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Polishing extracts

Some MMJ applications require greater purity and potency, so it is desirable to remove inactive ingredients like fats, lipids, and plant waxes, as well as any chlorophyll and other water solubles.

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.  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.

Water also dissolves and washes away the Chlorophyll binding proteins and exposes the Chlorophyll to the solvent used.  Chlorophyll is highly soluble in alcohol and slightly soluble in butane.

For further discussion of that subject, please see: /chlorophyll-pickup-in-extractions/

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.  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.

See: http://www.nlm.nih.gov/medlineplus/ency/article/002893.htm  for details.

In a nutshell, many water soluble non cannabinoid ingredients come along for the ride when a polar solvent is used and water is present. While it is easier to use a process that minimizes their extraction in the first place, if that is a moot point, because you already have an extraction with excessive non-active ingredients, here are some ways to clean them up:

Filtering:

After re-dissolving the extract in ethanol or hexane, it may simply be filtered to remove the material that is insoluble.  We usually use coffee filters for this purpose, or if we have a larger amount, we use a Whatman # 1 lab filter, with a vacuum assist.

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.

Winterizing:

When using non polar solvents like butane and hexane, some non-polar waxes, fats, and lipids are extracted as well.  An easy way to get rid of them is to simply re-dissolve the non-polar extraction in 190 proof (~95.5% azeotropic) polar ethanol and stick it in the freezer for about 48 hours at -18C/0F, for the waxes to coagulate.

The waxes will precipitate out of solution as the temperature drops and clump together so that they are easily filtered out with a standard coffee filter, or a Whatman #1 lab filter.

Here is what a winterizing filter cake looks like, while still wet. After filtering, the alcohol is evaporated or vacuumed off, to leave a pristine Absolute.

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.  By re-dissolving their extracts in hot ethanol and then placing that in the freezer overnight, some of the undesirables will precipitate out and may be filtered out.

Removing minor green coloration:

Because butane is non polar and considered insoluble in water, it is the longest chain alkane that is still slightly water soluble at 0.0325 vol/vol (3.25%).  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).

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.

These light green hues are easily removed without the more involved and extreme measures that I will follow up with, and is as simple as putting a jar of the oil suspended in an ethanol tincture, in sunlight or a light from a high UV source, like a grow lamp.

The UV radiation in the sunlight will quickly break down the chlorophyll and the breakdown products are amber, so the green color disappears. Alas, UV radiation also destroys cannabinoids, but fortunately at a much slower rate, and three or four hours in the sun is usually enough.

OH MAH GAWD:    

Oops!  Soooo, what if the extraction is really, really messed up, or if you just want to see how purdy you can make an extract?

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.  Fortunately there are ways to remove undesirables, though at the expense of yield and some of the other terpenes, so there is compromise involved.

Alcohol/Hexane wash:

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.

We use an HPLC Reagent grade for this purpose, which we get from the local scientific supply store. Shake well and then lift the lid long enough to burp any pressure, before setting it in a stand to stratify into layers.  After it has separated, bleed off the water and emulsion layer.  They contain both the undesirables, and the alcohol as well, with the cannabinoids left with the hexane.

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.  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.

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.

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.

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.

I filtered the hexane and poured that into a Pyrex pie plate, which I blew air over with a fan to evaporate off.  Attached are pictures of the amber oil that I extracted.

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.

I am not suggesting this process for reclaiming ashtrays, but simply to make a point.

Hexane/Saline water wash:

Joe came up with this process, which has produced our most pristine creations.  It involves  re-dissolving the oil in a hot highly non-polar solvent such as hexane and repeatedly washing the solution with saturated salt water until it is mint quality.

Salt water washing uses a separatory funnel as above, but we start out dissolving the extraction to be cleaned directly into hot n-Hexane, and then washing the hexane solution with saturated salt water.

The magic trick is two fold.  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 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. We buy the salt cheap by the bag, using salt intended for water softener use.

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.

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.

At that point we stop washing and evaporate off the hexane. While we use HPLC grade hexane, light naphtha containing only Pentane & Hexane will also work for this process.  Check the MSDS because the word light naphtha only means it boils between 30C and 100C, so it can contain Benzene..

Purging Hexane:

While n-Hexane is a delightfully non polar solvent, that enables us to do some amazing things, it has two more carbons and four more hydrogen atoms in the chain than Butane, and so due to the greater Van der Waal forces involved, is not as easy to get rid of as Butane.

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.

To wash with ethanol, redissolve the hexane honey oil in ethanol at a ration of about 10 to one and boil off the alcohol.  When it is almost all gone, do it again, and repeat, until there is no decernable hexane odor.

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.

N-Hexane boils at about 69 °C/ 156 °F and has a high vapor pressure, so it is easy to evaporate, but harder to completely purge.  Given our 30ppm taste sensory threshold and our 130 ppm odor threshold, we can detect its presence, long before we reach levels of concern.

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 first clue of course, is that it doesn't come in nearly as attractive a container, and the second is the MSDS information which tells us, that in excess, N-Hexane attacks our nervous system.  The following is a typical MSDS Section 8:

http://www.sciencelab.com/msds.php?msdsId=9927187

Section 8: Exposure Controls/Personal Protection

Engineering Controls:

Provide exhaust ventilation or other engineering controls to keep the airborne concentrations of vapors below their respective threshold limit value. Ensure that eyewash stations and safety showers are proximal to the work-station location.

Personal Protection:

Safety glasses. Lab coat. Vapor respirator. Be sure to use an approved/certified respirator or equivalent. Gloves (impervious).

Exposure Limits:

TWA: 500 (ppm) from OSHA (PEL) [United States] Inhalation

TWA: 1800 (mg/m3) from OSHA (PEL) [United States] Inhalation TWA: 176 (mg/m3) from ACGIH (TLV) [United States] SKIN TWA: 50 (ppm) from ACGIH (TLV) [United States] SKIN TWA:

500 STEL: 1000 (ppm) from ACGIH (TLV) [United States] Inhalation TWA: 1760 STEL: 3500 (mg/m3) from ACGIH (TLV)

Section 11: Toxicological Information

Routes of Entry: Absorbed through skin. Dermal contact. Inhalation. Ingestion.

Toxicity to Animals:

WARNING: THE LC50 VALUES HEREUNDER ARE ESTIMATED ON THE BASIS OF A 4-HOUR EXPOSURE.

Acute oral toxicity (LD50): 25000 mg/kg [Rat]. Acute toxicity of the gas (LC50): 48000 ppm 4 hours [Rat].

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.  Note also that oxygen in a breathing atmosphere greater than 75% pure will kill us dead!

A review of the hexane Material Safety Data Sheet shows that the oral rat LD50: is relatively high at 25000 mg/kg.

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).

Studies of shoe repair folks suggest that long term chronic exposure at lower limits can have long term effects, because the liver converts n-hexane to Hexane 2.5 dione.  Their chronic exposure was many times what you would encounter in purging residuals left in oil that is below sensory threshold.

Besides NIOSH, we also have U.S. Department of Health and Human Services, Food and Drug Administration, Center for Drug Evaluation and Research (CDER), Center for Biologics Evaluation and Research (CBER) regulating what you can use and what you can leave behind:

/blog-images/http://www.fda.gov/downloads/Drugs/GuidanceComplianceRegulatoryInformation/Guidances/ucm073395.pdf

They list n-Hexane as a class two solvent with 290 ppm concentration limits, and a total PDE of 290 mg/day.

The good news is that if you are out of the stink or taste, you are less than about .01% of TLV, but the bad news (?) is that although it is relatively non toxic, hexane still tastes like lighter fluid below toxicity levels, with our 130 ppm sensory threshold far below the Threshold Limit Value.

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485 Comments

  1. tashiherzmark

    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? Thanks for your efforts.

    Reply
  2. Matt Muzio

    Hey guys, Let me first say thank you so much for the work you are doing! This is great information and I really appreciate the efforts you've made to bring knowledge to the masses. I had a couple of questions to ask for clarification. 1. I live in CA and the highest proof ethanol that can be bought in a liquor store is 151 proof. I went to a chemical supply store and bought 200 proof non-denatured Ethyl Alcohol instead. Is there a problem with winterizing with 200 proof? Does there need to be some water for the process to work? 2. At what step would one normally expose the solution to UV light to lighten the oil? After winterization and filtering but before the purge is done? Can I just do this in a sealed mason jar in the sun for a few hours? And then do a heat purge after the sun time? It gets pretty hot here during the day, could you do a sun purge of the ethanol? Would this kill 2 birds with 1 stone? Thanks so much guys. Keep tokin SG420

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  3. doobie

    greywolf, i recently built a lil terp. i am using a 50 micron screen gasket at the bottom of the column. My first batch came out a little green. I was wondering if you had any input on why this happened? should i be using a different filter?

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  4. Hashcat

    Thank you for your quick reply. I'm glad to hear back so soon :) I'm doing further research on hexane extractions and have found prolonged exposure results in the formation of a " toxic metabolite hexane-2,5-dione" . I'm sure you have most likely addressed this question but I can't seem to fin the answer. What is your take on this? Do you suggest using Hplc heptane or pentane? Also last question, is the solubility of cannabinoids and monoterpenes in hexane over a 12 hour exposure comparable to using butane and a quick wash(using a blasting tube)? Again thank you for all your help. I'm going to research a bit more on the extractions of terpenes from natural sources. I'm excited to put these ideas into practice!

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    1. skunkpharmresearch

      Concern for Hexane 2.5 dione metabolite is a real concern for chronic exposure, so proper purging techniques to remove the hexane below sensory detectable limits of 130 ppm is important. The Permissible Exposure Limit for Hexane for Hexane is around ten X the detectable sensory limits. If you can't smell or taste it, you are below PEL. Exposure Limits per MSDS:http://www.sciencelab.com/msds.php?msdsId=9927187 TWA: 500 (ppm) from OSHA (PEL) [United States] Inhalation TWA: 1800 (mg/m3) from OSHA (PEL) [United States] Inhalation TWA: 176 (mg/m3) from ACGIH (TLV) [United States] SKIN TWA: 50 (ppm) from ACGIH (TLV) [United States] SKIN TWA: 500 STEL: 1000 (ppm) from ACGIH (TLV) [United States] Inhalation TWA: 1760 STEL: 3500 (mg/m3) from ACGIH (TLV) [United States] The issue with hexane is with the 2.5 dione metabolite from our bodies breaking it down. The NIOSH standards are based on an 8 hour time weighted exposure and don't reflect what lower levels of chronic hexane exposure over a longer period of time may do. It has already been established that chronic exposure to hexane below PEL can have toxic effects, by studying shoe repairmen who use an adhesive that contains Hexane. http://www.ncbi.nlm.nih.gov/pubmed/22863898 J Occup Health. 2012;54(5):376-82. Epub 2012 Aug 2. Electrophysiological studies of shoemakers exposed to sub-TLV levels of n-hexane. Neghab M, Soleimani E, Khamoushian K. The results weren't pretty and in summary: RESULTS: The TWA exposure to n-hexane was estimated to be 83.2 mg/m(3). Electrophysiological studies showed that the amplitudes of sensory nerve action potential (SAP) for median and sural nerves were significantly lower in exposed subjects than in unexposed normal controls. Additionally, a significant correlation was found between these decreases and the urinary concentration of free 2,5-hexanedione. CONCLUSION: The significant decrements in SAP amplitudes for the median and sural nerves may be considered as appropriate indicators for early detection of n-hexane-induced peripheral neuropathy in asymptomatic workers with current exposure to sub-TLV levels of n-hexane. From that it is clear that regular chronic exposure at only about 17% of PEL and 83% of sensory threshold creates health issues, so that bring us to how much hexane will be present at one time given an average dose of 100mg. If we ASSume that the residual hexane is at 129 parts per millionth, or just under sensory threshold of 130 ppm, and a standard 100 mg dose, then we would ingest .0129 ml per dose ( (100______X 129 ppm = .0129 ml). 1,000,000 It would also be a momentary exposure, not 8 hour, so my own concern is low enough that I use it myself for alchemy, just remove it to save levels afterwards. Heptane is harder than Hexane to get rid of, because of its longer chain and accompanying higher Van der Waal forces involved. Pentane is a joy to use, but expensive.

      Reply
        1. Ryan

          Isn't the extract itself nonpolar? I remember a thread where a guy washed the hash oil in hot water. Cooled it, which solidifies the hash oil, and filtered out the hash. The hot water should remove most of the polar contaminants. Is this a suitable substitution to salting out with hexane. The reason I ask is because hexane is hard to find. It is also my understanding that the hexane will still have a detectable odor even after proper purging is performed. Is this correct?

          Reply
          1. skunkpharmresearch

            The Carboxylic acid form is polar and the phenolic form is non polar. Hot water won't remove the same stuff that polishing with hexane and brine will. Hexane can be removed below 130 ppm, which is the sensory threshold for most folks, so no that isn't correct. What is correct, is that you have to work at it, as it doesn't purge as easily as butane or pentane.

            Reply
          2. Ryan

            Is there a taste of hexane still left. Isn't the taste threshold 30 ppm and could I get it below that? Is salting out with hexane used for concentrates that are to be vaporized, or is it really only for topicals?

            Reply
            1. skunkpharmresearch

              The average person can detect Hexane to about 130 ppm and gifted palates down to about 22 ppm. We remove it to below sensory thresholds, by washing in ethanol and vacuum purging. We polish extracts for both oral and vaporization as well. The vaporized product will be hashy in taste, vis a vis floral, because most of the monoterpenes are gone.

  5. hashcat

    Hello, Graywold I wanted to start out by giving thanks to your website for providing knowledge about safe and alternative extractions. Education for harm reduction! Anyways i had a couple questions: Im currently performing a hexane extraction and I do recall reading a comment suggesting using a liebig condenser to efficiently save solvent. I was wondering if you find any positives or negatives with using a graham condenser?(i currently own a graham condenser). Also, I've written up an sop for hexane+winterization and am currently tweaking small variables with each run in attempts to preserve terpenes. I've read your posts on Thcfarmer about introducing terpenes from alternative sources during the extraction. I was wondering if you have any tips on terpene preservation? I've been doing a cold boil to minimize exposure to heat I was just wondering if theres any other suggestions? (i vac @ 115f at 29hg for 3 hours typically? Sorry for the abundance of questions. Thank you for all the knowledge I am humbled to have exposure to such knowledge base.

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    1. skunkpharmresearch

      Thanks for the good thoughts! A Graham will do the job and work best in a vertical position. It's only drawback that I can see, is that they putt in a horizontal position, because condensing liquid plugs the low spots and pressure builds up until it is enough to blow it through, so they tend to expel in puffs, rather than a steady stream. No, 115F at -29.5" Hg is my best shot at retaining monoterpenes, and hexane is so hard to purge, that few remain when its gone, so adding them back in is probably the best bet

      Reply
  6. Johnny Redthumb

    So I left some trim in a jar out in the sun for a few days and it turned yellow/bleached. I had previously gotten a very nice waxy blonde concentrate from the same trim. Now after leaving it in the sun, the butane extraction yields a slightly darker amber oil and turns to puddy and almost shatter, but never waxes, and seems to take much longer to purge. Obviously in the summer sun the trim decarboxilated, but did it break down the plant waxes as well? Any insight as to what happened? Is it worth trying to winterize or re-carboxolate to firm it up? How would you guys continue to refine this?

    Reply       Edit
    1. skunkpharmresearch

      It is doubtful that the sun had significant effect on breaking down the plant waxes, as they help protect the plant from drying out in the hot sun. I know of no way to re-carboxylate, but winterizing will take out the soft waxes. We would probably winterize it and vacuum purge it at 115F and -29.5" Hg, to get the best effect, but the end result would be heavily influenced by what has already happened to the oil, and it might not be shatter anymore.

      Reply
  7. scott

    I made about 3 grams of bho and after heat purging I put it all in a small mason jar with about 20 ml of everclear. Let sit in freezer for 48hrs. And strained with a coffee filter. I only ended up with 1 gram. Do you know why I ended up losing 2/3?

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  8. chris

    I am currently trying to get rid of chlorophyll. In my bho just been experimenting with winterizing bho. But i used 99 isopropyl. Can i still attempt a NaCL brine wash?

    Reply       Edit
    1. skunkpharmresearch

      Isopropyl isn't as polar as ethanol or methanol, but it will remove some of the non polar plant waxes. Ethanol would be better and methanol would do the best job. Polarity is a scale of least to most polar, as opposed to polar or non polar, but a dielectric constant of 15 is accepted as the breaking point, with Isopropyl only a 19.9. As a point of reference, ethanol has a DC of 24, methanol 32.7 and water 80. As to whether you can brine wash away the chlorophyll with a hexane/brine wash, it should still work.

      Reply
      1. The Butes

        Leave the solution under sunlight or UV light. It really does help break down most of the chlorophyll. I had some second run Iso turn out pretty green and the sun turned it back to golden amber within a day or two. At the price of degrading some of your cannabinoids, you can probably get it to look the way you want. Best is to avoid solvents that bring so much through in the first place. Butane keeps it purddy.

        Reply
      2. chris

        First id like to thank you for your replies a expert opinion alwaya helps so thank you. So i was able to remove chlorophyll through uv exposure, im aware it destroys some cannabinoids and terpinoids but it was all the resources i had. My next step is purgeing out the solvent. How can i tell if its been purged propery its isopropyl alc. And i dont have a vaccum system. I care about my patients and gealth is first concern its very molasses like like it spent one day in a clean tent for heat purging then 3 in open air, 45 mins at 112° over a double boil system the thickness is concerning because i feel like its trapping vapors can you give me a ratio or formula for removal of solvent. Thank you so much for alk the help

        Reply
          1. chris

            Planning on having it donated to medical patient's for personal use. I would assume vaporization, but some of the older aged persons would orally apply if there is a way to show you a picture. Or pictures i could show you. I'm pretty proud of its appearance but is lacking terps i would assume because its has a very low oder no excessive heat was used. Thank you for your knowledge you've shared been really busy working sorry for my delayed response

            Reply
  9. MB

    Can I use 192 Proof Grain Alcohol to winterize BHO? I know everclear has been mentioned but I can not find that exact brand / kind.

    Reply       Edit
  10. Hydrostatic

    I have soaked roughly 20 lbs of ground up high quality trim in CRC QD Contact Cleaner (product #: 72131, MSDS: http://www.crcindustries.com/faxdocs/msds/72131E.pdf). I've run it through coffee filters 4x, but the product is still pretty dark. What can I do to polish this extraction? Should I do a salt water wash? What steps do I need to take to get the end product to be free of solvents/debris, while keeping as much of the CBD's intact? Thanks for your time and consideration, it is very much appreciated.

    Reply       Edit
    1. skunkpharmresearch

      I would suggest a vacuum purge at -29.5" and 115F in thin films. Besides Hexane, Hexane isomers, and Iso, the contact cleaner also contains a 1 1-difluoroethane hfc-152a propellant. Here is the MSDS for 1 1-difluoroethane hfc-152a, which shows that it isn't particularly toxic, but note that the breakdown byproduct is Hydrofluoric Acid, which will even dissolve glass. That makes purging more important than if you were just removing the simple alkanes and alcohol. http://www.refrigerants.com/msds/r152a.pdf

      Reply
  11. Jp

    I have some dark sappy bho I want to polish up about 14 gs. Using heated up ethanol ill pour it into a stainless steel bowl and then add my bho. Is their a tempature that i should have the ethanol at? How much ethanol should i use? Is it crucial to seal this bowl or find something that can be sealed instead? I have a feeling like this batch has some tane trapped in it so would this be eliminated as well as the greenish tint after winterization and purging it without a vac?

    Reply       Edit
    1. skunkpharmresearch

      I heat the ethanol until it starts to simmer and then dump it into the container with the oil. I mix as fast as possible, as the alcohol cools rapidly and doesn't readily dissolve the oleoresins cold. Not sure what you are planning to make as an end product, but I seal mine in a canning jar before sticking in the freezer. Not enough residual butane to be an issue at that point and it will leave with the alcohol. You may or may not loose the green tint during winterization, but if you stick the jar of alcohol in bright sunlight, it will usually break it down in a few hours.

      Reply
      1. Hands

        At what point in your polishing process would you use the sunlight to take out green color? Must this be done before winterizing or can you take the winterized solution after filtering it and achieve this?

        Reply
  12. c

    vac pump oil in the good oil.I know, Big mistake. Sucked it back from my cold trap cuz it was to full. Dumb guy I know. Never happen again I tell you what but any way so now can it be separated back out or is it trash?

    Reply       Edit
    1. skunkpharmresearch

      We redissolved some in ethanol and then added hexane and salt water to wash out the contaminants for an associate, which turned out well. Check the process at http://skunkpharmresearch.com/getting-the-green-and-waxes-out-afterwards/

      Reply
  13. Johnnyzxc

    Rapid, Solvent-Free Microwave Extraction (SFME) of Essential Oil Analysis of essential oils The analytical procedure for essential oils or aromas from plants or spices comprises two steps: Extraction by steam distillation or hydro-distillation. Analysis by GC or GC-MS. While the analysis step is complete after 15 to 30 minutes, the extraction step of essential oils represents 70 percent of the total processing time. The NEOS System The NEOS system is based on the Solvent-Free Microwave Extraction (SFME) technology for rapid extraction of essential oils from aromatic herbs, spices and dry seeds. These novel processes can produce essential oil in concentrate form, free from any residual solvents, contaminants, or artifacts. The NEOS system confirms that microwave isolation offers net advantages in terms of yield and selectivity, with better isolation time, essential oil composition, and is environmental friendly.* The NEOS system is the result of the partnership between Milestone and the "Laboratory of Chemistry of Natural Substances and Food Sciences” of the Université de la Réunion (France), which lead to the grant of the European patents 1439218, 1618798 and 1629725. SFME is not a conventional microwave extraction process which utilizes polar and non-polar solvents nor a modified hydro-distillation method.

    Reply       Edit
    1. skunkpharmresearch

      Thanks for sharing with us JZ! I will check out the patents for details! You've noted that their process includes GC; did they do tests comparing their terpene profiles to other methods of solvent extraction?

      Reply
  14. Johnny Redthumb

    I have a question regarding getting the final product back to a waxy consistency. Refining and polishing extracts is great for potency, but what the California market demands is crumbly wax. I have successfully made many batches of wax, but I've had a few runny looking batches too. Very gooey. I understand this can be from water trapped in the oil, which is possible considering those we're the batches with the highest condensation (we have since corrected our technique). What techniques and solvents would you recommend, if any, to return these batches to a waxy consistency? Ethanol and freezing, then decanting?

    Reply       Edit
    1. skunkpharmresearch

      We have the best luck making light blond waxes, but starting with a young Sativa, and extracting at about 85F to 100F, before purging at 115F and -29.5" Hg in thin films. We first make shatter at 115F in a thin film and then fold the oil into a patty and cook and vacuum at ~100F until it waxes up.

      Reply
      1. c

        Does it still wax up after winterizing? I am very curious as to why it turns to a waxy substance if the wax is removed first. Some by product of being under vacuum for so long? thanks.

        Reply
          1. c

            so wax is then mostly inferior. Unless they take the time to winterize it is carcanegenic as in vaping parrafin etc,correct? So is more flavor or just ease in handling supposedly the driving force in wax liking? I would think that the more people get educated the less popular the waxes will become. Though if winterized and then turned into wax I guess it would be very popular do to its ease to handle.

            Reply
            1. skunkpharmresearch

              Plant waxes are mostly non active ingredients, that reduce potency through dilution, but aren't a know carcinogen. If you vaporize them and inhale them, they will coat your lungs though, and require expectoration. That is why we winterize our oils that we vaporize. As I understand it, the popularity of man made budders and waxes is ease of handling, as it is easier to produce shatter with the same aromatic properties and higher potency.

  15. Robert

    Why is there no ome talking about a co2 oil I own a co2 extractor it is capable of reaching 7500 psi bho is killing people stop this Next years high times winner remember Gaschromatography will reveal half of the fake co2 extract there Be ready

    Reply       Edit
  16. connor d

    Just curious, if I did an initial extraction with naphtha, and then mixed the naphtha with some water in a jar 50/50 and shook for a bit to do a water wash, could I just put the jar in the freezer and let the water layer freeze so I could just pour off the naphtha layer since I don't have a seperatory funnel?

    Reply       Edit
      1. connor d

        Damn, couldn't find an answer on that quick enough so I've already gone through with it. Haven't evaporated it all yet though so can't say how much I came out with, but I just figured since the cannabinoids were in the naphtha and it wouldn't freeze it'd be a good idea.

        Reply
  17. Keith

    How effective would winterizing be on Isopropyl extracts? We are trying to remove the excess impurities and clean up our oil. Thanks

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  18. jameson

    Hi thank you for all the work from the skunkpharm team. Can a decarbed sappy oil that's been winterized in ethanol still become shatter given enough time in a thin layer at ambient temp? or does it need to be under vacuum? Will 115f/28.5 hg be sufficient to become brittle Thanks and Peace

    Reply       Edit
  19. samyaza

    Hello all. I have a ( rather ) stupid question. What would happen if I did so : Let the plant material slowly extract in pure alcohol for a while, filter it and then add a lot of water ( maybe salted ? ) in it. How would the water-soluble alcohol, the water insoluble cannabinoids and the water itself behave ? I suppose the alcohol + the cannabinoids would dissolve in the water at the beginning, but when the alcohol concentration will get very low after adding so much water, would the cannabinoids still be soluble ? Could they salt out in any manner ?

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      1. samyaza

        So, the emultion could be filtered and dried ? Ethanol is a bit dangerous to evaporate at home because it's flamable. You need to water-cool the vapors. If the emultion is mostly solid and poor in ethanol, it could be easier and quicker to extract à fatty, waxy paste. I may try to recycle molted material also. Cheap, safe recycling must be interesting.

        Reply
  20. Brandon

    Do I need to winterize before I do a hexane/saline wash? Or does the hexane leave all the undesirables in the alcohol? Would it be good to winterize the alcohol anyway, just so i can keep using the same alcohol as long as possible? Thanks B

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  21. joe

    Hi, I've been winterizeing my b.h.o. for some time now with everclear 175. In search of a cleaner product I tried ISO 99% and everclear 190 .Both gave me similar worse results, first when pouring my higher grade alchohols into my butane/oil solution (I let the tane burn off almost completey but not enough to get hard) ,when using the 175 everclear there is an instant seperation of butane and alchohol and once all butane is gone there will be debris in the alchohol solution. This doesn't happen when using the ISO or the 190 everclear..the poduct comes out WAAY DARKER . The only thing I get in my filters when filtering the higher grade alchohols is a very white slime, .I usually freeze my soultion 14 hrs before filtering..any thoughts would help ..thanks

    Reply       Edit
    1. skunkpharmresearch

      I would freeze for at least 48 hours before filtering and take it down to -18C/0F. I've still had waxes precipitate out after 24 hours. Using heat will darken the solution. If you can cold boil it in a vacuum at 115F, it will stay light colored.

      Reply
  22. C

    WOW just wow, I've known about both winterizing and water washing for quite a while but have never taken the time to do it. So I took some full extracted "RSO" style 12 hour everclear soaked oil and washed it. Yuch what a lot of stuff. For the cancer patients I always left the stuffin because as far as I know it could be any combo that is making it destroy the cancer cells so, ,,, but I decided to try this out for some pain patients to vaporize. wow. I made a trichrome extract from straight sieved clean trichromes and it was clear and strong but when winterized that same oil is amazing. My question now o wise ones is , 1) can sap oil be turned into shatter or is it always more liquid because it is so pure? 2) Is the "wax" BHO caused by the unfiltered out plant waxes? 3) Thanx bunches!!!

    Reply       Edit
    1. skunkpharmresearch

      Oil can be retained in the shatter form by using low heat. The plant waxes seem to play a part in producing "Wax", but are not the whole answer. Not universal agreement on the subject, but it appears to me that water is forming an emulsion with the wax and oil, which turns into wax and oil hydrates.

      Reply
      1. C

        thanx ,I'm very curious as to what all the different things r that wash out. What is a low heat? 120 f,130,140, or even lower? thanx again this is very new to me and I really appreciate the know how help.

        Reply
        1. skunkpharmresearch

          Any water solubles and chlorophyll will be removed. Low heat depends on the context and whether there is a vacuum present or not. 115F works in a 29.9" Hg vacuum, while 125/140F might be required without a vacuum. It is also different for an oleoresin and a solution. In what context do you have in mind?

          Reply
          1. C

            Thanx for the responses, First it would be in solution and as it evaporates turn more into an oleoresin. So if I run it at 140 F until it gets smaller and then put it under a vacuum at 115 F for the remainder ( using Hexane ) Then redisolve the oil in everclear and winterize it,then evaporate under vacuum again at 115 F then pour out and evaporate any solvent left will the final product be shatter ? or will the 140 F temp cause to much decarboxalation? I'm sure all the oil I have made so far is sap because of temps I've been getting the solvent off at. Good strong oil just kind of hard for people with muscle shakes etc to use easily. I'm thinking that the shatter is prolly the easiest form for them to vaporize with. Though the decarbed sap is great for medibles. thanx and hopefully I'll get to meet you in person sooner than later. I've been reading and rereading this site for a while now and I am so glad I found it. Thank you so much okay enough of that words aren't near enough peace.

            Reply
            1. skunkpharmresearch

              Sorry H&HN, I got behind with classes and this got buried on a back page. If you are running under vacuum, there is no need to go above about 115F. 140F will produce a softer, partially decarboxylated oil. If you use a large evaporation surface and keep the films thin, you can boil off and purge relatively fast. We don't do large quantities, so a 6" Petri dish works well in our vacuum desiccator, at 115F and 29.9" vacuum. At our saturation level, we pour in about 3/16 or so of liquid, and end up with a film 1/32" to 1/16 " no more than 1/6" thick, after cold boiling off the alcohol, and the residuals are purged. If it is a fresh frozen extraction of young material, it will produce a flint hard brittle extract, that fragments at room temperature when bent, and as the material gets older, or as more heat is applied, it will become more decarboxylated and softer as well as darker.

  23. Nathan

    Hey! I am into IPA washing of cannabis. And I've been using a syringe for filtering for a while now. But after seeing the syringe you folks have, Im wondering how I can get my hands on one! Any help would be appreciated. looking for glass.

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      1. Sppete13

        I have a question.... How do you operate the syringe filter? Do you: a) dip the filter tip into the solution to be filtered, then remove filter and squirt filtered solution into desired purging vessel. b) take the plunger out of the syringe and fill syringe w unfiltered solution and push thru the filter directly into purging vessel? I opted for "b" and it was very very difficult to push the solution thru....

        Reply
        1. skunkpharmresearch

          Wet the filter with some clean ethanol or other solvent first. Suck the solution to be filtered into the syringe with a stainless meat injection tip. Trade tip for pre wet filter and push into a new container. Or pre wet then try as you did before. If it is still difficult dilute it more and try again. Also make sure your filter and the housing are compatibile with your solvent. Also think about filtering with a larger pore size first. Then follow up with a smaller size. Joe

          Reply
  24. sally

    I don't put any water in when I purge. I take it from the butane machine then put on pyrex on a hot plate. Cook until butane is gone. The trim is also dry...

    Reply       Edit
    1. skunkpharmresearch

      You don't have to add water, as the plant material still contains some, unless powder dry, but the principle source for us has been atmospheric humidity. It freezes out in the form of ice at the edge of the evaporating pool, and then melts into the oil during purge. The way we got around it, was to use a deep catch and evaporation container, sitting in warm water, so that the ice formation was eliminated.

      Reply
  25. tilopa88

    Thanks for the info. I just did a simple hexane process that ended up a little too green (because I left the plant matter in the hexane for 2 days), and reading your cleaning article have this question. You say you can clean your product by dissolving it in 95% ethanol and then filter out the Chlorophyll (green stuff). But if chlorophyll is completely soluble in ethanol how can it be filtered with a coffee filter or other filters? And if I did this would I not be filtering out the THC? I'm assuming THC is not soluble in ethanol?

    Reply       Edit
    1. skunkpharmresearch

      If you already have a Hexane extraction, there is no need to redissolve in ethanol to get rid of the chlorophyll, as simply washing in brine will accomplish that end. The reason for redissolving in ethanol and then freezing, is to coagulate the waxes, so that they can be filtered out.

      Reply
  26. concentrait

    for winterizing, if its more like a normal house freezer, should it stay in the freezer longer since its not 0 F? also a milky white liquid formed when the everclear was nearly all evaporated, what is this and is it bad?

    Reply       Edit
    1. skunkpharmresearch

      The lower end of most household freezers is about 0F, but longer at a higher temperature will work. In fact, if you just set it aside for long enough, it would drop out most of the waxes at room temperature. GW

      Reply
      1. Sean

        Hi GW, Thanks for your help - earlier this year in a forum you graciously informed me of the hexane /saline wash, in an attempt to remove neem oil from a few harvests. My first and current batch has seen nearly 5 gallons of saline, however there still is an emulsion layer that appears between the water and hexane when my separatory funnel bleeds out nearly all the water. Initially my first reaction was thinking I wasn't dissolving enough salt into the water to be effective, which seems partly correct, and I started using roughly 500g / liter. However, is it possible that my lack of winterizing the solution in advance is causing the necessity of so much washing? Or, do you think the emulsion layer will eventually stop showing up if I just keep bleeding it out and washing with enough saline? The solution has been filtered with a coffee filter but I was waiting for the emulsion layer to disappear before finally running it through the syringe filter. Thank you very much for any insight, as I have a few more harvests in line =) Sincerely, -Sean

        Reply
        1. skunkpharmresearch

          Hi Sean, forgive me for not remembering the forum you mention and if I led you astray on Neem oil. The procedure will remove a lot of undesirables, but is doubtul if a saline wash would be effective in removing hydrophobic oils from hydrophobic oilss. Not sure what the emulsion is, unless there is some alcohol present. Did you use alcohol anywhere in your process? GW

          Reply
  27. Rob

    When doing the Hexane/alcohol wash how do you prevent an azeotropic mixture from forming between the hexane and the alcohol? Or how do you reclaim the pure hexane? I tried your method and after distilling off the hexane (stuff's too expensive for me to just evap, and not really eco friendly either) it is cloudy indicating that it has formed an azeotrope. BTW, I love your site, it's nice to see others doing the same type of extractions as I am and seeing how they handle the different aspects of the process. Keep up the good work.

    Reply       Edit
    1. skunkpharmresearch

      We prevent an azeotrope by adding salt and vinegar to the solution. There will be some comingling at the interface with the alcohol/hexane simply because the one end of the alcohol molecule is non polar (CH3-OH). I just pee it off slow out of the sepratory funnel and generally end up with a little alcohol left or a little less hexane. We attempted to recover hexane with a distilling condensor but couldn't get it dialed in such that we didnt smell hexane fumes escaping. I hear Greywolf has been tinkering with a stainless rotory evaporator for recovering hexane. I think we are still in the developement stages so it may be a little while before you see anything posted on our site. We are all waiting with baited breath......

      Reply
      1. Rob

        About how much salt and vinegar do you use per... say 100ml (or some other arbitrary volume)? I've had good luck with my distilling setup (liebig condenser) I solved my leaking problem by Dow using high vacuum grease.

        Reply
        1. skunkpharmresearch

          I would have to look at my lab notebook at the chemistry lab to know for certain. But I believe it was around 100g salt / liter. It was pretty time consuming to dissolve. You could probably use less. Salt makes the alcohol insoluble and exposes hydrophobic surfaces of proteins and causes them to precipitate. What are your polishing goals if I may ask? I could help paint a better picture if I have a better view.

          Reply
          1. Rob

            My wife has Primary Spinal Stenosis (narrowing of the spinal canal) and I make her extract to smoke and for making a transdermal topical. I use a soxhlet with hexane to extract the crude and am triying to find a good procedure to wash the crude to get a purer oil. I am doing your "winterizing" procedure right now and am excited to see how much wax/lipids/etc precipitate out. And the geek in me just wants to fiddle around and try to make it as pure as possible.

            Reply
          2. Rob

            OMG you were so right about the winterizing just finished distilling the extract. My procedure next time is going to be soxhlet extract with hexane, distill till "dry" then disolve in EtOH, freeze, vacuum filter, distill till "dry" disolve in hexane then distill and evap to leave my absolute. The reason I'm redisolving in hexane is on the equipment I have I couldn't get the EtOH to stop bumping even with boiling chips so It's just easier for me to use hexane as the last step. This last batch of extract now looks just like yours at the top of this page, thanks so much for being willing to share your knowledge/experience with me over the last few days. Rob

            Reply
          3. Rob

            One more question for you, is your absolute after winterizing always a liquid (viscous, kinda like gear oil)? Even a room temp my absolute is a liquid, just wondering if this is the norm. Rob

            Reply
          4. Rob

            ok this batch was decarboxylated, I'm looking at getting my wife an Omicron vaporizer, should I decarb or not for this kind of application?

            Reply
            1. skunkpharmresearch

              It will work either way, depending on the cart. Since you are vaporizing, it also isn't necessary. We use a 510 cart with the wick removed for the carboxylic acid forms, and leave the wick in for decarboxylated. The issue is that the decarboxlated will leak or run out of the cart when it is laid on its side, unless kept suspended in the wick.

  28. scottie15

    I do not know which forum is 'Greywolf's' forum of choice, otherwise I would post this there.. but I came across a research paper from the University of Toronto where they use acids to precipitate chlorophyll out of canola oil (Canadian rapeseed has alot of chlorophyll). The acid/solvent ratios are close to that of the isomerization process, so I wonder if this same process can be used with hash oil without damaging the cannabinoids. https://docs.google.com/viewer?a=v&q=cache:vwzM16J-XTsJ:www.cyut.edu.tw/~ijase/2005/IJASE%25203-2-1.pdf+remove+chlorophyll+canola&hl=en&gl=us&pid=bl&srcid=ADGEEShYZ-lbdR6c4qVNwcFk1THJDN5uH-ti3J3MKHIG3MGTXwLpsjOiKUG83tBsRe3eMJN3IO4cvj6TMJ3NWRtNLsryFRGl11SffNSvn0MgcHT7OtBwkTClpThGLFyZHEEdbLKXTbBO&sig=AHIEtbRXHV8blDgK-8n8BoctGDaAgvsSOA I figure you guys'll make sense of this more than I. Much appreciation for all the knowledge you are putting out there.

    Reply       Edit
    1. skunkpharmresearch

      Thanks for the link Scottie! It look like an interesting process and my guess is it would produce a phosphate ester. Alas, I'm not a chemist so I will ask Joe, our resident organic chemistry brain trust, to review the process and make more educated observations and comments. GW

      Reply
  29. for_science!

    Grad student here, working on a terpene extraction process for an entomology study! I just wanted to thank you, I'm trying to clean up chlorophyll and wax in my samples before putting them through a GCMS. If I incorporate your steps into my method, is there some way I should acknowledge you if this gets published?

    Reply       Edit
    1. skunkpharmresearch

      We understand if you are not comfortable with acknowledging Skunk Pharm in you research paper. The stigma may affect your career in the future. We would appreciate a comparative analysis of your extracts chlorophyll content before and after you perform the procedure. Our GC is not in operation currently and we would love to know quantitatively the effect of our procedure.

      Reply
  30. leo

    and how would i treat these differently? I am both interested in both using them for extraction and polishing up crappy butane products I come across.

    Reply       Edit
    1. skunkpharmresearch

      Here is how we use them for extraction. Note the different soak times. http://skunkpharmresearch.com/qwet-extraction/ http://skunkpharmresearch.com/qwiso/ You would use them the same for polishing, Iso just doesn't work as well as Ethanol for that purpose, because it is more agressive.

      Reply
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