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Right to left: 1x, 2x, 3x distilled[/caption]
There's been a lot of interest in turning less than appealing concentrates into a quality product. Recently we were loaned a Kugelrorh and tasked with standardizing a method to produce a consistent product.
The basic work flow prior to distillation is very important. There are two steps that must be completed prior to short path; winterization and decarboxylation.
Winterization:
Dissolve the extract in 190-200 proof ethanol at a 10:1 to 15:1 ratio depending on particulate load. Chill to at least -40c but ideally -80c for 24 hrs. Filter in a buchner funnel using coffee filters on top of 2um fast flow filter paper. Distill alcohol in a still or rotovap.
Quick winterization:
Follow as above, except place dry ice directly into the ethanol solution and maintain for 2 hrs at -80C then filter immediately.
Decarboxylation:
Heat oil to 121c on a heated stir plate until all of the tiny bubbles are gone. If you get impatient and remove too early you'll likely have issues during the following steps.
Short Path distillation equipment:
A simple boiling flask with Vigreux condenser can be used to produce distillate. This is the most economical option but, also has the lowest yeilds.
A good example of can be found on Google or here.
The next step up in production efficiency is the Kugelrorh thin film distillation apparatus. Currently there are 3 companies manufacturing these; Sigma Aldrich, Buchii and Jkem. 
The next step up in production is the wiped film evaporation. A good example would be a Pope or similar apparatus.
A similar but, larger unit that uses a rolled film rather than a wiped film would be the Terp Trommel.
Process:
There are 3 distinct fractions in this procedure; 1) the light volatile's that have boiling points below or slightly overlapping 2) the Cannabinoid's and 3) non volatile's.
Dual fraction systems, those that separate one fraction at a time, temperature is raised gradually to remove the volatile fractions in order of their respective boiling points. Generally the lowers are removed below 185-195C depending on level of vacuum and film thickness. The Cannabinoids are separated next up to 260C in some devices and the black non volatile fraction is discarded.
Three fraction systems, such as the Terp Trommel, separate all three fractions in a single distillation step. Accomplishing this feat of engineering requires close attention to thermodynamics and residence times to separate the volatile's from non volatile's in continuous operation.
Post process:
Distillates can be re-distilled several times for improved color and stability. Mono-terpenes or vape ready flavorings can be added for improved flavor and viscosity for vape pens. Distillates in the raw can be vaporized or put into edible products for improved flavor over RSO products.
Pharmer Joe
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I don't understand why you need 2 distillation systems (rotary evaporator and short path distillation). Why not just use a short path distillation setup to remove solvent, and then gradually bump up the heat to separate other compounds? Why use a rotovap at all?
I don't understand why you need 2 distillation systems (rotary evaporator and short path distillation). Why not just use a short path distillation setup to remove solvent, and then gradually bump up the heat to separate other compounds? Why use a rotovap at all?
Hey there, I tried to watch the vid but it requires a password. I would love to see your work.
Hey guys, I was curious if this process could be done on a smaller scale? I live in Mexico so good weed let alone distillate isn;t readily available so I was hoping to start with a 50-100ml of refined oil. I talked to the guys at Summit Research briefly and was told with such little starting material it wouldn't have the pressure to move through the system. I'm wondering if it won't work at all or is just inefficient? I can live with inefficiency because it is for personal and the plant material I start with is super cheap.
Hey guys, I was curious if this process could be done on a smaller scale? I live in Mexico so good weed let alone distillate isn;t readily available so I was hoping to start with a 50-100ml of refined oil. I talked to the guys at Summit Research briefly and was told with such little starting material it wouldn't have the pressure to move through the system. I'm wondering if it won't work at all or is just inefficient? I can live with inefficiency because it is for personal and the plant material I start with is super cheap.
What do I do with the Terps of the short path? They always have a weird smell. Would it be better to buy a steam distillation system? Any info would help Please and thank you Josh
You could separate them by doing a slow and very careful fractional distillation varying both the pot temperature and vacuum.
Does the potency increase or decrease the more you rerun product?
The percent of pollutants falls, but the heat also changes the product some. For instance it can reduce delta 9 THC to delta 8 or CBN. GW
Heat on its own will not convert the thermodynamically more stable delta-9 THC to delta-8 THC. To convert THC to CBN one needs to oxidize THC with oxygen or extreme heat (heat that will do much more than just convert THC to CBN). However the distillation process will change the ratio of these compounds in various fractions, with earlier fractions being enriched with the lower boiling compounds, as each of these compounds have different boiling points (CBN = 365° F/185°C at 50 mTorr; d9 THC =392° F/ 200°C at 20 mTorr (~214 °C at 50 mTorr); I could not find an accurate and reliable bp for d8 THC, but it should be close to d9-THC). If you want to avoid oxidizing your material, especially while distilling, vacuum purge (below 100 Torr, lower is better but 1 Torr is good enough for this process) and fill your equipment/storage vessels with grade 5.0 or higher nitrogen or argon, repeat at least a total of 3 times. I've seen mention of other methods of removing oxygen, such as using sodium metabisulfite, however they introduce chemically reactive species into the process which can cause all sorts of fun problems...
A good point that oxygen is limited at 20 microns, but still present, making time at temperature an element. GW
Guys, my distilled CBD change color (inside vacuum distillation unit) from yellow to very dark red. How to avoid that process. I really like to have yelow cbd not dark red.
You need to protect your product from light and oxygen (purge your still with an inert high purity gas before you begin your distillation, and when you are done refill it with the same gas until everything has cooled to room temperature). It is best if you refrigerate it as soon as possible and store it under an inert atmosphere.
hi,i got my self short path distillation equipment 5l ,from open steel source ,got my self welsh vacuum pump 1400,trying to distill bho oil,no reaction starts before 300c to 350,i know it should start from 192c-245c,what am i doing wrong .please help
Do you have dry ice vacuum traps inline with your vacuum pump? Have you used vacuum grease to seal the joints? Is your pump full of vacuum pump oil? What pressure are you reading (you'll need a gauge able to read into the 1 mTorr or 1 mircobar range)? What is the distillation head temperature? What is the pot temperature?
Oh, have your insulated the still?
no, top of the 5l flask is not insulated
hi thank you for your respond 1.yes dry ice trap,2.yes using grease joints,3.vacuum pump full of oil up to the middle level,4.don't have that kind of gauge but have regular one and it shows -30hg of vacuum,don't have temp of distillation head(but what i noticed that the head stays little warm, till pot it gets to about 295c )
Hi, You need to get a much better vacuum gauge. If you can, please post pictures of your greased joints. Also, go to Home Depot and get a roll of fiberglass insulation and wrap a layer around the top of your still (unless you already have a upper heating mantle). This will reduce your heat lose, making the distillation more efficient. By what you've posted, you have a leak in you system and are not getting to a low enough pressure (you'll need to be at least in the 50 mTorr range, which will give you a boiling point around 200C). You also need to be measuring the head temperature, the pot temperature will ALWAYS be much hotter then head temperature (better insulated, the lower the pot temperature).
Do you have a micron vacuum gauge in the system? Your absolute pressure appears to be too high. GW
hi,no only have regular vacuum gauge shows -30hg
Aside from the variables surrounding the material itself, temperature and partial pressure are the two principle process parameters, so it pays to be able to measure those two variables accurately, for process predictability and to figure out what is wrong when things don't work as predicted and planned. If you can't afford a micron/militorr gauge, but know for sure what the temperatures are, you can stumble through by inferring the partial pressure, by watching what does or does not happen. If we ASSume that is the case here, you have a leak. How many joints in the system and what kind are they? As TW notes, the critical temperature is the vapors in the head. The pot will be at the boiling point of the mixture. How are you measuring the temperature there? GW
I infer from the temperature reading something that I have noted several times myself, albeit my rig is a 250 ml boiling flask. You are measuring the temperature of the gas/vapor at the exact point of the thermometer. Your statement said no reaction takes place which could mean a great many things but I assume that you mean you do not see drops forming on the vigereux indents before this? So at least you boiled extract! At any rate, you have a 5L boiling vessel. The formula for computing the surface area is 4 pi r squared. A five liter boiling vessel has an inside radius of about 4.25 inches. The calculation computes to about 227 square inches. By contrast my 250ml flask has only about 36 square inches of internal surface area. For fractional distillation to proceed every square inch of the internal surface area up to the point of the fractioning column must be heated to the boiling temperature at any given pressure in order for the gas/vapor to work in the system. The fractioning column itself must be insulated very well up to the top of the head. For extract the stuff weighs about one gram per milliliter. Even at 250ml my flask is huge as I mostly never use about a tenth of that capacity. Moreover, the average 250ml flask weighhs about .6 pounds. Amazon shows the shipping weight of one 5000ml flask to be ten pounds. The task of heating all that glass up must fall to external heat sources all the way to the point of the fractioning column. ANYTHING like exposed external glass will cause nothing but headaches because the rig is not fractioning the way it needs to. At 5 liters of diameter this alone is likely the cause of your frustration. I even bought a 50ml flask with 24/40 joint to do this! I use 24/40 because it is what I have though in theory a smaller diameter would have even less surface area and mass to keep heated. I have used thermocouples to test glass temps and together with my analog thermometer notice that the flask temp is at leaat 15C higher than the head temp. I doubt this would be the case if I had more than a bottom half heating mantle. It is a good setup for hobby but for even the 250ml flask I really need a full top and bottom heating mantle. For now I wrap the top potion of my rig in hobby grade fiberglass matt from Amazon. I wrap it several times with the fiberglass leaving a looseness to it that insulates very well. I pin it with a metal pin to stay. You also did not mention the vacuum regulator setting used, but as you can see my hunch is that you are fighting a very large surface area and mass of the glass itself that is not allowing the ENTIRE boiling vessel to reach the temperature you have set. It is definately not an easy task to do what on paper seems simple. Be prepared with back up glass - the price of learning as you go is broken glassware. Trust me. 🤔
You are probably left with some black or very dark extract from boiling it. Here is how to clean it up; Disolve all extract in isopropyl alcohol. Place in freezer until the first cloudiness happens. An hour or two. Then put a half inch or so of aluminum oxide on top of a fine frit buchner funnel. Using a vacuum pull it through. Lots of sludge on top. Then take mix after first run through and add 30% again by volume of water. Mix well and into the freezer again. Then with fresh alumina in the Buchner funnel pull it tthrough again. More sludge. yuck. Repeat freeze/alumina cycle until mix pulls through without leaving sludge. Evap off or distill off the isopropyl alcohol/water mix. I heat thte oil very hot and vacuum chamber it to dry it. The alumina makes clean up a cynch compared to the sludge building up on the fine frit of the funnel. Alumina sure stops the darker gross stuff from getting through and is a great way to clean up a botched extraction too. Note: the exact ratio of iso to water does not seem important - qty shown is nominal https://vimeo.com/205242532
I should mention that this will turn the oil a beautiful deep red color. The water added to the isopropyl alcohol when boiled or evapped off will seperate from the isopropyl and combine with nice fruity smelling terps which will turn the water white/chalky colored. At this point the red oil will have nearly completely seperated from the water. Place this whole thing back in the freezer to begin final drying by freezing the oil hard and allowing the water/terps to easily be poured off. If the water is not chalky white but more red or orange/white there is still good extract in it but not a whole lot. Either boil this down further if possible or centrifuge it at 4000 rpm after a freeze to facilitate final seperation. The resulting red oil has to date always been of exceptionally high quality and smoothness when vaping. It is EXTREMELY potent when refined this way and often takes me by surprise after a hit as to the potency. I believe most of the potency is from the fact I can inhale the purified oil much deeper and take a much bigger vape hit because there is generally zero respiratory irritation as opposed to fresh extract without refinement, but also the delightful fruity taste encourages deep inhalation.
Here is the oil from my own messed up experiment but cleaned up in the video above with the buchner funnel/alumina combo. This started as black tar which I cooked in the oven at 300F for an hour or so after a botched short path attempt. Very fine red oil and this is my favorite of any 420 product. I finished it up this morning. https://vimeo.com/205242532
oops. Wrong link above lolz. https://vimeo.com/205396195
Here is a video on making clear concentrate using my short pathh distillation aparatus. In this case there is no vacuum used The energy used instead to pull over the clear concentrate is steam. The steam injector is a 150ml flask with a stopper. Into the stopper is the glassfitting from an old Vape Bothers vaporizer which is glass and is tall enough to keep the liquid water from surging over into the hot oil. Water vapor is less dense than standard air. When two immiscible liquids are boiled together it is possible to co-dostill them at the same time versus a fractional distillation. This has been done for many eras of men and is a great way to recover oils from plants. I am starting with an extraction that is sold in dispensaries so the purity of the starting product is high to begin with. Watr co-dostillation can clean up any extraction. Even extractions made with the dark tar colored RSO style extractions clean up into pure. Moreover, the product becomes fully decarboxylated at the same time. Not shown in the video are shots of the lower boiling point liquids being distilled over, which smell nasty and make the water cloudy. My iPad has the Magisto App. I tell it to use all the photos and videos of a certain day or time and it puts them in order.tpThe video shows a complete run with photos in order. It let me choose my own music from my personal library. Note: Steam distillation MUST NOT be underestimated regarding burn potential. I grew up in farm fields changing irrigation pipes as a kid in mint fields of Madras. They use steam distillation in VERY large units that get tractored into the field and are made of steel which they use to pull mint oil out (I stole the idea). I prefer to cover the glass boiling portion of my 250ml unit with fiberglass matt (hobby section on Amazon) by wrapping it around the unit. It helps the heat retention but also is a barrier should the boiling flask rupture for some reason. If the steam generator malfunctioned and puked a huge volume of water into the flask this could be enough to make the unit at last seperate at the joints from the pressure. A top heating mantel would help as well. https://vimeo.com/196677515
The very last shot in the video is when I put the thermometer into the boiling flask, replacing the steam injector right after I shut down the heating units. The temperature in the head unit took a sudden nose dive, then jumped up to over 100C. This hapenned when the unit had stopped producing clear concentrate in the head. Very wierd, but if you look at the last thermometer shot you can see the temps of he vapor in the flask are over 220C, while the temps at the head unit are that of the steam; 98C.
authors (stoners) note: This is a hobby for me only. I appreciate the email offers for $$$ in return for consult but that would spoil the whole concept of retirement! I do not accept offers of work or compensation of any kind.
why extract has to be dewaxed before distilation ? Whats happend if I start to distilation undewaxed extract ?
Hi tom, from what I understand plant waxes have a similar boiling point to that of the cannaboids. If you dont pre winterize you may end up with waxes in your distalate.You may want also decarboxilate also, it makes the distalation process smoother, less prone to bump.
"wax" is a term used not to describe a single compound at all in a normal sense. The plant waxes will begin to break down almost immediately once the temps exceed about 330F from my own personal experience. Without analysis it is impossible to know what the oxidation and thermal degredation compounds will be. Keep in mind that in any given extraction there are a number of volitile organic compounds (VOCs) that act as solvents (known as terps) that also act upon the constituents of the plant waxes when heated. I do not dewax when co distillng with steam because the constituents of the extract never exceed a temperature of about 115 C in the flask and about 98 C in the distillation head. I choose not to dewax because the plant waxes and the THC are miscible. Any wax removed will remove THC which I covet. Plant waxes offer very little to no harshness without the prescence of the VOCs (terps) which the steam distillation easily fractions out. I frankly much prefer the velvet feel of the wax left in when not burnt to a in the distillation. When you do a steam distillation and remove the low boiling terps you can always choose to save them and add them back although it is beyond my understanding why a person would do that once you sample extract without them included.
Hi Guys Could you explain me proces shown on that movie https://www.youtube.com/watch?v=dgfPI0MbLho from 2.07min Dehydrogenated oil is mixed on molecular level with alcohol - emulsification - then cristalized ?? how to do it step by step ? anybody know ?
They seem to be describing winterizing.
Hi Guys I have a question. Is it possible to remove THC from hemp concentrate and leave there only CBD ? I have paste 20% CBD and 2% THC. I need to remove THC to level 0,2%.
Boil the paste in a flask until it stops producing a pine scent/menthol scent fume, ten continue the boil until it reduces by another 5% or so by volume. This will eliminate all of the pinene and lower boilng components and the clue is ofactory. The scent when it begins to boil off the pinene is strong and the boil is brisk. The boil will settle down considerably when the majority of the pinene is gone. This is the point of purification that I tend to cease the boil because the next thing thtat boils off is thc which I am wanting. I have boiled many ounces as the first step in purification. Irregardless of purge method used, without boiling the extract residual volitile components will remain in the extract after a supercritical extraction. When extract reduces it becomes dark. Keep the heat just low enough to initiate a boil. A tiny flask in top of a 24W heat lamp turned up as a base will heat the mix gently to achieve this. The mix will froth considerable at first and I use a glass stirring stick to mix it so it does not boil over. When you keep smellling the vapor it will be at first extremely harsh to smell but as it proceeds it will become to have a very sweet odor . This is when I stop - that is the odor of thc mostly. Patience is key but men have been slow cooking marijuanna extract for several thousand years for a very good reason.
Here is a short vid I I did of my own boil yesterday. I targetted 10% to cook off. Past efforts indicate that 10-12% by volume of the extract that I get to be pinene. This cook comfirmed (from odor) that 10% was the point that odor dropped off. Inhalation close to fume went from stinging to nearly undetectable. This is typical. Vaping is pristine and medicine grade potent. This was not winterized or filtered in any way. Just plunked into a beaker topped with fiberglass mat and activated charcoal and brought up gently in heat to a boil. On my stove it ends up at about 70% of the way up on the knob. The odor can become very foul as it cooks and the color turns (in this case) from yellow to red to black as it cooks down. Its actually so red it gets black if that makes sense. https://vimeo.com/190684160
Same flask. Oil after boil is thick and hard to light on fire. Dame extract but before boil is highly flamable. A tiny dab produces considerable flame before boiling. This is an intermediate step to the final polish of sweet sweet cherry oil. The nex step is in process as this vid is posted. It is a boil in iso/water (rubbing alcohol). A vacuum chamber purge will follow evaporation. There is no better oil than cherry, and no loss from winterization and wax removal saves me money on med. https://vimeo.com/190712411
Hi Tomas, I'm a PhD chemist with 15 years experience, most of which was in the pharmaceutical industry doing drug discovery and process R&D. Yes, it can be done, however distillation is not a practical solution as one would have to run the material many times while carefully splitting fractions and suffering large material loses due to hold-up and issues with pot-residues. It can be done via chemical reactions, however you'd destroy most of the rest of your material in the process. Crystallization at the stage you are at, won't work as successful crystallization usually requires fairly pure starting materials. This leaves chromatography, which can be done manually (requires a lot of patience and skill to make the columns, especially large ones) or via automation. Chromatography systems that can process up to 300 g of crude per run (1 run takes about 1 hr) run around $80,000 and require a means of removing/recycling large amounts of solvent. Things get easier if one has not decarboxylated the material, as the acids easy to separate from the rest of the material, however you have to be in a proper chemical lab/manufacturing plant to do this (also true for doing chromatography) - it is a building/fire code and EH&S (environmental health & safety) issue. If you'd like to know more I charge $100 per hour to consult, and I can be reached at wahl.troy@gmail.com
green photochemistry inorganic organic
A supplier friend brought by some black goo lolz and wanted to see what could be done. Waxes were removed by disolving in rubbing alcohol, adding a small amount of alumina to the solution, then freezing. Out of the freezer into a centrifuge at 4000 rpm for 15 min, then into a clean tube and repeat the freezer cycle until all waxes were removed. A test run on the dewaxed portion confirmed that pure short path was impractical with my gear on this particular sample, so I decided to use the short path apparatus to co-distill the extract with water. Co-distillation solved the problem but a new question popped up; why did this batch require a head temp well above the nominal co-distillation temperature? The batch co-distilled nicely and the green goo left in the boiling flask will be flushed and the refined product run through a second time after all glassware has been hand washed and run through th washing machine. Co-distillation does not produce the hideous smell that regula distillation does but the fresh pine scent in the water is enough fresh pine scent for six neighborhoods lol! Now my drains smell like pine trees 🙈 https://vimeo.com/180018203
Hello, redturtle984! My name is Beny and I wanted to know if I can ask you a few questions regarding Short Path. I have been doing it for 3 months and have had relatively good results. I have a few questions regarding process. I have read many of your posts and watched your videos and would like to pick your brain if you are opened to it. I live in Los Angeles CA. Thank you
Hi beny, My email for questions is redturtle984 at gmail dot com. I would be happy to share anything about what I'm doing. I do understand why others see an economic need to hold back info but my interest is in health of using the product. I replaced a great deal of morphine/opiate pain management along with management of severe PTSD (Marine Corps) with these extracts. The problem I faced a few years ago while still in a wheelchair was that I sensed the medicine was working but the dosages required so much vaping that my lungs could not take it. I developed a smokers hack and felt the constant tickle urge of wanting to cough all the time. However, I noticed that the deep irritation and coughing during consumption was primarily only while vaping a dab and not smoking it using a lighter AND that my vaporizer aerosol mellowed out considerably on my second and third large hit off the vaporizer. This is how my hobby started lolz. I had shattered my right tibia plateau into several shards along with a punctured lung, four broke ribs, massive internal bleeding, and a REALLY nasty set of complications. What I was learning was that the harshness of the hits I was vaping was at both ends of the temp spectrum. It was always harsh to me at the lower temps and at really high vaping temps, but in the middle was a real sweet spot. The low end temperature harshness is pinene. The upper end is limonene. Pinene is harsh the moment I inhale. Limonene is a deeper burn and is delayed a bit. Coughing from from a deep hit of high temp vape I noticed at times can make the high zoom up to a good rush, but I noticed that coughing and hacking at the lower temp of a new dab only really interfered with the intensity of effect I need. At first I believed that it was the waxes in the product causing this. I was wrong. I also noticed that the info I could get from online did not match what I was learning, plus an enormous amount of time on my hands led me to making videos about it on my iPad. Since starting to refine my own extract the coughers hack went away entirely. No tickle in the chest anymore. My energy levels zoomed up, housework started getting done and I just felt better.
Here is a vid my cool iPad app spit out from pictures. I have found that covering extract in Aluminum Oxide then running that at high temp and very low vacuum in a cryogenic sublimator will utterly deoderize the extract. It removes or converts all pinene which collects abundantly on the cold finger. This is a sublimator but used as a modified short path to fraction just the first fraction. The other parts of the mix can be recovered selectively from the Alimuna by timing the soak of the extract covered alumina in a fairly polar solvant and/or adjusting solvent polarity to extract the desired fraction from the alumina. The oil becomes blood red and is evaporated of the solvent then vacuum purged and boiled in H2O. Boiling it removes a lighter than wat portion of the oil, a very small part, and the rest is dewaxed and enjoyed to great effect. I suspect I am isomerizing nut not oxidizing a number of substances and it becomes a very pleasant flavor. Very simple setup but only for personal use quantities as can be seen in the video. I do not use flower but theorize that bud brought up to high temp in a vacuum like the sublimator will also release the pinene (very nasty smell) without destroying the thc. Enjoy. https://vimeo.com/178249458
I have petitioned the Olympic Committee to consider Separation Alchemy as an Olympic Sport! Please sign the petition.
A short vid showing a sublimatoe being used as a short path distillation. It turns extract into clear which is wiped from the cold finger. https://vimeo.com/176391754
The extract wiped from the bottom of the cold finger is clear light yellow thc oil. I have not tested any in a lab and likely will not as my home hobby lab is suitable for me. I have a column chromatography tube ($35 at Ctech glass) and have used an airbrush air pump to assist (rudimentary flash chromatography) and am using aluminum oxide between 100-400 grit also for seperation and I am setting up the unit to test the purity but it will not be congruent with certified results so would be meaningless comparatively. I will caution about my video using the Chemglass Sublimator ($350 from Amazon). The dark oily portion of the extract left in the bottom on my first run had visually ceased producing vapor and was a fraction of the beginning gram. It looked like vaporizer residue, nearly black to black but under vacuum still seemed like it was all done. Until I released the vacuum and broke the seal of the sublimator....wow! The residue on the cold finger is just fine, but once atmosphere hit that hot oil - instant nasty, make you want to vomit smokey fume filled the vessel bottom vessel. I suspect the smoky vapor was volitile from the odor. Not necessarily a safety issue, but next time I am going to use my infrared camera that plugs into my iPad to confirm lower temps before releasing vacuum. It takes less than 30 min start to finish to produce clear from raw extract using this device. One vacuum pump, one sublimator, Nalgene vacuum hose ($17 per foot on Amazon), a hot pad, stands, and ice water, and one iPad to document all this foolishness is all it takes. I do not grow but my hunch is that any extract from iso, hexane, or any other suitable source and not just supercritical fluid extract could easily be purified this way.
For safety, one should use an oil bath (a deep frier would work) as a heating source instead of setting the sublimation chamber directly on a hot surface as is shown in the video. By setting the chamber directly on a hot surface, one risks uneven heating which can crack the chamber. Also, the oil bath will heat the sides of the chamber making the process more efficient. Finally, let the chamber cool to room temperature before releasing the vacuum; this should help reduce/eliminate the smoke.
Copy and paste from the manufacturers website, the specs on the unit are specific and the instructions were followed per specification. Please contact the manufacturer with your concerns Dr. Wahl. I am gonna vape some of the clear now lolz. CG-3038 SUBLIMATION APPARATUS Two-piece grease-free sublimer with a flat bottom to enable heating on a hot plate stirrer. Condenser has a large top opening for use with dry ice / acetone or liquid nitrogen. Connection between the flask and condenser is made with a flat o-ring joint permitting parts to be gently separated for maximum product recovery. The capacity listed is that below the bottom of the cold finger. Vacuum control is provided by a 0-8mm grease-free Chem-Cap® valve. Complete apparatus consists of the condenser, flask, Viton o-ring and horseshoe clamp.
Generally, glassware is heated in oil, sand or other types of baths or heating blocks which ensure uniforming heating both to improve heating efficiency and to avoid heating induced stress cracks (this is a major problem with flat-bottom flasks, like ChemGlass CG-1502). That said some glassware is designed to set directly on a hotplate: beakers and Erlenmeyer flasks. All that aside, you well get better performance if you use an oil bath, especially if you work with more than a gram of material (none of the solids will form on the other wall of the chamber). For the scale you are doing, it probably doesn't matter all that much.
Kudos to you Dr. Walz for the suggestion of the crock pot. I filled the bottom with sand so the sublimator can be positioned easily the n fill the rest with fractioned coconut oil from Amazon. the label says it is good up to 350F for cooking and my last run purifying extract was substantially below that. The main advantage I have for,personal use is small sample size - just a few grams or so. The sublimator vacuum gets very low, pegging the gauge at the 30" mark (analog gauge). Obviously the sublimator is like a vacuum chamber all by itself but one that is heated on one side and cooled on the other. I think the cooling of half of the vessel contributes to a great vacuum. The first fraction off smells just like pine needles being crushed. Without that substance, pinene, in the extract I am vaping now without resperatory burn even without dewaxing. The extract, referred to as "Hulk" has zero odor at room temp after process and is quiet odiferous before. Thank you again for the tip.
My main problem during this lab really was I used completely unprocessed extract straight out of the package. Anytime raw extract is cooked it tends to pop and sputter. Dabber know this lolz even though their temps used are much higher. I have found this behavior in all purchased extracts so it is nominal. I have a process using iso that we previously discussed until the dog done died that stops this sputtering completely. I suspect that the sputtering is from hydrophilic substances present in a mostly hydrophobic mixture because the iso process I use removes most of the former plus the waxes. The sputtering in this lab popped a little up on the glass sides and cold finger. I am still pondering a mechanical solution as the iso wash is very involved comparitively. Maybe a lower temp as well. Vacuum gauge was pegged at 30 on the mechanical gauge and I am notoriously impatient so heat things quickly. Now I just have to wait until payday to afford the next sample lolz! Can you write a grant for me? 🤓
hi,message is for Mr. Troy Wahl.hello sir i am ready to spend $500 and to sign NDA agreement ,how can can get in contact with you.thank you.
I can be reached via LinkedIn (I'm the only Troy Wahl in the Portland Area of Oregon). Just send me a PM and we can talk there.
Another run done in the sublimator. Started 5g fresh extract, removed .5g clear pinene (pine scent). Sublimator tipped causes drip of pinene to fall out of boiling crucible. Activated carbon pellets are very hard and retain heat and absorb volitile organic compounds (VOC) like pinene nicely. Vape is chalky sweet, waxes left in, zero respiratory irritation and as potent as it gets. Started with "Hulk". Temperature of oil/sand bath constant at 147C (296F)(421K) and the vacuum held constant at 30" on the vacuum gauge. Clear condensate seen on finger is pinene. I estimate that 12% of this extract was alpha-pinene. MSDS for that recomends no inhalation or skin contact. https://vimeo.com/177770547
I put activated carbon pellets into the oil cup on my dab rig and dab onto those. They really smooth out the vape plus make smoking it a good option for me.
https://mobile.twitter.com/pancakespoons/status/758340051944169472/photo/1 Here is the wipe using silicon mat.
I just vapes some. Faint aftertaste of pinene . Same quantity of vape I normally dose with of this has produced a profiundly potent high and an unusual body rush. Very potent. yay. 😗❤️👌🏼
Hi, whats a good condenser temp to start with? I was also thinking about flushing the apperatus with nitrogen prior to pulling a vaccme on it. Do you think that this would minimize side reactions caused by oxidation? Aslo what is the purpose of decarboxilating prior to distalation? Is it so the cannaboid fraction will have a similar boiling point? Does it somehow make the tastes bad? Whats going on in there when thca is distilled?
I would need to know more about which system you are using to give you a temperature for your condenser. The purpose of decarboxylation prior to distillation is so that the solution doesn’t foam and bump during distillation.
Hi, going to be using a short path distalation apperatus with a small vigerux section, the condenser is about 175mm. The glassware is 24/40 and I plan to use a 1000ml boiling flask with 3 100ml receiving flasks on a cow.I have a welch high vaccume pump and savant refrigerated cold trap.Im heating it in a pid controlled oil bath/ mag stirrer. Any advice?
The answer to condenser temp is both easy and complex: The easy part: it needs to be warm enough so that the distillate does not solidify but not so warm that it does not condense. What makes this issue complex is that mixtures (common in extract distillations) melt at lower temperatures than pure compounds and that the distillate can dissolve small amounts of compounds that would otherwise be solid. For a distillate containing THC start around 75C, but you'll need to experiment a bit as different set-ups will have different requirements (remember, the distillate has to remain warm enough to flow into your receiver and not just out of the condenser). Purging your equipment of oxygen prior to use (either for extractions or distillations) is a good as oxygen reacts with your product. The best way to do this is to close your equipment, evacuate it to less than 100 Torr (~ 1/8 atm), fill with nitrogen, and repeat twice. It is best to use a check-valved bubbler (such as a CG-4522 from ChemGlass) when supplying gas to sealed glassware so as not to over pressurize it. For solvent based extractions (other than butane or propane) using a continuous supply of nitrogen will help minimize oxygen. However, for distillations the nitrogen supply should be turned off unless one is doing a distillation at 1 atm and it is connected after the condenser (if it is connected at the stillpot it will screw-up the distillation). One can not distill the cannabinoid acids, attempting to do so will decarboxylate them. If you want to isolate them as pure compounds, contact me directly.
You can't mechanically remove other oils from the extract.
I did not say anything about the methods one can use, just that it can be done. That said, you are correct, purely mechanical methods will not work.
Sorry this was supposed to be on another post about mystery oil. My phone is having issues.
No worries.
I am going to attempt to use my cryogenic sublimator to obtain pure. I washed the extract to nearly pure using mostly info from a patent on purifying citrus oil. The problem I see is that I cannot get all the higher boiling point terps out with just a wash described in thte patent. I even centrifuge, like the patent decribes. I took videos of it so I could analyse it but my main concern prior to doing a lab plan for the sublimation just how to go about it. My belief is that the temperature needed to get the stuff into gas will heat the terps and change them. I know what burnt terps/shatter tastes like and it is foul to me. So I am at an impasse as how to,procede. The first part in the patent worked magic. Pulled put waxes and undesirable terps to a great extent. End product nearly clear. Citrus oil seems to have about the same challenges involved with the pirification of it, and it seems to me after using the info that it works for raw marijuanna extrat also. I am at the last part requiring fractioning. I have evaporated off the binary solvent and the terps that it took with it, so now am to the distillation part using e cryo sublimer. Any input anyone has on set up cautions and safety considerations please feel free to input. I am planning the ice bath to be iso and dry ice because I can get it pretty easy. My mobility is limited so easy is good! What pitfalls does anyone see in the plan I outlined above for getting to pure?
I have a helium tank here at home that I use to fill balloons for kids in the neighborhood. Since I have this gas and I am just a hobbyist in this, can I ourge the system of ambient atmosphere with the helium in the same manner as described for nitrogen?
Yes but it's much more expensive and I recommend a two stage regulator.
Actually helium is less effective than nitrogen for maintaining an inert atmosphere. Argon , also pricy, is probably the most effective choice.
I have been doing more research and ran across alot of people saying that their distillate has an unpleasant odor, is this a fraction present in the starting material or is it molecules being destroyed by heat? Also how would I prevent this?
As I recall the acid form of thc boils at 90 deg F lower than the converted Delta 9 form. Since than conversion takes time I think it would mean the boiling point would be plotted in an unpredictable curve. I think that a substance that slowly changes boiling point because of decarboxylation would through off a reflux unit, wouldnt it? I just got a cryogenic sublimator and plan to,try to sublimate thc crystals on it. I am planning to decarb the sample sully prior to,the test because I do not want to sublimate the acid form. Any suggestions or comments are welcome. I appreciqte this forum.
There is more going on than simple fractioning. At very high temps limonine breaks down into isoprene I believe, and isoprene boils at about 140 C lower than limonine. I believe that in the moment limonine breaks down it boils out as isoprene. I allowed my extract to boil until refluxing on a beaker. It got black and nasty looking and the fume smelled bad. The next day I vaped some and it was perfect. Deep smooth vape hits, no hacking or choking followed by a very fun high. Highest potentcy. There is a taste that I can only describe as pleasantly toasted. Like carmelized sugar but not so sweet in the vape. Fruity. I am making more lolz. The beaker cooking the extract was on my stove top. I had the stove nearing med high and over 350 F when I put the thermometer down to cover the mix from popping a bit. It boild but got VERY hot before it did. I hope some of this helps. I am gonna vape some of this deep red to black but clear and stony sweetness now. Is that wrong?
While limonene can be oxidized, it is extremely difficult to decompose it into isoprene especially in the presence of oxygen. This is also true for the rest of the terpenes/terpenoids. The other issue one needs to consider is that heat and light (UV) can cause these compounds to polymerize.
I lacked the right thermometer to test my boiling puddle so i am, not sure the temp but it got very hot. The fume was repulsive to inhale when I removed the lid, but a sit in the freezer overnight led to some of the most pristine vaping I have every done. The stuff is glass clear but dark amber, almost red. Dr. Wahl at what temperature, given that the mix of actual components is unknowable, do you believe the limonene and other terpine break down into more volitile components like isoprene? My stove top was set between med and high to get it to finally boil in that beaker enough that it was feluxing down the sides. I llaced a dish of glycol I keep in the freezer for a cold bath on top of the beaker as a cold lid to help it reflux. I recorded all the things on my iPad on video this last run. Using the info in the patent of citris oil purification I have made nearly clear product using just the simple binary solvent listed in that patent and centrifuging to remove the gunk. I discovered that a paper filter rated "slow" to catch fine particulate lets cloudy material (DNA?) right though and this can only be removed in a centrifuge. The VAST majority of the cloudy nature of extract is quickly removed when following the steps in that patent. The results prior to any heat application but a vacuum chamber treatment at 29.5" of vacuum for 15 minutes were so,clear that I have to tip the beaker so it will run to see the yellow tint. I did not heat half the stash and it too is 10 out of 10 for potency, but still has a bit of that "mentholatum" type mediciney feel that the other half which was boiled doesnt. The other thing that might be affecting taste is a mystery substance that ALWAYS appears when I cook this stuff in the binary solvent used in the patent; it will start out clear, then long chains of white gunk slowly form in the clear liquid, They will appear enough to fill the dish, then after just a few minutes they begin to shrivel and turn black. They tend to drop out of solution then and fall to the bottom of the pot. Components like these are likely the cause of foul odors? What is it that rolls out of solution after filtering then shrivels up and turns black? I have a video that shows the form the shrivel the turn black. Thanks for letting me share. I am gonna vape some red now. I have the advantage of being my own test subject! I just have to wait until next payday for more testing material. Peace fom Oregon.
Pyrolytic cracking (breaking C-C bonds with heat) is typically done at over 300C (570F), several atmospheres of pressure and in the presence of catalysts. Remove the later two, and one will need much higher temperatures. Pyrolysis, however will not happen in the presence of oxygen. At this point, you've reached the end of my willingness to answer your questions without charging.
no worries. I knew a professional lady in Memphis that reached that point in just a few minutes! You have been more than generous with your intellect. Thank you.
Did your first runs have any bad odor? I saw a youtube video of a guy discussing fractional distalation of canaboids, he talked about an odor that was unpleasent. He also talked about the odor being removed by allowing it to overshoot the condenser into the cold trap whilst still collecting the cannaboid fraction.is it possible that this smell is degraded limonine? Because its boiling point is lower that the canaboids it could be possible that this is responsible for the odor? https://youtu.be/z5hFjExd8vc here is the video, the man isn't very educated the way he talks, but I think there is some information to glean from it.
Here is what dispensary extract looks like after the wash I talked about and after the vacuum chamber but before heating or attepting boiling. It is runny like molasses and the high is pristine. this is nearly pure medicine in this form but turns dark red to black when boiled as I mentioned above (this was the other half of my stash I did not boil but came out of the same stuff. https://www.amazon.com/clouddrive/share/Cun8EMFeznWqSstmPt5VqyfxfncQOqkTuUj9u6Mq3zj
this guy is fucking awesome he has the right information, i can't wait till the next one comes out
The foul odor he speaks about is alpha pinene which is the main component of turpentine. It is repugnant to smell and is ine cause of espiratory irritation.
I should add that alpha pinene is one of the only things in extract that is miscible at least partly in water. This is what the iso wash removes.
a-Pinene smells strongly of pine. It's fairly pleasant, actually, if you like pine. That's the main and virtually only fragrance note, and one of the most common and recognizable terpenes in cannabis. Pinene (alpha and beta) is also used in room fresheners and cleaning supplies. The foul smell you are getting may contain a-Pinene or its derivatives, but comparing your description to the large bottle of it that we have in our fridge, there is more to it than pinene.
Try heating that stuff you have in a bottle Captain up to the temperatures needed for fractional distillation in the process shown and take a good whiff. After you barf, tell me again you want that odor in your cardboard pine tree dangling from the rear view mirror lolz. You have the stuff. Give it a try.
Hello Skunkpharm, Just wanted to say thank you guys for everything you do. I work in a cannabis testing facility here in Colorado and I'm just curious if you have any potency testing results for these distillates. I'm sorry if I've missed this topic somewhere else, just came across this article in a quick search. Keep up the good work, I love this site!
Best place i know of to look at results is sc labs in california. They publish everything on their site. If you want baselines for any extract check it out.
I must confess that the purest oil I have made at home is in the sublimator, but I have found that by itself it is not as pleasant to vape as the iso/water wash treatment I do. The clear yellow thc oil is best when added back into the red hash oil that I make. When blended with the red, the perceived potency is much higher than vaped on its own, but beyond that there is someing intangible for me vaping the clear versus the red oil blend. I am diagnosed with severe chronic PTSD. I have been trained through therapy to identify when my limbic system activates signalling an onset of PTSD symptoms. This means that my blood becomes flooded with the same things that everyone else blood gets flooded with when they are scared. Adrenalin and all the other things a body needs to engage in either fighting or running from the danger. I have a cabinet full of pharmacuticals that address aspects of this but they do not do all that well compared to thc oil I make. Without any doubt, vaping the clear does produce a high but it simply does not difuse PTSD symptoms like a blended oil does for me. Producing pure is pretty simple. Turn a glass funnel upside down over a small bowl of extract. Put a test tube on top upside down on the funnel down spout to cover. Then simmer the extract on low heat. The first thing the funnel catches is nasty nasty nasty, clear pinene. Yuck. I wipe and throw away. Then the mixture will begin smelling sweet, and begin collecting on the funnel. I blow a fan over the top. Wih patience anyone can capture clear this way. I bought an iPad app that makes videos out of photos and stuff and made this one creating clear red oil. My next vid will be showing the blending of clear back into the red. If you watch the video and pause it you can see the kind of temperatures I use to produce the red. When that thermometer slips past about 300 or so F and the mix settles down and starts climbing to 360, the red is done cooking. There are normally three temperature plataeus during the cook. Compared to clear the red is hands down a better med, but blended with clear? boy howdy is it potent stuff. Not a lab test per se but I use a great deal of extract, normally an ounce or so a month between use and the botched experiments lolz but after several years I can identify potency pretty close. https://vimeo.com/171020414
While this is reasonable, more effective and efficient is chromatography. Even in it's most basic form, chromatography allows one to separate the waxes and non-polar (perhaps better to say, least polar) compounds from the cannabinoids, and the cannabinoids from the black junk. In more advanced forms, chromatography allows one to separate each compound without heat, which causes chemical reactions and degradation of product. If you wish to know more, please contact me.
I'd like to know more about the no-heat alternatives if you have some information you can share. Thanks!
Hi Mark, Please send me an email/pm through Facebook or LinkedIn - I'm the only Troy Wahl in Oregon City, Oregon.
I also would find interesting and helpful any information that you wish to share.
Steven, To be clear as a PhD chemist with 10 years of industrial pharmaceutical experience, I consult for a living and do not share much for free. If you are still interested find me on LinkedIn or Facebook.
I have a secret and I'm not telling.
Is there anything regarding azeotropic distillation that you can share, Dr. Wahl?
Sure: an azeotrope is a where two or more compounds distill in a fixed ratio, commonly at a temperature less than the boiling point of the individual compounds, and thus behave as a single compound - distilling an azeotropic mixture will not separate the compounds. The ratio of compounds depends on pressure. A binary azeotrope maybe, in addition to changing pressure, be broken by adding a third compound, an entrainer, that forms an azeotrope with one of the other compounds so the the new azeotrope has a lower boiling point than the original azeotrope. For example: Water and isopropanol form an azeotrope at 1 atm. with a boiling point (bp) of 80.1C, and a mass ratio of 12.0 % water: 88.0% isopropanol. Water and benzene form an azeotrope at 1 atm., bp: 69.25C, mass ratio 8.95% water: 91.05% benzene. Isopropanol and benzene form an azeotrope at 1 atm., bp: 71.74 C, and a mass ratio of 33.7% isopropanol: 66.4% benzene. Thus benzene can be added to rubbing alcohol (the isopropanol-water azeotropic mixture) to separate water from isopropanol. Is there something else you wish to know?
I am a patient and suffer severe respiratory distress from standard dispensary extract. Do you believe there is a safe way to render the extract safer for me to use (so I do not hack and choke) by removing at least some, or possibly all, of the irritants from standard lab tested extracts by using the extract as an entrainer in an azeotropic distillation of that binary azeotrope thingy you mentioned? It occurs to me this may be possible?
Hi Dennis, Unfortunately for you, no (at least not with water and isopropanol). For two compounds to form an azeotrope they must have equal vapor pressures at a given temperature and pressure. Cannabinoids have almost zero vapor pressure between 20 C and 100 C at 1 atm. There might be azeotropes between water or isopropanol and some of the other compounds in cannabis oil, such as one of the lighter terpenes, but that would only allow you to remove that one compound. What you need is a different technique to isolate individual compounds. I would also suggest edibles. Unless you have no other way of taking the cannabis, why subject your lungs to any type of irritation?
Your response comfirms for me many things I believe to be true about big pharmacutical types. Thank you. Of all the binary azeotropes listed on Wikipedia why did your response focus on the obscure notion that "rubbing alcohol" was the basis of my question Doctor Troy Wahl? Thank you for your time. It is rare that somebody as smart as Alex Trebek, or any other game show host for that matter, would take the time to help educated an old Marine with service commected PTSD and a litany of ambulatory problems. Especially a doc from big pharmacutical. I can find no appropriate words to share with you that you took the time to respond the way you did. I hope your career path finds for you the place in our community you deserve Dr. Troy Wahl. I know I will remember this! Just remember to phrase all answers in the form of a question for Final Jeopardy lolz - it will keep everyone guessing! Be well citizen
https://patentimages.storage.googleapis.com/pdfs/US2938028.pdf
Speaking of vape pens and short path distillation, doesn't decarboxylation give the oil a roasted almost nutty flavor, and if so, is it good to sacrifice flavor for color? What is the process for decarbing that won't have the oil going nuts, or is the nutty flavor here to stay? Can that taste be processed out of the oil? What's the word? Big THANKS.
The nutty flavor you are referring to is the result of side reactions. To minimize this, it is best to separate the acids from the rest of the cannabinoids before heating the acids to decarboxylate them. If you wish to know more, please contact me.
I've gotten to a completely flavorless state from distillation.
The distillate's I've tasted have not had the characteristic taste of decarboxylated oil. I've even achieved completely flavorless state from distillation.
It took an impacted left lower molar on me and a weekend wait with just extract for pain to fully understand why I personally need to completely decarboxylate my extract. The nutty flavor is just a side benefit really. When I had raw nerves yanking my brain around from the impacted molar I would seek relief by trying to vape. God explains things to me through my nervous system. When I vaped "uncooked" extract, I discovered it triggered intense pain the instant the vapor came into contact with the painful tooth. Don't worry. I survived the tooth, but without any doubt I know that fully cooked extract did not trigger that tooth pain on contact. I surmised that my extract therefor was not becoming fully bioavailable to my body, on both a belief that it was the acid form of thc that was triggering the pain in the raw nerves of my tooth on contact, and experience in dosing in which the same medicinal relief I get from extract is greatly intensified if I "pre-cook" the extract until it stops bubbling in a small dish. About 10 mins or a bit more. The high is intensified orders of magnitude when the extract is made fully bio available. Thre is no way the extract is allowed sufficient time in a vaporizer to decarb the acid for of thc fully. It takes several minutes. The belief that the thc degrades substantially during full decarbing is understandable, but false. There is no evidence I have seen of any informational worth that confirms thc is capable of degrading spontaneously in just the presence of heat after it has degraded from the acid form (decarboxylation) into the form that makes me high (destressylation). There is much dogma surrounding marijuanna and the products thusly derived. There are a lot of folks in Oregon now sniffing around trying to catch scent of where the end of the rainbow is ($$$) I think lolz. I suppose everyone needs to pay their bills. I suggest using the product fully decarboxylated, which will turn browner (browner is a word if you are stoned so shut up!), and will inherit a delightful nutty flavor as it is heated. It bubbles like fizzy cola then stops bubbling completely and has a delighful sweet smell that makes my mouth water a bit. Yum. I use a 60 watt onfared heat lamp sold at Petco to do this because it is flat when pointed up and my small stainless steel pot sits nicely on it. About 10-20 min until bubbles cease completely works wnders on the stuff. Petco has best stuff for sophisticated extract users. Reptile section. Humans really do not do all that well with most uncooked things I have learned. Cooking the extract does not destroy thc in extract in a spontaneous fashion or I am a damn fool. hmmmm..... ;)