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Single solvent winterization (with Pictures)

Discussion in 'Concentrates' started by jdee, Jan 4, 2014.

  1. jdee

    jdee Well-Known Member

    Messages:
    219
    Location:
    Canada
    Finally got around to trying winterizing and wanted to share. Living in Canada and not having access to Everclear 190 I thought my only option was IPA. Recently I learned Canadian Tire caries BioFlame ethanol http://www.recochem.com/en/products..._living/item/bio_flamesuptm_sup_ethanol_fuel/ you can find the MSDS here http://64.26.129.203/_profiles/_msds/14-414.pdf it's 95% ethanol 5% isoproply alcohol and nothing else, making it suitable for winterizing. However you do lose terpenes with an ethanol/iso purge because of the higher (relative to butane) boiling point.

    I wanted to dewax/winterize but preserve as much flavor as possible, so a single solvent winterization seemed perfect. Only problem is you need to keep your butane in a liquid state at atmospheric pressure, temperatures of -18c/0f are recommended. People in warmer climates buy dry ice for this, but I live in Canada and it's cold enough to keep butane liquid outdoors, so I did just that.

    I kept the butane in the freezer and used dried buds that once packed in the glass extractor were put in the freezer with the 50ml beaker. It seems when you winterize you want 10ml for every 1g of oil and since my 7g glass extractor usually puts out 1.5g of oil I figure as the final volume in my beaker around 15ml would be good. Covered it and left it out for a day. Here is the result after pouring out the liquid butane without using any type of filter because the wax is so cold its frozen to the bottom and isnt going anywhere.

    [​IMG]

    After this I did my usual cold boil vac purge 115f @ -29.5hg to preserve the maximum terpenes. Final result pictured here.

    [​IMG]

    The oil on the dabber is reclaim from regular oil, and on the end of the dabber is small piece of non winterized oil
    on the parchment is the single solvent winterized cold boil purged oil.

    amount used: 7g (indica, which usually makes a darker oil than sativa)

    weight of beaker with the wax: 30g
    weight of beaker after cleaning: 29.35g
    amount dewaxed: 0.65g

    weight of dewaxed oil: 0.7g


    Usually I yield 20% so 1.4g, I guess this test shows that half of that weight is useless filler junk like epicuticular plant waxes.

    Is it worth the 50% loss in yield? well, it tastes amazing. I suspect it's in part because when I take a dab it vaporizes instantly giving a rush of flavor, rather than a usual dab that is 50% wax that vaporizes slightly slower and definitely tastes less pronounced. It should certainly be easier to make eliquid mixes in this state as well, slightly warming the oil and mixing it with some propylene glycol, some users are having no issues with mixtures as high as 60% oil for their e-cigs, using just pg.

    That was fun, what if I wanna do it again? well it looks like I have to either
    -wait until it gets cold enough
    -do a 2 step process, butane extraction / ethanol winterization (at the expense of terpenes)
    -buy some dry ice (I prefer to reduce the amount of consumables required)
    -purchase an industrial freezer capable of temperatures anywhere from -20c to -85c from http://www.krackeler.com/products/1969-Refrigerators-Freezers-Equipment/15623-ScienTemp-Freezers.htm (seems a bit much for the -85c model that I want) or if that one isn't explosion proof than this one http://ontarioovens.com/85_17industrialfreezers.aspx

    With this sweet freezer I could also keep my butane at -70c and according to gray wolf this is the temp he extracts at and it doesn't even require winterizing because it barely pulls any waxes at those temps, or I could purchase dry ice and prevent it from sublimating thanks to the -85c temps. Never thought I would be considering industrial freezers in my quest for perfect extracts but here I am. That's all, have a great day!
  2. kingtut106

    kingtut106 Well-Known Member

    Messages:
    237
    Location:
    'MERICA
    Nice process and thanks for sharing. I had one question about using a vac chamber with heat to assist in evaporating out the everclear (post freezing). Is 115 F too high, I thought ethanol boiled at room temp when you are at full vac (http://tables4ethanol.webs.com/boilingpoint.htm) ? Just thought the mixture might explode in the vac when you go to open the chamber.

    How long does it take you to evap the everclear for your amounts used?
  3. weedemon

    weedemon enthusiast

    Messages:
    2,712
    Location:
    Ontario, Canada
    super post @jdee ! thanks so much for sharing. days that cold in my neck of the woods are kind of rare, but we do see em from time to time. I totally wanna do the open dish soak style extraction using butane someday :) I expect the yield to go way up. i usually see about a 12% extraction when I do em.
  4. jdee

    jdee Well-Known Member

    Messages:
    219
    Location:
    Canada
    Alternate approach...

    Liked the results, don't wanna spend 4k+ on an explosion proof -85c freezer, or purchase dry ice for each run (minimum $65 order),
    Freezers are supposed to be -18c, what about safety. People winterize with ethanol in the freezer all the time, except it's liquid at room temp unlike butane, and doesn't evaporate the same. Butane is heavier than air so falls.

    http://www.mathesongas.com/pdfs/products/Lower-(LEL)-&-Upper-(UEL)-Explosive-Limits-.pdf
    butane lower explosive limit 1.8%
    ethanol lower explosive limit 3.3%

    Made a double boiler out of 2 beakers, except the larger one filled with propylene glycol pre chilled to whatever the temp of the freezer is (melting point of pg -59c). The double beaker chiller goes inside a sealed container. Blasted using pre chilled butane as it picks up less waxes. After 24hrs around 40% liquid butane evaped into the sealed container. Waxes not forming larger grains as before, only slight finer grains. Only 0.25g worth. Either the temp was not cold enough or the plants had less waxes or the duration was too short (was evaping too quickly with the freezer temps to go longer than 24hrs). Opening the container and blowing you can see the butane vapor that pooled at the bottom escaping. This doesn't seem 'safe' unless you have a pressure rated vessel to contain the evaporating butane.

    When I did it first time was around -27c outside, colder is better. Next up refrigerated immersion probes, capable of temps as low as -100c, ethanol has a melting point of -114c, no need to buy dry ice each time.
    [​IMG]
  5. Bouldorado

    Bouldorado Well-Known Member

    Messages:
    929
    Location:
    CO
    I might be a little confused by the first post, but do you blast directly into the beaker and winterize with the butane that was used for the initial extraction?
  6. jdee

    jdee Well-Known Member

    Messages:
    219
    Location:
    Canada
    Yep, blasting direct from a packed glass extractor prechilled butane into a prechilled beaker.

    It's super cold again (-26c) so had to try again. This time I wanted to stop extracting at exactly the amount of solvent needed to dewax (in this case 10:1 solvent to oil ratio). Expecting around 1.5g output I stopped at 20ml and 12hrs later it was down to 8ml due to evaporation. Normally people use a whole can for an ounce (300ml) so for 7g 75ml would make sense, except I only did 20ml, because the first time I overfilled it and found it difficult to remove the excess without increasing the temps too much as it needs to stay really cold. Rotating the beaker and tilting it is a slow way of removing excess solvent.

    7g in, stopped at 20ml out, after 12hrs at between -20c to -26c here is what it looks like

    [​IMG]

    after pouring it out onto pyrex without a filter before scraping to purge

    [​IMG]

    end result
    wax removed 0.8g
    dewaxed oil 0.6g
    Should be noted there was a bit more left to extract in the tube since I stopped blasting at 20ml in the first beaker, that I blasted into another beaker that actually completely evaporated (probably because it was a larger beaker and the liquid was more shallow), so no dewaxing happened, and it was a really small amount.

    [​IMG]

    It's very very thin oil, trying to pickup a dab is challenging as it rather just melt and spread everywhere it's so damn thin. So a 20% yield becomes 8.5% after further refinement. What is this magical wax I'm removing, it smells great, unlike the oil the smell is strong. Tried a dab of the oil, same as last time, a cleaner more pronounced taste, yet smoother allowing you to take bigger dabs. I had to take a dab of the wax just to see what I'm removing. I was expecting it to be harsh, but actually it was quite flavorful and was only harsh if vaped at too high a temp. Since I took a dab before trying the pure oil-less plant wax, it's hard to say if it added anything, but I feel like there was something removed from the oil that you may not necessarily want removed, some terpenes for sure. It seems like it's possible to overdo the winterizing, or that single solvent using butane is not ideal for preserving as much terpenes as possible.
    Last edited: Jan 21, 2014
    Fulvic, havealight101 and 2clicker like this.

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