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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. WARNING: THE LC50 VALUES HEREUNDER ARE ESTIMATED ON THE BASIS OF A 4-HOUR EXPOSURE. Put the filled dish and crystallization vessels into a vacuum oven using a drying temperature between 18-30. The mind change is unmistakable. I put the dispensary extract in a couple of tea bags. Be careful, though, as too much solvent or solvent that is too warm will dissolve your THCA. Garden. My last batch was all small diamonds. May do it with an ounce or a pound, advice on both quanties would be great. Do you have an email graywolf? I noted above how it inhales. Leave the vacuum on to dry the crystals at the end. GW. and what if it is brown? Youre not a bad person for consuming cannabis, Dale says. 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. Then, reduce the pressure in your system to -30 mmHg, or as low as you can go based on elevation, using your vacuum pump. Ever try winterizing at -80C (or anything lower than 0?). I added several drops of pentane in order to get the remaining BHO crumbs to dissolve. Pleasant tasting frankly. My plan is to just keep doing this to see if they continue to grow. Whether the diamonds are smoked or added to flower, some people are gravitating to purer products across categories, and 99 percent THCA is grabbing attention. We tried a third time, it seems that no matter how we approach it, it looks like, the water only washes off the chlorophyll, but other dark colored stuff that methanol pulls initially stay in the hexane along with the goodies. I figured I can just add it to something and drink it (my body is not a big medibles fan, only what slid down as leftover in my mouth from sublingual use), but would love to be able to simply RSO it. The following is a typical MSDS Section 8: http://www.sciencelab.com/msds.php?msdsId=9927187, Section 8: Exposure Controls/Personal Protection. When you are cleaning up really gunky stuff it might be more practical to use 10% increments. Easy to visually identify each substance mostly by color this way. Could you please tell me what that bottle top filter contraption is? THCA is white when pure (or close to pure). It didn't dilute very easily (???). When performing your extraction, its important to chill your jacketed extraction system to -50, C or colder. 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. From your post I assume you are also after THC. It has a burnt taste not normally present when vaped above 365F but is sweet below that. Without testing you cannot know these answers. We did a quick wash and it still came out dark. I remove the liquid with a vac chamber but how do hou keep that sample from decarbing? The "splat" part that held to the cool glass and did not run down when tipped is almost opaque and looks grainy like wax in a honey jar at the top. The process is known generally as Dry Column Vacuum Chromatograph (DCVC) although the only references I find online relate to the method as used with silica gel as the stationary phase. There are solvent polarity charts online. Acetone is polar with a dielectric index of about 20.7 and is miscible in all proportions with water. Quick question oh wise one, it is difficult at times to purge the extract before heat and agitation render it waxy and sealed in. 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. . 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. I hope all this helps. Next month I plan to do a vid from start to finish and present the results in a video to show it. The water will drop through the iso layer and into the bottom layer at first, oulling polar compounds with it. Thank you so much! 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. This means it is designed to sublimate frozen water into water vapor, skipping the liquid phase. Repeated washes from then on got a huge amount of the green out and fats and so forth. Hi Thanks for the valuable knowledge. If the sample crosses state lines, it ostensibly falls under the aegis of the Feds. I would love to see photos! Ingestion. But, vaping the extract baked liked this turned me on to the fact I wasn't inhaling fully converted THC. I started with a bunch of old green oil that was made with older auto trim material so it picked up a ton of chlorophyll. mandurah news body found Login. On April 29, 2023, Melissa Reidof Cannabis Now talked extensively about the film in a review called Higher Ed.. If you have a dewaxing column, you can utilize this to assist in further removing undesirables. The reasons we use warm methanol are the following Have a great New Year! I evaporated and purged at high vacuum the yellow layer by itself and the dark hexane layer. Kleen xtract has been the wash to get it back into a "purgable" consistency. 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. The poison is in the dosage, so even for a salubrious ingredients like chlorophyll, some people can get too much of a good thing, producing digestive tract upsets, with attendant vomiting, cramps, and diarrhea. A couple of points, and as the first seems to be based on an ASSumption on your part, I will give you the benefit of the doubt and infer it is from ignorance, as opposed to malice. Did anybody realize the pictures show this person with the dab out on the sidewalk with a vacuum or blower dude that shit has so much dust and dirt in it you are an idiot if you smoke that shit and I'm sorry for the people you sell it to. CHEMICAL AND PHYSICAL PROPERTIES 1. I'm pretty much retired these days maybe considering a bit of a comeback who knows? Make sure your work area is dust/contaminate free. This will remove approximately one-third of the remaining solvent. It is also incompatible with strong acids, alkalis, and oxygen. 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. Clean and nice smelling, but 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. There is a SURE fire way to remove the polar substances from your extract, and furthermore purify your compound to either a pure cannabinoid product or nearly pure. Stay Connected. How can I clean up my wax if I bought it from a friend and it looks like poop soup and very hard to work with? It was nearly pure THC, sweet chalky flavor and delicious. Put back into freezer for a couple of hours and repeat 2 more times so you have a good clean product. To try and make that layer easier to see and remove I have tried heating up the salt water, and cooling it down. I generally see the best results going from the most non polar solvent (hexane) and proceeding towards the least polar solvent one step at a time in the seperatory funnel. May Life not life on you too often. at a certain point the polarity will become just right for the cannabinoids to pass through the column. 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. After shaking it well, I hung it from one corner, to let it stratify, and after it had, I clipped off the lower corner of the Ziploc bag, and by pinching it, and controlling the bleed rate, I was able to bleed off the water, alcohol, and emulsion layer, so that only the now gold hexane solution remained. No fear. We must have repeated this at least 10 times. I pre-heat my oven to 250 F. I put the iso/extract mix now onto a preheated cookie sheet. 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? Looks like a 1000 ml Sep they are using in the photo. Great info. Dale talks about fighting to free cannabis prisoners, staying active in cannabis advocacy, and reducing the stigma around the plant. A personal disclaimer; I involve one more step that requires flame to volitize the remaining hydrocarbons out of the extract. 10.3 Pentane/Hexane/Heptane and brine wash - GrayWolf's Lair Nucleation is when atoms begin to bond together due to reaching a specific temperature called the solidification temperature. When you say acetone/water experience, is this including salt water? I use HPLC greate 99% hexane. do a vac purge? When I class chlorophyll with the water solubles, it is not in the same vein as the term is used in inorganic chemistry and is more involved. Here is what a winterizing filter cake looks like, while still wet. As you may know, anything above 15 is considered polar, with water at about 80. Cthis will preserve your terpene profile. #8run dissolved liquid into coffee filter back into a clean jar this is to prevent unwanted seeds from starting, #9(room temp) Hence floats on water. Once that's done, seal the concentrate in a container and leave it for two to three weeks. Hi All, Hi, It is not correct to say that using hexane is not highly effective at recovering thc from any form of extract. You've picked yourself a challenge brother! This presumes that your goal is to remove the chlorophyl only. GW. Simple filtration, even at that micron level, takes stuff out of suspension, but not out of solution. Your "pasty mess", from your description is H2O still in your Onion. The hexane was much brighter, but when we purged, it came out pretty black. GW. Preliminary research into THCA has shown this cannabinoid possesses anti-inflammatory, neuroprotective, anti-emetic, and anti-proliferative properties. Isopropyl alcohol always has water in it so that was involved. 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? does not really works, am I understand it morrect? Are you up for a challenge ? The Pam was used to lubricate the blades on an automatic trimmer and contaminated the trim used for this particular extraction. Do you do this with your cold crash crystals ? 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. Close the vessel and very slowly increase the temperature to 25-35. The deviation from routine extraction begins here. My ISO process is done after I have done other primary extractions, so I am extracting whatever is remaining in the plant. I will post another way to "clean up" goopy wax or shatter. I rarely use flower because I do not extract, but this reply is in hopes of helping you out. So from now on, I will only do "mixing" outside of my main mash tin - that way I can still reclaim the little bits of precious. The water layer underneath was clear. Once dissolved, I place the mixture in a 0 degree freezer for 48 - 72 hours. Can anyone suggest me an effective method for the - ResearchGate Same with the eggs and so forth. Run the rotovap again. 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. Begin adding COLD water in a pippette, about 1ml-5ml at a time to the seperatory funnel. Does this help? A vacuum of -15 to -20 mmHg should be used to assist the purging process. 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. Chlorophyl is not soluble in water. Besides name calling your post has little data to support your claim that environmental elements found in normal day to day living are hazardous beyond the hazards already present in the product. Clarified neem oil is said to be hydrophobic. 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. Combining THCA with cannabinoids like cannabinol (CBN) and terpenes that promote relaxation, such as linalool, could assist in recovery or rest. GW, could you by any chance assist in us getting in touch with a lab that would accept a sample and cash payment via mail? It runs smooth and pure at this point and doesn't snicker or pop when dropped through a flame (Bix). But how are these diamonds made? After it is lit I turn the cigarette up so anything fluid drips out and I let the icky part flame off. #12 once pentane gets to the point where your crystals are not covered or your impurities are getting too concentrated ,remove the wanted seeds then fast crash the pentane solution by keeping the lid off repeat steps #4+ once solution has evaporated the pentane leaving unwanteds+ THC-A, Thanks @Terpjesus. 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. :). feel free to add any advice fam. Lab coat. I use 5% increments as an example. I have gone to using activated carbon pellets only in the vapor stream of my Vapir One vaporizer which is packed with carbon pellets in the chamber that the vapor passes into prior to the breathing tube. Diamonds, otherwise known as crystalline tetrahydrocannabinolic acid (THCA), have started to become more popular in the cannabis industry. Shake well, stick it in the freezer fro two days. There wasn't really enough that precipitated out to smear onto paper to see. If you need to explain it, maybe the person you are explaining it to shouldn't be doing it. you will dissolve more thca than wanted No matter how hard I dry the the ethanol, the pastiness exists. Step Five: repeats several times. Be careful, though, as too much solvent or solvent that is too warm will dissolve . Because brother, I have found when refining dispensary extracts; fitting grease, eye lashes, tiny flies, unidentified dust bits and have added on accident some of ose those things myself. It is amber and clear and can vape with very little respiratory irritation. Check the MSDS because the word light naphtha only means it boils between 30C and 100C, so it can contain Benzene.. It appears however that azadirachtin by itself is hydrobolic and miscible in water. This doesnt mean it isn't effective it just means that more understanding is gained with each effort. We were able to justify the cost based on the number of samples we ran and the cost to have a lab run them for us. Sometimes bad things happens to good oil, and evil spirits need to be exorcised, or sometimes the most economical process, or indeed the only available extraction process, extracts undesirables. Given the extremely low toxicity of the product to humans I personally would not hesitate to vape the oil after I did the above procedure. What evidence can you provide that suggests the lungs are not capable of dealing with this? Alumina is basically the grit on sandpaper and is as toxic as sand. Your wax is probably between 60% and 80% which is much better than pure stuff anyways (imo) because you get the full spectrum of the plant. GW. When you smear it on white paper, is it green or brown? N-PENTANE is incompatible with strong oxidizers. Bigger chunks bake at 275F instead of 300F to avoid burning. Cleaning and Disinfecting Surgical Instruments | STERIS Perform your extraction as normal but maintain a ratio of solvent to biomass between 6:1 and 10:1. Individuals with nausea may want a capsule or tincture that has a ratio of THCA and cannabidiol (CBD), another cannabinoid with potential anti-emetic effects, and some myrcene to help alleviate their discomfort. Join the Movement.Sign up to receive email updates for more opportunities like this, cannabis job postings, events, and more. I think this is why there is no simple answer to solvent questions because after all extract itself is solvent heavy (terps) and the ratios of the different solvents will always be a bit different. This is my sop (without getting into minute details) it really only is efficient for 100+ grams of thc-a otherwise there is a significant loss If symptoms such as redness or irritation develop, IMMEDIATELY call a . easily avail at any glassware supply lab supply, or with the correct search term, on amazon . I wish I could post pictures, but what it looks like, is a perfectly clear big thick layer on bottom (of salt water) and a gunky, kinda fatty layer in the middle (I'm assuming this is the emulsion layer though I'm not entirely sure what that means because it wasn't explained) and then the dark hexane mixture up top. Pentane recrystallization - Extraction - Future4200 Your time is always much appreciated, Skunk Pharm. Even at the hobby level for me it gets spendy to just evap it all. I wring the tea bags and am left with white waxy stuff and other solids. If we wish to filter it further, we run it through 0.45 or 0.2 micron syringe filters, which takes out any remaining plant material, as well as any bacteria present. This separates the iso from the water and immediately concentrates the iso above the water. You can continue to grow larger diamonds utilizing super-saturated hexane and to improve the clarity of your diamonds using chilled pentane washes. Please try again. I decided to cook it into a decarbed QWET oil (I follow your HOA recipe, sublingual) after straining, freezing, and straining again, but when it came time for the final 1/8" of mash that was left, it just wouldn't (visibly) go to decarb at 250F (I noticed a rainbow sheen to the bubbles), so I stopped and decided to try and air dry the remaining ethanol off. Safety glasses. I have never had any evidence that an acetone/extract mix can be "washed" with water. You seem to be blissfully unaware that we don't sell any concentrates to anyone, period. The reduced yield is not as much as you might think, once you eliminate the non targeted element pickup. For some reason, my alcohol, Hexane and water mixture does not bringing chlorophyll down. Experience has proven to me that this is the moment to stop heating it and put turn it up for the drip to form. Are you using 70% ISO, thus taking advantage of the containment of water to dissolve the salt? 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. Very interested in being able to remove as much amber color as possible. First off ,freeze your alcohol and plant material separately for a good 24 hours ( never wash at room temperature! Nowcan limes extract oil? It will pop under vacuum when those water pocket burst under the oil so a cover is necessary on the dish. 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. 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. Joe came up with this process, which has produced our most pristine creations. btw 98% is completely false. 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. Here is a link to a DIY evaporator that addresses that issue. I use isopropyl alcohol and water as a solvent system because it is inexpensive and much safer from a fire hazard and fume point of view than systems that use hexane. Please try again. In my humble opinion, you are doing it absolutely right. We still send out samples for others material to test for pesticide, but if you know the history of material that you've grown yourself, you should know what you used. I have seen various layers form but trying to repeat the results is hard. Diamond Mining is all about encouraging separation of cannabinoids from terpenes. Diamonds and Washi - YouTube 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? The THCA content of these crystals can be as high as 99 percent but can fluctuate depending on residual solvent and terpene content. washing diamonds with pentane 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. I surfed the links and discovered that the active ingrediant in neem oil is azadirachtin. I lit the picture on fire and warmed myself. Acute toxicity of the gas (LC50 rat): was 48000 ppm using 4 hours exposure data and the Threshold Limit Value for an 8 hour weighted average in breathing air is 500 ppm with a Permitted Exposure Limit of 1800 mg/M3 (~ppm). We are way over budget and we thought this would be the cheapest way to achieve high yield with one wash. So put in a large seed. We buy the salt cheap by the bag, using salt intended for water softener use. Then the person begins to adjust the solvent (called the mobile phase) as he adds it to the column in progressive increments which slowly makes the mobile phase more and more non polar. it is 94.5% thca and I was trying to figure out how I may clean it further. I tried many times to repeat the process but couldn't get the same thing to happen again. So waiting for the rubbing alcohol to evaporate or not having any rubbing alcohol present, I will tell you another sure fire way to "clean up" small amounts of wax and shatter; 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. In my attempts to polish with hexane I have done the following: One article cannot cover the m" >. I modified the screen a bit to accomodate extract. Excerpt from NIOSH Pocket Guide for n-Heptane: Eye: IRRIGATE IMMEDIATELY - If this chemical contacts the eyes, immediately wash (irrigate) the eyes with large amounts of water, occasionally lifting the lower and upper lids. Excellent post, we'll definately look into this in the future, sounds quite interesting. Ive tried to read as many threads as I can find on the subject, but most use butane for THC-A or if pentane is used, its to recrystallize CBD. We still have just one question - does the Hexane/Saline water wash impact the yield? I use a medicine dropper to remove the amber layer.