A clear colorless liquid with a petroleum-like odor. We are working with oil extracted through warm methanol extraction. C or colder for 48 hours. Perform your extraction as normal but maintain a ratio of solvent to biomass between 6:1 and 10:1. This presumes that your goal is to remove the chlorophyl only. Vapor respirator. In column chromatography, which takes HOURS for even small samples and simply cannot handle larger samples, a solvent gradient works by passing a solvent through the column that has very little or no ability to disolve the sample and carry it through the stationary phase. I pre-heat my oven to 250 F. I put the iso/extract mix now onto a preheated cookie sheet. . Hello Mr Gold, Thank you for your book, it must have been hard work publishing a book of this nature back then. Polishing extracts | Skunk Pharm Research Following this I dissolve the winterized oil in n-hexane (Ratio 20 g ISO to 100 ml hexane). Step 3: have 6-8 filters , jars &funnels ready, i usually have my alcohol oil mix into 2 liters glass mason jars so i can filter as quick as possible so the waxes, chlorophyll etc..does not dissolve back into the alcohol ( which will happen if the alcohol starts to reach room temperature). 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). Gently wash all affected skin areas thoroughly with soap and water. Metal-organic frameworks (MOFs) are highly nanostructured coordination polymers that contain metal cations and organic linkers and feature very large pore volumes and surface areas. Thank you! Put makeup on. TWA: 500 (ppm) from OSHA (PEL) [United States] Inhalation. I have found the following site to be a good source on information on this sort of thing. And filtering through AC and DE? 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. As you may know, anything above 15 is considered polar, with water at about 80. Boiling point 97F. GW. Combining THCA with cannabinoids like cannabinol (CBN) and terpenes that promote relaxation, such as linalool, could assist in recovery or rest. The mix will clearly seperate into multiple layers. I cover them with rubbing alcohol. Instead, we'll wash our current solution with hexane and water, removing chlorophyll and whatever else goes out with it. Could you please tell me what that bottle top filter contraption is? CHILDREN IN INDIA ARE GOING WITHOUT!!! The second time we washed, the water was lighter. The THCA content of these crystals can be as high as 99 percent but can fluctuate depending on residual solvent and terpene content. My starting material is BHO which has been CRCd and dewaxed inline. We warmed the oil and solvent in a pyrex dish in water bath. 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; Diamonds may be tough, but avoiding knocking them against hard surfaces (or dropping them) can go a long way toward keeping your gems sparkling. 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. I'm pretty much retired these days maybe considering a bit of a comeback who knows? Use a fan to evaporate off the alcohol (about 15 minutes) then place the almost dry extract on some cooking paper. 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. The reason we are trying to yield pristine oil is so we could advise accurate dosage to our patients as the medicine is illegal here and no lab testing is available. Be careful, though, as too much solvent or solvent that is too warm will dissolve your THCA. I have really messed up extracts through a variety of experiments and this method cleans them up to pristine. In my attempts to polish with hexane I have done the following: Ostensibly Methanol would do an even better job winterizing, but would require tighter purging standards. In a nutshell, many water soluble non cannabinoid ingredients come along for the ride when a polar solvent is used and water is present. What were your perameters for that thing?! Insoluble in water. I siphon off the amber precipitate with a medicine dropper. The water will drop through the iso layer and into the bottom layer at first, oulling polar compounds with it. Nowcan limes extract oil? Growing cannabis is a fun and exciting hobby unless your plants produce less flower than you had hoped. The web says PAM is water soluable. We deeply appreciate your support and what you do! Here is what I would do with a glob of black tar as you describe. Hope it helps. We used 20 grams of oil and around 200ml of Pentane & Hexane mix. - Should we 'winterize' before washing or that is not necessary? Less volatile means it'll be harder to remove.. I have done this many times. GW, I've asked our chemistry brain trust Pharmer Joe to also share his thoughts, but my first thought is that a warm methanol extraction would be chock full of extra stuff, that as you've noted is difficult and time consuming to remove. Pour off mix into seperatory funnel. Do you have data that shows ordinary dust found in every single food product, tobacco, and marijuanna leaf to be more hazardous to human health than the MSDS shows for either pinene or limonene? When you say acetone/water experience, is this including salt water? Clarified neem oil is said to be hydrophobic. 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. Would have a question for you. 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? The most effective way that we've found to remove the residual hexane, is either with multiple ethanol washes, usually around three, or thin film vacuum. I use HPLC greate 99% hexane. The relatively pure iso evaporates off much much quicker after the rubbing alcohol has been "salted down". I will need a hexane-group solvent or other alcohol to work with acetone/salt water to create various fractional layers. I am thinking of peppers. Nice and cheap is great! You can make nearly pure iso propyl alcohol for pennies by salting down rubbing alcohol. The Pam was used to lubricate the blades on an automatic trimmer and contaminated the trim used for this particular extraction. Commercial n-hexane is a mixture of n-hexane isomers with a small amount of cyclopentane, pentane, and heptane isomers. Chlorophyll itself has a polar head and hydrophobic tail, so it is mostly non soluble in polar water, but can be removed from the plant and conveyed by water as micelle. A vacuum of -15 to -20 mmHg should be used to assist the purging process. Thank you so much! There are orders of magnittude less solvents used in this process compared with Flash Chromatography. See: http://www.nlm.nih.gov/medlineplus/ency/article/002893.htm for details. From your post I assume you are also after THC. 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. Acetone is polar with a dielectric index of about 20.7 and is miscible in all proportions with water. No matter how hard I dry the the ethanol, the pastiness exists. I accept the danger in my own kitchen and simplyhave not found a way to finalize the polish without it. easily avail at any glassware supply lab supply, or with the correct search term, on amazon . Two Dawgs It seems like the colder I got the salt water, the more of that gunk I was able to pull out each time. The oil becomes hard and taking the dish out, the water left melts first abd pours off easily. The magic trick is two fold. I'm looking for an older link you posted to terps you bought off line. Or 7-10? The sorption and desorption of n-pentane vapor by porphyrin aluminum metal-organic framework Al-MOF-TCPPH2 where TCPPH2 is tetrakis(4-carboxyphenyl)porphyrin linker were studied by a novel method of in-situ . Ended up a little dark so I ordered a gallon of hexane, warmed some up, and dissolved oil in it. 10.3 Pentane/Hexane/Heptane and brine wash - GrayWolf's Lair 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. I cannot know if this would work for you because every parameter often gets adjusted "on the fly" as I do my own. Some questions that we have If it is not chalk white, evaporate and oil will be recoverable. We would be happy enough If we found a way to test the potency of our extract. This means it is designed to sublimate frozen water into water vapor, skipping the liquid phase. Light smoking will occur if particulate is present - the goop oil will stop smoking though. Two Dawns here Bro, I have a project that you need to be involved in ! I stuff it in there real tight. No matter the strain it always seems to taste fruity and pleasant. I can't waste this material. Pleasant tasting frankly. Invalid username/email. I have tried this saline/hexane wash before on some oil few years ago. I immediately place the dish used while still very hot into my vacuum chamber and pull it down until the gauge shows 30" or the pump starts complaining lolz. 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! I usually make a QWET into your HOA formula, batches of 1-2 ohzees per batch, and so I usually just add the coconut oil, cinnamon oils, etc. Set aside and come back in 1/2 hour. I am wanting to wash them clean and use them for various purposes; starter diamonds, season them with previous terpene separations, distill for amusement, whatever. N-PENTANE | CAMEO Chemicals | NOAA Now the crystals are left to dissolve in pentane, which extracts more parts per million of non-THC material. Extract doesnt like salt. In that patent they mention the same kind of azeotropic behavior shown here when using hexane and water as well as the primary patent application that soecified isopropyl alcohol at 91%. At this point, after draining, we added 300ml of saline water and 300ml of methanol. Salting alcohol is well known. ( depending on your material and type of alcohol you use). EXTREMELY potent when captured in a Vapir party bag. Starting with the solvent and working our way to the crystal, lets explore the best methods to create the finest diamonds. When enzymatic cleaning chemistries are used in washer/disinfectors, they typically work best between 100-140 F/32-60 C with detergents typically being used in ranges between 122-180 F/50-82 C. This can vary . Bleed off bottom layer (or what I can semi distinguish as the aqueous phase) and replace with clean water. Very interested in being able to remove as much amber color as possible. Skin: SOAP WASH PROMPTLY - If this chemical contacts the skin, promptly wash the . Thanks for your time, Reverse Osmosis is sort of like pumping a solution through a blotter paper straw. Hexane grabs all of the medicine for sure, but the real point of this article is to show one posssible use of it. Once the desired diamond size is achieved, pour off the remaining layer thats comprised primarily of terpenes. It runs smooth and pure at this point and doesn't snicker or pop when dropped through a flame (Bix). 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. 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. Preliminary research into THCA has shown this cannabinoid possesses anti-inflammatory, neuroprotective, anti-emetic, and anti-proliferative properties. ********* 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. Acetone is hands down the solvent of choice for cleaning extract and the residue it leaves in a boiling flask. QUICK READ: How can one obtain a shatter consistency with an ethanol wash/winterize, if not what is the best way to evaporate Ethanol? Garden. Saw @Future4200 did a pentane reX on his ig a while back was trying to find some more guidelines before I try it. 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. Deadly poison if you drink it. 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. Specific gravity (water = 1): 0.66 at 20 degrees C (68 degrees F) 4. Inhale this dense vapor, and you might even talk to the Man on the Moon. (broad and obviously erroneous generalization; but sound advice nonetheless). Link to a pdf of the issue here. After the fats and waxes have separated, I use a Whatman #1 Lab filter, accompanied with an unbleached coffee filter. No matter how you consume cannabis, the idea is to treat something that ails you physically as well as mentally. With all of the listed items above done as a hobby one thing is very clear - the results are highly variable. No chemicals involved ! I better gothe Vapir is getting cold. Kleen xtract has been the wash to get it back into a "purgable" consistency. Water also dissolves and washes away the Chlorophyll binding proteins and exposes the Chlorophyll to the solvent used. Pentane is a highly non-polar, light hydrocarbon solvent, that acutely dissolves THC instead of plant matter. Solvents in Class 2 (Table 2) should be limited in pharmaceutical products because of their inherent toxicity. Any ideas? The smoke is horrible so I don't believe any THC is left at this point. Put back into freezer for a couple of hours and repeat 2 more times so you have a good clean product. Have you personally smoked or vaped extract with dust in it? When left outside for 20min (45-50F) the solution solidified. 2023 Wise Education Technology Inc. All rights reserved. Does this help? Combining THCA with cannabinoids like cannabinol (CBN) and terpenes that promote relaxation, such as linalool, could assist in recovery or rest. 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, Fractions are collected as the process proceeds and the ones identified by the right color (light yellow in this case are saved out and evaporated off. Then I use either a battery power hot iron for wood burning craft, or a light to puddle the goop with heat so it is completely liquid and bubbling. What is left of the plate is black, and runny at room temp. Next Post: Faculty Feature: Stefanie Gangano, Ph.D. How to Get the Most Flower Weight from Your Cannabis Grow. 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. For our in house information, we picked up our own gas chromatograph used for $12K. We let it settlte and drained, it looked as if it was going as planned, the water was colored (but no percipitation). If the sample crosses state lines, it ostensibly falls under the aegis of the Feds. I have not observed salt having any significant impact in my own experiments, but it was cool to see salt crystals form in the extract upon drying. I leave my refined extract in an uncovered petri dish in my home. Washing Diamonds: There are a few ways to go about this. I wanted to know the best way to clean the 8 oz of green wax. To further refine the THCA you can wash it in another hydrocarbon such as pentane to try to remove the remaining . I notice the first pull down to -29.5Hg lets the extraction boil off very rapidly, then slows to a crawl. 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. Diamond Hazard Value Description; 4 1 0 Health 1: Can cause significant irritation. 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. Preliminary research into THCA has shown this cannabinoid possesses anti-inflammatory, neuroprotective, anti-emetic, and anti-proliferative properties. For some reason, my alcohol, Hexane and water mixture does not bringing chlorophyll down. Cite. I think of water and hexane as two extremes - most polar I have and least. A couple bucks at the Chevron mart. Extract can take a VERY long time to decarboxylate. Here is a link to a DIY evaporator that addresses that issue. 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. It has a burnt taste not normally present when vaped above 365F but is sweet below that. We poured the soution in the separatory funnel along with 1 liter of saturated saline water. The result is thick liquid at room temp, but hard as a rock in the refigerator. Thanks! What I just typed is how I would attempt it. I have redissolved it into fresh ISO and have it in the freezer separating from a saline water infusion. It sputters and pops and crackles something fierce. I came across a problem with onion extraction in ethanol and I ended up with a pasty mass. 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? Could I just skip the first step of extracting from the plant material and evaporating that off just to re-dissolve in a solvent, and just go straight to salt water washing after the original extract from the plant material is in the acetone? Youre not a bad person for consuming cannabis, Dale says. When performing your extraction, its important to chill your jacketed extraction system to -50oC or colder. I am having a great deal of difficulty acquiring non-denatured alcohol for the scrubbing of the hexane, what other solvents can be used to get rid of the last of the hexane, or is using denatured alcohol (denatured with MEK boiling point 79.6 C) ok? What would happen if you put an oil extract through a reverse osmosis system? Shake well and then lift the lid long enough to burp any pressure, before setting it in a stand to stratify into layers. Alas, UV radiation also destroys cannabinoids, but fortunately at a much slower rate, and three or four hours in the sun is usually enough. We buy the salt cheap by the bag, using salt intended for water softener use. I wish to retain the antibacterial properties of the extract as well as wish to obtain a powdery product. Part two. By googling, I learned (contrary to my vast knowledge beforehand lolz) that some things, like iso and water, cannot be separated by distillation. 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 find that IPA cleans up dispensary extracts quickly, safely, and from this simple process I obtain nearly pure THC/CBN/CBD/ terpenes etc. 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. If you have a dewaxing column, you can utilize this to assist in further removing undesirables. 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? "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. So just to check in case I'm being a bit thick IPA can be used to purge hexane from an extract instead of the ethanol mentioned in the above article, bearing in mind the less-than 0.1% water content of my IPA? Boiling point (at 760 mm Hg): 68.9 degrees C (156 degrees F) 3. See what happens. That means that a liter of n-butane will actually hold as much as 32.5 ml or mgs of water (1000ml X 0.0325). Well go through the typical method of creating THCA diamonds using liquid petroleum gas (butane/propane) extractions. washing diamonds with pentane. After winterizing and seprating the wax, would it be wise to keep oil solution cold like very cold? However the general process is a great tool if you realize that this is not a simple cookbook recipe. It's a syringe that wont hurt a mouse lolz! 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. Should you add the everclear to the butane/oil before it has evaporated? WARNING: THE LC50 VALUES HEREUNDER ARE ESTIMATED ON THE BASIS OF A 4-HOUR EXPOSURE. In meterology this is called "condensation particulate" and dust was once added to clouds in an attempt to seed the rain. It tells the full, untold story of the Oakland-based underdogs who risked everything to spark a global revolution in cannabis policy. But how are these diamonds made? Without additional processing, it produces a more full-spectrum product called a high-terpene full-spectrum extract (HTFSE). During this time, the THCa naturally crystallizes at the bottom of the container. The water layer will be milk to chalk white. I modified the screen a bit to accomodate extract. Leave in freezer the whole time? This time, a lot of stuff percipitated. Thanks. I wring the tea bags and am left with white waxy stuff and other solids. Run the rotovap again. Processes that use a polar solvent and reflux or soxhlet to maximize extraction, also maximize and concentrate chlorophyll, which can be a problem for some people. do a vac purge? Looking forward to your video! It turns out that I don't mind or notice a bit. 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. Based on this, my "go to" method of removing the irritant azadirachtin would be to attempt to disolve it in water. Below 10 degrees celsius, outdoors, not frozen 90 seconds wash. I strain off the salt water and gunky middle layer. Depending if you want to recapture your Ethanol or not, the next step is to remove/reclaim your Ethanol. Purged the pentane/hexane, the oil hasn't changed its color, it was still black. About 2-3 inches. High clarity and a lack of color is a sign of a high potency crystal; any other characteristics will diminish the potency. GW Step V : Here's where the chromatography machine comes . The flame gets intense. The UV radiation in the sunlight will quickly break down the chlorophyll and the breakdown products are amber, so the green color disappears. I'm also allergic to chlorophyll so I'm trying to kill two birds with one stone and stick to alcohols which I react much better to. This low and slow method will encourage more nucleation due to increased temperature and pressure and larger crystal growth. http://www.collectioncare.org/MSDS/naphthamsds.pdf Routes of Entry: Absorbed through skin. One way to clean up an alcohol extraction, is to reduce its volume to a manageable level given your resources, and pour it in a separatory funnel to about the one third level, followed by the same volume of n-Hexane and then of water. 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). Run the rotovap again. C over the course of 5-30 days. Only tiny bits of immiscible particules. We've got a bulk quantity of medicine that we would like to polish. May do it with an ounce or a pound, advice on both quanties would be great. What would I do in this case? Boy Howdy!!!! I have a half pound of green wax, Maui Waui, it's orange when looked at in the light. keep in mind evaporate too fast at this time and you will get unwanted contaminants trapped in the crystal lattice you want to evaporate reaaal slowy but not just sitting there or it will pause the process ( crack a ball jar lid as little as possible)
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