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Sweet Mary's Charms

It is understatement to say that only "clean" flowers of the highest quality should be used in the process that I described above. ANY pesticides, mold, mildew or other nasties will certainly volatilize in this process and be caught in the condensers and traps. Since only separation techniques are used with no solvents, these will likely contaminate the collected terpenes and have very bad effects when vaped. In short, unless you know for certain how the flowers were grown, it would be highly unethical to do this extraction tech for resell, unless of course if entire terpene batch was sampled and subjected to thorough lab analysis.

The original impetus of my efforts centered on taking world class flowers and creating a world class extract that mirrored the effect profile of the mothers. I am currently extracting terpenes, doing a -50C ethanol extraction, purge to shatter and add back terpenes for vape carts. Blind tests, which are ongoing, have noted a huge difference in effect when cannabis terpenes are added. .1ml per gram (.9 ml) of shatter is some of the most potent vape imaginable with the right strains. I have tested some Chem D hybrids that have been devastating.

So just to be clear ...... you are taking fresh frozen buds .... extracting the terpenes which will equate to no more than 5% in total, naturally occurring.......... in the process destroy the buds and then add back double the amount of terps that were present in the original flower ???? Is that about right ?
 

WaterFarmFan

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So just to be clear ...... you are taking fresh frozen buds .... extracting the terpenes which will equate to no more than 5% in total, naturally occurring.......... in the process destroy the buds and then add back double the amount of terps that were present in the original flower ???? Is that about right ?

Destroy buds? Not in the slightest. Maybe there is a small bit of decarbing, but I make flawless shatter with material after terpene extraction. Am I missing something in your question?

What you are describing (destroying) is when you do steam distillation with water that drenches material. My process drys the fresh material so that an ethanol extraction can be done sooner. I do let the material sit on large baker pans for a couple of days to completely dry before qwet.
 

WaterFarmFan

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As to adding more terpenes then were present, that can obviously be done after the fact, but fresh flowers have more terpenes (think rosin) then dried, due to evaporation over drying cycle. I am simply catching the terpenes as I accelerate the drying process with a vacuum oven using fresh material. I am still experimenting with different strains that have different terpene and cannabinoid amounts, but if I get 7 grams of shatter per ounce, terpenes could vary from .3ml to .7ml (from fresh) and obviously have different ratios.

You are very fair to bring up the health effects of consuming larger quantities of terpenes. GW's original article in post #1 addresses some. But you have to contrast that with the real world alternatives of third-party non-cannabis terps and PG/VG mixes.
 

WaterFarmFan

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As I currently understand it, here is what is going on in my process:

Nitrogen is not a carrier, only an inert gas that bounces around the oven and helps to volatilize terpenes locked inside trichomes. Oxygen can alter the chemistry of terpenes easier while in gas form via oxidation. I pre-heat the Nitrogen to speed up the extraction process and create a repeatable internal environment, where I am not guessing about the residence time that the Nitrogen needs to reach oven temps. It simply enters as the same temps as my oven (~215F) .

The vacuum oven allows precise heating to keep the terpenes from escaping or condensing, volatilize trichomes with nitrogen interaction and radiant heat, and allow easy Nitrogen backfilling with reliable controls - all the while keeping decarbing to a minimum. Need to keep in mind that cannabinoids are still locked inside the trichome at the point and not directly exposed to atmosphere. Member GO Joe gave a great response in Decarboxylation of flower material under vacuum - "Water and alcohols absorb and release a lot of heat, yes keeping the temperature below 212. Yes condensation in a vacuum situation keeps the overall temperature low and heat for decarboxylation is effectively lost to change of state.".

I believe some people are using freeze drying systems to do something similar, but I think my process is superior for its collection process via the ability to volatilize terpenes in collection chamber at higher temps. I believe the material must be in freeze dryer for much longer as well. The benefit of freeze drying is obviously at preserving the terpenes in their most original form, as heat similar to oxygen can alter components. I have attempted to work in as many of the elements of the freeze dry logic that I could by using ln2 and dry ice for attempts at sublimation and decreasing decarbing.

I am not saying that this is perfect, only that it is what I could cobble together using off the shelf parts to test the logic. I have gone through (and tested) more than a dozen different configurations, and I believe that can now say that this process is technically sound, but obviously open to improvement. The finesse required on the vacuum oven controls to not over-pump (suck the terpenes through the system so fast that can not be condensed or frozen) is something serious that should not be overlooked.
 

Gray Wolf

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As I currently understand it, here is what is going on in my process:

Nitrogen is not a carrier, only an inert gas that bounces around the oven and helps to volatilize terpenes locked inside trichomes. Oxygen can alter the chemistry of terpenes easier while in gas form via oxidation. I pre-heat the Nitrogen to speed up the extraction process and create a repeatable internal environment, where I am not guessing about the residence time that the Nitrogen needs to reach oven temps. It simply enters as the same temps as my oven (~215F) .

The vacuum oven allows precise heating to keep the terpenes from escaping or condensing, volatilize trichomes with nitrogen interaction and radiant heat, and allow easy Nitrogen backfilling with reliable controls - all the while keeping decarbing to a minimum. Need to keep in mind that cannabinoids are still locked inside the trichome at the point and not directly exposed to atmosphere. Member GO Joe gave a great response in Decarboxylation of flower material under vacuum - "Water and alcohols absorb and release a lot of heat, yes keeping the temperature below 212. Yes condensation in a vacuum situation keeps the overall temperature low and heat for decarboxylation is effectively lost to change of state.".

I believe some people are using freeze drying systems to do something similar, but I think my process is superior for its collection process via the ability to volatilize terpenes in collection chamber at higher temps. I believe the material must be in freeze dryer for much longer as well. The benefit of freeze drying is obviously at preserving the terpenes in their most original form, as heat similar to oxygen can alter components. I have attempted to work in as many of the elements of the freeze dry logic that I could by using ln2 and dry ice for attempts at sublimation and decreasing decarbing.

I am not saying that this is perfect, only that it is what I could cobble together using off the shelf parts to test the logic. I have gone through (and tested) more than a dozen different configurations, and I believe that can now say that this process is technically sound, but obviously open to improvement. The finesse required on the vacuum oven controls to not over-pump (suck the terpenes through the system so fast that can not be condensed or frozen) is something serious that should not be overlooked.

As you've touched on, delta temperature and residence time are the major players in heat transfer. You can increase residence by slowing down the flow, or lengthening the heat exchanger, and speed up the heat transfer efficiency by adding turbulence.

Slowing down the flow can mean the same flow through a larger diameter tube or plate and tube condenser.

A small mag drive pump circulating alcohol and dry ice or LN2 make it easier by increasing the delta temperature and reduces the need for area and longer residence time, if you can get them.
 

WaterFarmFan

Active member
Veteran
This is a tricky process because you have to deal with both evaporated water and the terpenes/organic volitiles. My solution was to use Graham condensers with ice water at ~1C, short stemmed take off adapter into receiving flasks and then my stop my dry ice sleeve for receiver flask at the base of the neck (exposing upper neck to room temps). This allows water/oil/hydrosol to drip cleanly into receiver flask and instantly freeze. When I wrap the upper neck and expose to dry ice, the water can freeze in the take off adapter and clog the system. The last stage cold trap into 1000ml boiling flask has a long stem adapter that goes to within 1/2" of bottom of flask, but virtually all water is gone and it is only collecting the most volatile compounds at that point.

I would love to experiment with the mag drive pump for other processes, or maybe even modifying this one with a new final stage. Can you recommend an affordable model available on ebay or amazon? Thanks!
 

Gray Wolf

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This is a tricky process because you have to deal with both evaporated water and the terpenes/organic volitiles. My solution was to use Graham condensers with ice water at ~1C, short stemmed take off adapter into receiving flasks and then my stop my dry ice sleeve for receiver flask at the base of the neck (exposing upper neck to room temps). This allows water/oil/hydrosol to drip cleanly into receiver flask and instantly freeze. When I wrap the upper neck and expose to dry ice, the water can freeze in the take off adapter and clog the system. The last stage cold trap into 1000ml boiling flask has a long stem adapter that goes to within 1/2" of bottom of flask, but virtually all water is gone and it is only collecting the most volatile compounds at that point.

I would love to experiment with the mag drive pump for other processes, or maybe even modifying this one with a new final stage. Can you recommend an affordable model available on ebay or amazon? Thanks!

None cheap, but check out Graingers.
 

WaterFarmFan

Active member
Veteran
In honor of the spirit of this thread (and ICMag!), I present one of the finest terpene/cannabinoid rich strains (Sweet Mary Indeed!!!) on the planet:

picture.php


Sundae Driver by Cannarado Genetics
Genetics: Grape Pie x Fruity Pebbles
Terpenes: Myrcene, Beta-Caryophyllene
Flavor: Grape, Fruity Pebbles cereal
Effects: Relieves pain & anxiety; Happiness, couch lock

Grape Pie - (Cherry Pie x Grape Stomper) - Cannarado Genetics
Fruity Pebbles - (Green Ribbon x Grand Daddy Purps x Tahoe Alien) - Alien Genetics

Jungle Boys made this strain famous at TLC, and it was one of my most difficult online snipes - gone in seconds, but I truly understand the hoopla. This is the total package, with face melting potency and the absolute best tastes imaginable.

I selected 3 keepers from a total of 7. Left to right, #1 (Grape Pie dom), #5 (50/50 mix) & #4 (Fruity Pebble dom). Flavors and smells range from pure grape/blueberry syrup (#1) to milky sweet cereal (#4) to an impossible to describe mashup of creamy fruit with a hint of fuel (#5). If scratch and sniff was a thing, you would break your screen trying to get at this stuff!

I searched but could not find terpene profiles for this line, but JB listed Sundae Driver as Myrcene & Beta-Caryophyllene dominant. Would love to have this tested and really see what the terpene composition actually is. What terpenes could grape and sweet milk scents be linked to?
 

WaterFarmFan

Active member
Veteran
None cheap, but check out Graingers.

Is there any reason why this would not work for ethanol and dry ice only (>-78C)? It does not have to last forever. Seems like O-ring is the weak spot on other mag drive models.

https://www.amazon.com/CHUGGER-PUMP-CPSS-CI-1-Transferring-Compliant/dp/B01N9HERFS/

Stainless steel pump head, Magnetic Drive w/ base, Teflon thrust washer, Clear Silicone O-ring, Ryton/Teflon Impeller, 55" cord with plug. Featuring a max flow rate of 7 GPM and 18 Feet of head to handle back-pressure. Capable of handling liquids up to 250 degrees F. The CHUGGER PUMP is the only home brew pump with ETL certification and USFDA food compliant materials tested for safety and performance standards.
 

Gray Wolf

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Is there any reason why this would not work for ethanol and dry ice only (>-78C)? It does not have to last forever. Seems like O-ring is the weak spot on other mag drive models.

https://www.amazon.com/CHUGGER-PUMP-CPSS-CI-1-Transferring-Compliant/dp/B01N9HERFS/

Stainless steel pump head, Magnetic Drive w/ base, Teflon thrust washer, Clear Silicone O-ring, Ryton/Teflon Impeller, 55" cord with plug. Featuring a max flow rate of 7 GPM and 18 Feet of head to handle back-pressure. Capable of handling liquids up to 250 degrees F. The CHUGGER PUMP is the only home brew pump with ETL certification and USFDA food compliant materials tested for safety and performance standards.

The issue with temperatures that cold, is the elastomers lose their resilience, so pump seals are eliminated by using a magnetic drive pump. -78C is cold for even a mag drive pump.

I know of someone who used a similar pump at -50C short term, but not how long it lasted.
 
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PDX Dopesmoker

Active member
The chart at http://www.leffingwell.com/odorthre.htm is really eye opening, but it seems incomplete. I found linalool & limonene listed, but a lot of the other familiar names are missing.
The concept that chemicals have high variability in smelliness is important and quantifying it could be extremely valuable. I've witnessed bud with modest terpene results overpowering ones with high overall scores before and I always assumed that all those number were telling me was that the lab reports on terps aren't consistent, accurate or meaningful. Now I wonder if I went back and multiplied the mass per gram of each individual terp on those lab reports by the inverse of their odor detection threshold and tallied them I would have a kind of smelliness index number for that batch of weed (assuming that the terp numbers on the lab resorts were accurate).
If there were odor detection thresholds for everything on the list in Sweet Mary part II we could have calculated loudness numbers for each strain. I can only assume that odor detection threshold for each chemical varies with temperature somewhat unpredictably, but having such a number would be the next best thing to exchanging odors via the internet.
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
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ICMag Donor
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The chart at https://www.leffingwell.com/odorthre.htm is really eye opening, but it seems incomplete. I found linalool & limonene listed, but a lot of the other familiar names are missing.
The concept that chemicals have high variability in smelliness is important and quantifying it could be extremely valuable. I've witnessed bud with modest terpene results overpowering ones with high overall scores before and I always assumed that all those number were telling me was that the lab reports on terps aren't consistent, accurate or meaningful. Now I wonder if I went back and multiplied the mass per gram of each individual terp on those lab reports by the inverse of their odor detection threshold and tallied them I would have a kind of smelliness index number for that batch of weed (assuming that the terp numbers on the lab resorts were accurate).
If there were odor detection thresholds for everything on the list in Sweet Mary part II we could have calculated loudness numbers for each strain. I can only assume that odor detection threshold for each chemical varies with temperature somewhat unpredictably, but having such a number would be the next best thing to exchanging odors via the internet.

One indicator of how loud the odor is, is its vapor pressure.
 

Pangea

Active member
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Check out:
"Characterizing the Smell of Marijuana by Odor Impact of Volatile Compounds: An Application of Simultaneous Chemical and Sensory Analysis" https://journals.plos.org/plosone/article?id=10.1371/journal.pone.0144160

Excerpt:
Fig 4. Compounds with high odor impact are not always the most abundant in concentration.

Horizontal axis is peak area counts (PAC) of mass detector response on logarithmic scale, assuming equal response for all compounds. Vertical axis is calculated OAV (Eq 1) for each compound. Highly odorous compounds emitted from loose marijuana (blue circles) and through packaging (yellow triangles) over 68 h at room temperature are 1) Benzaldehyde, 2) Myrcene, 3) Decanal, 4) Heptanal, 5) Methyl anthranilate, 6) Octanal, 7) Hexanal, 8) Methylisohexenyl ketone, 9) Linalool, 10) β-caryophyllene, 11) α-humelene, 12) Acetic acid. Highly odorous compounds emitted from fresh evidence of marijuana through a duffel bag (black diamonds) over 68 h at room temperature are A) Nonanal, B) Decanol, C) o-cymene, D) Isobutyraldehyde, E) 1-chloroacetophenone, F) Nerol, G) Propylamine, H) o-guaiacol, I) Linalyl acetate, J) Methyl anthranilate, K) Benzaldehyde, L) Limonene.
 

PDX Dopesmoker

Active member
One indicator of how loud the odor is, is its vapor pressure.

That would be a measure of the atmospheric density of potentially odoriferous chemicals without factoring in each chemical's individual odor detection threshold, wouldn't it? I have no idea how the detection threshold numbers are calculated, did you see anything about that? I'm guessing its something assembled from surveying test subjects like how they do wind chill factor & heat index calculation, it seems like it's too subjective of a number to calculate from a formula.

This is a really fascinating area of research when you start to scratch the surface. This part of the TAR article made me wonder how much of the je ne sais quoi of various places and times have something to do with the medicinal properties of the chemicals in the air:
A dab of linalool for instance produces that calm, serene catholic eye in my own system, and b Myrcene leaves no doubt where a large portion of couch lock comes from, while d- Limonene and a-Pinene sharpens my alertness.
A Dead concert is one thing, I know the atmosphere there is meaningful to how I feel, but the idea that the smell of the pines is affecting my psychology via medical routes when I'm out in a pine forest on the east side on a sunny afternoon in the autumn is really mind-blowing.
Kurt Vonnegut wrote about "positive viruses" or something like that in one of his books and his idea was that you'd get a bug and it would make you feel great for a little while or make you smarter until your immune system dealt with it properly. I thought that was a funny idea, but now you're suggesting that random smells in the air really do affect my mood and alertness, wild and crazy stuff for sure. Have your other guinea pigs had similar experiences? Are the effects as long lasting as the effects of dabbing THC enriched material?

Also I think you can combine your geraniol with citral to make THC in the lab, I read about it a couple years ago so I'm dim on the details, but that seems like it would be a really neat trick to pull off.
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
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Check out:
"Characterizing the Smell of Marijuana by Odor Impact of Volatile Compounds: An Application of Simultaneous Chemical and Sensory Analysis" https://journals.plos.org/plosone/article?id=10.1371/journal.pone.0144160

Excerpt:


The first three on the list have vapor pressures ranging from 2.29 to 0.207, but not in order of vapor pressure, so seemingly chemical composition has the dominant effect.

One thing I learned co writing Sweet Mary' Charms, is that extremely small amounts of some of the esters and diols can have significant effect. Mercaptans are a diol for instance, and are detectable by our sensory system in low parts per billionth.
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
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ICMag Donor
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That would be a measure of the atmospheric density of potentially odoriferous chemicals without factoring in each chemical's individual odor detection threshold, wouldn't it? I have no idea how the detection threshold numbers are calculated, did you see anything about that? I'm guessing its something assembled from surveying test subjects like how they do wind chill factor & heat index calculation, it seems like it's too subjective of a number to calculate from a formula.

This is a really fascinating area of research when you start to scratch the surface. This part of the TAR article made me wonder how much of the je ne sais quoi of various places and times have something to do with the medicinal properties of the chemicals in the air:

Check out aroma therapy. Our lungs are one of the gateways to our bloodstream.

A Dead concert is one thing, I know the atmosphere there is meaningful to how I feel, but the idea that the smell of the pines is affecting my psychology via medical routes when I'm out in a pine forest on the east side on a sunny afternoon in the autumn is really mind-blowing.
Kurt Vonnegut wrote about "positive viruses" or something like that in one of his books and his idea was that you'd get a bug and it would make you feel great for a little while or make you smarter until your immune system dealt with it properly. I thought that was a funny idea, but now you're suggesting that random smells in the air really do affect my mood and alertness, wild and crazy stuff for sure. Have your other guinea pigs had similar experiences? Are the effects as long lasting as the effects of dabbing THC enriched material?

Also I think you can combine your geraniol with citral to make THC in the lab, I read about it a couple years ago so I'm dim on the details, but that seems like it would be a really neat trick to pull off.

Check out, "The Total Synthesis of Cannabinoids", by Raj K. Rasdan, which reviews multiple processes for producing the cannabinoids out of other terpenes. http://onlinelibrary.wiley.com/doi/10.1002/9780470129678.ch2/summary
 

SkyHighLer

Got me a stone bad Mana
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Check out, "The Total Synthesis of Cannabinoids", by Raj K. Rasdan, which reviews multiple processes for producing the cannabinoids out of other terpenes. https://onlinelibrary.wiley.com/doi/10.1002/9780470129678.ch2/summary

(-)-delta-1-3,4-trans-THC is a resin that is optically active and is generally referred to as delta-1-THC. It is also known as delta-9-THC based on dibenzopyran numbering system. The other physiologically active isomer is delta-6-THC (alternate name delta-8-THC)


Link to a free download via Library Genesis (click on 'GET')

https://libgen.io/scimag/ads.php?doi=10.1002/9780470129678.ch2&downloadname=
 
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