Refine Iso Hash Oil?

Discussion in 'Concentrates & Processing' started by TrichromeFan, Oct 2, 2011.

  1. TrichromeFan

    TrichromeFan Well-Known Farmer

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    Does anybody know if it is possible to refine iso hash oil into a more pure oil, maybe like a honey oil?

    Thanks guys.

    -TF
     
  2. Graywolf

    Graywolf Well-Known Farmer

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    Yes! You can clean it up a little or a lot, depending on how involved you want to get.

    I would start by re-dissolving it in 190 proof ethanol and leave it in the freezer for a couple days before filtering. That will coagulate and clump the waxes, so that they can be removed.

    It will also drop out some of the water solubles, as ethanol is not as aggressive a solvent as ISO.
     
  3. mrdizzle

    mrdizzle Active Farmer

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    theres pretty good thread on another site, absolute amber, from what I understand is, you can clean it up, but it doesnt effect much from the inhaling standpoint
     
  4. TrichromeFan

    TrichromeFan Well-Known Farmer

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    Graywolf,
    Thanks for the response. I assume that you mean everclear 190 proof? Any other sources for 190 proof ethanol? Chemistry supply store? Are the waxes the good part? I assume that you have to evaporate or cook off the ethanol at the end as well. Thanks for the info man.

    Dizzle,
    Hmmm. I googled absolute amber. You dirty devil. You know I like the big booty. Mighty nice of you, but I'm talkin about hash oil:D

    You got a link to that site?

    -TF
     
  5. jump

    jump Farmer

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    Refine is always harder than preventing pollution.

    In addition to winterization, you can use cleaning alcohol solution with activated charcoal.
    This is effective but takes a portion of the good resin together with mud.

    Dissolving the Iso-extract in a non-polar solvent also will leave behind the polar dirt that was extracted by isopropyl.

    Try to dissolve the iso-extract in hexane or petroleum ether, add the salt water, shake, allow to settle and separate the layers,
    collect the upper non-polar layer to evaporate and collect the refined resin.

    I suspect the link is probably not welcome by TOU,
    ask google the full title “Absolute Amber from Banana Silver Ladyboys”
    and/or “Absolute Amber From Sugar_kremlin Ladyboys”.
    Waxes are the useless part.
     
  6. Graywolf

    Graywolf Well-Known Farmer

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    What Jump said! Here is a post I made on getting the green and waxes out.


    Public opinion appears to be split on the salubriousness of including chlorophyll and other plant water solubles in our extracted oils, so this is written not to stir controversy, but specifically for those of ya'll whom do not wish ingredients other than cannabis in your extracts.

    Those whom wish to preserve those ingredients are invited to please ignore this posting, rather that debating whether it is a mistake or even a crime against sweet Mary's natural wholeness.

    In a nutshell, many of those non cannabinoid ingredients came along for the ride because there was water present and they are water soluble. It is easier to use a process that minimizes their extraction in the first place, but what if that is a moot point, because you already have an extraction with excessive non-active ingredients and wish to remove them?

    Next best to a process that doesn't pick up many water soluble ingredients, is one to take them out, so let's talk about a couple processes that we use at skunk pharm:

    If the extraction just needs final polishing, we may simply re-dissolve it in 190 proof (~95.5% azeotropic) ethanol and stick it in the freezer overnight at 0F, for the waxes to coagulate and the excess water solubles to precipitate out.

    We then carefully decant and filter the alcohol mixture, to remove the coagulated waxes, as well as the chlorophyll, and plant alkaloids which precipitated out as sludge in the bottom of the container.

    We routinely use this step to clean up extractions using Isopropyl or Methanol, because they are far more aggressive than ethanol in stripping everything, and much of the non active ingredients fall out when re-dissolved in hot ethanol and subjected to the above step.

    It also works well to remove the minor water solubles picked up in a butane extraction, but has its limitations because alcohol is polar and 190 proof is still almost 5% water.

    As far as filtering, I prefer a 0.45 micron or a 0.2 micron syringe filter, but got good results with a coffee filter until Joe turned us on to syringe filters. We have picked both the syringes and filters up off of E-bay, as well as from our local scientific supply store.

    Now, if we really need to clean up an extraction, we have had good results by 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.

    You can even skip the re-dissolve step, by just mixing the alcohol extraction with the highly non-polar solvent before evaporating it off, and the alcohol will leave with the first water wash, after the non-polar solvent has stolen away sweet Mary's succulent and titillating charms.

    Salt water washing is easy, easier with a separatory funnel, but you can even do it with a few gallon Ziploc bags in pinch, or any number of ways to siphon off, blow off, etc., to achieve that purpose.

    To use a Ziploc bag, simply hang by one corner, and clip off the lower corner to drain, pinching to control flow and shut off point.

    The way we do it is to start out by making four or five liters of saturated salt water in glass (or ceramic) containers, 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.

    The magic trick is that because the saturated salt water readily accepts the alcohol, but no longer has any room for the water solubles due to its salt saturation, they fall out of solution and are filtered off in bottom sludge or left stuck to the sides of the funnel.

    The rest of the magic is just as predictable when you mix the polar solvent holding sweet Mary's charms and the lustful non-polar solvent that covets them deeply, given that because of her own polarity, sweet fickle Mary herself lusts after the new suitor, so participates willingly and with a passion.

    The alcohol and water are left giggling like idiots and the sludge is probably left puzzled.

    To perform the salt water wash of the hexane mixture, simply pour the salt water and hexane into the separatory funnel together in about equal parts and shake well, before allowing the mixture to separate out into layers.

    After carefully bleeding off the bottom layer of water, alcohol, and sludge, we replace the salt water that we bled off and shake up the mixture again to mix well. After bleeding that salt water, et al, again, and repeating the procedure several times, the hexane mixture becomes pristine and bell clear.

    At that point we stop washing and evaporate off the hexane. While we use HPLC grade hexane from the local science store, naphtha will also work for this process.

    To get rid of the hexane, we first evaporating off the visible liquid hexane, and then add 190 proof ethanol to the extracted oil and boil that off. We repeat that procedure several times, until there is no discernible taste or odor of hexane left.

    That means that the remaining hexane is below about 30 ppm, which is (~) our sensory threshold perception level. What does that mean as far as our health means?

    For starters, 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.

    OH MAHGAWD, but do check out at what levels this is so and note that oxygen in a breathing atmosphere greater than 75% pure will kill us dead! Poison is in the dosage, so leave us please keep N-Hexane's potential nature in perspective, which includes never losing sight of it!!!!!!

    Despite our worst terrors, a review of the hexane Material Safety Data Sheet shows that the oral rat LD50: is relatively high at 25000 mg/kg. At that rate it would take about 4.5 pounds to kill 50% of a population of 180 lb men.

    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).

    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 sensory threshold far below the Threshold Limit Value.

    Not an unexpected taste treat, because as many of ya'll know, lighter fluid is in point of fact light naphtha, which is a blend of pentane (5 carbon atom chain) and hexane (6 carbon atom chain).

    Most of skunk pharm oil goes into oral or topical medications, though some is vaporized. Both the oral and the vaporization applications require residual hexane below human discernable (threshold) perception levels, so out of practicality, we standardized on zero perceptible solvent content on all our oils as just a matter of policy.

    Lawrd knows that there are enough people kissing and licking at least some of the more provocative foxes and hunks in our folds all over, that we voted to use the same taste standard for topicals as orals.

    The last issue, is of course residue and color, when using topicals! Besides undesirable taste, and non-active bulk in your extractions, there is the pregnant issue of how much residue they leave behind on the skin and how badly they stain our clothes.

    Yet another reason to take care in extracting and subsequently processing our topicals, despite the ostensible threshold perception standards being lower.

    We could also add that after we have removed the bulk of the non-active ingredients, our oil is more uniform and so our mixing ratios in our menstruums will be more precise and the results more uniform, as a bonus to not leaving a mess on our skin and clothes!
     
  7. squiggly

    squiggly Well-Known Farmer

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    GW--Have u considered using a drying agent like magnesium sulfate or calciumn chloride to remove water? Doing this would allow you to do one water wash, you'd maybe see a better yield. The water washes do affect yield, as the cannabinoids are not completely water-insoluble.

    Let me know if ur ever in the market to hire a chemist :) You've really done your homework.
     
  8. Graywolf

    Graywolf Well-Known Farmer

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    Yes, we sometimes use magnesium sulphate or Dri Rite to dry stuff out.

    Thanks for the insight and offer bro!
     
  9. squiggly

    squiggly Well-Known Farmer

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    re

    No problem dude its always a pleasure to see someone with a respect for the science behind all of this--you don't see alot of that in this field. Thats part of the reason im looking at this as a possible career path post school. Ive got a ton of experience on both sides of the fence. Its really important to me that this industry be legitimized, and i see the first necessary step towards that as being the use and proliferation of scientifically sound and legitimate practices/methodologies.
     
  10. kamdavs

    kamdavs Farmer

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    Qwiso solvent

    What is the best value solvent that is easy to purchase online to use for a quick wash iso coffee press method for trim extraction?

    Http://www.YouTube.com/watch?v=015oFyX5beo


    I'm think of using:

    99% iso

    190 proof ethanol

    Ethanol reagent

    http://www.amazon.com/Pro-99%-Isopr...6M/ref=sr_1_15?ie=UTF8&qid=1319903130&sr=8-15

    http://www.amazon.com/Ethanol-190-P...DO/ref=sr_1_45?ie=UTF8&qid=1319903248&sr=8-45

    http://www.amazon.com/Alcohol-Reage...3IQ6/ref=sr_1_4?ie=UTF8&qid=1319903425&sr=8-4
     
  11. budboy299

    budboy299 Active Farmer

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    Graywolf....I was wondering about a RO housing and cartridge to run my winterized bho though.
    I took the BHO and mixed it with Iso...and put it in the freezer.

    As I have an extra RO housing and 1 micron filter....what do you think of the cleansing rate if I ran it through that? I do have a vacuum pump that I can pull a slight vacuum. But as the vessel is designed to withstand municipal water pressure...probably best to increase the pressure on the other end.


    As I am always delighted with your insights into the extraction processes, any thoughts on this would be appreciated. If it works to any extent I will post pics in a week or so. -BB
     
  12. squiggly

    squiggly Well-Known Farmer

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    The reagent grade is the best. Reagent grade means meant for use in chemical reactions (i.e., it is to be used as a reagent). This means that it is chemically pure, about 99.9% Ethanol is also almost completely non toxic, but keep in mind that it will pull out many unwanted substances and it is miscible with water.
     
  13. kamdavs

    kamdavs Farmer

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    Re agent

    What are your thoughts on reusing the ethanol solvent with new trim material after the first wash? I was wondering how many washes could be done using the same ethanol solvent before it goes through the coffee filter.
     
  14. TrichromeFan

    TrichromeFan Well-Known Farmer

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    squiggly,
    where would you suggest picking up reagent grade Ethanol?

    Thanks,

    -TF
     
  15. squiggly

    squiggly Well-Known Farmer

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    Im not sure what limitations there are to obtain it. I know its a huge pain for me to get it as a student and im 25 so the age isnt an issue. However the stigma of college drinking may be why ive got so many roadblocks. Any supplier should have it, anything that says 100% should be reagent grade for the most part, but the extra verbage gives you an assurance this is the case. As far as reusing the solvent, eventually it will become saturated, and its more likely to fill up with crap than desirables. Ethanol is not the best solvent to be using here. Imo it should be used to purge other solvents only--a job it is perfect for.
     
  16. Graywolf

    Graywolf Well-Known Farmer

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    1 micron vacuum filtration should work for filtering the waxes out after winterizing.

    If you want to take out mold and bacteria, you need to get down to 0.2 micons.
     
  17. 51R50G

    51R50G New Farmer

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    Im surprised this hasnt been mentioned, and if it has i passed right over and i apologize!!!

    But due to iso being a polar solvent, it obviously has the ability to dissolve the polar compounds...

    So they will be in the final oil, regardless of the quality of the filtration, some will have already dissolved into the solution and will pass right on through.

    Now the trick with oils made from polar solvents, is if they are redissolved into a non polar solvent, only the non polar compounds will dissolve, while the polar compounds will remain suspended, but not dissolved into the new solvent.

    Then, if you take, or make something like a separatory funnel, and pour in the new solent mix, and pour in water, and shake. The water will then pull out the polar compounds from the solvent. Then you let the solution separate (the water will "settle" at the bottom, where the drain valve is) then you drain out the water until it is just the solvent mixture left, and repeat until the water is clean after shaking.

    Then purge the solvent (i prefer to use hexane for this, as its non-polar and easily kept as a liquid, while also being easily purged) and what you have is a nice refined clean oil!!!!!
     
  18. Graywolf

    Graywolf Well-Known Farmer

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    Try:

    http://www.thcfarmer.com/forums/f60/getting-green-waxes-out-afterwards-35029/?highlight=green

    For how I typically do that.
     
  19. 51R50G

    51R50G New Farmer

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    Yes I've tried that method, well not the full method... but parts of it haha. However I am close enough to a science supply co with cheap hexane, and I have a separatory funnel already as it is. This process takes all of 10 minutes when done correctly, and it will remove the water soluble compounds no questions asked!

    Though hexane usually isn't cheap or easily accessed by people, so I would understand why no one does this

    But I like to keep it more simple for the water wash, and I don't mind the excess waxes so I don't bother processing them out haha. Your process is quite extreme though
     
  20. Graywolf

    Graywolf Well-Known Farmer

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    Good point that extracting with a non polar solvent cuts to the chase, but not to forget that the longer carbon chain alkane hexane, doesn't purge gracefully and additional stips may be required.