I need help!! It is a frost free freezer. If they are growing slowly this is the ideal saturation level. Do you honestly believe the extracts you obtain do not have dust, eyelashes, bug parts, and every other thing that floats around in our atmosphere? Is it safe to smoke? if not add small amount of pentane ( a few mls) untill you see a close to white color in the thca layer dont add too much ! You can continue to grow larger diamonds utilizing super-saturated hexane and to improve the clarity of your diamonds using chilled pentane washes. illustrated walkthrough of doing a hexane wash (Cannabis) Without additional processing, it produces a more full-spectrum product called a high-terpene full-spectrum extract (HTFSE). Close the vessel and very slowly increase the temperature to 25-35. What is left, is "Absolute" Onion extract. Is it possible to reverse the auto buddering process? Then the idea behind DCVC is that a continuos solvent gradient is fed through the system starting with an extremely polar solvent. This will remove approximately one-third of the remaining solvent. I can think of a lot of things I would like to have extract from. June 29, 2022. There is a very small amount of salt left in the extract, because when I chew it the salt is detectable. Can I put it in a jar of Eveclear in the sun for 2-3 hours, then rubberband 2-3 coffee filters on the jar and filter out the green Everclear? At 250F, there won't be alcohol or water left. PDF SAFETY DATA SHEET - Airgas Silica would likely work great but comes with a few problems regarding toxicity when inhaled, plus very tiny percentage will disolve in isopropyl alcohol and end up in our sample. I am absolutely certain, from personal experience that these two things are true. This one ended up a little over 100g, took maybe 10 cycles ? Thank you for sharing such wonderful information. If the sample crosses state lines, it ostensibly falls under the aegis of the Feds. The report states that at oral doses of 5 - 10 ml (extract is almost precisely 1 gram per ml) that some children begin to display nausea and other icky feelings. I have done a LOT of seperatory funnel work, centrifuge work, filtering, cooking, distillation, and have even oxidized away Volitile components of extract with Hydrogen Peroxide by carefully creating an emulsion of extract at elevated temp with (drop by drop) 35% food grade hydrogen peroxide. ISO wash done at room temperature, overnight. As far as the other components the answer is that I have found it to be unrepeatable as to the results. For further discussion of that subject, please see: /chlorophyll-pickup-in-extractions/. Fire Hazard When I helped a friend yesterday to clean up RSO into THC oil (REALLY messy lolz), we started with a hexane/water wash. At first there was no visible seperation visible which should not be possible, right? Also, when mixing multiple solvents into extract it can be a pain in the rump to purge them out, and forget about recovering the solvents lolz. 2) I would transfer what you desribe to an oven safe piece of glass or stainless steel and turn the oven to 275 F. Place the goop into the oven with lid off. After giving it some more thought, we settled on halting precessing more bud until we can comfortably do more than one quick wash. Vapor respirator. My lab thermometer goes down to -10 C and it is colder than that. While the black color was gone, slight ashtray undertones could still be tasted, so further refining was necessary with activated charcoal, but we will cover that as a separate subject. Eventually the oil wil seperate from the alcohol in the seperatory funnel as fresh water is added. This low and slow method will encourage more nucleation due to increased temperature and pressure and larger crystal growth. However, methanol and ethanol being chemically almost identical, shouldn't differ at all as solvent, do you agree? Close the vessel and very slowly increase the temperature to 25-35oC over the course of 5-30 days. God damn! . When left outside for 20min (45-50F) the solution solidified. By observing closely it starts get a bit easier to see when an amount of H2O needs to be adjusted, or the temp needs to be changed, or the solvent strategy needs to be adjusted overall. btw 98% is completely false. Sigh. You can remove the C-30 size molecules like the color pigments, using column chromatography, or short path distillation, but I will leave that up to Pharmer Joe, who took his organic chemistry classes this century and is our brain trust on those subjects. Two Dawns here Bro, I have a project that you need to be involved in ! Experience has proven to me that this is the moment to stop heating it and put turn it up for the drip to form. Good luck. Very interested in being able to remove as much amber color as possible. So time, temp, state of decarboxylation(therefor boiling point and acidity), residual solvents from extraction, and a littany of other "little" things can and will have a big impact on results. Hey Skunkpharm, this post, while interesting, is contradictory and confusing: first you say: "After it has separated, bleed off the water and emulsion layer), and then: "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" Which is it, and why? We must have repeated this at least 10 times. Before delving into how to make that process work, may I ask why you've chosen to extract with warm methanol. Was looking for more info on dissolving an recrystallizing in pentane. 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. I can even take the extract so cleaned up and when placed on a cool glass surface can seperate the components easily with a flame above the goop and a tilt to the surface. We haven't figured that one yet. I have a fireplace at home, but normally do this on my stove top and I agree with Skunkpharm that a burn danger does exist. Have a great New Year! Drained again. Powered by Discourse, best viewed with JavaScript enabled, https://future4200.com/search?q=CBD+pentane. CHILDREN IN INDIA ARE GOING WITHOUT!!! Specific gravity (water = 1): 0.66 at 20 degrees C (68 degrees F) 4. You can purchase these on Amazon. How do I know? How long/how many washes did it take to achieve this size rock? Creating unique mixes from THCA is precise chemistry that will spawn thousands of future products. Trade secrets and forbidden solvents in today's cannabis extracts The hexane/oil remained dark, but though we must have done it right already We purged - the oil was still black. We are thrilled that our documentary American Pot Story: Oaksterdam continues to get favorable reviews. Clarified neem oil is food stuff - lipids and fats. Creating THCa Crystalline | Cannabis Tech GW Extremely potent this way, likely owing to the possibility of DEEP lung inhalations without coughing. It will pop under vacuum when those water pocket burst under the oil so a cover is necessary on the dish. They list n-Hexane as a class two solvent with 290 ppm concentration limits, and a total PDE of 290 mg/day. We used around 8 liters of water and 3 liters of methanol. Even at the hobby level for me it gets spendy to just evap it all. I take the glass which is cool to the touch and dab my goop (wax or shatter or scrapings) onto the glass which is held horizontal. How long should i wait before the ethanol is gone, always seems to have a slight smell to it. Step Two: I load my raw extract into a ceramic cigarette. I just did my first ever wash in a buchner funnel with pentane. The relatively pure iso evaporates off much much quicker after the rubbing alcohol has been "salted down". It appears however that azadirachtin by itself is hydrobolic and miscible in water. Just asking as I have not much access to hexane or usable light naphtha, all I have access to are generally acetone, isopropyl alcohol, ethanol alcohol, and water/salt water. The alcohol will disolve into the hydrophobic components of the extract and neem oil present and give the water (which forms an azeotrope with the alcohol) a way to be presented to the hydrobolic component like azadirachtin and alpha pinene. My starting material is BHO which has been CRCd and dewaxed inline. Provide exhaust ventilation or To try and make that layer easier to see and remove I have tried heating up the salt water, and cooling it down. - Do we really need salt in the water? ISO readily dissolves and holds chlorophyll as a solute, as well as the anthro cyanin color pigments, water, and water solubles. What temp to let sit out at? 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. The THCA content of these crystals can be as high as 99 percent but can fluctuate depending on residual solvent and terpene content. GW, Hi Then to pull the methanol out, chemists put the mixture back in the rotary evaporator again. I see stuff on Google in this thread but I can't find it. The section for Gerbils and Hamsters has syring type eyedroppers for feeding medicine and test tube size tubes with rubber stoppers and a hole in them for watering the rodents. You've picked yourself a challenge brother! I then capped the vial, placed it on a digital hotplate, and have been alternating between 95F and room temperature for the past day or so, all while capped. 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). Vapors are heavier than air. It came up in the only the strong thread, but lookin for a little more info. add pentane (-20 -50c seems to work best) too cold and you wont dissolve undesireables too hot you will dissolve too much thca .too much pentane will dissolve too much thca as well , too little wont dissolve enough Plus, putting your jewelry away safely while you bake, apply cosmetics, or garden helps keep debris from building up in and around the setting. How To Make THC-A Crystalline, The Most Potent Hash On Earth - Herb I even asked nice. Diamonds have unique colorations and clarity that are derived from terpenes and the purity of the crystalline structure. After this time, remove the vessel from the cold environment, open the vent valve, and allow the solution to reach room temperature. But how are these diamonds made? Flash point 57F. 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. ;). Floor dust,doggie hairs, and (yuuuuck) I walk barefoot on my floorsand did not get the cooties, just a little athletes mouth. Vapor density: 2.97 5. This separates the iso from the water and immediately concentrates the iso above the water. GW explained that activated carbon can clean up extract and he is right, however i have used it extensively in tests and irregardless of how I extract with it the activated carbon will indeed absorb cannabinoids along with the other material. In minutes it hardens into tiny air pocket ridden pieces. When I clean up 80%-90% lab tested extract (mostly wax removal) with IPA I am left with extremely pure and pristine THC, which leaves nearly zero residue in my vaperizor. Test tubes would work but I got mine at Petco down the street. Anthony DeMeo is Co-Chair of the Extraction & Manufacturing Department at Oaksterdam University. Any ideas? I placed ~2-3 grams of extract in a 20mL GC vial. https://vimeo.com/181396690. Perform your extraction as normal but maintain a ratio of solvent to biomass between 6:1 and 10:1. Ingestion. Invalid username/email. GW. ! What were your perameters for that thing?! Very interesting. ( depending on your material and type of alcohol you use). 100% no moisture. In the video I am processing extract into a more refined product which I vape happily, and the video starts as the centrifuge of the isopropyl alcohol and extract mix are finish slinning the waxes out. Filter is "slow" rated for fine crystals. Let the mix settle for a few minutes then stir in non-iodized salt so it is a layer about a 1/4 thick or so on the bottom of the vessel (small tube or jar). thank's for the information. Your time is always much appreciated, Skunk Pharm. Yeah once they get that big it becomes difficult to get enough thca to continue to grow them even bigger. Cleaning and Disinfecting Surgical Instruments | STERIS #8run dissolved liquid into coffee filter back into a clean jar this is to prevent unwanted seeds from starting, #9(room temp) I have tested a multitude of solvent/lab techniques to accomplish what you are attempting. Note that my system is based on iso/water because it is simple, effective and extremely inexpensive compared to other systems but without a doubt other systems of solvent used as a gradient thusly would likely be more efficient. That hasn't been my experience where over saturation had helped to precipitate out of the fats, definitely hard to find that balance and I'm not sure the advantage would be worth it, It only matters if your going to put into your crack pipe.. So I am working on extracting some lovely compounds from plant matter only problem is I left it in alcohol for several days longer than expected. 3.25% by volume is also enough water to bring along some water solubles like chlorophyll and leave an otherwise pristine extraction with a green tint, usually light and sometimes a gorgeous electric hue. Secondly, this polishing article on ashtray reclaim was simply to make a point, not suggest a source of dabbing concentrates. > redturtle984 commented: "It is not correct to say that using hexane is not > highly effective at recovering thc from any form of extract. Put the filled dish and crystallization vessels into a vacuum oven using a drying temperature between 18-30oC. The flame gets intense. What am I doing wrong, can someone please help! I already posted a very simple way to do this, however I am a stoner. What is the difference between hexanes and petroleum ether Reactivity Alerts Highly Flammable Air & Water Reactions Highly flammable. Gently wash all affected skin areas thoroughly with soap and water. I will post pics of my crystals when they are bigger. 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. C over the course of 5-30 days. This article was written by Michael Sassano and Anthony DeMeo of Somai Pharmaceuticals. I don't think it matters as far as protocol, you'll just need more heat and time to remove the heptane once you're done with the wash. People use butane/propane because of its low boiling point, not because it's safer. Repeat and wash the crystals as many times as needed. I get acetone from Amazon labelled as "Pure Acetone Nail Polish Remover" by the quart. Sweet amber dreams. I am not suggesting this process for reclaiming ashtrays, but simply to make a point." I handle the oil using a medicine feeder for rodents I got at Petco. everyone recrystallizes their CBD. Already among organometallic compounds there are examples in which obtaining crystals at all is an enormous struggle and having single crystal quality is simply a matter of hope. The only thing I have extracted by intense boiling in water is some pinene which is partially miscible in water (no idea about salt water here). The water layer will be milk to chalk white. Orders of magnitude more potent than ground up herb in the unit which the unit is really meant for. Sorry, we don't have an account for that email. 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. Because I didn't want to mess up a separatory funnel with the black foul smelling mess, I poured the solution in a 1 gallon Ziploc bag, to which I added equal amounts of water and hexane. Saw @Future4200 did a pentane reX on his ig a while back was trying to find some more guidelines before I try it. Purged the pentane/hexane, the oil hasn't changed its color, it was still black. 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. Step Three: My trusty lighter is held just off the end of the cigarette and both are held over a smooth cool glass surface. C. A vacuum of -15 to -20 mmHg should be used to assist the purging process. #5 if top liquid pentane layer is too dark and crystals on the bottom are not close to pure white let the thca settle, slowly pour off/siphon off top layer, try to stop if you see some thc-a grains coming with it.Now If liquid layer is light in color with a water like viscosity proceed to buchner funnel filtration. I wish to retain the antibacterial properties of the extract as well as wish to obtain a powdery product. Salting down is a method of fractionalization for this solution. And then repeat steps 1-7? Pentane is about .004% water soluble and Hexane is about .001%, so not a lot goes out with the water wash. https://erowid.org/archive/rhodium/pdf/solvent.miscibility.pdf Dissolving Acidic Cannabinoids for a THCA Tincture by Cat Scientific, FDA Rating and limits on various solvents, Washington State Emergency Rule on Flammable and CO2 Extraction, http://www.nlm.nih.gov/medlineplus/ency/article/002893.htm, (/flacktek-speedmixer-grinding--milling/) Comments. Will this work? Pentane and Heptane are Class III solvents with FDA residual solvent limits of 5000 ppm: Hexane on the other hand is a Class II solvent with limits of 2.9 mg/day and 290 ppm residual. I've been fighting with this process and I'm trying to figure out exactly what I'm doing wrong or still need to do. dissolve it in rubbing alcohol completely. I have really messed up extracts through a variety of experiments and this method cleans them up to pristine. #4 feed hc into jar slow agitation swoosh liquid around in jar you will see it start to pull the unwanted parts of the thc-a out. the first trip through the flame it is quite a light show. Part two. Same concept applies to pentane vs heptane. Its made specifically for extractions and concentrates. 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. They contain both the undesirables, and the alcohol as well, with the cannabinoids left with the hexane. Isolating cannabinoids to their purest form, such as THCA diamonds, and recombining them with terpenes is the first step in creating treatments that target specific symptoms. Put back into freezer for a couple of hours and repeat 2 more times so you have a good clean product. 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. We let it settlte and drained, it looked as if it was going as planned, the water was colored (but no percipitation). It works without question and the only product loss will be the polar compounds which will not pass the alumina column. Four month old trim will be significantly darker than fresh trim. Smell testing is important. I have used salt in my trials but only to get pure isopropyl from rubbing alcohol. I cannot know if this would work for you because every parameter often gets adjusted "on the fly" as I do my own. If you have a dewaxing column, you can utilize this to assist in further removing undesirables. Let it sit still for a few day, and the two fluids separate. I have tried this saline/hexane wash before on some oil few years ago. The end product can be incredibly flavorful and potent, and many dabbers who prefer live resin also prefer the crystallization of "terp sauce." . Rock on Oregon. Doing so will evaporate most of the butane. What the meaning of "treated with ether and water after cooling"? A rice grain size vaped into my Vapir 1 bag fills the bag twice with a dense foggy cool sweet orgasmic vapor. Looks like a 1000 ml Sep they are using in the photo. I've looked into carbon filtration a lot, but this is the first time someone gave an actual number as to what is lost. The resulting RSO concentrate is a dark harsh wax/tar (50% THC). D. Gold. Then, reduce the pressure in your system to -30 mmHg, or as low as you can go based on elevation, using your vacuum pump. Excellent post, we'll definately look into this in the future, sounds quite interesting. We typically freeze everything and do a subzero quick wash to avoid as much of them as possible, but soaking overnight at ambient, is pretty much guaranteed to extract them all. I have been tasked with helping a producer in Oregon who extracted with isopropyl alcohol to clean his stuff up as well as several various batches over time from others who extract with SCF extraction methods. Here is one techique that can remove any impurities soluable in water - specifically alpha pinene. The third time it was even lighter, but the hexane/oil was still dark. At this point, after draining, we added 300ml of saline water and 300ml of methanol. How to obtain clear terps? Pentane wash? Vacuum Distalation? What I just typed is how I would attempt it. might be a little off but it will at least give you some starting points . Hello Mr Gold, Thank you for your book, it must have been hard work publishing a book of this nature back then. I better gothe Vapir is getting cold. It always tends to leave traces and crystals in the extract The issues I am having is that I do not get a distinct phase separation between the water, emulsion and hexane layers. Make sure the vessel condenser is cooled to -20 C. During this time, the THCa naturally crystallizes at the bottom of the container. 5) Spin the tubes at 4000 rpm for 20-30 minutes. Hexane and water do not mix. This means my ability to be patient and wait only exist when I am stoned.lolz. 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. Alas, UV radiation also destroys cannabinoids, but fortunately at a much slower rate, and three or four hours in the sun is usually enough. Hey skunkpharm! The good news is that ethanol is not insalubrious below 5000 ppm, according to the FDA pharmaceutical standards. GW. It has a burnt taste not normally present when vaped above 365F but is sweet below that. GW. feel free to add any advice fam. I do not recall any experiments with salt water and acetone. TWA: 500 (ppm) from OSHA (PEL) [United States] Inhalation. These unique characteristics show the quality of the crystals; the more yellow/gold color means more terpenes are present, and fogginess or lack of clarity in the crystals means there is solvent present. Pentane recrystallization - Extraction - Future4200 Hands down DCVC produces purified and seperated results and generally is useful for the ounce size quantities I process and likely much larger quantities.. I saturated the oil in ethanol, ran it through a vacuum assisted filter using a watman 1 filter, pulled out a ton of gunk, then dumped hexane and saturated salt water into the seperatory funnel as instructed, poured out the water and ethanol mixture, using the funnel, saving the hexane and terpine mixture that was the dark color on top, just like the picutres, and I have been running salt water though allllll day and the color isn't getting any lighter. They worked well for our purpose, and we cleaned them when they clogged, by alternating a hot aqueous NaOH solution and a HNO3 solution, to break organic bonds. This method is as safe as any method and I personally consume 100% of all extracts I process. I have done this many times. Following this I dissolve the winterized oil in n-hexane (Ratio 20 g ISO to 100 ml hexane). It would be a huge help to my career, thanks! Absolutely. I am not suggesting this process for reclaiming ashtrays, but simply to make a point. I would suggest chilling both the material and the alcohol to below -18C/0F and doing multiple quick washes, keeping them separate, or switching to a non polar solvent at the same temperatures. WARNING: THE LC50 VALUES HEREUNDER ARE ESTIMATED ON THE BASIS OF A 4-HOUR EXPOSURE. Each time you pour off the terpene layer and leave the crystals behind, the potency increases. The layer that is amber and clear is the good stuff. Dissolve the entire batch in just enough rubbing alcohol to make it dissolve. Instead, we'll wash our current solution with hexane and water, removing chlorophyll and whatever else goes out with it. What would your recommendation for maximizing the yield be, without doing a warm extraction? I know I need to, or can use a cold hexane or pentane to wash them through a Buchner. I think I am on the right track, but just wanted to get some feedback from the community. I'm wondering if it will be possible to remove pam cooking spray from a run of bho. 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.
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