I remember reading about it on trollitup or some shit years ago now at this point and it seemed boof for a butane alternative. And they kept pushing it as ‘organic’. Lol
I imagine it has it’s uses, but those were bs claims back then.
Worst terpenes I’ve ever smelled were extracted with dimethyl ether. I’ve only had terps extracted with this solvent once but they were so bad I don’t think the solvent was doing it any favors. Also extremely dark.
Deep vac + condenser
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Exactly, can even do it in a closed loop manner, recycling the same solvent through the material if required as well.
Ive tried it with my regular butane blend, put about a pound of gas through a column, didnt get anything but could be done better, probably didnt get the gas warm enough. Jackets everywhere is def key, but I think pre warming the gas in coil would probably be wise in addition to jacket temp control.
I think that perhaps pressure vs decreased might have some good possibilities.
This is my favorite subject.
yeah dont need nothing fancy!
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Me too!!!
Hot propane vapor. Then stick some jimmied terp condenser on the separator when it comes to boil off
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Exactly, im thinking refrigeration like path. Hot gas through material at higher pressure then forced through a small orifice into reduced pressure condenser, flash freeze out the aromatics whilst leaving the propane as gas.
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They also say if you thought of it someone else has. Not sure how i missed this thread back around the time i thought i was onto something.
Lifes been crazy. Never made time to dick around with this one
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I’m doing some forced RnD with ether, not extracting flower with it. More like a vehicle for filtration if the terps alone. I made a thread on it. Check it out give me your input. Also those terps I refined had a nice lemonene smell and didn’t look dark, rather reddish instead.
I talked w @magisterchemist on the phone the other day, he said people have been extracting in pentane and then running his membranes for solvent recovery. Supposedly the terps separated from the pentane after solvent recovery are super good.
Not something I’ve heard about many people doing, might be something to look into!
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Here’s one method of extracting preserved, in-tact, non-degraded terps with high efficacy; using fluorohydrocarbons to extract In closed loop systems. The properties of these fluorohydrocarbons allow for easy high pressure, low temp conditions in situ.
Check out this patent:
https://patents.google.com/patent/WO2008071985A2/en
This is an excellent read on the use on fluorohydrocarbons with very unique properties for selective extraction of terpenes, aldehydes, terpenoids and other fragrant compositions.
Here’s an excerpt:
Processes for extracting a desired compound or composition from a raw or bulk material which contains that compound or composition as a constituent part using an extraction solvent are known in the art. In these known processes, the raw material is contacted with the extraction solvent, often under vigorous mixing conditions so as to facilitate the dissolution of the desired compound or composition into the extraction solvent, and the resulting solvent liquor containing the desired compound or composition is then separated from the raw material for subsequent processing, e.g. distillation to remove the extraction solvent. Multiple extractions may suitably be carried out on the same raw material sample so as to maximise the amount of the desired compound or composition which is extracted from that sample. Typical examples of extraction solvents which have been used in the prior art extraction processes include hexane, methyl acetate, ethyl acetate, acetone and methanol. More recently, hydrofluorocarbons such as 1,1,1,2- tetrafluoroethane (R- 134a) have also been used for extracting products such as flavours and fragrances from materials of natural origin as disclosed in EP-A- 616821.
Although solvent extraction processes are used on a commercial scale, many of the extraction solvents that are currently used in these processes are not wholly satisfactory. Thus, when solvents such as hexane are used to extract flavoured or aromatic oils, such as are used in the food and cosmetic industries, from plant matter containing those oils, unwanted materials contained in the plant, e.g. high molecular weight waxes, tend to be eluted along with the desired oil. This problem necessitates subjecting the resultant hexane liquor or product concentrate to further processing in which the unwanted components are removed by extraction, e.g. using ethanol. Furthermore, many of the extraction solvents which are currently in use have fairly high boiling points, and the elevated temperatures which are employed in the distillation process to remove these high boiling solvents from the extracted material can cause problems. For example, the flavoured or aromatic oils contained in certain plants are complex substances containing a large number of individual compounds some of which are relatively volatile or relatively thermally unstable. Consequently, high distillation temperatures can tend to result in a loss of product either through co-evaporation of the more volatile compounds with the extraction solvent or thermal degradation of the more thermally unstable compounds. Hydrofluorocarbon solvents, such as R- 134a, can exhibit certain advantages over traditionally used solvents, being both selective and low boiling so that they can be more easily removed from the extracted material. However, the global warming potential (GWP) of hydrofluorocarbons is higher than is desirable.
Solvent based purification processes, such as liquid chromatography and high performance liquid chromatography (HPLC), are also known. In these known processes, the crude material to be purified is contacted with a solid adsorbent known as the stationary phase and the resulting solid is then eluted with a suitable solvent known as the mobile phase to progressively and selectively remove various compounds held on the adsorbent. The particular compound or compounds of interest can be collected in essentially pure form by monitoring the solvent eluate as it is recovered from the adsorbent.
In many liquid chromatography processes, the crude material to be purified is charged to the top of a chromatography column packed with a finely divided adsorbent solid as the stationary phase and is effectively washed through the column at a controlled rate by means of a flow of solvent. As the solvent flows through the column, it carries the crude material along with it, but the various components of the crude material are carried along at differing rates owing to the differing affinities that those components have for the adsorbent/solvent pair.
Thus, as the crude material passes through the column it is gradually separated into its component parts, and by appropriate selection of the packing material and solvent medium the desired compound or compounds can be collected off the column in essentially pure form as a solution in the solvent medium.
It also shows the comparative yields of specific fluorohydrocarbons:
Here’s part of the description of the small closed loop apparatus used:
In use, the plant biomass to be extracted was ground in a blender and the required amount of biomass placed in the glass aerosol tube. The metal cap and attached three-way valve were then secured in position over the open end of the glass aerosol tube and the tube evacuated using a vacuum pump connected to the three- way valve. The vacuum pump was then disconnected, leaving the glass tube under vacuum, and a pressurised container containing the solvent to be tested connected to the three-way valve via a quick-fit connector and the required amount of liquefied solvent transferred to the aerosol tube from the container. The aerosol tube was then shaken and allowed to stand for about 30 minutes.
Also this looks interesting:
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Well that’s good to know lol. Strike DME from the list
Also it’s worth noting that @Swet254k is using diethyl ether and not DME. Pretty sure they have substantially different characteristics.
That fluorocarbon method looks interesting, essentially just column chromatography in a closed loop. I’m not sure why 134a would make for a particularly good mobile phase though
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Purest terps I’ve had is from vacuum distillation. Either from flower or crude material. If flower, connect vac oven to mechanical cold trap, put oven to 100° F, pull vac for a few days. Flower method is really time consuming so it may be better to extract the flower into crude and put that into a boiling flask, set mantle to 50° C, and pull vac thru a cold finger/cold trap. Could put nice HTE in the flask as well, but you might as well use the HTE for carts as is.
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Flower in a vac chamber is slow because the the usual heating methods rely on conduction, when the flower that is contact with the heated surface area is dried out it acts as a insulator to the rest of the material, slowing down heat transfer. Adding a infrared heat element into the vac chamber is a good solution. Ive done it with some epoxy and a reptile light. Sped up the drying process significantly.
@Ruwan Very interesting post and paper! They go one to describe how to make “terpeneless” oil that is described and explained as more desirable. And how r134a is utilized to reduce levels of terpenes from essential oil extracts.
Essential oils are typically extracted or expressed from plant materials and are used for flavouring, fragrance and medicinal purposes. These oils typically contain quantities of undesirable compounds, particularly the terpenes, and the desired organoleptic compounds, which can be structurally related to the terpenes, but carry heteroatom functionality, e.g. oxygen containing functional groups such as hydroxyl, carbonyl or ether groups. One particular class of organoleptic compounds contained in essential oils is the terpenoids.
The terpenoid content of essential oils often contributes significantly to the desired organoleptic properties of the essential oil. For example, the aroma and flavour of citrus peel oils is largely determined by the presence of citral (an aldehyde), nerol and geraniol (alcohols) and their ethyl esters.
However, the terpenes are often present in large quantities in essential oils and tend to dilute or mask the desirable properties of the organoleptic compounds.
The use of hydrofluorocarbons such as R- 134a in the production of essential oils having a reduced terpene content is taught in EP-A-1332201.
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My buddy up in Oregon knows a group that have been isolating some world class terpenes using a pretty sweet technique that I’m not sure is out there yet. So here we go. I got around to trying it and it works very well. This method of isolating terpenes from crude hydrocarbon oil is a game changer. Not only are the quality of the terpenes about the best I’ve ever come across but they found out that this simultaneously decarboxylates the oil while extracting the terpenes- and it decarboxylates under more mild conditions and quicker than other methods I’ve seen.
The set up is basically a 5L distillation set up with some modifications. Use a 3-neck flask. One neck has a rubber septa with a small water line running through it and is used to inject small amounts of water at a time into heated cannabis oil in the flask (for proof of concept purposes you may use a long metal needle tip attached to a syringe with water in it, but eventually you will want to automate the process- easy enough with an inkbird unit and a couple of parts hehe). Center neck is equipped with a distillation head. A standard bump trap is placed in between the boiling flask and distillation head to keep bubbling oil from spitting up into the distillation head during the process. The third neck is equipped with a thermometer.
Crude oil is placed into the flask, no more than half full. Heat the oil to 90 C. The system is brought under vacuum and stirred using a rare earth magnetic stir bar. Water is then injected into the heated oil in small amounts (a few milliliters at a time). As the water is introduced into the system under vacuum it boils very actively and rapidly releases the small amount of water that was injected as vapor into the distillation head. This small amount of water carries with it a surprisingly large amount of terpenes. The oil rapidly cools down once the water is evaporated out, perhaps by 10 degrees C, and the oil takes a minute to heat up again to 90 C. As soon as the temp reaches 90 C another injection of water is shot into the hot oil and another portion of terpenes is carried over into the collection with the water vapor. The cycle is repeated until no additional terpenes are collecting with the water in the collection vessel.
The entire process takes 1-2 hours to capture all available terpenes. The percent yield of terpenes varies largely on the starting materials but they were getting 4%-7% on average from starting weight of butane extracted crude oil. Come to find out the process completely decarboxylates the cannabis oil too. My buddy said sometimes they ran it just to decarb material because it worked so much better than all of the other methods (quicker, etc…). Anyway give it a try, try to prove me wrong if you think it’s impossible.
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and with a rotovap?
Stick to hydrocarbon if you can. Steam grabs a lot of stuff that needs to be refined out in most cases kinda like co2. There’s always exceptions though. Technology advances quickly.
Never tried it, but my nerd hard on says this.
Terpene extraction isn’t new. Classical and advanced methodology applies.
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that’ll be five dollars hehehehe
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Testing Strip the terps in the roto and decarb at the same time at 90-95c and vacuum, thinking make a few modifications and upgrades because work better than i was think.
The first test come out water clear, the second test come out yellow and with some contamination(cbd) because i go to the limit of the tech for learning fast. I wash with water the terp fraction and dry with sodium sulfate. Smell very similar to the farm where i get the biomass.
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Cold distill your HTE
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