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: http://skunkpharmresearch.com/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:

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.

505 responses to this post.

  1. Posted by Bobbybud on February 27, 2014 at 9:47 AM

    I want to make sure all of the ethanol is purged from a dissolved solution of oil/ethanol. Heat alone takes a very long time and I am concerned about fumes. Is there a vacuum chamber setup that one could recommend for this?

    I’m also working out ventilation for the Ethanol fumes, if anyone has a good suggestion I would love to hear it.

  2. Posted by Joe C on February 24, 2014 at 6:35 AM

    What would you recommended as a good amount of 190 proof per ml of bho to winterize? and what is the best way & @ what temp to evaporate ? Sorry for all the Noob questions & Thanks again for your help!

    • About 10:1.

      Depends on what you want to make. Cold vacuum boiling works best to retain it in carboxylic acid shatter form for vaporizing, but if you are going to decarboxylate anyway for oral consumption, then a still works fine. With just atmospheric pressure, it will boil very close to 173F at sea level.

  3. Posted by david on February 22, 2014 at 4:47 PM

    I got Bhopal from someone and it’s green with some specs of marijuana in it. Is there any way I could get rid of it?

  4. Posted by Greasy on January 18, 2014 at 9:14 PM

    You have the vacuum as 29.9″ and temperature at 80 degrees for hexane. Is this completely necessary, or could I vacuum distill at 28.3″(cheap vacuum) with maybe a slightly higher temperature before adding ethanol and repeating, since I’d be winterizing afterwards? That way I could save the majority of the hexane.

  5. Posted by Hands on January 16, 2014 at 7:50 AM

    Hey there Masterminds! Just was wondering if an extended time soaking in ethanol (possibly a week – two even) and stored in the freezer would hurt the oil, or change the results after winterizing? I ask because I am having to wait for a week or two for a .2u filter come in the mail, I was thinking I could wash out after Thermos run with the ethanol (eliminating scraping/transferring) and store it in the ethanol until ready to finish the winterizing process but am not sure about how the extended soaking might affect the end product or would it? Thanks yal… bless

  6. Posted by thirdstone on January 11, 2014 at 5:57 PM

    will winterizing also remove any leftover butane?

  7. Posted by thirdstone on January 11, 2014 at 12:27 AM

    Will winterizing also remove any left over solvent? I don’t have a vac so I’m kind of worried. thanks

    • Depends on the solvent. What are you trying to remove?

      • Posted by thirdstone on January 13, 2014 at 2:12 AM

        Butane and I was also going to try it with my iso extracts. I Guess I was wondering if I could use winterizing as an alternative to using a vacuum chamber. I’m not so worried about the waxes and all of that mainly any leftover solvent, and my bad I didn’t realize comments showed up at the top of the page lol

  8. Posted by Kevin on January 2, 2014 at 9:57 AM

    I am winterizing using 190 everclear and I’m having a problem with an alcohol odor left in the purged oil. I have upped the temps 10 degrees at a time and continued vacuum till no more bubbles but the smell is always still there. I’m over 48 hrs in vacuum, and up to 180 degrees with no change. Every time I release the vacuum to check for odor and start again, I get a vigorous amount of bubbling action between 28-29.5hg that lasts approximately for an hour even if the temp is lower, the same as last run or greater. Your site and information is amazing. Keep up the great work. Thanks.

  9. Posted by caseyh on January 1, 2014 at 4:46 PM

    Will Pentane work for the saltwater wash? If so, why are you guys using Hexane instead of Pentane?

    It seems like you have access to anything you want and have mentioned the additional effort needed to purge Hexane.

  10. Posted by none on December 28, 2013 at 7:51 AM

    after reading your page, i can only conclude that you, in the past, have made dmt =) same chems, same language, same process (mostly), etc.

  11. Posted by robert on December 20, 2013 at 4:09 AM

    Why’d me last post get deleted? GW is there anything different abuot making things like sap, shatter etc using hexane instead of butane? I don’t have a vacuum anymore so I haven’t really had the option to make any of my favorite extracts. Is there anything I could do with some hexane washed qwiso or qwet besides just evaporating and curing? WAs hoping I could make some shatter from that somehow at least. thanks.

    • I haven’t deleted anything, I am just about sixty comments behind, what with other demands.

      The primary difference is that the hexane is harder to purge, so you lose more of the monoterpenes in the process. It also extracts non polar waxes, so winterization helps. Winterization also helps urge the hexane, especially if you don’t have vacuum purging.

      You can get rid of most of it with just a fan, so not a lot of heat required, and easy to make shatter if you purge in thin films.

      • Posted by robert on December 21, 2013 at 3:29 AM

        Ok, thank you I’ll give it a try then. Originally I was just asking if I had a dark extract made crown VM&P naphtha, would dissolving in acetone/saline and washing with hexane lighten it up, or would it just carry the dark impurities withh it?

  12. Hello
    Thank you for all the information you give on your site.

    I just have one quick question – if you want to winterize 10ml of Hexane oil, how much alcohol will you use for it?

    Thank you
    Gil

  13. Posted by caseyh on December 17, 2013 at 8:01 PM

    FYI: I was able to filter the winterization waxes after a few hours.

    I got impatient and filtered the solution as soon as I saw the wax form a cloud. As you might expect, it did not work. But when I did it again an hour later it did. I think the first try “primed” the filter and the second time the particles in solution bonded to the particles on the coffee filter.

    The final product is just as clear as usual.

  14. Posted by caseyh on December 17, 2013 at 7:45 PM

    You said, “so further refining was necessary with activated charcoal, but we will cover that as a separate subject” but I don’t see any discussion about it anywhere on your site.

    Am I missing it somewhere? If not would you elaborate.

    I am interested to know if charcoal would be an effective way to reduce mystery oil getting into the final product. I have considered putting zeolite or charcoal in the blast tube or in the ethanol solution but I don’t want to mess things up.

    What would you recommend?

    • Charcoal can be used to scrub the butane, but it will absorb cannabinoids if used to scrub the extraction.

      I recommend vacuum distilling the butane using a 85F cold trap to remove mystery oil. From there further scrubbing with charcoal, zeolite, bentonite, DE, molsieve, etc, can be used to further reduce residual contaminants.

  15. Posted by robert on December 17, 2013 at 11:38 AM

    so if I have some dark oil made with Crown VM&P would washing with hexane and salt water lighten it up or would the hexane just pick up the darker impurities the naphtha picked up?

    • Varnish and Paint Makers naphtha doesn’t typically extract dark colored elements, because they tend to be polar. You can give it a try and wouldn’t need to use hexane to wash it either. Just mix the salt water with the naphtha and use a separatory funnel. Stop adding salt water, shaking, and letting settle, when the water at the bottom stays clear.

      • Posted by robert on December 25, 2013 at 12:02 PM

        Ok, sorry I didn’t notice you had answered this I repeated it in another comment. Why do you think when I use it my extract always comes out dark brown and even pretty much black when it’s thick enough though?

        • I would have to know more about your process to comment, but the Beers Lambert effect will cause one thin film to be clear and almost colorless, while two layers will be almost opaque.

          • Posted by robert on December 29, 2013 at 8:27 AM

            Is that something that can somehow be more of a factor depending on solvents used or something? Should I just stop using naphtha? I don’t always use it, it’s just so convenient because the home depot’s 10 minutes away. But when I use it I pretty much just throw some buds or low quality bubble hash in a jar cover it with naphtha and swirl it around for 30 seconds to a minute and strain. Winterizing helps but for some reason there’s been a couple times where I just couldn’t see any waxes to filter at all. It’s always turned out the same color though, amber whehn smeared thin and almost black when it’s scraped or dabbed. If I use it from now on I might just start doing an acetone extraction and extract it with naphtha but I guess I might as well just use hexane for that.

          • I don’t recommend using naphtha or acetone. Can you get hexane and ethanol?

  16. Posted by Mario on December 16, 2013 at 10:03 AM

    Which brand butane do you prefer grey wolf? I had switched to colibri but it is nothing special for the price. Thank you so much for all your help, you are incredible, one more quick question which type of vacuum pump is a good choice.

  17. Posted by Mariojuana on December 16, 2013 at 2:45 AM

    I use 99.9% virgin acetone for winterizing with great results! but I really respect your opinion of this! I switched from ethanol to acetone because of the lower evap temps. Thank you GW

  18. Posted by Dylan on December 12, 2013 at 2:18 PM

    Would a buchner funnel with a fritted glass style filter be suitable in a vacuum assisted setup in stead of what you suggested?

    I want to make e-juice using a tincture style method*, rather than oil extraction due to its simplicity and safety (and ability to be done indoors etc).

    *Seeping cannabis in ethanol, straining, adding PG/P, then boiling off and filtering.

    Any tips on this, allbeit less effective, method too?

  19. Posted by caseyh on December 10, 2013 at 3:50 PM

    I have noticed a white cloud when I spill a THC saturated solvent into water. I suspect this is the oil being purged from solution as the solvent dilutes in water and losses its dissolving power. Is this correct and if so do you see any use for this as an extraction tech. I tried this once and it worked to separate something that sure looked/smelled/felt/tasted like hash…tried again and got nothing.

  20. Posted by Ron on December 9, 2013 at 1:14 PM

    I live in Ca.and they stopped saleing MEK, Toluene,Xylene,and Naphtha.
    The replacement contains, P etrolleum disttillates and Ethyl Actate. will
    this work or do I have to go out or state !
    Thanks
    too dawgs

    • You need to know what kind of petroleum distillates it contains, to tell how suitable it is. Can you get the MSDS to see if it is spelled out, or if it at least gives the boiling point ranges?

      At 170.6, Ethyl Acetate boils between hexane at 154.4F and heptane at 209.1F, so how difficult it would be to remove, depends on what it is in. I suspect that they wouldn’t use it, if it was easy to remove.

    • Posted by Ron on January 3, 2014 at 2:36 PM

      Hey,
      Wanted to say thanks. your answer makes a lot of sence.
      I’m kind of stuck. I have a bunch of last years trimings and so
      so far I have only been able to come up with a dark product.
      using Nap.and Denatured alcohol.
      Thanks
      Two Dawgs

  21. […] to it. Especially very high quality oil. Here is a link to winterizing using different solvents: http://skunkpharmresearch.com/gettin…ut-afterwards/ They refer to it as polishing extracts. You have it right on the freezing and 45 seconds. The […]

  22. Posted by Fernando on December 7, 2013 at 4:24 AM

    First off I’d like to thank you guys for sharing all of this information, it has been both interesting and educational! Second, I have something of an odd question: I’ve been considering methods of extracting oil from wormwood with the goal of isolating its active ingredient thujone (C10H16O). If I perform a methyl hydrate extraction, would the hexane/saline wash method be able to polish it successfully without carrying off any of the thujone? If not, which method would you recommend? What could I do to prevent picking up the chlorophyll during the extraction process itself?

  23. Posted by Gbroque on November 30, 2013 at 5:51 PM

    Three questions about the polishing stage;
    Can denatured ethanol be used in place of drinkable ethanol?
    Can methanol be used in stead of either and is it better?
    How can one purge denatured ethanol or methanol, and tell if it is fully purged?
    I ask because they are cheeper and more available than 190 proof ethanol.

  24. Posted by Sam on November 27, 2013 at 3:36 PM

    Hey I love your site very informative, and unlike most others your not full of shit. Any way, I make BHO and QWISO, here’s a quick run down. Since butane is expensive and I can’t afford your fun toys, I blast into another chilled jar with material, usually pack my column 3 times a can each, blast into a jar with material and keep it in the freezer, once I’m done blasting I seal the jar and keep in the freezer at least an hour, every 15-20 minutes I take it out and get it warm enough to make it boil, shake then return to freezer. After 60-90 minutes I filter it into a Pyrex dish as usual, hot H2O bath OUTSIDE EVERYTIME. I’ve seen a dumbshits blow himself up…..twice. Anyways, once I have thick oil I pop the bubbles and mix a little, I then let it “cure” for a week just covered with air flow cloth. When it’s cured( totally matte not sticky) I disolve in Everclear Yes you can get in California, I do legally, my secret. I’ll tell ya if ya pay me. So I dissolve add those charcoal gel caps minus the cap the triple filter after winterizing. It’s good stuff, what do you think I could do to make a better product? Is it true that simmering trim in water isomerizes cbd? Not to the extent as true isomer adaption tho? I also have an excellent thc e juice recipe if you’d like to know.

    • No isomerizing CBD with hot water. We have done it with sulfuric acid.

      Always interested in hearing someone elses recipes! What ya got?

      • Posted by Sam on November 29, 2013 at 8:46 PM

        I posted it in pen vaporizers, I’m not qualified enough to perform a true isomerization, I just read that on a “reputable” site surrre. I knew it couldn’t be true, I do visit your site daily, I live in Sacramento, am a MMJ patient and I love alchemy. And growing, this summer I took my first ever clones, made a CFL grow light for my closet 12 bulbs 26,000 lumens for 2×2, n grew the clones to harvest, my 1st cloning attempt was 70%. And my indoor grow way Surpased my expectations. And I’m an outdoor organic geek, I love growing n don’t sell shit!

      • Posted by Sam on November 29, 2013 at 9:29 PM

        So when you do the saline/hexane wash doesn’t that just break the emulsion layer chemically?

  25. Posted by GEEW on November 27, 2013 at 1:36 PM

    Gread read. I need some help here. I have older trim material that i have made some into bho and the extraction is very dark (not green) but very dark. i use a vessel that holds 4 cans of butane….not a pass through. so the method and the beginning material both lead to a very dark end product. I purged at low heat in a vac chamber so its not dark due to high heat.
    What would be the best approach to turn this into a light(er) color end product that isnt as harsh from the plant oils etc. THANKS!!

    • Winterizing and filtering to 0.2 micron will help some, but to really lighten it, I would suggest redissolving it in a non polar solvent and using chromatography beads in a packed column to strip out the polar elements, which tend to be colored.

      • Could you describe exactly what is needed and how this [process is done = “chromatography beads in a packed column” ?
        Thanks as always.

      • Posted by Sam on November 29, 2013 at 8:52 PM

        Did you use Vape poo in the extraction? I experience that u can use the same everything to the T, but the weather has a large influence on end product, mine are only dark If I use vape poo in the material(green n poo) is bet that it’s from the age of the material, after so long the cannabinoids oxidize just like thc in decarbing, I’ve found that the more CBN in your oil the darker, when I extract right from the plant it’s lighter than ghee.

  26. hello everyone i am trying to get some feedback here, i am wondering what people suggest i do for extracting, i can get n-hexane fairly easy, but what do you all suggest butane and a glass tube then cleaning it with the method given above, or do a hexane wash and clean it with the method above? i am looking to get a tasty highly potent like a budder or a honey comb.. not so much a shatter.. i am a noob at making this stuff and i need all the help i can get please and thank you

    • A good BHO or HHO doesn’t require polishing, because it doesn’t extract much in the way of undesirables to start with, except for non polar plant waxes.

      If you do either a hexane or butane extraction and then winterize in ethanol, you should get a tasty highly potent extract. If you want budder or honeycomb, you might be happier leaving the plant waxes in and going directly into a vacuum oven for finishing into wax.

  27. could i use 99.8% ISO instead of ethanol? for the hexane purging process?

  28. i was just wondering if i could use 200 proof ethanol denatured with methanol IPA, for the hexane purging step?

  29. Posted by richboy on November 23, 2013 at 4:04 AM

    If you don’t mind me asking, where could one locally obtain a syringe with “safe” rubber materials in it for winterization, if they already have a syringe filter.

    • We use ground glass syringes, so haven’t done much of a survey on plastic ones. My few tries met with disaster when the piston cup froze and I pulled the plunger out of it, trying to withdraw.

      Viton or PTFE would be two good choices of polymers.

  30. So I would like to be able to filter through charcoal as an option sometimes when needed to remove green colorant. What grade of charcoal and size would you suggest to minimize product loss in the charcoal during the filtration process? I am thinking a simple filter using a funnel packed with the charcoal and a stopcock on the bottom to control speed of flow. I was going to do it at the top of the mk iii column but after hearing the heat/friction/restricted flow issues I am thinking that after may work better. I figured to have the oil in a everclear base at the point of charcoal filtering prolly right after winterization. thanks. and hope tour staying warm and dry.

  31. Posted by ben on November 18, 2013 at 8:17 AM

    Can you put liquid ethanol mixture in a vacuum chamber to evaporate off under low pressure?

  32. Posted by Schrodingers Marmoset on November 16, 2013 at 6:27 PM

    Where did you get that sweet orange Buchnell funnel adatpter thing. Looks like it’d be cheap and work great.

  33. Posted by connor on November 15, 2013 at 9:46 AM

    Hi I have a question about winterizing..should the oil/solvent be diluted to a certain amount to work best? Just wondering because I put my oil into some acetone, but I wanted to use as little acetone as I could so the solution was extremely dark, I could put it into the light though and see if it was clear or not though. But after a couple days I still can’t see anything in there and I know there’s wax in there. Would making it more diluted help?

  34. Posted by step on November 10, 2013 at 8:45 PM

    Not sure where the best place to post this question would be, but I decided here!

    I am having a heck of a time separating the non-polar plant waxes from BHO produced in my MK IIIA. After dissolving my collection pot in ethanol, I am using 47mm filters (a glass microfiber stacked on a whatman 1) in a Pall filter funnel with vacuum assist to separate out the waxes. I remember reading somewhere on this site that you all do a filtration right after washing the collection pot and after winterization.

    My issue is my filters clog immediately. There is simply so much wax that even if I let it slow to a drip, a 1/2″ of wax has built up on the filter in a matter of minutes.

    I am extracting with below 32F butane in an effort to limit wax pickup, but this really has me miffed.

    I have seen pictures of you all using huge whatman filter papers.. is this how to counter the wax layer build up? Do you all use a massive Buchner funnel?

    • Some of the oil does have a large amount of wax dropping out at winterization and as you note, they don’t filter readily.

      We use a Whatman #1 filter with vacuum assist. I slows down as it clogs, but eventually finishes and we just do something else while it is pumping away.

      You can speed it up some, by using a long handled stiff artists brush and keeping the filter surface brushed clean.

      If you are careful, you can also gather the top of the partially filled filter and gather them at the top, before folding them over and gently squeezing the remainder of the alcohol out, I say gently, because it is easy to rupture the filter and squirt filtrate into the finished product.

  35. Posted by Reptar jr on November 9, 2013 at 1:14 AM

    I should be more descriptive. It is almost like a shatter when cold much closer to sap in relation to consistency.

  36. Posted by Reptar jr on November 9, 2013 at 1:10 AM

    In regards to removing of the green tint wirh UV light will this work if it is dark green? I have a run that is clear but dark green. Will this also remove chlorophyll ? Many thanks

    • Dark green will eventually break down, but so will a lot of the cannabinoids as well, so not a good plan.

      • Full Extraction Chlorophyll (really black-green) oil was UV light treated for 3 hours in a semi-mirrored formed enclosure, then winterized. The crud removed was substantial and black (as opposed to green), the chlorophyll ‘bite’ removed and the oil seemed to have plenty of kick. Many patients and caretakers present a morbid fear of further cleaning with chemicals and this procedure does conform to an ‘agricultural process’. Any thoughts of length of time in UV light treatment? How far does the light penetrate? or other observations?

  37. Posted by Walter White on November 5, 2013 at 5:03 AM

    If you had access to a research facility with ceterin things including a tissue lyser, ultra sonicator, centrifuge and a vent, wouldn’t using chloroform be the best method of extraction? It made some prettty dank shit, but i added methanol to the mix ( assuming this is why it turned dark green? ). Would using just chloroform make it brown? I also have access to 200 proof la grade ethanol. How could i use this?

  38. Posted by Tyler on November 3, 2013 at 9:44 PM

    Hello there! I’m almost finished collecting everything to polish the collection of roach flower I have aquired. My question is, does it matter if the syringe filters you use are sterile or not? I wasn’t sure if the ISO or hexane would sterilize the filter. Thanks for the help!
    Regards,

  39. Posted by Sean on October 31, 2013 at 9:15 AM

    Any tips to achieving a more shatter-like consistency after winterizing? I have produced this consistency before with this method, but find sometimes my end product remains very sticky with a more oil like consistency. I prefer an end product that is easier to handle occasionally.

    • Thin film vacuum at around 115F is the best way that I’ve found.

      • Posted by Sean on November 1, 2013 at 7:38 PM

        sorry should have been more specific, what if I don’t have access to a vacuum?

        • You might try heating it with a heat gun in thin layers on parchment.

          • Posted by Joel on November 23, 2013 at 5:30 PM

            I too have this problem. I tried winterizing with 200 proof ethanol and then used light heat on my stove top over night to try and evaporate the ethanol. I used a metal pot with water and placed my pyrex dish on top of the pot with water and placed parchment paper in the pyrex dish with the product on top of the paper. I am not sure if it the product got too warm or not. I do know that when I woke up all of the water in the pot evaporated. I also used 300ml of ethanol to 80 grams which dissolved completely in a very beautiful dark liquid. After about 30 hours in my vac oven at around 90 to 105f (my oven is old and fluctuates heat) it is still very soft and oily. Do you think if I give it another wash in the ethanol solution and let it air dry with a fan then place it into my vac oven that it will fix my problem? Or is the only way to fix oil is to use a seperatory funnel? the product looks beautiful, extremely clear and smooth. The only thing I am unhappy with is the Constancy.

          • Two thing typically make resin oily, retained solvent and decarboxylation.

            If you will place it in your vacuum oven in a thin film at 115F and -29.5, the bubble activity will tell you which it is. Retained solvent will promote random sized bubbles and decarboxylation bubbles are smaller and more fizzy. If there are no bubbles, you are most probably already fully decarboxylated and are stuck with the loose oil.

  40. Posted by Bigbank on October 30, 2013 at 3:43 PM

    Dude you are a boss this is by far the most informative website i have seen on this subject thank you and keep up the good work

  41. Posted by Kyle on October 28, 2013 at 9:57 AM

    Quick question regarding the finish product after Winterizing. After reading around a lot here and there I’ve come to the conclusion that Winterizing done right with the correct temps could very well leave me with a shatter finish, correct? I’m wondering if it is possible to get a honeycomb finish from Winterizing? I’ve been after a honeycomb finish for awhile now. I’m using dry indoor trim that I dehydrate then I water bath for 120-130 then vacuum at -30 at about 110 but it still doesn’t wax up. AT ALL. Just a sticky finish that is not touchable at all. Any suggestions for that as well? Thanks again. Love this site.

  42. Posted by Jedd Jones on October 28, 2013 at 9:03 AM

    Long time lurker, first time talker. I am running an experiment on some budder I was given. I took 5 grams of 3 strains (SD, OG, Sweet tooth) and dissolved it into 190 Everclear and put it in my freezer for 48 hours. Then filtered the OG through an unbleached coffee filter, and placed it into my desiccator and turned on the vac. Shortly after (5 minutes or so) my OG/Everclear mixture volcanoed inside the desiccator. The same happened with SD. I have the mixtures in a drinking glasses. Is this issue due to surface tension from the liquid cooling or is the cylinder type container working as a cannon and shooting out the liquid due to atmospheric pressure. I put the last mixture into a container with more surface area. Hoping this will reduce the problem. All help is appreciated. Thanks GW

  43. Posted by kevinf on October 26, 2013 at 2:40 PM

    will dehydrate my material to withdrawl more water when using iso 99..will this help prevent indica doment from auto buddering in chamber without heat..i having hard time keeping heat in chamber even..using extrationexpert one..have it floating in hot water at 1600f..with towel over it i have heat gun so can appy heat but hard.. any tips?

    • If you withdraw all the water, you will lose all of the monoterpenes. I prefer to freeze the material and the alcohol, so that the water locked up as ice and is not available to the alcohol.

      • Posted by kevinf on November 20, 2013 at 7:14 AM

        I do def freeze every thing for iso always in freezer i jus store it there all the time..and prod i freeze once get so it is in there for 48rs+….i think i just wasn;t thinning it out enough on my parch…because this last run went freaking awesome so nice and shatter like ..melts nice not popping

  44. Posted by Bobby G on October 23, 2013 at 9:58 AM

    would it beneficial to get to colder than 0F with 190?
    I’m having some problems of it warm up to fast.

    what do you consider hot ethanol?

    how long should it sit in the hot ethanol? just until it dissolves?

    what happens if its just room temp until it dissolves? does it matter?

  45. Posted by corey pearson on October 20, 2013 at 2:44 PM

    Hey gw I’m a long time lurker and I’ve been hearing a lot about single solvent extractions lately. I don’t know much and would like to know more. I figured if there was anyone to ask it was you.

    Thanks in advance. I’m really curious as to how to go about this process. We’ve played with winterizing and we have access to hexane just haven’t decided to open it up yet and try the process. Although we do have a jar full of roaches hmmm. Anyways very curious about this as its just come to my attention and I feel like the kid in math class who missed a week of school.

  46. Posted by Eric Sparks on October 19, 2013 at 10:25 AM

    Hi Greywolf,
    First of all, like many others have said, your website is a godsend and I truly appreciate the lengths you go to learn more and spread knowledge.

    I recently have been doing my first BHO extractions and have decided I would like to winterize them. I recently read that silicone, like the silicone found on parchment paper, is resistant to polar compounds like alcohol. My question is, in order to guarantee an almost 100% return of my winterized product, would it be safe to let the alcohol mixture evaporate directly on the parchment so I could simply fold and freeze the oil until its the size I would like. I understand non-polar solvents like butane cause swelling and would damage the silicone, but would this be true at all of alcohol? I truly appreciate the help and look forward to your insight.

  47. Posted by jeff on October 15, 2013 at 10:01 AM

    Hey I’m currently winterizing my product with 151 ever clear, filtering and evading under a fan until oil starts to fall out of solution. I then siphon this dark yellow liquid on top and place in a separate container. I’ve evaped all this mystery liquid liquid down and it forms a red hard concentrate that smells like impurities when burned so I’m assuming this is the 49% water I’m using that cannot readily evap and is picking up gross polarities. My main question is when I throw my product in the vac oven around 110-115 under -29.5 hgs its looks glass but eventually starts to nucleate after a couple hours in the vacuum. Could this be from the high % of water that is present in my secondary solvent? How would u suggest I go about keeping my concentrates “glassy”?

  48. Posted by country_strong on October 13, 2013 at 1:05 PM

    Ok so question iso mix of oil added to a saturated solution of NaCl is not removing the
    Chlorophyll. Should i try iso mix with H2O instead? I know they are miscible with each other but if there is oil in the mix shouldn’t it precipitate out of the solute?

  49. This site is packed with Wisdom and Utilized to help ease pain and suffering. God bless you. In Jamaica, the Rastaman at times uses propane termed ‘rocket fuel’. The ‘overstanding’ here is that a pipe is capped and valved at both ends, stuffed with cannabis flowers. Then, commercial propane is introduced at one end, the ‘goo’ flows out the other. Seemingly, this ‘goo’ could be field refined with commercially available ethanol/H2O 5% and frozen with available dry ice, filtered, etc. Also, field work with ‘bit of buds’ and ‘buckets of trim’ from the California fields present the same quandary when cost effectively processing in bulk. Questions. Could you all recommend a design? Our goal is to process barrels of bulk cannabis for distribution of conforming RSO through ministry. Seems, there could be the cost effective solution utilizing these easily available commercial solvents. And, the concrete forming industry utilizes a field vibrator that I’ve always considered attractive if ‘stirring’ is required.

    • You can run propane or butane in a fully enclosed Terpenator design extractor, and is how I would proceed in your position.

      We expect to process about 5 pounds per hour with the latest Mk V design, and there are others out there with competitive designs that hold more.

      Vibration speeds up dissololution, because it keeps the solvent/resin boundary layers refreshed.

  50. Posted by Parker on September 23, 2013 at 8:51 AM

    Hey you guys,
    First off, great work you guys are always doing and thank you for publishing your findings. You’re helping revolutionize the industry keep up the great work. I had a question regarding ethyl alcohol used in winterization. From looking around for trusty online sources of ethyl, I’ve also seen that part of the other 5% contains methyl, the stuff that made those original moonshiners go blind. Depending on the source, it will vary in amounts such as lab-grade; high, in everclear;low. What’s your take on the levels of methyl present in the finished product? And can it be fully purged? Does it evaporate off with the ethyl? Thanks again.
    -Parker

    • The levels of methanol in Everclear 190 proof is minuscule, as it and the ethyl acetate are removed in the foreshot.

      Methanol has a lower boiling point (148.5F) than ethanol (173F) and evaporates away first.

      Methanol is the product of fruit pectin, which is low in the grain that the alcohol was made from to start with. You would get more methanol in your morning orange juice, than the equivalent amount of 190 proof Everclear.

  51. Posted by korupt on September 23, 2013 at 6:16 AM

    I have to ask, if done correctly, which method produces the most pristine extract? My theory is that QWET is the answer here but I’m really not sure.

    Which method, if filtering now would be allowed, produces the most pristine? I’m thinking that the starting method doesn’t matter here since you will filter out most the contaminants. My theory is that if you are to filter you could even go with slow soaking.

    Background for my theories, please correct me if I am wrong:

    The way I understand it is that QWET is one of the methods that pulls the least amount of unwanted products but also slightly less THC than BHO and QWISO.

    ISO has the ability to pull out a lot a lot of unwanted things, but with the QWISO it should be limited.

    Butane pulls out least amount of chlorophyll but can pull out more waxes than both ISO and ethanol.

    • The most pristine extract would be a non polar solvent like propane, butane, pentane, or Hexane, and then winterizing it with ethanol to remove the non polar waxes.

      They are extremely forgiving with regard to undesirable water, water solubles, and polar elements, but do extract non polar plant waxes, so removing those afterwards produces a gorgeous bell clear extract.

      • Posted by korupt on September 24, 2013 at 6:46 AM

        The more I keep reading, the more questions I have..:(

        Questions on brine/hexane wash:
        1: What is considered hot hexane? 69c?
        2: Does hexane temperature matter besides making the oil easier to solve?
        3: How long do you normally let Hexane/brine sit?

        /K

        • 1. Under its boiling point.

          2. Unless you are reflux boiling, warming the hexane just speeds up the process.

          3. We don’t let it sit any longer than it takes to separate into layers.

          • Posted by korupt on September 25, 2013 at 12:29 AM

            Thanks yet again brother.

            Do you guys have like a donation link or something? The fact that you take the time and anwser our question is really one of the things that sets this site so far appart.

          • A couple of folks have been helping me pay for the Mystery Oil experiments, but we have no donation links.

            If you have a specific project that you would like to support with a non tax deductable donation, you can send donations to:

            Skunk Pharm Research
            xxx Project
            3439 NE Sandy Blvd, Box 683
            Portland, Or 97232

          • Posted by korupt on September 26, 2013 at 12:13 AM

            I’ll send it today. You guys should REALLY get a http://flattr.com/ or PayPal account, possibly even add a bitcoin address. You have a different grade of information on your posts that I know people really appreciated.

          • Good idea! Working on this!

  52. Posted by Helping-a-friend-out on September 21, 2013 at 5:11 PM

    Hello,

    First off, thank you so much for all of your efforts for the community!

    Regarding polishing and the use of Syringe Filters, a friend of mine is looking at purchasing a few 0.45u filters but had a few questions.

    First, can you name a preferred filter material for working with Butane? Her filter choices seem to be PVDF (Polyvinylidene Fluoride), PES (Polyethersulfone), MCE (mixed Cellulose Ester), Nylon and PTFE.

    Second, would this choice change if she used Hexane instead of Butane?

    Third, do you know if syringe filters never/occasionally/sometimes/usually/always are of the “Luer taper” variety in terms of fittings to a syringe?

    Forth, can you recommend a syringe by type/material/brand/supplier? The one in your picture appears to be glass–true? Reusable? My friend usually only has a few grams of oil at a time to process so it doesn’t need to be very big.

    Finally, is it preferred to filter by injecting or ejecting oil into/out of the syringe?

    Thanks in advance!

    • Ptfe for both. Draw in syringe then attach and eject through the filter. Ebay or American scientific for glass syringe. Don’t use plastic syringe for either.

      • Posted by stephen d on September 22, 2013 at 9:48 AM

        Got a question, I’m making some BHO from some dark bubble hash, was just wondering if it would even need to be winterized? Or would it have to be the other type of wash for polar solvent extracts (forgot what it’s called, brine wash?) Saw you mention doing this on another thread so I decided to ask, right now I just have a jar of saturated acetone, looks like dark apple juice. Should I winterize or just water wash? Thanks.

        • Not as much plant wax in the hash. If you already have it dissolved in acetone, I would just freeze and filter it.

          • Posted by stephen d on September 24, 2013 at 1:53 PM

            What about taking out the color? I know solvents get darker the more saturated it is but I can tell this stuff is still gonna be darker when it’s dried. I’ve used activated charcoal but that was kind of a pain. Kinda figured it would turn out cleaner looking after dissolving and filtering the solids.

          • Most of the darker elements are polar, so we’ve had the best luck removing them, without losing an inordinate amount to the filter media, by using chromatography resin beads in a column.

          • Posted by stephen d on September 26, 2013 at 8:00 AM

            Man I thought winterizing and water washing well enough was supposed to make it come out looking more pure. I always tend to end up with darker oils no matter how much I do them. So just some ion exchange resins? Could you maybe link me to a place to get the kind you’re using please? I don’t know much about them.

          • I would contact joeoakes@skunkpharmresearch.com for that information.

          • Posted by stephen d on September 26, 2013 at 9:14 AM

            Also is there any benefit doing a hexane/saline wash with bubble hash/non polar solvent extracts or does it really only make a difference in alcohol extracts?

          • Non polar extracts have non polar plant waxes in them, but usually not much polar stuff like chlorophyll, water, alkaloids, etc.

            I’ve used the process to clean up non-polar extracts, that got subsequently contaminated from other sources, but it is generally not necessary.

          • Posted by stephen d on September 27, 2013 at 9:07 AM

            Well yeah I understand that but I’m just not sure what this stuff is in my dish so I didn’t know which way to clean it. Just to be specific what I did was I got some bubblehash and dissolved it in some butane, but part of the way through I just decided to use acetone though, so I poured that in and let the butane evap off, so technically I guess it’s not BHO anyway. But anyway I filtered all the solids in the freezer, everything looked perfectly clear putting it up to the light, no particulates.

            But now that it’s evaporated on the dish, the thinner areas of it the dish are light brown/golden but there are some areas where these brown specs are all bunched up and it makes it look darker in general. Didn’t expect anything else to show up after getting rid of the plant matter from the hash. But I figured maybe a brine wash could work, if whatever it is was soluble in the acetone before it evaporated? Sorry if I’m not being clear enough, first time making anything from bubble hash.

          • What you have is an acetone extraction, so it will have some polar elements in it.

            There ie also the Beers/Lambert effect, by which one layer is clear like stained glass and two layers are almost opaque.

          • Posted by stephen d on October 13, 2013 at 3:33 PM

            Hm, never heard of that. I just decided that I’m just not going to use naphtha anymore, even if it’s more convenient. Not sure what it is, but no matter what I do the stuff comes out dark. Water washing didn’t seem to really change anything either. Would it just be best to redissolve the oil in minimal amount of acetone and wash with a larger portion of fresh naphtha? Would that somehow be better than washing a naphtha/oil solution with water?

          • What it takes to lighten the oil, depends on why it is dark. We lighten oil a shade by filtration to 0.2 microns to remove more fines.

            Brine washing removes water solubles and chlorophyll, with little affect on other dark polar elements like caramelized plant sugars and anthocyanins.

            The best way that we’ve found to remove those polar elements, is is column chromatography. That involves dissolving the oil in a non polar solvent like hexane and passing it through a column of chromatography beads. The beads pass the non polar cannabinoids and retain the polar elements, until those fractions are subsequently washed out using a polar solvent.

          • Posted by stephen d on October 19, 2013 at 9:14 PM

            Alright thanks. I just ordered a separatory funnel and I’ll probably get some .2 micron syringe filters also. But I may get some ion exchange resins if I need to. But since Ill have a sep funnel, if I wanted to dissolve some hash oil in something pretty polar like acetone, and evapped that down and mixed with naphtha, that should yield some pretty clean oil supposedly. But should I put in the effort and wait to have some hexane delivered or do you think with that method the naphtha would work fine?

          • I don’t recommend using naphtha, because it is uncontrolled. It can not only have boiling points from 30C to 200C, but it can contain things like benzene.

          • Posted by stephen d on October 19, 2013 at 9:15 PM

            Sorry I meant to say if I used bubble hash from the start, not oil.

          • Posted by stephen d on October 20, 2013 at 8:30 AM

            Alright I guess I’ll get some hexane or maybe pentane if I can find it to use for that then. But I have already used vm&p naphtha on this bubble hash. It shouldn’t be too big of a deal though should it? Just figured it was fine since that was what a lot of people used for RSO.

          • Varnish Makers and Painters naptha contains different components, depending on manufacturer. I would suggest pulling a MSDS sheet from that manufacturer, and seeing what is in it.

          • Posted by stephen d on October 24, 2013 at 2:01 PM

            I don’t know if I’m not looking hard enough or something, but I can’t seem to find exactly what’s in it. I think I’ll just put it off and order some hexane to do that with. Is there any safe/convenient way to use butane in a separatory funnel though? Probably a dumb question lol. But it could be really convenient for me.

          • You could use butane, if you kept it cold enough. n-Butane boils just under 32F.

      • Posted by Helping-a-friend-out on September 22, 2013 at 1:20 PM

        Very much appreciated, thank you!

  53. Posted by Tallulah on September 20, 2013 at 12:53 PM

    Hi GW et al,
    Would the winterizing and/or cleaning/polishing methods discussed on this forum work with RSO?
    thanks,
    Tallulahgirl

  54. Posted by drizzle on September 18, 2013 at 2:26 AM

    wanted to do the hex/salt wash, having troubles sourcing a supply of hex.
    ever use coleman camp fuel which contains naphtha? might that be suitable? msds say light hydrotreated distillate. what about ronsonol lighter fluid? msds says 95 aliphatic/light naphtha 5 medium aliphatic. are there any other alternative sources i could use or does it have to strictly be a mix of pentane and hexane? is vm&p naphtha like mineral spirits?
    thank you truly for your guidance.

    • Should work just make sure there are no nastiness added to discourage using it

    • Posted by drizzle on September 18, 2013 at 11:02 AM

      Hydrotreated Light Distillate, C
      AS # 68410-97-9, OSHA-500 ppm, 100.0
      This product contains:
      *Cyclohexane, CAS # 110-82-7,
      OSHA-300 ppm, ACGIH-300 ppm
      *Nonane, CAS # 111-84-2, ACGIH-200 ppm
      *Octane, CAS # 111-65-9, OSHA-400 ppm, ACGIH-300 ppm
      *Heptane, CAS # 142-82-5, OSHA-500 ppm, ACGIH-400 ppm
      *Pentane, CAS # 109-66-0, OSHA-1000 ppm, ACGIH-600 ppm
      these are the ingredients for the coleman camp fuel. doesnt seem like enough hex/pent.

      the ronsonol lighter fluid medium naphtha component has hydrocarbons c9-c12. the light component has h/c c5-c10. also has ethylbenzene 0.1-0.2% by weight.
      the “right to know “chem list states there is hexane 2+3 methyl. 2 is 3-4% weight, while 3
      is 3-5%. heptane 2-3% and octane 10-16% weight.

      neither seems enough. im at a loss. i know you said hexane/pentane and light naphtha has 5-6 hydrocarbons(wikipedia). i wanna write off the camp fuel b/c ive never heard anyone mention the other chems listed. however, the ronsonol contains ethylbenzene, a possible carcinogen(not in a severe enough concentration? any seems senseless) and the hex/pent content seems low. which do you think is a better choice.

      ever thought of just making a list of acceptable solvents, with tolerable additives/components and their acceptable percentages? maybe a list of chems to absolutely avoid. hell if you give me the info ill write it up for posting, so that doesnt take your time. something of a guide so people like me dont waste your time with beginner questions. just a matter of time before more of me show up. :)

  55. Posted by itschad on September 17, 2013 at 8:37 AM

    Could I winterize multiple different oils together? I have a bit of some really green wax that tastes great but it’s really soft and really cloudy, and I also have some other stuff that has more of a darker brown color. Anyway they’re both a little too soft for my needs, I was wondering if winterizing would be a good way to clear it up and possibly get it to a bit firmer texture/solid?

  56. Posted by chris on September 16, 2013 at 9:56 PM

    Im a quality not quantity person i use dual solvent extraction to get to my absolute. But i seem to be losing alot of my original yield throughout my winterization process i even rewashed my filters and the filtered again but i lost 33% of weight granted my quality difference is day and night. But i would like to learn a higher yielding process to then clean to a absolute. Give me a name and ill research my self to save the time and so i can personally know the process better, soxhlet? Or any ideas i wouldn’t mind doing a nacl wash to remove chlorophyll. Plus my plant matter still seems to have a decent amount of cannabinoid rich matter still attached i do not wish to remove carboxylic acids

  57. what if…. someone used a 1/4″ plexiglass on a vac chamber and when it imploded it contaminated the bho with glass and plexiglass? Can the bho be broken down enough with iso to separate the contaminants through a filter….? hmmm?

  58. Posted by tanner on September 14, 2013 at 9:25 AM

    Hello
    First off I love your tutorials/ I’m in the processe of making hexane oil. I purchased some laboratory grade hexane off Amazon and had a few questions that I think will help everyone including my self.

    My steps
    Hexane soak> semi purge> ever clear winterization> hot hexane with saturated water wash and separate etc to remove chlorophyll …> final purge with ethanol

    1. If I did the initial extraction with hexane and I have a nice vacuum pump is it necessary to purge the hexane with ethanol on the final purge? Thin film? Do you mean make thin layer with the oil when you purge

    2. What temperature is good to purge ethanol in the oven or a heating plate Temperature for hexane?

    3. Should I still do a water wash to remove the chlorophyll if I did the initial extract with hexane or is the mostly necessary if you started with a polar extract

    4. Im using hash. But didn’t see any ratios. Say 28grams hash so how much hexane, I Used 42 grams hexane is that enough

    5. Is 190 ever-clear ethanol? Or can I go a lot better and what will this change in the end product

    6. Will the quality be better if I winterize my hexane extraction in ever clear? I should use hot ever clear when I do this?

    • Hexane is detectable to under 30 ppm to some folks, and isn’t real easy to purge below those levels without an alcohol wash, or extended vacuum purging.

      We use 115F for the vacuum purge.

      The Hexane extract shouldn’t have water solubles and polar elements, so no brine wash is typically required.

      If the hash was extracted, it was enough, but I typically use up to 10:1 for extracting hash.

      190 proof is ethanol and is what we use.

      Hexane does extract non polar waxes, so winterizing in ethanol will improve the effects.

  59. Posted by kevinf on September 13, 2013 at 9:20 PM

    Hi guys, I am doing a run here with 5xrefined butane..after heat purge on oilslick pad/skillet/vacuum chamber for like 10/hrs..i should have about 3g of bho. After all bubbles are gone and well purged will it be wise to dilute in 2 table spoons of Iso only stuff i can get in mason jar then put in freezer for day or two. Pull out set out in sun for 4 hours/ strain through 3-4 coffee filters then pour back onto oil slick pad and re-water/heat purge tell all iso is gone? is this better then nothing?I just usually 3 hot water baths/heat purge tell bubble are all gone then toss in vacuum chamber/pump tell 25hg and lock in for 4 hours then re heat purge and continue tell purged.. I have hand pump vacuum chamber from extractionexperts.com with a heat lamp and double broiler style and griddle/skillet..

  60. Posted by korupt on September 13, 2013 at 2:10 PM

    Got a quick question on saltwater/hexane wash.

    I was left with some white powder on my lasagna dish after the wash, I assume this is salt. It was clumping together in so i just took a razor and took it out. After that i added some water to my dish and spun it around a bit and then threw it out.

    My question is, are these white powder clumps salt, and if so, why? Did i have to much salt in my solution or was there maybe wrong ratios of saturated saltwater to hexane? Maybe I didn’t bleed it of good enough, even though I thought I was very though.

    Thank you yet again:)

  61. Posted by chris on September 9, 2013 at 9:05 PM

    Is it possible to achieve a honeycomb or wax texture with a absolute in a vac chamber?

  62. 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

  63. Posted by korupt on September 9, 2013 at 3:29 AM

    I have a few questions on the Alcohol/Hexane wash. First is, what is considered hot hexane? Second is does this remove the need to winterize. I mean does this method also clear out the waxes.

    Thanks in advance, you can’t imagine how good this blog has been.

  64. Hey skunkpharm! Was curious about any other ways to dewax your concentrates without a secondary wash, i.e. : using dry ice to freeze your stainless steel extraction tube prior to butane extraction to freeze the solubles, so not extracted in the first place? main concern being terpene retention, and elimination of waxes etc. also, possibly using a 5 micron screen on the end of extraction tube to eliminate extraction of waxes in first place as well? Thank you for any info!

    • Chilling the butane reduces the amount of plant waxes extracted. If you chill the receiving vessel low enough, some of the waxes will also fall out of solution, and you can filter them out.

      You might consider setting the receiving vessel in denatured alcohol and dry ice.

  65. Posted by Dill on September 3, 2013 at 1:41 PM

    Can I winterize using 99% isopropyl instead of ethanol. I have some readily available and would need to order ethanol. Thank you

    • Iso isn’t as polar as Ethanol and doesn’t work as well, but it will remove some of the non polar waxes.

      • Posted by drizzle on September 11, 2013 at 1:15 PM

        hello, i live in canada and ethanol/everclear/access to sci supply store are4 hard to come by. however i have a bottle of hospital hand sanitizer. ingredients are active- ethanol 70%// non-medicinal- purified water, iso alc, glycerin, glyceryl laureate. is this ok or should i just use 99 iso?(im trying to take out the green). thank you in advance.

        • Don’t use hand sanitizer! 99% iso is useable if you heat the extract past the bp of iso. Iso is toxic to consume.

          • Posted by drizzle on September 11, 2013 at 7:16 PM

            so could i do the saline wash with iso? would that be better than freezing it? here is some other info- my extract was made with colibri and i have a vac.
            thank you for helping this dim bulb.

          • I don’t see a reason why not other than it holds onto the green more.

          • Posted by drizzle on September 11, 2013 at 9:14 PM

            and when you say heat past the bp of iso, do you mean cook it off? i was reading about your qwiso process and it doesnt say anything about heating past the bp. it says just to put a fan on it, so could i just vac?

          • Yeah. You can but in a thin film. Its risky if you aren’t testing it to make sure its completely purged.

          • Posted by drizzle on September 11, 2013 at 10:37 PM

            so i foun 99.953% pure anhydrous iso for cleaning electronics, useable?
            and finally, what constitues safe denatured alcohol(marine stove fuel 90-10 mix, or fireplace fuel dont know the mix)? what additives are ok, which should i avoid.

          • The anhydrous iso is safe if used for topical or is completely purged. We use denatured that is just a methyl/ethyl blend.

          • Posted by andre baptista on September 14, 2013 at 9:15 AM

            so the marine stove fuel is what i want with 90% ethanol and 10% methanol? a 95 ethanol to 5 propanol(fireplace fuel) is no good?

            On 13 September 2013 20:59, Skunk Pharm Research LLC wrote:

            > ** > Skunk Pharm Research,LLC commented: “The anhydrous iso is safe if used > for topical or is completely purged. We use denatured that is just a > methyl/ethyl blend.”

          • You can extract with it, but need to be rigorous about purging. Does it also show any embittering agents on the MSDS.

          • Posted by andre baptista on September 14, 2013 at 9:45 AM

            i dont think so, but maybe i missed something. this is for the fire place fuel. trying to get it for the marine alcohol….

            On 14 September 2013 09:20, Skunk Pharm Research LLC wrote:

            > ** > Skunk Pharm Research,LLC commented: “You can extract with it, but need > to be rigorous about purging. Does it also show any embittering agents on > the MSDS.” >

          • Posted by andre baptista on September 14, 2013 at 10:35 AM

            hers the marine alc. again from what i read there isnt any. it does say the mix is 85-15.

            On 14 September 2013 09:45, andre baptista wrote:

            > i dont think so, but maybe i missed something. > this is for the fire place fuel. trying to get it for the marine > alcohol…. > > > > On 14 September 2013 09:20, Skunk Pharm Research LLC comment-reply@wordpress.com> wrote: > >> ** >> Skunk Pharm Research,LLC commented: “You can extract with it, but need >> to be rigorous about purging. Does it also show any embittering agents on >> the MSDS.” >>

          • 85/15% will work, if there aren’t other agents present, which should be listed on the MSDS.

          • Posted by andre baptista on September 15, 2013 at 8:03 AM

            i freakin hate canada sometimes. love the healthcare though….. so blue it is. thank you for your guidance. it is greatly appreciated.keep my email, if you come to canada i got your medz, they might be be blue but…hey if you come up maaybe you can bring me some hexane!

            On 15 September 2013 06:30, Skunk Pharm Research LLC wrote:

            > ** > Skunk Pharm Research,LLC commented: “85/15% will work, if there aren’t > other agents present, which should be listed on the MSDS.” > Respond to this comment by replying above this line > New comment on *Skunk Pharm Research LLC > * > > > *Skunk Pharm Research,LLC* commentedon Polishing > extracts . > > in response to *andre baptista*: > > hers the marine alc. again from what i read there isnt any. it does say > the mix is 85-15.

          • Alas, my daughter doesn’t have as long as I planned, so doesn’t look like we will make it further than Port Angeles. A pity too, because BC is so beautiful this time of year.

          • Posted by andre baptista on September 15, 2013 at 6:35 PM

            well, im sincerely sorry to hear about your daughter. all you can do is make the most of the time you do have together and not worry about the time that is lost. obviously im joking about the hexane, but if you do come up this way and dont contact me i will be mad that you would have prevented me from showing you my gratitude for the assistance you have provided me.

          • Thanks for the good thoughts bro! We’re having a good time, even if this is the last day!

          • Posted by andre baptista on September 16, 2013 at 12:08 PM

            this is probably the wrong area for this but… heres another question for you. my mom just had cervical/ovarian cancer surgery 4 months ago or so. there doesnt seem to be any growth or spread. however they think she has had it for a while, just wasnt detected. she doesnt take anything for the cancer, other than a japanese mushroom called reishi(ever heard of it?). they wanted to give her the chemo spa treatment, but she doesnt want the side effects. what sort of medication should i use? she also has diabetes and high blood pressure and is taking the usual suspects to combat. the diabetes and high bp are under relative control. my parents(mainly my father, who doesnt have any known health problems ) are under the impression they can eat and act(lack of physical activity or the promotion of) however and…presto magico! pop a pill and everything is hunky dory. her eye sight, hearing and mobility have all gotten worse. there has been a steady increase of dependance on pills just to maintain proper health, as opposed to curing these ailments which is the direction i’d like to head. She doesnt like the taste of cannabis, but if i can slip it to her and it can help, and she doeasnt have to rely on pills i am down to do it. so back to my original question, what direction should i take/advice can you give in regards to mmj medicating and heer health problems.

            On 15 September 2013 08:03, andre baptista wrote:

            > i freakin hate canada sometimes. love the healthcare though….. > so blue it is. thank you for your guidance. it is greatly appreciated.keep > my email, if you come to canada i got your medz, they might be be blue > but…hey if you come up maaybe you can bring me some hexane! > > > On 15 September 2013 06:30, Skunk Pharm Research LLC comment-reply@wordpress.com> wrote: > >> ** >> Skunk Pharm Research,LLC commented: “85/15% will work, if there aren’t >> other agents present, which should be listed on the MSDS.” >> Respond to this comment by replying above this line >> New comment on *Skunk Pharm Research LLC >> * >> >> >> *Skunk Pharm Research,LLC* commentedon Polishing >> extracts . >> >> in response to *andre baptista*: >> >> hers the marine alc. again from what i read there isnt any. it does say >> the mix is 85-15.

          • Not a doctor, not qualified to offer medical advice, but cannabis has been shown to aid diabetes and high bp patients, as well as being an anti tumor agent, so if it was my body, that is what I would be trying.

            Suggest that you try the Holy Shit sublingual formula, if she likes cinnamon, or consider a cannacap if she doesn’t.

            If you can find a balanced CBD strain like Cannatonic or Hawaiian Bubble Gift, it will be easier to build up her tolerance, without discombobulating her.

            Good luck!

            GW

          • Posted by andre baptista on September 14, 2013 at 4:20 PM

            the marine fuel is blue too.

            On 14 September 2013 10:35, andre baptista wrote:

            > hers the marine alc. again from what i read there isnt any. it does say > the > mix is 85-15. > > > On 14 September 2013 09:45, andre baptista baptista.andrealberto@gmail.com> wrote: > >> i dont think so, but maybe i missed something. >> this is for the fire place fuel. trying to get it for the marine >> alcohol…. >> >> >> >> On 14 September 2013 09:20, Skunk Pharm Research LLC > comment-reply@wordpress.com> wrote: >> >>> ** >>> Skunk Pharm Research,LLC commented: “You can extract with it, but >>> need to be rigorous about purging. Does it also show any embittering agents >>> on the MSDS.” >>>

          • Alcohol isn’t blue, so that it at least has a dye added.

  66. Posted by doobie on August 31, 2013 at 2:28 PM

    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?

    • Sounds like fines. I pack the column with two wadded coffee filters, and finish up with two coffee filters, which the screens hold in place. The screens just hold them in place, and they do all the work.

  67. Posted by cory on August 30, 2013 at 10:15 AM

    When winterizing, after waxes/lipids have precipitated in the ethanol solution do I have keep it at freezer temperatures while filtering to prevent it from redissolving, or can I do this all at room temp? Can I pour more room temp ethanol over the filter when finished to try to reclaim some oil that may otherwise be lost to the filter?

  68. First of all thank you for publishing all this great information … it is so needed!!!
    My question is about ‘winterizing’/producing an ‘Absolute’.
    I have followed your procedure and extracted with Butane, redissolved-filtered with 190 proof grain alcohol and put in the 0f temperature freezer for 2 days … and was amazed at all the waxes etc. that were removed.

    I would like to produce an absolute … without the butane/hexane step, if possible. I grow my own medicine, organically …. and as I have just harvested (today) what I plan on doing in a week, is reducing my bud, to high purity kief (very little plant material). If I extract the kief with 192 proof ethanol, filter the THC laced ethanol into a container and into the freezer for 2 days (to possibly further eliminate contaminants) then re-filter into the evaporation dish and if necessary, into some sunlight to deal with any hint of green that might have been picked up.

    After evaporation would this then be considered an absolute, and if not, is there any way to get an absolute without using a petroleum product?

    Thank you in advance … I have other questions/comments, but will leave them in the appropriate sections.

    I hope to be be able to meet you all this September at the alcohol extraction and/or Alchemy classes…. if there is room for me.

    • Technically, an absolute is extracted using a non polar solvent and the non polar waxes then extracted, using a polar solvent, so the answer is no.

      As far as a quality extraction goes, a polar extraction using ethanol doesn’t pick up that many (non polar) plant waxes in the first place, so winterization is mostly a waste of time.

      What ethanol does pick up, is polar elements like chlorophyll and water solubles, making temperature control during extraction a critical element. If you do your extractions at -18C/0F, and limit soak times, you can also side step the water solubles and chlorophyll, and produce a pristine end product.

      I have you on the roster for both classes in September, which are at 170% of the optimum 10 student capacity at this point. There are no more Alcohol classes this year after September, and only one more Alchemy class, so you slid in under the wire.

      See you in class!

      GW

      • Posted by Steve Weglein on August 24, 2013 at 8:29 AM

        Ok, that makes sense.  Soaking (extracting) kief in ethanol at 0c could be a fairly slow process ….. how long would you suggest ….. and would one still follow with a second wash/soak …. a 3rd water extraction (it is surprising how much is returned on the water wash when leaf/bud are extracted)?? My harvest is now in day 6 drying …. perhaps I’ll begin the kiefing process in the next couple of days …. I expect to have between 100 and 200 grams (1-1.5 lbs of dry flowers) of kief to work with/learn from.  I’m thinking that I will likely end up with 70% weight in oil … is that overly optimistic?

        As to polishing ….. I have noticed that when I extract in Ethanol, leave the filtrate in the sun for several hours (to deal with chlorophyll), and evaporate the ethanol with low temps (110f) and a fan in a very thin film, after the ethanol is evaporated, there is still a small puddle of whitish liquid left on the plate.  I have assumed that it is water which evaporates at a higher temperature and may contain a high concentration of unwanted plant materials. In the past I have just evaporated this as well with more time, not more heat.  It occurs to me that this water puddle, may have a high concentration of those water solubles, and very little of the psychoactive/medicinal properties, and perhaps not be evaporated with the rest.

        Would you think it might improve the overall quality of the oleoresin, if before the water evaporates, I suck this remaining liquid up into a syringe (or other suction device), and remove it?

        thank you as always …. and looking forward to meeting you’all and having an  extremely interesting (and lucky) Friday the 13th Alcohol extraction class in about 3 weeks !!!

        >________________________________ > From: Skunk Pharm Research LLC >To: sweglein@yahoo.com >Sent: Saturday, August 24, 2013 6:22 AM >Subject: [New comment] Polishing extracts > > > > WordPress.com >Skunk Pharm Research,LLC commented: “Technically, an absolute is extracted using a non polar solvent and the non polar waxes then extracted, using a polar solvent, so the answer is no. As far as a quality extraction goes, a polar extraction using ethanol doesn’t pick up that many (non polar” >

        • I would soak the kif the first time until I got as much as it will dissolve, and then wash the filtrate one more time to get the rest.

          70% may be a tad optomistic, depending on the dry sieve, but you are in the ball park.

          The beige liquid is mostly water. You can continue to suck it off and if you stick the tray in the cooler for a bit, the oil will solidify and you can pour the water off.

  69. Posted by HoldTheMustard on August 15, 2013 at 10:36 PM

    Hey SF, you guys are doing great stuff and thanks for sharing everything with us. I was a heavy blunt smoker and have a few ounces of shelled roaches, after trying a 28g iso run I’ve ended up with a thick, ashtray smelling oil that has seemed to pull a lot of tar/carbon through the extraction, I filtered 3 times and winterized with little difference in the taste. I would like a little more info on your roach reclaim method because after weeks of researching, you guys seem to be the only ones that have successfully tried this. Any help would be greatly appreciated!

    • I dissolved the roach material in denatured alcohol, added equal parts of hexane and flushed it with water in a seperatory funnel, until the water ran clear. I still had to filter the material through activated charcoal to get rid of the remaining taste.

  70. Posted by Hashcat on August 14, 2013 at 1:11 AM

    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!

    • 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.

      • Posted by Ryan on August 31, 2013 at 1:05 AM

        Why does hexane needed to be used? Salting out using isopropyl alcohol is very common.

        • Hexane, or other non polar solvent is necessary to be able to brine wash, because a polar solvent like isopropyl absorbs water.

        • Posted by Ryan on September 3, 2013 at 4:29 PM

          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?

          • 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.

          • Posted by Ryan on September 4, 2013 at 12:00 PM

            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?

          • 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.

  71. Posted by hashcat on August 12, 2013 at 10:57 AM

    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.

    • 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

  72. Posted by Hands on August 8, 2013 at 3:01 PM

    I didnt know which thread to post this but this one seems most appropriate. The subject is “Centrifuge Extraction”. Most recently in the SFO area there is a new product in the clubs being called “The Clear”, they claim it is solvent free and that they start with a concentrated extract (I assume kief given “solvent free” although water is commonly dismissed as such by the average consumer). It comes in a variety of colors that are dependent upon the strain from which it was extracted, orange-red-gold-yellow but all completely translucent. Texture described to be as a pure decarboxylated oil becomes in its sticky, dabb-able form. All information and thoughts on forums found on this subject to date are all conceptual theories leading to essentially “purification of a solute extracted with a solvent”, but this also was just released to the public recently so Im not surprised whoever cracked the code hasn’t released any info yet. With my newly researched understanding of the centrifuge I have been trying to wrap my brain around how this would work without even water as a solvent, could it be as simple as loading some 100-120u kief into the test tubes and turning it on? What a dream come true that would be… Ok, any thoughts on this would most appreciated and as always… You Guys Rock!

    • Sounds like centrifugal chromatography. Joe does chromatography to remove the dark colors, but just uses gravity and a simple packed column of chromatography beads.

      By flushing it through the column in a non polar solvent like hexane, the polar elements are removed. Different mixtures of hexane and other polar solvents are then passed through the column, to selectively pull off the different fractions. The final full polar flush clears the column for the next run.

  73. Posted by TorrenG on August 8, 2013 at 8:55 AM

    Hey skunk pharm, this information is wonderful. I am about to attempt to make some oil for the first time (iso), and would like to know what you suggest about my tek. Here is my procedure so far:

    Grind trim/bud to a fine consistency, put in a ziplock bag and let it freeze in a box of dry ice along with the iso I will be using (99%)

    take a few 2 liters and cut the tops off right after the bottleneck, turn said tops upsidedown and put them in the bottles to act as funnels. put a reusable coffee filter in the funnel

    QUICKLY (as in have all necessary parts ready) put the product into the reusable filter and pour the freezing iso through it at about 1L:1/2oz. wash the product a second time (mulling over separating the runs as to preserve quality), then dump the product back into its ziplock, cut the corner, and squeeze the rest of the iso out.

    filter the slurry through 5 coffee filters

    reduce iso/oil mix to make it easier to work with

    use joe’s hexane/brine tek to clean it up.

    dissolve hexane/oil into ethyl alcohol and wash it

    purge the rest of the alcohol using a preheated double boiler.

    any tips? anything I missed?

    thanks again

    • I recommend not breaking up the material any more than necessary, when doing a polar extraction. The fewer broken leaf boundaries, the less chlorophyll pickup.

      The rest of your technique looks solid.

      The pour through funnel technique that you describe is an alternate technique also works well. You stop pouring the alcohol through it when the color starts to change.

  74. Posted by Johnny Redthumb on August 7, 2013 at 3:34 PM

    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?

    • 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.

  75. Posted by scott on August 2, 2013 at 7:43 AM

    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?

  76. Posted by Hands on July 27, 2013 at 4:17 PM

    Interesting Experiment using Subcritical Water:

    Started with 5 g’s of kief that came from a 1lb. dry ice sieve at 8 mins. in a 145micron 1500G drum which resulted in 54.6 g’s.
    Goal was to see if at all possible I could extract a clean powerful oil with subcritical water not having to ever expose to any other solvents besides water at different temps.

    Took distilled water, heated on double broil in pyrex cup to to around 120-130F, added 5 gs of kief massaged into mud with small amount of ice water, dropped into water in pyrex and let sit maintaining 120-130F for 1 hr. Removed from heat, set in freezer until water was frozen yet still liquid, strained through coffee filter, cooled down again, strained through #1 Bubble bag. Took water (Extremely Golden) and evaporated in pyrex dish at 100-110F down to a very light amber/blonde liquid that still had 50-100% water in it. I then took that pan and put it on reptile heating pad that maintains with a few degrees of 80F. Let this sit for a couple hrs until the left result was an eye candy amber-ish blonde transparent what looked to be the same as winterized BHO looks. Let sit at room temp for a night and it turned to exactly what pristine shatter looks/feels like. I was excited but when it was smoked it bubbles like those charcoal snake fireworks, expanding 3 times its size into a charcoal like shell that then slowly burns away as you smoke it. My thoughts are maybe the cellulose being extracted in the warmed water is being infused the oils, and if this is the case then is there any possible way to use water to re-rinse at maybe a cold temp to get the cellulose out?

    Break Down:
    Ratio: 5 g’s kief in 2 cups 130 degree water for 1 hr yielded almost 2gs “oil”?
    Looks: Amazing, like perfect high quality translucent shatter.
    Smells: Like high quality bubble hash with a skunk floral essence, much like if not better than the bubble hash I have made from the same Cheese trim but twinge of something I cant pin-point.
    Smokes: strange bubble mentioned above^^^ aside from that the taste is very yummy hash flavor with the definite presence of the strain it came from.
    Affects: Surprisingly cerebral melting down in the nervous system I could feel it in my muscles strongly as well. Similar effects to smoking the 2% cream off the top, not near as clean though I could still feel a slight cloudy feeling probably from the cellulose.

    Thoughts are appreciated. Bless

    • Wow, good experiment! Haven’t tried it before, but my thoughts are:

      Cellulose is insoluble in water, so it won’t be in solution.

      Carboxylic acid fizzes when decarboxylated by heat and you probably still have some water in it. That may be the source of our snakes.

      • Posted by Hands on August 2, 2013 at 1:42 PM

        Thanks for your thoughts! So maybe the “cloudy” feeling was just the heavy concentration of CBD? Also I did take the oil out, put it in a smaller bowl to dry further and after about a day it turned so hard it was a task to chip the small amount out with a razor blade. Then as soon as it touched my fingers it would soften a little like a soft “wax”. Tried to dab it and it would melt to a black coating on the crystal, which makes me wonder about its purity unless somehow you could over decarboxylate to a point where the structure would change dramatically enough not to dab? Thanks for your time…

        • Posted by Hands on August 2, 2013 at 2:50 PM

          Another thing I should say is I cant find anyone who has used Subcritical Water (SW) for THC extraction, I have searched all over the net, asked a few valued resources and still nothing has come up. Im a total novice in chemistry but from the research done on SW I have read it seems valid, I just wonder if I might be defying chemical law somehow or could this really be a valid method to extract oil?

          • The perfume and essential oil industry uses steam to extract the lighter terpenes, but usually have to resort to a solvent for a molecule as heavy as a diterpene cannabinoid. That might be a place to search, but so far I haven’t seen information suggesting that they use that process.

        • If it hardened up, it was still in carboxylic acid form.

          I’ve seen oil forgotten for several days in a hot oil bath and which was pretty dense at ambient temperature, but wasn’t desiccated and was still dabable.

          It was however intensely sedative and left me with a morning hangover.

    • Posted by oliver twist trees on August 25, 2013 at 12:14 AM

      I place my oil in a jar with rice and put it on a seedlings mat for 24hrs to remove water. Heating it in a pot with oil works too but is harder to control temp. If it still crackels i found freezing then placing back in rice jar works. I’m not sure how but I’ve had great success.

  77. Posted by The Butes on July 14, 2013 at 12:09 AM

    Hello Skunk Pharm, I want to start off by thanking you and your team for pushing the envelope to where this medicine can go and openly sharing your experiences. So I got an idear, watch out. In efforts to make the most pristine meds in the most efficient manner I was wondering if it were possible to do the entire extraction in butane as it has such a low boiling point and purges easily. If I froze a thermos, butane, and material, do the initial extraction through a filter then throw it back in the freezer will the undesirables still coagulate or winterize out? I believe redissolving in another solvent is may be beneficial as it breaks the bond between the thc and the butane making it purge easier, I could be wrong. But these extra solvents such as ethanol or methanol have higher boiling points than I want to bring my temperatures to and definitely does not make the purge easier. Methanol evaporates at 148F, Ethanol 173F according to wiki and I want to try to keep temps under 120F. Is there anyway to get to an absolute without the extra solvent? Thanks in advance. Hats off to you guys.

    • No, it is the non polar waxes that we are trying to get rid of.

      Winterizing is extracting with a non polar solvent like butane and then redissolving in a polar solvent before freezing and subsequently filtering to remove the plant waxes that fall out of solution.

      Sticking an open container of butane back in the freezer is a bad idea, as it can easily explode from the freezers electrical. The butane will pool and flow somewhat like water to the low spots. Even if you don’t have a leak in the door seal, when you open the door, the butane will flow out and run down where the running motor is.

      I know of no other way to make an absolute, because it is defined as above, but you can keep the temperatures down by just using a vacuum to purge it off. At -29.5″ Hg, Ethanol boils closer to 90F.

    • You could dilute acetone with 5% h20 and winterize. It has a higher vapor pressure and will purge at room temp over time. The water will then present the same problem with temp. You could skip the water but it won’t be as effective.

      • Posted by The Butes on July 14, 2013 at 10:24 AM

        Thanks Skunk Pharm for your quick response. Would you still consider this dangerous if the container was completely sealed? My thoughts are I could do a wash for as long as I want (well a whole lot longer than iso or ethanol) without pulling through chlorophyll too. I feel I could also conserve a lot of butane with this method. I mean why not, people put cans of butane in the freezer all the time. There has to be a safe airtight container for this, even a mason jar. I would just blast it but I have kief to process and I feel a wash would be best. After fully extracting I could then winterize with the ethanol to grab the non polars. If your thoughts are an ethanol wash instead would you add an additional solvent to winterize? Peace and Pot!

        • There are sealed containers that you could safely put in a freezer with butane in them, but a thermos isn’t one of them.

          You could extend the thermos soak time with additional insulation and placing in a styrofoam cooler, without having to resort to a freezer as well.

          Ethanol is another good way to extract kif with long soaks, but not with the plant material still present.

          Hexane will work well for long soaks and doesn’t require freezing.

      • Posted by korupt on September 26, 2013 at 2:17 AM

        Since acetone is more readily available where I live I was interested in this. Do we have any guidelines on acetone winterization or is it just 95%Acetone + 5% water and in to the freezer?

        Best regards
        korupt

        • Ostensibly, acetone doesn’t work quite as well as ethanol for winterizing, because it has a 20.7 dielectric constant, while ethanol has a 24.3.

          Acetone is also a known mutagen and teratogen, making purging that much more critical.

    • Posted by Dilly on July 25, 2013 at 7:08 AM

      THC does not “bond” to the butane. Butane already has all of its “bonds” taken up. I think grey wolf went over this way lower on the page.

  78. Posted by chris on July 12, 2013 at 11:12 PM

    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?

    • 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.

      • Posted by The Butes on July 14, 2013 at 9:43 AM

        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.

      • Posted by chris on July 18, 2013 at 12:45 AM

        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

        • Posted by chris on July 18, 2013 at 12:49 AM

          And to the butes i used butane and extracted chlorophyll then used iso to refine it.

        • What are you going to make out of it Chris? Will it be vaporized or used orally?

          • Posted by chris on July 22, 2013 at 12:23 AM

            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

  79. Posted by Hands on July 11, 2013 at 6:24 PM

    First off, thanks so much for all the extremely informative blogs on this site!
    Right now I am in the process of finding an easy way to break down concentrates I have available to a pure shatter without using a vac oven. The reading that I have done here and there of your blogs has lead me to the following winterizing experiments. The best I have available to my immediate use is 99% Iso, I would have used ethanol if available but I figured for an initial experiment the iso would do. So, using your instructions on I have done the following:

    - 14.4 gs of high quality small buds mix of cheese strains, followed your instructions doing three washes (first two with ISO, third with Water). Strained, filtered, evaporated, re-dissolved in iso and set to winterize.

    - Dry Ice sieved 14.4 of the same bud ^ which resulted in 1.8 g of pristine kief which was then rinsed in iso for 3-4 mins, filtered and set to winterize.

    - 2 g’s of kief made by Dry Ice sieved trim of same bud ^ , washed in iso for 3-4 mins and set to winterize.

    - 2 g’s of purged BHO (butane free) simply dissolved in iso and in set to winterize.

    At this point now I have 6 jars in the freezer at around 24-32 hrs waiting for the final filtering. My end goal in this is to see what ratios I get from the differently extracted concentrates as well as the varying qualities and compare them to see what might be the best way to get the right balance of quality and quantity that I am looking for.

    So I would have some questions for you but instead I will leave you room to share your thoughts of my experiments before I venture further. Thanks so much for your time and consideration to create and maintain this website…. Blessings to you all there at SkunkPharm!

    • Looks like a righteous experiment to me bro, and look forward to seeing your results!

      • Posted by Hands on July 27, 2013 at 3:18 PM

        Results:

        Exp. 1> 14.4g Iso wash -
        1st: (wasnt as prepared as I should have been when combining solvent in the material and it ended up in the solvent for more like 45-50 sec.) Yielded 1.7g of some mostly clear darkish/amber oil.

        2nd: Yielded .8g of some oil with darker and slightly amber hue.

        3rd, water wash: I suspect that I over dried this pull, while still in the water it dried to a hard shatter like form. When I tried to dissolve in the iso even after slight heat couldnt get it to break back down. Did my best and tried to winterize but after filtering resulted in daaark red waxy mess getting stuck in the filter. Pulled this out and set it aside in freezer.

        Exp. 2> 2g BHO Polish – Yielded 1.3g of amazing golden translucent oil which originally was in a blonde stiff peanut butter like texture. Was told it was purged with short exposures of sun of the period of a month or more.

        Exp. 3> 1.8g Bud Kief wash/polsih – Yielded .9/1.0 bouncing …. oil was very similar to “Exp. 1, 1st” results yet mush less dark.

        Exp. 4> 2g Trim Kief wash/polish – Yielded .07/.08 bouncing …. looked the same as exp. 3 results in color and translucency.

        Notes:
        “Exp. 1″ was done following all your instructions. The other 3 experiments I skipped the one step of evaporating the alcohol down the first time before winterization in consideration of the concentration of the starting material. Looking back now I think that I will include that step for extractions with kief. Im hoping it would make a larger difference in the translucency of end product between using bud or kief as starting material although there is a definite difference as the results stands.

        Exp. 4 material came from a 8 minute tumble in a 1500 drum on 1lb. of trim from high quality cheese strains with 2-3lbs of dry ice. This resulted in 54.6gs of kief.

        Comparing Exp.’s 2 to 4 while letting both sit puddled at oil state in pyrex for 3-4 days at room temp. I have noticed a dramatic difference at which the rate in they are stiffening to shatter texture. Exp. 4 is surprisingly stiffening at 4 times the rate as the exp. 2 and is almost like glass while 2 has a 1/4 thick hardening film on top of the puddle. Maybe more impurities making it harden faster?

        I will leave it at that for now, hope you find this interesting and that all you there are well and happy… simply, me

  80. Posted by MB on July 7, 2013 at 4:51 PM

    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.

  81. Posted by pdxtracts on June 26, 2013 at 7:42 PM

    Hey guys! I would love to polish to a blonde, crumbly end product from such extractions that are dark and waxy, or just not drying up in my vac oven. I have zero problems making any other finish beautifully (thanks to this site’s incredible info) I use a closed extractor if that helps. Are hexane and brine washes the way to go ? And should I procure a soxhlet if I go this route.

    • Polishing with a non polar solvent and brine, will remove water solubles and chlorophyll, but won’t removed caramelized plant sugars.

      You can remove most of those using activated charcoal, but you also lose some of the cannabinoids and have to filter out the charcoal.

      The best solution so far appears to be a column of chromatography resins that grab the polar elements and passes the cannabinoids. Joe has done enough work to prove the process and is working out the details and methods, but isn’t ready to publish yet.

  82. Posted by Hydrostatic on June 20, 2013 at 11:16 PM

    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.

    • 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

    • Posted by Hydrostatic on June 21, 2013 at 5:05 PM

      If I vacuum purge @ 115F will it pull out the R152a? Or do I have to bring it down to -29.5 ?

  83. Posted by Jp on June 19, 2013 at 5:24 PM

    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?

    • 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.

      • Posted by Hands on July 11, 2013 at 6:58 PM

        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?

  84. Posted by c on June 18, 2013 at 6:18 PM

    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?

  85. Posted by scott zcollett on June 17, 2013 at 8:23 AM

    i am winterizing and it is taking a long time to completely redisolve. Does ethanol have a eutectic point, i put 60 g in that i needed to clean up further and it has been setting at 115 for 5 hours and still isnt redissolved.

    Ps im using shine that wasn’t quite 190.

    Tnx

    • You either need to stir a lot or raise the temperature of the alcohol to get the oil to dissolve. It doesn’t readily dissolve at low temperatures.

      It will mix at any ratio with the oil, so just add enough for the consistency oil that you want. For winterizing, we use about a 10:1 ratio

  86. Posted by Johnnyzxc on June 11, 2013 at 6:31 AM

    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.

  87. Vac purge it

  88. Posted by C4h10 on June 6, 2013 at 1:25 PM

    Hello again, This might not be the right place for this question but I’ve heard a lot of talk lately of “solventless extracts” and I was wondering how this is being accomplished? Here is an example http://www.clearconcentrates.com/#!concentrates/c1anq .

    • Posted by C4h10 on June 6, 2013 at 4:42 PM

      Someone was saying it might be made with a process called fractional distillation. If you have any info on this I would love to know more about it. Thanks for all your help this site is a great place for info!

      • Sorry, losing continuity, what might be made by fractional distillation?

        • Posted by C4h10 on June 10, 2013 at 2:36 PM

          Sorry if that was confusing clear concentrates make concentrates but they say their process uses no solvents. The concentrate they make looks like BHO but I don’t know how you would get it to look like that without a solvent. I think the lab you saw on the site was the lab they use for testing to help back up the solvent less claim. I’m just interested on how you could make a BHO like concentrate with out any solvents? Thanks

    • It looks to me like the lab that you referenced is not making solventless extracts, but testing for solvent.

      We use a gas chromatagraph to check for residual solvents, but you can taste and smell the solvents that we use far below levels of concern, so one way you can tell is with your nose and sense of taste.

  89. Posted by connor d on June 5, 2013 at 3:06 PM

    Actually nevermind, that works. Now I’m wondering if it would be ok to use some Isopropyl diluted to 96% to winterize?

    • Good question, and so I ran it by Joe, who says that adding water to about 95 or 96% would add polarity and make it better for winterizing.
      GW

      • Posted by connor d on June 7, 2013 at 10:08 AM

        Ok, thank you. Just one more question though. My naphtha is evaporating pretty slow, I know it’s common to evaporate on a heat source of some kind but does it matter that much how long it’s on the heat source, as long as it’s not too hot? I’ve had it sitting on an electric grill on 150 for at least a few hours a day, but it’s probably not at 150 though anyway, it feels a little too cool to be 150.

        • The longer it on the heat source, the more decarboxylation will occur and more of the THC will be converted to CBN. Did you pull an MSDS sheet for your brand of naphtha to see what the highest boiling point component is and what all it contains?

          • Posted by connor d on June 10, 2013 at 8:36 AM

            Got everything figured out. I forgot how much a good fan can help with evaporation, it’s been a while. My room mate didn’t like the smell so I brought it outside but I didn’t have a fan to use out there til recently and it sped up FAST. Also, the question I mentioned earlier about letting the water and naphtha layer sit in the freezer so I can just decant the naphtha did work. Only a slight emulsion layer that had a minuscule amount of naphtha trapped, so I just thawed it and added a little more again. Sorry I feel like I’ve been wastin your time cuz I’ve been makin it work anyway lol. Gonna go on to the winterizing and carbon wash next. Thanks for you help

          • Your welcome! Yup, a good fan does speed things up.

          • Posted by connor d on June 14, 2013 at 11:22 AM

            One last question promise!! So is there a certain ratio for iso/ethanol:oil? Pretty sure I put in too much oil for the amount of iso I had (8 grams in half a quart jar). The iso turned some kinda dark green that turns yellow when in front of a light, and I can see a lot of swirling action goin on at just room temperature. It turns more of that darker urine kind of color if it sits for a while, then there’s a bunch of milky swirls at the bottom of the jar. Are these the waxes showing since the iso was so saturated? I have twice as much iso in the jar as I did before now though but it’s not like the solution is clear, still cloudy particles.

          • If the oil is loose like alcohol, you have enough. If it is heavy and roily, I would add some more.

            The milky swirls are water. They will go away when you reduce it down.

            I would stick it in the freezer for a couple days at this point and then filter out what falls out.

          • Posted by connor d on June 18, 2013 at 10:54 AM

            Any reason that I’d only have a portion of my oil winterized? Just evaporated last night, and most of it just looks the same as what I first put in the alcohol, but it is smoother for sure. But as it was getting to be almost completely evaporated another milky layer started to form which I know is normal, and I actually poured that into its own tray to evaporate, and it’s lighter colored and forms like silly putty, can stretch it really far and snaps if I pull it fast so this is obviously (more?)winterized. Anyway I didn’t wait 48 hours to filter, because I seemed to get a ton of wax in one filter after waiting around 12 hours maybe, but after another 12 the iso solution didn’t change at all, still looked clear. So should I just try winterizing the darker stuff again or is this some other issue? By the way, I bought 70% iso and dried it a few times with magnesium sulfate then diluted that to 95%.

          • We’ve tried different soak times for winterizing and use 48 hours because we still filter out additional material up to about that point. You may not have removed all the wax.

            The milky layer is a water emulsion. You still have water present.

            Isopropyl isn’t as polar as ethanol or methanol, so doesn’t do as good a job of removing non polar waxes by winterizing.

            I would try again with a longer soak time and using ethanol for best results. You can get 190 proof ethanol shipped to you, if it isn’t available at your location.

          • Posted by connor d on June 27, 2013 at 6:04 AM

            that’s so odd though because the milky layer ended up being a really stretchy puddy like hash with no harshness when smoked so that was winterized of course, but the oil that was starting to form underneath it looked the same as what I started with. dark sticky extract. And now I used acetone like I’ve heard of plenty of reputable people say works, and I hadn’t really seen anything after 48 hours in the freezer. I don’t understand what’s going on lol. This should be soo simple but for some reason either I don’t get all the waxes or none form at all.

          • Winterization is dissolving a non polar extraction in a polar solvent, and dropping the temperature far and long enough for the non polar plant waxes to precipitate out, so that they can be removed by filtration.

            Acetone is polar and will work for winterization, but not as well as Ethanol or even better yet, Methanol.

            It has a diaelectric constant of 20.7, with Isopropyl at 21.8, Ethanol at 24.3, and Methanol at 33.1.

            If you are trying to winterize a polar extraction like propane, butane, Pentane, or Hexane, and not getting any waxes to precipitate out, I would take a look at the temperature. It should be down to -18C/0F for around 48 hours before filtering and it works best with a more polar solvent like Ethanol or Methanol

          • Posted by connor d on June 30, 2013 at 9:00 PM

            Ok, just didn’t know what was happening really, I was doing everything I read to do. So about the methanol, could I use HEET? I guess I could go to lowes and pick up some of their denatured alcohol though.

          • HEET has an unidentified proprietary additive, in addition to the Methanol. http://zenstoves.net/MSDS/MSDSHeet.htm I don’t accept unidentified solvents under any circumstances.

            If you pick up anyone’s denatured, do Google their MSDS sheets, to see what they’ve put in it. Some put embittering agents in, that foul the extraction.

  90. Posted by Johnny Redthumb on June 4, 2013 at 5:48 PM

    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?

    • 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.

      • Posted by c on June 12, 2013 at 2:39 PM

        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.

        • Yes, you can wax oil after winterizing, though it isn’t as easy.

          • Posted by c on June 13, 2013 at 10:19 PM

            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.

          • 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.

    • condensation on your extractor or extraction tube ?

  91. 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

  92. Posted by connor d on June 3, 2013 at 12:13 PM

    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?

  93. Posted by Keith on May 23, 2013 at 2:50 PM

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

    • Winterizing with ethanol or methanol will remove some stuff from Isopropyl, but not much. The best way to clean up and iso extract, is with a non polar solvent like Hexane and a brine wash.

  94. Posted by Jeremy on May 23, 2013 at 4:45 AM

    Thank you Grey Wolf,
    I did not think moonshine would be as clean as ever-clear. Thank you for your time.

  95. Posted by Bkdelux on May 21, 2013 at 7:33 PM

    Man, I just want to say thank you!!! What a wealth of information this is. We’ve been extracting/purging into Pyrex on hot plate with great results but want a cleaner harder outcome. If we purge into Pyrex and then wash with 190 everclear and wash immediately with everclear we can go straight to jar and into freezer for 48 hours? Once we filter back onto clean Pyrex what’s best non-vac purge? Hot plate again at 130? Never purged winterized so how can you tell when fully purged?

    We’ve been using a vaporizer pen with great results and a harder product does very well in our 510 pen with kanger cartomizer.

    Thanks guys!!!

    • If you want a harder product without using vacuum, I would consider placing the alcohol mix in a thin film on a hot plate at about 125F.

      Besides watching bubbles, I tell by taste and smell when the alcohol is gone.

  96. Posted by jameson on May 21, 2013 at 6:19 AM

    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

  97. Posted by Robert on May 17, 2013 at 1:25 PM

    Where’s the resin come from…in a pipe or is it the trichromes>?

  98. Posted by samyaza on May 17, 2013 at 5:08 AM

    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 ?

    • The cannabinoids are not totally insoluble in water, so my guess is that it would mostly make an emulsion.

      • Posted by samyaza on May 19, 2013 at 12:15 AM

        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.

  99. Posted by bob on May 16, 2013 at 4:55 PM

    WHat other solvents do you rreccomend instead of hexane for refining oil with iso and water?

    • Pentane works well too. More expensive and easier to purge, but not as hydrophobic.

      Heptane will work, but is harder to purge due to its longer chain and higher Van der Waal forces.

  100. Posted by Brandon on May 13, 2013 at 7:53 AM

    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

  101. Posted by Bill on May 8, 2013 at 2:17 PM

    Does hexane remove terpenes as does ethanol? And is it true that ethanol removes terpenes? If I was to re dilute the extract in warm hexane and do saline washes as stated above will any terpenes remain? I have proper fume hood and lab glassware to try this method safely. Thank you

    • Terpenes are aromatic Alkene hydrocarbons, soluble in both simple Alkane hydrocarbons like Hexane, as well as a simple Alkane alcohol, like Ethanol. They are all 100% miscible in one another, including alcohol and Hexane.

      The terpenes are mostly lost when evaporating away the solvent, especially the lighter monoterpenes, because they are alcohols, ethers, keytones, aldehydes, esters, and carboxylic acids, with high vapor pressures. They also form azeotropes with the solvent.

      The terpenes are also not 100% insoluble in water, so the saline wash also depletes them. An extract that has undergone a brine wash in Hexane, has little monoterpene flavor left, and tastes mostly like the diterpene cannabinoids.

      The best way that we’ve found to preserve the lighter terpenes, is to do a clean extraction in the first place and vacuum purge away the solvent at low temperature.

  102. Do you think it might be possible to use slightly dilute isopropanol for winterizing? The thought being that iso+water could be adjusted to achieve 3.9 polarity index so it is the same as azeotropic ethanol.

  103. Posted by scottschwake on April 18, 2013 at 2:14 PM

    Hi GW,

    I do a super cold qwiso with dry ice and get amazing results very inexpensive. I use a large stainless salad bowl and a large stainless stew pot. First place a little crushed dry ice in the salad bowl place stew pot on top. Now fill void around stew pot with more dry ice and pile up the sides as high as you can pack it hard. then wrap it with towels. put 18 pints of 99% iso in the pot and let stand until iso turns viscous. I like to wait until it is as thick as motor oil I put a few pieces dry ice straight into the iso to speed this up. Then add 1 lb frozen material and stir up to 5 minutes with a few chunks of dry ice in the mix. Note after 5 mins. in wash no chlorophyll. Then one filtering through cheese cloth to get the course debries then 3 times through commercial coffee filters to get the fine sediment.Then I cook it down in a rice cooker until it stops bubbling. Amazing results every, time leaf and shake turn out clear reddish great tasting very potent oil every time. anyone else doing anything like this?

    Thanks

  104. Posted by ketabyte on April 16, 2013 at 11:48 PM

    My first winterization:

    I ran my bubble into a pyrex pie dish that was sitting in a hot water bath.

    I then poured my everclear into the pie dish then set in freezer.

    I know I should have let it sit longer but I noticed a mishap.

    I purged the tane in the hot water bath too long and let it dry, then added the everclear. MISTAKE

    What I should have done was blast into a pyrex measuring cup, added the ethanol while the tane was purging, stirred ALOT gently, then stuck to freeze overnight.

    What I did was panic, pour out the ethanol (that didnt mix), and scrape my remainder out then, which was almost nothing afterward.

    If I plan to remove said chlorophyll, lipids, fats, etc. What should I blast my tane column into (vessel)?, how much should i allow the tane to purge? whats the lowest grade of ethanol i can use? how much ehtanol should i add?

  105. Posted by Tyler on April 14, 2013 at 4:33 PM

    Hey SPR,
    I slowly heated my extracted matter until it was soft and whip-able. Question: will prolonged heat ruin my extraction? It was over a low heat for a few hours while i waited for it to stop bubbling. Bubbling I understood was the butane evaporating. Am I misunderstanding? I was worried about the effects of prolonged heat so I removed it.

    • When you heat oil to purge the solvents, it also decarboxylates the oil at a slow rate and produces CO2 bubbles. The solvent bubbles are random sized and some are quite large, while the fizzy CO2 bubbbles are small and of uniform size.

      Decarboxylating an oil, makes it softer and more runny, but not necessarily bad for the purpose that it was made. We typically decarboxylate all of our oil for oral application, so that it will pass the blood brain barrier and be orally active at the CB-1 receptors.

      Some of the heat that converts THCA to THC, also converts THC to CBN, a sedative, so a decarboxylated oil is typically more sedative than a shatter.

      We also routinely vaporize decarboxylated absolute amber, but also make some oil especially for vaporization bragging rights. We typically do not decarboxylate that oil, so as to maximize THC content, and minimize CBN.

  106. Posted by joe on April 10, 2013 at 3:40 PM

    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

    • 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.

  107. Posted by Kevin on April 9, 2013 at 8:08 AM

    Hello Skunk Pharm Research, I had a question regarding my bho melting and sticking together to the wax paper it was stored on. I winterized my oil in an attempt to separate the oil from the paper however after the 99% IPA evaporated out today it still has a similar texture as before, is there anything I can do to salvage this oil?

  108. [...] And then clean it with a brine solution. then and only then would it be acceptable to smoke. see http://skunkpharmresearch.com/gettin…ut-afterwards/ for instructions. Reply With [...]

  109. Posted by Jeffrey smith on March 26, 2013 at 9:33 AM

    Ive been experimenting with winterizing my BHO extracts, Which winterizing solvents preserved the best flavor and aroma in your oils out the 3, Hexane, ethanol, and Iso propyl alcohol?

  110. [...] but what if his process was followed by Gray Wolf’s method of “ getting the green out ? http://skunkpharmresearch.com/gettin…ut-afterwards/ Reply With [...]

  111. [...] and then wash away the water solubles and chlorophyll with a brine wash. Check out the procedure at http://skunkpharmresearch.com/gettin…ut-afterwards/. Reply With [...]

  112. Posted by arun on March 14, 2013 at 11:01 PM

    I have extracted green leaves with ethanol. how can i remove the green color in the extract..plx help me for this

    • Some green color can be removed by setting the ethanol and oil mixture in bright sunlight, but if there is very much you will need to dissolve the extraction in a non polar solvent like hexane and wash it with brine.

  113. Posted by johnnyzxc on March 14, 2013 at 12:16 AM

    Do i need to heat the Ethanol first to dissolved the purged BHO? or can i spray the BHO directly into the ethanol and freeze for 12 hours then filter, then purge. i did not purge out all the butane and i can see a seperation of oil and ethanol in my jar. Is this normal?

    • Ostensibly you could spray directly into the alcohol, though I never have.

      If you redissolved the BHO in ethanol, it is normal for the waxes to separate from the alcohol solution.

      • Posted by johnnyzxc on March 24, 2013 at 10:26 PM

        I normally winterize using ethanol and i can see cogulation within 5-6 hours of a deep freeze.

        this time i decided to use 99% ISO when it’s in the freezer i checked after 5 hours and nothing has solidified. will it take alot longer to winterize using 99%iso than ethanol?

        i hope i didn’t mess up my oil =(

    • Posted by Johnnyzxc on March 24, 2013 at 8:44 PM

      I sprayed bho into a measuring cup let some of it purge and then I poured in 99% iso to winterize it. It’s been in a deep freezer for 5 hours already and I don’t see any waxes or solids. I’ve used ethanol before and I would have seen this by now. Did I do something wrong???

  114. Respect as always.

  115. [...] Are we allowed to link to other sites? http://skunkpharmresearch.com/gettin…ut-afterwards/ Reply With [...]

  116. 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!!!

    • 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.

      • 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.

        • 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?

          • 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.

          • 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.

  117. Posted by Walldawg on February 18, 2013 at 7:27 AM

    So i have just started ‘polishing’ some extracts i have been getting and I have a few questions…

    I am having an issue “polishing” my matter… i am working on a small personal scale and i experienced success with nice amber absolute my first two polishes and then i tried to polish another wax and it is looking really good until right at the last second when under vacuum pressure and light light heat from a heating pad it waxed back up… I am using 100% acetone as my solvent and making sure it is fully removed before trying. I have narrowed this down with my understanding to a few possible issues…

    A. Is it the heat? if the heat, i used the same amount in my first two tests and it was successful but i know it can react differently with each matter

    B. is it the solution? is 100% acetone from a supply store different than a lab quality acetone? Should i switch to iso? i couldn’t find ethanol where I live.

    C. Is it the matter: this seems like the most likely to me but it really confuses me because the first two tests i did were a success and the material was worse off and had a visible amount of plant material in it via a blow out (but was a ridiculously good deal). so this reason also confused me because the cleaner golden looking starting concrete matter isn’t cleaning up nicely.

    D. Could it be possible because the second batch of matter that was cleaner looking was bright gold wax so it might be that it has a less amount of plant waxes and undesirables but was actually just whipped and beaten to shit to much by the processor? (it also has a strange taste, harshness, smell {unpolished i am referring to here}} it will affect its ability to turn into an absolute consistency?

    So i guess i want to know on a small scale is it best to do what i am doing or what recommendations safety issues can you advise me of before i try my finished product.

    • My first thought is Botrytis mold causing your issue. Try dissolving and filtering with a 0.45 or 0.22um syringe or vacuum assisted filtration unit. Check compatibility of your plastics beforehand to prevent dissolving them and the membrane. Cellulose nitrate and PTFE membrane are my recommendations.

      Joe

  118. Posted by Lance on February 16, 2013 at 12:27 AM

    How long do the alcohol/hexane, saline/hexane washes normally take to separate fully? I’ve followed all the steps and can’t seem to get the layers to stratify with any ease. Do you recommend doing the alcohol/water/hexane wash first without any salt, and then do another step with just saline and hot hexane? or does it work if they’re combined into one step, with the salt and vinegar at the beginning? Do you usually have to wash the same oil a bunch of times to get it not black? Last thing, what do you think about using Petroleum Ether ACS/ Reagent Grade 30-60 boiling point from pharmco-aaper in place of hexane? its much cheaper. Any recommendations would be very helpful!
    Thank You,
    Lance
    Abstract Extracts

    • If you are having emulsion issues decrease or eliminate the alcohol. I would add a little vinegar to heavily salted water. You still need some interaction between the layers to get stuff to partition. You just need to be able to drain off what you can tell is water soluable. As you decrease salt in the mix you get more alcohol diffusion into the water and then you can bleed that off too. When the alcohol is gone add more salt back to the solution to decrease emulsion and drain off the water. This may take several washes. I use hexane because its not soluble in water or alcohols and is reasonably non hazardous. Pet ether has safety issues that need to be addressed and ether is polar so it is soluble to some degree with water and no doubt soluble in alcohols. Which in this case wouldn’t be desired.

      Joe

      • Posted by Lance on February 18, 2013 at 6:29 PM

        Right on thanks joe! Theres not very much alcohol, most was evaporated off. We did use vinegar with the saltwater, and it did finally seperate but not very well, probably because we used petroleum ether I guess. Thats very confusing to me though because I always knew petroleum ether to be non-polar, it definitely isn’t mixing with a pure water layer. Have you ever seen the books Marijuana Chemistry or Cannabis Alchemy? They both recommend doing this process with petroleum ether…I don’t get it…? Thank you for your help, you guys have obviously put your time in on the subject!!

        Peace,
        Lance

        • Posted by Lance on February 18, 2013 at 6:42 PM

          Sorry one more question. Just curious about the safety issues you mentioned with pet ether, at least anything more than possibly blowing yourself up with fumes. I assume you might me talking health risks, which worries me since I just got 5 gallons to work with :( Thank you again

          Lance

          • I was referring to explosive peroxide crystals that form with ethers. Apparently though the EPA advises that pet ether is not ether and not a peroxide forming solvent. The Lower carbon chains are still soluble or form emulsions. So same fire safety measures and general safety practices. Try high bp varieties like 60-80 for less issues. Happy extracting

            Joe

        • Ethers aren’t all water soluble just those that don’t have many carbons. Ether is a carbon chain that has an oxygen atom connecting it in the middle. That oxygen is polar and is attracted to water. The hydrocarbons all want nothing to do with water. If there’s enough carbons it will form an interface with water if not the carbons get dragged in. The more charged ions (salt) in solution the less pull the water has.

  119. Posted by Jake on February 13, 2013 at 6:49 PM

    For the saline wash, is the hexane necessary? That is, if liquid (warm) oil was introduced to hot salt water, could that be agitated sufficiently to remove chlorophyll? Could the desirables be removed by lowering the temperature to around 0 degree c and filtering out the semisolid oil? Or does chlorophyll precipitate out of solution at low temperatures as well?

    • Oil is slightly miscible, but not nearly enough to wash it without the aid of another solvent. It mostly just clumps together and floats on top, with some forming an emulsion.

      Separating the molecules with a solvent, allows the water molecules access to the water solubles and those things that fall out of the hexane solution.

      Chlorophyll actually isn’t water or hexane soluble, though it is in alcohol and is readily transfered by water as micelle, because the molecule has one polar hydrophylic end and one non polar hydrophobic end.

      GW

      • Posted by marie on March 7, 2013 at 4:45 PM

        I have a question regarding chlorophyll extraction from my bho. I have made bho a number of times with desirable results. This last time didn’t come out so well, it came out pasty with a jade green color. I am assuming that I have chlorophyll in my extract based on my readings. I don’t have a vacuum or anything lab-like at hand, the information you provided is sound but a bit over my head. In reading your answer to Jake’s question, came my own question: would I be able to break down oil with regular 70% isopropyl, evaporate alcohol, then do hot salt water wash to bring extract to desired state and rid it of chlorophyll if indeed that is my problem?

        • Posted by marie on March 7, 2013 at 5:16 PM

          I want to add that the process looked successful, this change in color and consistency took place when I reheated extract over warm water a few days after extracting with butane. Until then the result was an ideal amber color with a glass like consistency. when it warmed up and became gooey I started stirring. Ten minutes later, a thick, green, pasty clump was the ending product. This was a large yield with great starting material so I’m hoping to be able to rescue what I have. Could warming it over the water have resulted in this even though I’m positive none came in contact with it? Thank you for your time and know-how.

          Marie

          • Pretty sure you can save it simply by winterizing it, but if that doesn’t work, we have more tricks.

            We average about 8% loss of the raw oleoresin weight, when we winterize our own indoor strains, but a much greater loss sometimes processing donated outdoor grown material. How was yours grown?

            I didn’t ask for the details of your process, because the Jade paste sounded like a one time thang with no changes in process. Might you tell me more about the material that you are using, and how you are processing it?

        • Pasty Jade green BHO sounds like the presence of plant waxes, water solubles, and some chlorophyll. The slight green tint is usually due to overwashing, or grinding the material too finely using a grinder such as a food processor or coffee grinder, which produces a lot of fines.

          Plant waxes will cause cloudyness, so I would first recommend that you simply winterize the BHO extraction to see where you are at first. That may solve your problem.

          Alas no, there has to be a non polar solvent involved to do a brine wash, so unfortunately that won’t rid you of the chlorophyll and water solubles.

          Without the wax, you may still have a light electric green, but at those low levels it shouldn’t be harsh, so you might check it before processing it further. Processing it further to get rid of the light electric green, will cost you some of your terpenes, including some of the cannabinoids.

          • Posted by Andrew on April 21, 2013 at 10:59 PM

            I’m no expert on bho, having only done a handful of small runs, but I’ve definitely turned a batch of beautiful translucent shatter bho into the kind of dull jade butter described above.
            The bho was made from high grade pollen and the initial end-result clarity was top-notch, so I’m assuming the oil was low in plant fats/chlorophyll.

            The transformation from shatter to paste occurred suddenly after about a week of gently reheating the oil via water bath in preparation for each use (so usually once daily). The oil wasn’t ever intentionally “whipped,” only agitated when pulling out warm stringy dabs.
            Each time after use, when the oil was allowed to cool back to room temp, it would return to shatter, until one day after about a week, pulled it off the water bath and it instantly got cloudy then opaque as it cooled.

            So I can attest to repeated heatings causing buttering up.

            (On second thought, if using warm water baths like this frequently, could the steam from the bath be slowly hitting the oil forming emulsion?)

          • It may have been both the heat and steam. Old dry material doesn’t appear to autobudder as frequently as newer stuff.

  120. Posted by Nathan on February 5, 2013 at 8:14 AM

    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.

    • I got our last batch off e-bay. Before that, some were gifted to us, and Joe had one or two that he dug up somewhere. Several have since been dropped and broken, so I may be off looking again soon.
      GW

      • Posted by Sppete13 on February 17, 2013 at 8:27 PM

        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….

        • 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

  121. Posted by Little Trees on February 4, 2013 at 6:25 PM

    Great guides here. I have a couple questions: Where can I get that vacuum fitting for vac assisted filtering? I tried searching around on some lab equipment supplier sites but couldn’t find what appears to be a very simple setup that you have.

    And when you’re doing larger batches with the ethanol do you use a still for evaporation/recovery?

  122. Posted by dysomniak on January 16, 2013 at 1:28 PM

    So, I have some hexane, a vacuum chamber, and a sep funnel on the way. What I’m planning to do is extract with ETOH, then add HEX and separate. I may also winterize and/or do additional washes with ETOH/H2O/NaCl as needed. (this basic procedure was suggested to me by a chemist friend with quite a bit of experience in this *sort of* thing, but not this *specific* thing)

    I’m wondering if you experts think there’s any value to starting with an NP extraction and then redissolving in ETOH if I’m going to be going through all the rest of that, or if you see any other flaws in my plan.

    • It sounds like you have an understanding of what you would like to do. If you want to do a np extraction before winterizing it should work just fine. You should however review our pages on these subjects to make sure you have picked up all the nuances of each before starting. Good luck and let us know how it goes!

      Joe

      • Posted by dysomniak on January 20, 2013 at 1:00 PM

        Thanks so much for the reply, I’ll make sure I let you know how it goes.

        ” If you want to do a np extraction before winterizing it should work just fine.”

        I imagine it would, I guess I’m mainly just wondering if there is any reason I *should* do an NP first, considering I plan to end up with a hexane solution at the end anyways. In other words, is there any reason NOT to start with an ETOH extraction?

        “You should however review our pages on these subjects to make sure you have picked up all the nuances of each before starting”

        I’m working on it. At the moment “nuance” may be a bit too much to hope for out of me, but I’ve been doing some reading and I think I’m staring to wrap my mind around how this stuff works. If I’m not mistaken in the “Alcohol/Hexane wash” procedure described above the addition of H2O to the ETOH solution creates a microemulsion from which the HEX can readily dissolve the desirable substances?

        • My preference would be to extract with any number of solvents, winterize, decarboxylate, NP, decarb, NP, separatory funnel brine/EtOH/ Hexane wash, then drive the hexane off with EtOH when concentrating your final product.

        • The micro-emulsion helps to draw out charged and polar compounds that may remain in the extract. Some contaminates may be too hydrophobic to be in brine but once they get into the emulsion precipitate. If you vary the salt concentration or start low and move to a high concentration it will be a little more effective.

          Joe

  123. Posted by jakenm on December 15, 2012 at 6:16 PM

    I’m posting this here because I think I could get some good feedback from sfr, but there isn’t a dedicated section on cold water extraction so here goes- Is there a way to limit the pick up of plant waxes in the cold water extraction process? My bubble is to a point lately that it vaporizes almost completely leaving almost no residue, and tastes much like a dab of oil, but also leaves a slight waxy coating on the lips and tongue as some oils do. I’m also considering using your method of winterizing in ethanol to remove those waxes at some point, but would first be interested to know if there is something I can do differently in my cold water process to limit the pickup of plant waxes in the first place

    • Alas, I know the waxy taste of which you speak, but no ideas on how to minimize it with ice water extraction. Almost 100% of our icewater extraction is just an interim step toward oil.

      When I research ice water extraction myself, I find http://www.fullmeltbubble.com/forum/index.php a good resource.

      • Posted by Tyrelle Raymer on December 18, 2012 at 1:21 PM

        So you make oil from bubble? I always wanted to try this. Pass through column?

        • I made all of our oil extraction with ethanol, but you can extract with a column or thermos using butane. You must pay close attention to filtration using a column, less it clog.

          A proud new local Mk III Terpenator owner just ran an experiment extracting dry sieve using a 12″ column, which turned out well, so we will be doing more experimentation in that arena.

  124. Posted by pandawashere on December 15, 2012 at 4:40 AM

    Awesome writeup! Quick idea about a speed winterization… after solution is dissolved in solvent load into paint sprayer (would want it to be new never used for paint…) spray out with N2O as the air source onto a piece of glass. This results in super frozen cannabis resin almost instantaneously

  125. Posted by nate on November 28, 2012 at 8:21 PM

    Please e mail me I have a specific question thanks

  126. 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…

    • 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.

  127. Hey GW,

    When I purge on a hot plate after running thru the extractor with butane, there is a this bottom layer stuck to my pyrex that is white. I scrape with putty knife first and then the last thin layer with a razor blade and it is white. Do you know what this is or why it is turning white close to the pyrex?

  128. Posted by garrett on November 26, 2012 at 2:52 AM

    I have never heard of winterizing nor performed it on my bho…should I be worried about my health with all the non-winterized stuff I have been puffing?
    Do I winterize after I purge?
    Does adding ethanol affect taste or mess with terpenes?
    I appreciate this website immensely, so THANK YOU in advance for all your hard work!

    • Convoluted issue;

      Are the waxes removed by winterization toxic? No.

      Can they be turned into something toxic or carcinogenic if subjected to the pyrolysis of burning! Yes.

      Can they coat your lungs? Yes.

      Will removing them make the oil safe to burn? No, because the cannabinoids can also be converted to carcinogenic substances through incomplete combustion.

      Combusting cannabis oil is not a good idea, so we prefer vaporization, at which point the issue becomes residual wax coating of your lungs, if the waxes are not first removed.

      Winterizing will remove the residual butane as well, when the alcohol is evaporated off. You can skip that first butane purge step. We wash our oil out of the extraction pot with ethanol, and then stick that directly in the freezer for winterization.

      Winterizing with alcohol also reduces some of the lighter mono and Sequiterpenes, when it is purged, but still leaves nice floral undertones.

      We winterize most of our oil and yet when you first open a jar of oil and stick your nose in the opening for a deep sniff, it explodes with floral over and undertones, and with a little practice, you can easily tell what strain it came from, due to its distinct odor profile.

      The raw oleoresin that they are made from, have even more, but you can feel and taste the wax left behind in your lungs and mouth upon exhale. A matter of taste and choice….

      • Correct me if I interpreted that incorrectly, but are you saying that [in my case] after spraying into the pyrex resting above the hot tap water, one doesn’t need to apply a low-heat purge [in my case, i would have no vacuum and have yet to purchase a hot plate] and can instead directly scrape the oil and dissolve in ethanol for the winterization process?

  129. Posted by tilopa88 on November 19, 2012 at 6:26 PM

    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?

    • 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.

  130. I will check with my husband and have him inspect. I have a question about the Appion G5 twin. The gauge on it broke after about 20 runs. It seems to still be working and we use our own gauges. The Appion seems tempermental……. Sometimes it shuts down during our runs. Is there something we can do to preserve this machine and care for it a little better during runs and after runs are completed?

    • The gauges on the Appion are a joke, so I ignore them and use a good compound refrigeration gauge, that goes from 120 psi, down to -30″Hg.

      My first thought is that the Appion has a pressure limit switch, that shuts it down if you exceed its limits. That will happen if you build up excessive pressure, or start drawing liquid.

      I would have to look at your system set up to have any opinions on which it might be.

      As far as taking care of the Appion, beyond following the Appions manual, we no longer try to pull our pots below -22″ with the Appion, instead switching to a two stage pump at that point, to reach -29.5″Hg. The Appion is not only super slow at those vacuum pressures, but it wears out the upper end seals prematurely, because they are running essentially dry of lubricant at those low pressures and butane concentration.

      I had to install one $250 upper end rebuild kit in our unit, shortly after buying it, because I developed our process using it. We have hundreds of hours on it since that rebuild, with no indication that it’s performance is deteriorating.

      The difference between 29.5″Hg and 22″Hg is about 25% of the volume of the pot in vapor, and with a 233:1 ratio between butane gas and liquid, the cost is less than a penny for our largest pot.

  131. Grey Wolf,

    We seem to have problems with the fitting between the colum and the pot leaking. Seems to need to be replaced every 5 runs. Any suggestions?

    • Are you refering to a triclamp connection?

      If so, we haven’t had to replace any of ours in over a hundred runs, so I suspect you have either a mismachined gasket surface, or are not using a compatible gasket material.

      What material is your gasket? We use either Teflon, or Buna N, depending on which one.

      Is the machining on the two mating gasket surfaces smooth and undistorted? Any nicks or gouges?

      GW

  132. Posted by will on October 15, 2012 at 2:16 PM

    I would also be interested to know what that milky white liquid is as it has shown up in several of my isopropanol extractions. I can’t imagine its bad but I’d be interested to know what it is and what causes it to form

  133. Posted by concentrait on October 15, 2012 at 4:20 AM

    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?

    • 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

      • Posted by Sean on November 7, 2012 at 11:59 AM

        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

        • 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

  134. Posted by Rob on October 1, 2012 at 10:26 AM

    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.

    • 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……

      • Posted by Rob on October 1, 2012 at 9:58 PM

        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.

        • 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.

          • Posted by Rob on October 2, 2012 at 8:37 AM

            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.

          • I predict that you will be amazed at what drops out winterizing in ethanol and delighted with the results.

            Good job tinkering!

            GW

          • Posted by Rob on October 2, 2012 at 9:52 PM

            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

          • You’re welcome! Ohmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmm!!!!!!!!!!!!!!1

          • Posted by Rob on October 4, 2012 at 7:56 PM

            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

          • It is if it is decarboxylated as well. Undecarboxylated, it is a stiff resin, that ranges from stiff taffy to hard at room temperature.

          • Posted by Rob on October 4, 2012 at 9:18 PM

            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?

          • 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.

  135. Posted by Liam on September 9, 2012 at 2:37 PM

    So out of the above outlined procedures, which parts need i do to polish my qwiso extractions into an absolute using everclear? Or at least remove some more of the undesirables ive been picking up (relatively little). Also I’m considering making the switch to pure isopropanol for my qwiso extractions, will i need to make any changes to my current method or is there anything i should keep in mind?
    Many thanks to everyone whos contributed this wonderful information to skunk pharm, keep it up!

    • Thanks for your good thoughts!

      An Absolute is made by winterizing a non polar extraction with a polar solvent, to remove the mostly non polar waxes and lipids.

      Isopropyl is a polar solvent, so it doesn’t extract as many of the non polar elements, and technically can never be an Absolute, but can be cleaned up with Ethanol some, by simply re-dissolving the QWISO extract in hot Ethanol and then sticking in the freezer.

      Often you will find that everything won’t re-dissolve in the Ethanol to start with (redish waxes), and after about 48 hours, when you filter it, some more things may drop out. That is because Ethanol is not as aggressive a solvent as Isopropyl is. Isopropyl will strip in 20 seconds, what it takes Ethanol 3 minutes to accomplish.

      The best way to totally clean up a QWISO, is to redissolve in a non polar solvent like Hexane, and water wash it using brine and a separatory funnel, to remove the water solubles and the chlorophyll.

      As far as switching from 99% to pure Isopropanol, I doubt that you will be able to tell the difference in either the process or the end product. There is more water than that still left in the plant material, unless you have it desiccated powder dry, which is counter productive.

      GW

  136. Posted by ExtractorMarc on August 18, 2012 at 1:53 AM

    Thanks for the good info as always guys! I’m just having a tough time visualizing the Alcohol/Hexane wash… Any way to further clarify it or perhaps make a video? I have a gallon of reagent grade n-hexane, and shitloads of food-grade 95% ethanol (as well as iso and a bunch of other good shit, and all the required labware) so I’m really interested in this process to clean up my bho extractions.

    From what I understand, I dissolve my bho in the n-hexane, and then add saturated saline solution to the mix in the sep.funnel, let it stratify, bleed off the saline (which would also contain the impurities, no?), add more saline, rinse lather repeat until no more impurities precipitate with the saline, and then boil off the n-hexane.

    Another thing is that (living in CO) my vacuum desiccator won’t go above ~21-22inHg so I’m guessing I need to purge more and longer as well?

    And would the final product be an absolute or would I still need to winterize it, or should winterization be done before the hexane/saline washes???

    Again, thanks fort the info guys, keep up the AMAZING work!

    • Thanks for your interest and good thoughts!

      Adding videos is on our project list, but we didn’t like the quality of our first attempt, so are approaching it more cautiously this time.

      As we have a full plate wrapping up existing projects like the new skunk lab and Mk II Terpenator, don’t look for any until next year.

      Your understanding is correct; but add “shake well”, after mixing the brine and hexane mixture, and before allowing to stratify.

      Your vacuum gauge is reading relative pressure, but the actual absolute pressure would be the same. If you are using a pump capable of vacuum levels below 29.9″Hg at sea level, it will ostensibly pull the same relative pressure at any elevation.

      The definition of an absolute, is a non-polar extraction, that has been winterized using a polar solvent, to remove the mostly non polar waxes.

      We winterize before washing.

      Peace, GW

  137. Posted by scottie15 on August 17, 2012 at 1:44 PM

    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.

    • 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

  138. Posted by for_science! on August 3, 2012 at 11:53 AM

    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?

    • 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.

  139. Posted by leo on July 2, 2012 at 3:22 PM

    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.

  140. Posted by leo on July 2, 2012 at 3:05 PM

    I have easy access to 99 % iso but not ethanol. can these be used interchangeably ?

  141. Posted by jump117 on July 1, 2012 at 12:43 PM

    Hey Skunk Pharm!

  142. This is very exciting to see done. Thanks SkunlPharm for your reasearch.

  143. Such an informative and knowledged filled site, everyone interested in concentrates need to take a look at this!
    Go skunk pharm go!

    • Thanks for the good thoughts and bon appetite!

      • hey Skunk Pharm, i have a question, i am about to do a hexane wash i am going to wash some qwiso i made but i also will be adding half pound of fresh (just cut down) plant material buds and all,.. my question is can i do my wash, filter it, and as it is still in liquid form pour it into my separatory funnel with salt water and bleed off the water and emulation layer? will it layer up or do i need to add alcohol also? i am going to do the experiment as soon as i get a reply lol ;).. also thank you for all the information you have helped me so much lately

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