I ensured the solution was supersaturated by adding small amounts of BHO into solution, until no more would dissolve at room temp. One thing I notice is it takes quite a long time for bubbling to become visible. This is VASTLY more than our senses will detect, and is also VASTLY more than most bodies will ingest before violently regurgitating. Because it is a simple Alkane and relatively non toxic, hexane is used extensively in food extraction, but should not be viewed as being as salubrious as mother's milk. Was looking for more info on dissolving an recrystallizing in pentane. Cite. It has all dropped down to the glass. 2) THC does not significantly break down with the application of extreme heat so long as oxygen to oxidize the THC is present. slowly evaporate pentane untill desired saturation level is obtained you can check this by throwing a few test seeds in the pentane if they dissolve too fast you need to evaporate more if they dissolve slowly or remain their same size you are close. dissolve it in rubbing alcohol completely. What is not known is how effectively the separation of the extract components are when the extract is disolved in rubbing alcohol prior to salting it. More on hexane purging in the subsequent process description for serious scrubbing: To put this process into perspective, I once collected all of my pipe bowl scrapings and roaches until I had about a pint of them, and dumped that into the container of black denatured alcohol, that I had been cleaning my pipes in. What is left of the plate is black, and runny at room temp. I shook the mixture well and let it soak for a day to extract the material from the roaches and scrapings, before straining it through a wire strainer and then a coffee filter. It had 1/2 dram of LorAnn raspberry flavoring in it (PG, color, flavoring). Diamonds have unique colorations and clarity that are derived from terpenes and the purity of the crystalline structure. Winterizing ISO, Methanol, and Denatured alcohol extractions: Even though Ethanol is polar itself, it can still be used to remove some of the undesirables they pick up, because it is not as aggressive a solvent as Isopropyl and Methanol. If anyone has any knowledge of how this problem can be fixed, it would be greatly appreciated. You could short path vacuum distill the extract. Im assuming 7-10. I rarely use flower because I do not extract, but this reply is in hopes of helping you out. Finally, if you really want to see the separation, obtain a glass tube. No matter the strain it always seems to taste fruity and pleasant. Now the crystals are left to dissolve in pentane, which extracts more parts per million of non-THC material. Once the desired diamond size is achieved, pour off the remaining layer thats comprised primarily of terpenes. Be sure to use an approved/certified respirator or equivalent. Once youve achieved your desired crystal growth, purge the residual solvents from the terpene layer and crystals using a large glass (e.g., Pyrex) dish that allows you to create a thin layer of terpenes, maximizing the surface area. That long process results in 99.96% THC. Generally the whole process is about 15 minutes or less. We buy the salt cheap by the bag, using salt intended for water softener use. Are you using 70% ISO, thus taking advantage of the containment of water to dissolve the salt? I'm looking for an older link you posted to terps you bought off line. Did you actually read the article, or just look at the purdy pictures? I like iso because it falls in just the right niche polarity wise to target the medicine. ! Method #1, pour your fluid into a glass, Pyrex pie plate, place a small fan in front to blow over the top. Bigger chunks bake at 275F instead of 300F to avoid burning. Sorry, we don't have an account for that email. Diamond Hazard Value Description; 4 1 0 Health 1: Can cause significant irritation. Adding salt is not productive at all because it iterferes with the water in a way that prevents the water from pulling pinene out of the goop. I don't have access to butane, I am pretty much a double-boiler type QWET setup (NuWave w/candy thermometer for the cooking oil, stainless steel 2 cup UKonserve container for the mash/oil). In minutes it hardens into tiny air pocket ridden pieces. It is a sort of thin film chromatography separation and works surprisingly well for seperating the components of an extract. I have some Everclear. We perform the salt water wash of the hexane mixture, by simply pouring the salt water and hexane into the separatory funnel together in about equal parts and shaking well and burping, before allowing the mixture to separate out into layers. #6 filtering: pour slurry into buchner funnel after filter is ready and set. Here is a very short version of what I do to make my Pristine Oregon Pharmers World Class extract into a product that is vaguely fruity, makes DENSE foggy vapor, has zero, nil, no, and absolutely zed respiratory irritation even when held in a long time. 1) that a vaporizer, no matter the style, does not convert THC-A to the THC-YUMMY form that the body can use to speak with the animals and, QUICK READ: How can one obtain a shatter consistency with an ethanol wash/winterize, if not what is the best way to evaporate Ethanol? Based on this, my "go to" method of removing the irritant azadirachtin would be to attempt to disolve it in water. The manufacturer also provides classes on how to use it accurately for about $400. With all of the listed items above done as a hobby one thing is very clear - the results are highly variable. Set aside and come back in 1/2 hour. Eventually the oil wil seperate from the alcohol in the seperatory funnel as fresh water is added. I do not take lightly the handling of chemicals, but I will not either toss away opportunity to improve my existence because of fear. nobody recrystallizes their THC. If they are growing slowly this is the ideal saturation level. It works for cleaning extract up. With each solvent gradient the column progressively elutes the less polar compounds. Looks like a 1000 ml Sep they are using in the photo. It would be a huge help to my career, thanks! As the saying goes, the poison is in the dosage, so leave us please keep N-Hexane's potential nature in perspective, which includes never losing sight of it. I did mine with left over jar wash and trim runs that people had laying around, My first attempt yeilded bigger diamonds then the hot jar tek. During this time, the THCa naturally crystallizes at the bottom of the container. Trying to turn small diamonds into bigger ones. I only have one video which only shows one step and how effective the process works just as a pure filtration method rather than seperation. Ethanol however, is a very different story, being as I am in the UK and Everclear is not on sale here (nor do we have a limey equivalent). Next Post: Faculty Feature: Stefanie Gangano, Ph.D. How to Get the Most Flower Weight from Your Cannabis Grow. It will remove nearly all the odor and "terpene" rush you get too, but the medicine that I am after is THC and that is joyfully intact and as decarboxylated as it can get without further time and heat. We are working with oil extracted through warm methanol extraction. ********* Hello! Step Three: My trusty lighter is held just off the end of the cigarette and both are held over a smooth cool glass surface. Is it possible to reverse the auto buddering process? > redturtle984 commented: "It is not correct to say that using hexane is not > highly effective at recovering thc from any form of extract. The real question, putting aside your personal attack, is this; "What data do you have that suggests the dust or debris that might collect in your extract is harmful to human health vs. an advantage to human health? Wash with a cold alkane e.g pentane, hexane, heptane, or spin in a centrifuge. It also takes longer to work the emulsion layer with subsequent washes, and each wash leaves with some, so at some point need to make the call. It turns out that I don't mind or notice a bit. After carefully bleeding off the bottom layer of water, we continue to replace it and repeat the wash process of both the emulsion layer and the hexane solution, until the emulsion layer disappears and the hexane has bell clear clarity. The salt, if any, left in the extract is not detectable. Even then, pulling the product through will take horsepower because there will be so much unwanted material it will tend to plug up. Same concept applies to pentane vs heptane. Fire Hazard I just did my first ever wash in a buchner funnel with pentane. look in the CBD threads instead. But it's dark ! The far more hazardous thing (verifiable with medical data) to do from a healhwise perspective is to kiss another human or share a joint or pipe. Even at the hobby level for me it gets spendy to just evap it all. Lost your password? I was only given crude to do R&D with so every time I would get some id isolate the thca and add it to it, Nice! If you even leave a small amount uncovered in a closed room for a night it will collect dust. It has extremely low volitility. Use a fan to evaporate off the alcohol (about 15 minutes) then place the almost dry extract on some cooking paper. Put the filled dish and crystallization vessels into a vacuum oven using a drying temperature between 18-30. The light yellow fluid evaporated down, and then I purged. Isopropyl alcohol always has water in it so that was involved. But, vaping the extract baked liked this turned me on to the fact I wasn't inhaling fully converted THC. The MSDS sheets regarding the inhaling of terpenes says do not do it, yet people do it all the time and many believe it benefits them. Patient thinking is key. Its made specifically for extractions and concentrates. Creating unique mixes from THCA is precise chemistry that will spawn thousands of future products. See what happens. Step Two: I load my raw extract into a ceramic cigarette. Close the vessel and very slowly increase the temperature to 25-35. All I used was a 1 micron paper filter, DE and pentane. We let it settlte and drained, it looked as if it was going as planned, the water was colored (but no percipitation). (/d-gold-author-of-cannabis-alchemy-1971-shares-cannabis-extraction-history-unfolding/) Comments. Poof - extremely concentrated THC that vapes with zero irritation in the lungs and no hacking choking and so forth and..it is the most potent form I have used. Inhalation. The first relates to the adage that you can't make chicken salad out of chicken manure, so the best you can hope for is to make the best out of whatcha got. There are about a hundred variables that might present themselves with your extraction, but the general prodedure above has been employed by myself for a long time. They contain both the undesirables, and the alcohol as well, with the cannabinoids left with the hexane. I have used salt in my trials but only to get pure isopropyl from rubbing alcohol. I just scanned through the site and it doesnt look like Joe ever published his chromatography results, so Ill publish something using a picture of his samples, to explain the issues with color and other non-targeted elements. 100% no moisture. This low and slow method will encourage more nucleation due to increased temperature and pressure and larger crystal growth. Insoluble in water. Excellent post, we'll definately look into this in the future, sounds quite interesting. Repeating the last two paragraphs of the article for your benefit: This will remove approximately one-third of the remaining solvent. You can make nearly pure iso propyl alcohol for pennies by salting down rubbing alcohol. You can see a color gradient between the water and the hexane layer but it is impossible to tell where one starts and one ends. This new vid I made this morning boils the extract and also makes the water a bit murky. This time, a lot of stuff percipitated. BE CAREFUL I put the small jar with iso washed extract in a small jar and put that jar in front of a small fan so the surface just ripples. Note also that oxygen in a breathing atmosphere greater than 75% pure will kill us dead! 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For thin film evaporation, we place about .200 inch of it in a six inch Petri dish, which we place in a vacuum chamber and evacuate down to 29.5 mm Hg and ~80F for 30 minutes. Once dissolved, I place the mixture in a 0 degree freezer for 48 - 72 hours. When you add salt to the mix it is very tough to know how that impacts things. GW. We start out by making four or five liters of saturated salt water in a glass (or ceramic) container, by mixing sodium chloride (table salt) in hot tap water with a hand mixer until no more will dissolve. I realized I need to stop putting the eventual "carrier" type materials right into the just-finished cannabis oil while it is still in the mash container - that will keep me from having to salvage anything in a polish maneuver. This is because every extraction can be different. I wish to retain the antibacterial properties of the extract as well as wish to obtain a powdery product. Extracting frozen with subzero alcohol is intended to avoid extracting those molecules, but as you note does reduce yield on the first wash. We address that with two extractions, one higher quality than the other. Add water again and repeat the wash step until you are satisfied with the clarity, before evaporating off the hexane, to yield the pristine oil. They melt right in and are very pleasant to the touch, though they are highly irritating to the eyeball so washing hands is a good idea after rubbing it in. Put back into freezer for a couple of hours and repeat 2 more times so you have a good clean product. it is 94.5% thca and I was trying to figure out how I may clean it further. Thank you! I'm always looking for you folks to clean up my ongoing (and seemingly neverending) RSO apprenticeship :-) The deviation from routine extraction begins here. Here is a short video of the finished product with no solvents being shown burned off. There wasn't really enough that precipitated out to smear onto paper to see. @mylkingtrees Ummm dude3, hes referring to the filtering funnel on top of the bottle @Guapo sir the pirce of labware that you are refferring to and that this man is faiiling to correctly inform on is called a "Buchner Funnel" It is usually used in conjunction with an "Erlenmyer Flask" with a vaccum port feature, a filter paper is placed in the filter funnel an a vaccum is applied to the port on the flask, when filtering flow slows down from a clogged filter, vaccum is turned on to assist in speeding up the process. You will be able to easily identify the water miscible (hydrobolic) components versus the oil that we seek. As the mix evaporates off there is typically a milky white seperation of two immiscible layers that develop. Since you are posting on a marijuanna site I assumed of course your concern was neem oil as an insecticide which contains the naturally occuring azadirachtin. We've observed that when evaporating 1 liter of methanol, hash oil starts forming in the last 50ml. In a ball jar, with a lid put in your Onion, then add 3x the amount of Ethanol. The saline exposes any proteins hydrophobic surfaces, making them insoluble in water, so that they precipitate out, and the saturated water has no room for anything but the alcohol, which aids that process. We would be happy enough If we found a way to test the potency of our extract. Rock on Oregon. Once the vessel is filled, tightly close and chill it to -75oC or colder for 48 hours. or not? The resulting black gunk can easily be purified/purged much further until it is deep red (normally). I can think of a lot of things I would like to have extract from. Any tips or suggestions would be great! As a matter of fact, prior to winterizing I intentionally add dust or sand of some sort to the disolved mix which increases wax removal orders of magnitude better that filtered extract/solvent. In my humble opinion, you are doing it absolutely right. I just cannot manage to get it to become a shatter consistency. But I've run a ton of washes through it and I'm still getting a gunk layer (only when cold) but the color of the hexane mixture isn't getting lighter or more yellow at all. The light yellow layer mentioned with acetone evaporated into pure thc judging by the slightly sweet chalky flavor and my commitment to solving Einsteins problem with gravity as a constant in any given inertial frame after vaping some. :). #10 add big seeds( at this time your saturation and purity levels should be ideal.) Are people also idiots who do that too? Shatter consistency is caused imo by impurities in the extract. Your "pasty mess", from your description is H2O still in your Onion. When you say acetone/water experience, is this including salt water? You can reduce the pickup of water, water solubles, and other polar elements, by soaking in a non polar solvent, but if you do so at ambient temperatures you will still pick up the non targeted C-30 elements, and is more prone to pick up the ~C-30 non polar plant waxes.