. (I had already told Canyon thatI though mine was weak (I was estimating 10% & it's probably 12-15 max)) before I visited. I think he expected me to fall out of the chair when I hit his stuff.) Over the week, he threw the whole arsenal at me. He was a great host, what can I say? LOL! Eventually, he told me that my buds were probably stronger than I was giving credit. Then we got the results back and I understood why I thought that (20% loss in extraction).

Then my focus went to agitation. I was not wrong about that one. You must refresh the solvent's exposure to the thc constantly because evoo is a weak solvent. So is VG, etc. I have used ultrasonic, homemade mixers, etc. Now I have a magnetic stirrer hotplate.

Then liposomal encapsulation. I have that one under control. I am satisfied that I am making it happen. It is visually obvious. If I can figure a way to show it in a photo I will post. The dremel. Still need a better mixing blade. And to my new Canadian friend, that dremel competitor- name escapes me- well that would be perfect IF I hacked it and put in a variable speed controller. As is, it starts off wide open from what I can tell. I don't see any good coming from that. lol. RE Dremel: I once mixed VG, PG, Coconut oil, & 151 Everclear & CCO into a stable emulsion. No change after a full week. Can you tell I was in the weeds???? LMAO.

Now my focus is on getting the max trichs without the plant mtl. I think I will have clean oil, but expensive. Anyway, I will do it with keif at least once to test the flavor principle.
 
Canyon,

I think 20mg/ml sounds low also. But that's what the info in the patent said. And I don't think the patent was about achieving that per se. But I suppose we should see if we can verify that stat. I just wanted to pass it on. Also, that pool of water that formed, could you use an eyedropper or needle to suck it out?
 
Re: Decoding The Holy Grail: Terpene & Cannabinoid Retention - Decarb to Extraction

Kicknitup1 said:
Thank you Greatwolf. I was considering the same thing for the next run. I'm pretty sure using only keif will eliminate almost all of the taste problems. I am also going to eliminate grinding up the buds going forward. I suspect most of my woes come from that step. After I figured out that a dusting of PAM in the spice grinder would prevent loss of trichomes I thought I was home free.

Remember that the goal here was to try to get ALL the goodies without damage. I wanted every chance to get them all so by exposing every bit to the solvent was step one. I do not regret doing it that way for the sake of the experiments. But for actual use......ugg. Then I learned that ALL the THC is on the outside. So, that's different. Then the trick becomes getting all the trichs without all that grinding. Freezing & dry ice appear to be the best home style for that task. Skunk Pfarm looks at it with a 100x scope to see if he got them all.

Even with all that exposure, remember at Canyons- we still left 20% behind. I was seriously disappointed in that...and more than a little surprised. But, it answered a host of potency mysteries. It also explained why I thought our weed here was far worse than it was. -it's still on the low side of acceptable, even when you find the best you can. REMEMBER: I was testing the oil with the tcheck and working backwards to determine the potency of the weed. (I had already told Canyon thatI though mine was weak (I was estimating 10% & it's probably 12-15 max)) before I visited. I think he expected me to fall out of the chair when I hit his stuff.) Over the week, he threw the whole arsenal at me. He was a great host, what can I say? LOL! Eventually, he told me that my buds were probably stronger than I was giving credit. Then we got the results back and I understood why I thought that (20% loss in extraction).

Then my focus went to agitation. I was not wrong about that one. You must refresh the solvent's exposure to the thc constantly because evoo is a weak solvent. So is VG, etc. I have used ultrasonic, homemade mixers, etc. Now I have a magnetic stirrer hotplate.

Then liposomal encapsulation. I have that one under control. I am satisfied that I am making it happen. It is visually obvious. If I can figure a way to show it in a photo I will post. The dremel. Still need a better mixing blade. And to my new Canadian friend, that dremel competitor- name escapes me- well that would be perfect IF I hacked it and put in a variable speed controller. As is, it starts off wide open from what I can tell. I don't see any good coming from that. lol. RE Dremel: I once mixed VG, PG, Coconut oil, & 151 Everclear & CCO into a stable emulsion. No change after a full week. Can you tell I was in the weeds???? LMAO.

Now my focus is on getting the max trichs without the plant mtl. I think I will have clean oil, but expensive. Anyway, I will do it with keif at least once to test the flavor principle.
Click to expand...

First, as promised, photos of the caps. On the left is Tangerine Dream kief Daytime cap and the right is Blueberry bud Nighttime cap, both autos:

20180202_074455.jpg


The color of the kief cap is almost entirely from the lecithin, otherwise it would be a very light green in color.

I didn't think of the idea of using PAM on the grinder but it makes sense and I may have to try it.

I agree that dry ice sifting would be best but there is none local (within range I can comfortably sit). While my wife is wonderful and would try, I'm not about to ask her to drive and get that for me, it would be difficult for her to do. I can get additional screens, if I need cleaner material, and re-sieve it.

It is definitely more potent then the Nighttime caps, probably 3x or more. Took 1 at 5AM when I got up and again stopped spasm (Sunday's storm may be stronger than they're calling for or maybe I just over did yesterday making the caps, or possibly both). It's now almost 10 and still feel just a slight buzz, but easily able to function under it. I'll have to figure out the frequency of dosing for Daytime caps and start trying 3 Nighttime caps at night (and change that production method, obviously). All part of the grand experiment.

Decarbing in the Instant Pot appears to work (from visual exam, cooling now), I'll post a full report as part of pain cream production in a few days (it will be a multi-step process).

Cheers from the darkside
 
Greatwolf, I did the grinding because I could NOT find a definitive answer as tho whether there was any thc in the plant. I even asked our group once. Anyway, I would skip that even though there is no loss doing it. Try cutting the buds down with manicure scissors into thumbnail size pieces. I really think that is enough surface area exposed. I would do that before decarb.
 
Kicknitup1 said:
Greatwolf, I did the grinding because I could NOT find a definitive answer as tho whether there was any thc in the plant. I even asked our group once. Anyway, I would skip that even though there is no loss doing it. Try cutting the buds down with manicure scissors into thumbnail size pieces. I really think that is enough surface area exposed. I would do that before decarb.
Click to expand...

Now you tell me! :thedoubletake: j/k

I forgot to take a photo before, but here is a similar bud, from a jar with a boveda 62 curing decarbed on the left):

20180202_101206.jpg


Is this comparable to what you saw from the Nova?
 
Re: Decoding The Holy Grail: Terpene & Cannabinoid Retention - Decarb to Extraction

"Is this comparable to what you saw from the Nova? "

Yeah, it looks about like that.
 
"Is this comparable to what you saw from the Nova? "

Yeah, it looks about like that. As long as you are doing the equivalent to apx 240*f for apx 75 min + 15 min warm up + 15 cool down you are in the sweet spot for normal use. Yes, there are an infinite amount of ways to combine temp & time to get there. We just know this protocol decarbed 99% from memory. Hard to argue with that performance.
 
I have even considered freezing the bud and then razorblading off the entire outer layer to make sure I got all the trichs. It would add plant matter but I'm still miles away from soaking the entire bud. Thoughts boys & girls????
 
Bucudinkydow said:
Be happy to oblige, oldbear, but it's going to be late next week before I get back home to my supplies. My plans are to do a mix with some MCT oil to supplement some caps I already have prepared. I'll try a little of the mix by itself and give you a report.

Thanx for the photo upload directions. I'm gonna give it a try shortly.

BCDD
Click to expand...

Delighted to have a volunteer :) Looking forward to the info.

Where are you guys buying your terps? I do have a won't ship to Canada problem.
 
Oldbear said:
Click 420 Entertainment>420 Gallery take you to the upload picture option

They moved it
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Well, still having issues. I'm able to upload photos to "member galleries" for instance. Am I correct in assuming this should simultaneously load to my albums as well or is there a step I'm missing? It's failing to appear in my album photos. If I click on the "my album" tab next to "upload photos" I get this message: Sorry, Personal Albums are not enabled. Am I going astray in my process or is it time to contact a mod?
 
Oldbear said:
Delighted to have a volunteer :) Looking forward to the info.

Where are you guys buying your terps? I do have a won't ship to Canada problem.
Click to expand...

I'm buying from True Terpenes but they're supposedly being exclusively marketed through Buy Terpenes. Not sure if they're shipping to Canada or not. I made a discovery this morning that gives me concern about this company, however, and I'm going to hold short of an endorsement until I get it sorted out. I hope to share my findings here but I'm going to have to master my photo uploading skills first.
 
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