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What process will create vape oil?

coldcanna

Active member
Veteran
I see what your sayin now.... I myself have been mulling the same problem, reading through dozens of scholarly articles on essential oils. I have a separate thread on the science of curing in the advanced growing forum on here.

Some cats are doing steam distillation of terps prior to your typical solvent distillation for cannabinoids. I personally haven't tried this but seems interesting enough. Not sure how 230 degree steam is gentler on the terps than other options but who knows.

Problem here is all of our methods involve heat. Whether is vac purging butane or distilling off ethanol. Terps volatilize at room temperature from heat and oxygen so its really a tough problem. I would venture to say that freeze drying fresh nuggets then using those in a vaporizer would be your closest bet to near original oil content. But the point of this thread is vape oil so I'll get back on track.
 

Prime_Extracts

New member
I am certainly not advocating anyone to pay the current insane prices for cannabis derived terpenes. I am saying that if you have high quality flowers, then the terpenes are already there just waiting to be extracted, in a natural ratio that could be used for safe vape oil. If there is a way to safely extract terpenes in a repeatable fashion, just like the 100s of commercial and DIY products for extracting cannabiniods, I wonder why more people don't discuss these ideas.

Terpenes are terpenes, regardless of where they were derived from. The only "fake" terpene would be one that was synthesized in a lab, and I don't know if that is even being done or not. There is no difference in the chemical structure of these individual compounds across different species of plants.

Just because you extracted your terps from high quality cannabis flower does not automatically make them safe for consumption. We know they are safe to consume at levels found naturally in the flower, but once extracted they are further concentrated and no longer in a natural ratio. The same goes for the terpenes (and every other compound) found in your typical shatter or wax.. once extracted they are no longer anywhere close to natures intended concentration.
 

Hashmasta-Kut

honey oil addict
Veteran
Terpenes are terpenes, regardless of where they were derived from. The only "fake" terpene would be one that was synthesized in a lab, and I don't know if that is even being done or not. There is no difference in the chemical structure of these individual compounds across different species of plants.

Just because you extracted your terps from high quality cannabis flower does not automatically make them safe for consumption. We know they are safe to consume at levels found naturally in the flower, but once extracted they are further concentrated and no longer in a natural ratio. The same goes for the terpenes (and every other compound) found in your typical shatter or wax.. once extracted they are no longer anywhere close to natures intended concentration.



Nature has no "intention" as to concentration and consumption. People have smoked hash for thousands? of years, nature doesn't care.

also it has been shown that non cannabis derived terpenes added to cannabis products do not have the same synergistic effects.
 

Prime_Extracts

New member
Nature has no "intention" as to concentration and consumption. People have smoked hash for thousands? of years, nature doesn't care.

also it has been shown that non cannabis derived terpenes added to cannabis products do not have the same synergistic effects.

I would say nature definitely has its intentions. Plants evolved to produce their specific terpenes profiles for a reason. For example..
"Several terpenoids have their roles in plant defense against biotic and abiotic stresses or they are treated as signal molecules to attract the insects of pollination."
-https://www.ncbi.nlm.nih.gov/pmc/articles/PMC4362742/

Could those reasons include the consumption by animals/humans for their physiological/biochemical effects? Sure, its definitely possible and personally what I like to believe.

I never said that they were dangerous or that they shouldn't be consumed. My point was only that once the plant has been processed, the contents of your resulting material are no longer "natural". The only actual risks here, in my opinion, could be inhaling pure concentrated terpenes, or maybe even the "sauce" that people are smoking that is measuring 20%+ in terpene content. Would I still smoke it? You're damn right!

"it has been shown..." .. yeah that's a neat theory and all, but please get back to me when you find some sort of scientific backing for that one because I'm definitely interested.
 

WaterFarmFan

Active member
Veteran
Terpenes are terpenes, regardless of where they were derived from. The only "fake" terpene would be one that was synthesized in a lab, and I don't know if that is even being done or not. There is no difference in the chemical structure of these individual compounds across different species of plants.

I never said terpenes extracted from other plants are "fake". They are the exact same chemical compounds if distilled and handled properly. There are indeed terpenes that are synthesized in a lab, as certain vendors list options for both Natural and Synthetic for the same isolate. I read that many base terpenes are precursors for others, and thus open to manipulation.

Just because you extracted your terps from high quality cannabis flower does not automatically make them safe for consumption. We know they are safe to consume at levels found naturally in the flower, but once extracted they are further concentrated and no longer in a natural ratio. The same goes for the terpenes (and every other compound) found in your typical shatter or wax.. once extracted they are no longer anywhere close to natures intended concentration.

If flowers are safe to smoke, then the compounds inside are as well. Proper extraction does not chemically alter terpenes. My comment about natural ratio pertained to making shatter with same flowers after terpene extraction and adding back same terpenes to make vape oil. The terpenes are in the exact same ratio to the amount of thc, but of course in a concentrated format. That terp:thc ratio could vary from 1:10 to 1:20 (roughly), which is not enough for sauce, but perfect for vape oil. There is also a natural ratio of the terpenes themselves as well as other lesser organics. Labs only test for the main ones, which vendors sell, but as Gray Wolf noted in his sweet mary posts, very tiny amounts of esters can have very powerful effects.

Welcome to Icmag! Happy to have you!

WFF
 

WaterFarmFan

Active member
Veteran
I see what your sayin now.... I myself have been mulling the same problem, reading through dozens of scholarly articles on essential oils. I have a separate thread on the science of curing in the advanced growing forum on here.

Some cats are doing steam distillation of terps prior to your typical solvent distillation for cannabinoids. I personally haven't tried this but seems interesting enough. Not sure how 230 degree steam is gentler on the terps than other options but who knows.

Problem here is all of our methods involve heat. Whether is vac purging butane or distilling off ethanol. Terps volatilize at room temperature from heat and oxygen so its really a tough problem. I would venture to say that freeze drying fresh nuggets then using those in a vaporizer would be your closest bet to near original oil content. But the point of this thread is vape oil so I'll get back on track.

This is a diagram that is about 4 generations old. I have radically changed my condensers and cold traps, but can get the jist of my process.

https://www.icmag.com/ic/showpost.php?p=8133421&postcount=12

The problem with steam is that gets material wet which is bad if you make shatter like me. I have all the glassware, including wide-mouth chromatography reservoir, and will be testing steam distillation soon. I noticed that my post-etoh filter cakes still had a strong terp smell after extraction. So, my new working theory for extraction is below:

Vacuum terpene extraction with Nitrogen backfill
-50C Ethanol cannabinoid extraction
Steam terpene distillation of filtered material (after etoh evaporation and drying)
Add back terpenes to shatter to make vape oil

Would love to have someone try and replicate what I am doing!

WFF
 

coldcanna

Active member
Veteran
:tiphat: Very clever work @Waterfarmfan, this is the type of original content that really keeps the community moving forward, so thank you.

Couple questions:

1) when using the pestle and sieves to separate raw material, what type of efficiency are you seeing? does it take multiple attempts to fully break off all resin glands?

2) are you capturing any terps during sublimation

3) do you think you would lose quality by taking your frozen trich mixture and using a short path distillation apparatus under vacuum instead of vacuum oven manipulation?
 

Prime_Extracts

New member
I never said terpenes extracted from other plants are "fake". They are the exact same chemical compounds if distilled and handled properly. There are indeed terpenes that are synthesized in a lab, as certain vendors list options for both Natural and Synthetic for the same isolate. I read that many base terpenes are precursors for others, and thus open to manipulation.



If flowers are safe to smoke, then the compounds inside are as well. Proper extraction does not chemically alter terpenes. My comment about natural ratio pertained to making shatter with same flowers after terpene extraction and adding back same terpenes to make vape oil.

Welcome to Icmag! Happy to have you!

WFF

Yeah it doesn't chemically alter them (IF you keep your temperatures under control) but concentrates them. And that's exactly how I make vape cartridges also, about a 10% ratio give or take depending on the extract. I personally use TrueTerpenes though which are not cannabis derived.

My main point though was that if anything might be unsafe I would think it to be smoking the concentrated terpenes that you extract as they are, cannabis derived or not. Anyone who has worked with concentrated terpenes knows that some of those chemicals are crazy strong solvents! I would agree though that if you are diluting them by adding only a small amount to your product, mimicking the ratios found in nature, then the consumer should have nothing to worry about. Its the extracts we see today with crazy high terpene content that I worry about.. a lot of the time it burns the hell out of my sinuses or throat.

And thanks! I'm going to try and stop lurking and jump into discussions more. I very much appreciate this communities' passion for sharing knowledge :D
 

Hashmasta-Kut

honey oil addict
Veteran
Could those reasons include the consumption by animals/humans for their physiological/biochemical effects? Sure, its definitely possible and personally what I like to believe.

"it has been shown..." .. yeah that's a neat theory and all, but please get back to me when you find some sort of scientific backing for that one because I'm definitely interested.

You like to believe. With no evidence, and yet you make decisions based upon beliefs that you just like to have, that aren't proven? That will take you down a dubious path.


The terpene info I saw on here. You can look around if you like. I'm good.
 

WaterFarmFan

Active member
Veteran
:tiphat: Very clever work @Waterfarmfan, this is the type of original content that really keeps the community moving forward, so thank you.

Couple questions:

1) when using the pestle and sieves to separate raw material, what type of efficiency are you seeing? does it take multiple attempts to fully break off all resin glands?

2) are you capturing any terps during sublimation

3) do you think you would lose quality by taking your frozen trich mixture and using a short path distillation apparatus under vacuum instead of vacuum oven manipulation?

Thanks! I simply love to experiment.

1) - With Ln2 and fresh flowers (cut from stem less than 30 minutes), it takes little effort to break up the flowers into smaller pieces. About 90% will go through the top sieve with relative ease. You just tap the buds and they will break up, but you do need to work pretty quickly (or not put too bud on sieze at one time). After about 2-3 minutes the fresh material will thaw enough that it will no longer break up. I just move this material to one side of the sieve and dump in a fresh load of ln2 frozen flowers. When I remove the canister from ln2, I let the ln2 drip on the ~10% material to refreeze, and immediately do another grinding on both old and new material in sieve. I repeat this process 3 times (and only stems and leaves remain) and then remove the top sieve. After dumping contents of top sieve into a 2nd stainless bowl, I simply tap the walls of the lower sieve to separate the trichomes. Because the bottom sieve is ~500 microns, some plant material will get the bottom, but at this point you have fresh ln2 hash (with a high water content in trichomes). I dump the contents of the second sieve in the 2nd bowl and start the process over from beginning, but the ln2 hash in the bottom bowl remains until all flowers are processed. I can process about 500 grams of fresh flowers a hour with this method.

2) A good question that I can not answer with 100% certainty, but I have seen enough empirical data to say the terps do not come until I raise heat, which causes evaporation. This process only does sublimation initially, and terps could be condensing in parts of the oven that will only be volatilized for collection once temps are raised enough. Trichomes contain a waxy shell that must penetrated or degraded in a way that allows the terpenes to escape. A freeze drier does repeated freeze thaw cycles, but it very difficult to collect terpenes from these system. Another thing that I have encountered repeated sublimation from different parts of the traps. If you collect terpenes in cold traps, what is to prevent them from sublimating again, after they have sublimated from plant material? I have re-engineered my traps and receivers to alternate different cold temperatures (-70C, -20C & 0C). Still experimenting...

3) There are lots of ways to skin a cat, and I certainly think that you could do this with only glassware. It really just comes down to how you volatilize the terpenes. I have well over 100 pieces of 24/40 glassware and you can do just about anything (except high pressure applications) that can be done with stainless, just typically on a smaller scale.
 

coldcanna

Active member
Veteran
Awesome. To me, this is a very cool take on live resin. I don't think a lot of people realize how volatile the terps are, like for example even drying your buds for the normal 7-10 days then blasting them you're going to lose a lot of the original characteristics.
 

WaterFarmFan

Active member
Veteran
Yeah it doesn't chemically alter them (IF you keep your temperatures under control) but concentrates them. And that's exactly how I make vape cartridges also, about a 10% ratio give or take depending on the extract. I personally use TrueTerpenes though which are not cannabis derived.

My main point though was that if anything might be unsafe I would think it to be smoking the concentrated terpenes that you extract as they are, cannabis derived or not. Anyone who has worked with concentrated terpenes knows that some of those chemicals are crazy strong solvents! I would agree though that if you are diluting them by adding only a small amount to your product, mimicking the ratios found in nature, then the consumer should have nothing to worry about. Its the extracts we see today with crazy high terpene content that I worry about.. a lot of the time it burns the hell out of my sinuses or throat.

And thanks! I'm going to try and stop lurking and jump into discussions more. I very much appreciate this communities' passion for sharing knowledge :D

Hey Prime. I am very far from an expert, but I have been picking up quite a bit, both from reading and performing my own experiments. I think that heat can be a bad thing for terpenes, but IMHO it is actually heat plus oxygen and/or heat plus water (and certainly heat plus high pressure) that can cause adverse chemical reactions. These reactions don't happen (much?) in a vacuum with nitrogen backfill even with higher levels of heat. It is tricky because even with nitrogen at higher temp levels (greater than 100C), if you allow too much water vapor to form in your volatilization area, which for me is my vacuum oven, than you are in effect steaming the material in the oven, which drenches it with water and creates that dry hay smell. If you allow oxygen into your volatilization area, at higher temps you will get terps that smell like the wet sauna at the gym.

Lot of testing needs to done on the safety limits of inhalation versus orally consuming terpenes at different levels. My point about the ratio was really to draw a comparison to smoking or vaping huge quantities of flowers everyday. People that smoke 4-5 grams of flowers are consuming the same amount of terpenes and thc as 1ml of vape oil with 5%-10% terpenes, except without all the other inactive ingredient that get smoked as well.
 

WaterFarmFan

Active member
Veteran
Awesome. To me, this is a very cool take on live resin. I don't think a lot of people realize how volatile the terps are, like for example even drying your buds for the normal 7-10 days then blasting them you're going to lose a lot of the original characteristics.

I certainly would not recommend spending the money, and honestly I seriously doubt the efficiency of these units, but it will give you an idea how others are trying to make commercial products. These use steam, which will require a different approach to collect cannabinoids, to volatilize terpenes.

https://summit-research.tech/product/terpene-distillation-kit/
https://labsociety.com/lab-equipment/buy-terpene-distillation-kit/

Virtually everything is available here for a small fraction of the cost - https://stores.ebay.com/deschemsciencesupply/ However, I have to be honest that the Lab Society injection port (https://labsociety.com/lab-equipment/steam-injection-port-tube/) looks like something that I would love to have.

The ln2 method is fun as hell, but honestly not super practical. It uses about 2L-3L of ln2 per pound (wet weight) of fresh flowers and takes perfect timing from when you cut the plants for peak ripeness.

I will be trying my terpene extraction with cured material that is frozen to -70C using some of the methods below, but I will just freeze flowers in pot for 6-8 hours and then do all same steps of ln2 process (but without the ln2) with stainless sieve set. I want to duplicate the methodology using only dry ice and not ln2. I really think that fresh flowers need ln2 to be effectively processed this way.

https://www.icmag.com/ic/showpost.php?p=8201105&postcount=26
 

WaterFarmFan

Active member
Veteran
Now that I have all the True Terpene stuff, I am going to do a new round of analytical testing. I am going to place a glass container with 10ml of TT terpenes in my oven and watch the volatization as I raise temps. This will also let me test the efficiency of my condensers and cold traps and really see what is getting collected and where. It will also let me test my separation techniques. I could also do a separate test where I freeze the terpene mixtures at different temperatures and see if I can observe sublimation. More soon...
 

WaterFarmFan

Active member
Veteran
I am curious about the use of THC-A vs THC for vape pens as it pertains to chemical reactions and internal seals (ie leaking cartridges). Is the acid part of THC-A more aggressive than distillate or decarbed shatter? I understand that terpenes can cause reactions but was wondering about cannabinoids as well.
 

atosvitara

New member
This is called a Rotary evaporator.

https://en.wikipedia.org/wiki/Rotary_evaporator

It separates the alcohol from your extract. You do not need this. It does the same process as standard vacuum distillation only at a faster rate with higher throughput.

https://en.wikipedia.org/wiki/Vacuum_distillation

There are lots of videos that show these. Search videos for "vacuum distillation" for a start.

https://www.youtube.com/watch?v=TZo97aO4xbk



This is a totally different step from above. After filtering cannabis and cold ethanol, you have to remove the bulk of the alcohol at the lowest possible temps, and vacuum distillation (which includes the more expensive roto vaps) does this most efficiently. I said BULK (and this is a bit tricky) because you do not remove all of the alcohol in distillation. I try to get around 90% ethanol removed.

The step with the stainless steel kettle (or a more expensive vacuum oven) is to PURGE the last 10% (or so) of ethanol that remains in your extract. Again, using a vacuum allows you to remove alcohol with less heat.

Do some video searches for "vacuum purge". You will find a lot that reference BHO and show a different process sometimes, but the concept of purging alcohol is exactly the same as butane.



It is actually the vacuum that gets the process going, because it shifts the boiling points significantly. You need heat and thin film because the last bit of ethanol is very stubborn and gets trapped in the sticky mass. As for applying heat to your vacuum kettle, this can be done with in many ways. I referenced a dedicated heat pad with accurate PID controller that sticks to bottom of kettle. More expensive = more control over temperatures.



You really should use a cold trap between your vacuum device and pump, but honestly if you use a cheap pump and change the oil often, some ethanol getting to pump won't really hurt it.

https://en.wikipedia.org/wiki/Cold_trap
https://www.ebay.com/sch/i.html?_nkw=cold+trap&_sacat=0

WFF


This is great info.


One question, I always imagine the process being:
(short version)



1- Extract with ethanol
2- Filter x times in vacuum filter.
3- Rotary Evaporator
4- Distill? This is the part I don't get, do you always distill at the end to separate chlorophyll? Or you can leave it on the evaporation part?
 

SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
I was checking out ethanol availability and came across an inexpensive option.

UTILITY-GRADE ALCOHOL (NON-ORGANIC & NON-GMO PROJECT VERIFIED)

https://organicalcohol.com/non-organic-alcohol-utility-grade/


UTILITY GRADE 200-PROOF (NOT-CERTIFIED-ORGANIC) GRAIN ALCOHOL - 5 GALLON
IN STOCK
Excluding Federal Excise Tax: $125.00
NON-CERTIFIED-ORGANIC

Alchemical Solutions' 200-proof neutral non-organic, Utility Grade Grain alcohol is made from non-organically-certified grain (in other words, it is not certified organic, it is pure alcohol WITHOUT organic paperwork trace-ability).

We maintain the utmost level of quality and attention to detail, while at the same time adhering to environmentally sound practices.

Tested by an independent lab to insure that they meet United States Pharmacopeia (USP) standards, not all pure alcohol is pharmaceutical grade - only 190 proof and 200 proof pure ethanol which meets or exceeds the stringent standards of the USP.

Five gallon purchases ship in a single food-grade, high-density polyethylene container suitable for shipping high-proof alcohol.

https://organicalcohol.com/utility-grade-alcohol-200-proof-5-gallon/


Five gallons of 200 proof for $240 total delivered to Southern California, see attachment.
 

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