RSO purification and techniques

Nugbender

Active Member
Think I got the rona and am currently in quarantine so thought I might as well make some RSO to pass by time and boost the immunity.

Spending the last couple of days reading past previous posts and looks like Isopropyl Alcohol 99% (IPA) - USP-NF is what I will be going with.

I am wondering about how to properly purge as much ISO out of the extraction as possible and have yet to see much on vacuum pump times and purging techniques.

Also looking into picking up a vacuum pump and making a DIY container, was thinking of a 32 oz glass mason jar but after the purge it will be some what difficult to remove after the purge.

I'm looking for cheap DIY vacuum chambers, I have about a 4 ounces of flower and 4 ounces of trim with small buds i'm looking to turn into RSO in multiple batches as these are multiple genetics and this would also help me refine and improve on my process as I have not made RSO in a very very long time.

Items ill be using:
- Laser thermometer
- Freezer
- Glass Jars for soaking
- Isopropyl Alcohol 99% (IPA) - USP-NF
- PPE ; gloves and glasses
- Fan
- Carbon filter; will be purging in a small unused tent in doors with the windows open

Process:
- Freeze material and ISO 1 hour before use
- Crush but not turn the flower into powder
- Immediately place in milk nut bag (if there is a better micron size bag to use feel free to recommend it, I do have bubble bags somewhere but they are in storage and have to search for them)
- Place bag into pyrex or 32 oz wide mouth mason jar depending on the batch size
- Soak material with ISO immediately pulled from the freezer and set a timer for 20-30 seconds
- Vacuum purge material (Don't have the equipment for this yet as I am still looking into it also not sure how long to vacuum purge this for?)


Questions:
- If I get particulates that escape the milk nut bag what would be the best way to filter this out?
- What micron bag works best? (I do have bubble bags but will need to find where they are)
- Where can I find a DIY cheap vacuum purge set up?
- How long do I purge for and what do I look for as a final product?
- Does ISO remove the chlorophyl with a short 20-30 sec saturation from dried flower and trim? If so, what are the best ways to remove this? Just leave it in the sun for a few hours, a day?
 

Boatguy

Well-Known Member
 

Nugbender

Active Member

I've been going through that user guide and process as well
 

bez420

Well-Known Member
I've been told that sunbathing the green ISO or ethanol wash will only change the color of the chlorophyll, not remove it. Although when I refroze it after hours in the sun for many hours down to -15f and let it drip in the freezer through a 3-5 micron glass filtered funnel. A nice bit of brown material was left behind that didn't come out through the first frozen funnel drip. However the dabs still taste of chlorophyll.

So Apparently the best way to keep your RSO from ever getting the chlorophyll. Is to do the extraction in a smaller deepfreeze and dry ice at least down to -60f. In my experience it was very hard to get a larger deepfreeze that cold. Much less keep it that cold very long. Dry ice kept melting on me. When I used a smaller deepfreeze I was able to keep it at -80f for quite awhile with not to much dry ice.

Also, I don't think you'll be able to vacuum purge that liquid. I think you gotta get most the liquid evaporated first before vacuuming. At least I do.
 

Fadedawg

Well-Known Member


C-55 Chlorophyll is green because of the magnesium atom in the tail, and is turned into brown Pheophytin by removing that atom using UV light.

Chlorophyll is also polar because of the magnesium atom and becomes less so when deprotonated by removing it.

Winterization is a process by which a non-polar resin is dissolved into a polar solvent and then the temperature is dropped until the solution becomes super saturated and reaches its "dew point" for that resin, so that the less polar material precipitates out of solution.

A polar solvent will hold more polar chlorophyll than it will less polar pheophytin, so some drops out during winterization. Some is the key word, and the best way I've found to deal with chlorophyll, is to not extract it in the first place.

To do that I drop the extraction temperature below -50C using either dry ice or LN2. That allows a longer wash while minimizing dissolving the l molecules longer than the C-22 cannabinoids that we are targeting, like C-40 carotene and C-55 chlorophyll and pheophytin.
 

blueberrymilkshake

Well-Known Member
So all you do is just let it sit out and its good to go? How do you check residuals?
Yep. I don't check. I just let it dry completely before touching it. The biggest batch I've made took almost two weeks to dry, that's the downside. If you scrape it up before it's dry, I've found it never totally dries and definitely has residuals because it's harsh.
 

Nugbender

Active Member


C-55 Chlorophyll is green because of the magnesium atom in the tail, and is turned into brown Pheophytin by removing that atom using UV light.

Chlorophyll is also polar because of the magnesium atom and becomes less so when deprotonated by removing it.

Winterization is a process by which a non-polar resin is dissolved into a polar solvent and then the temperature is dropped until the solution becomes super saturated and reaches its "dew point" for that resin, so that the less polar material precipitates out of solution.

A polar solvent will hold more polar chlorophyll than it will less polar pheophytin, so some drops out during winterization. Some is the key word, and the best way I've found to deal with chlorophyll, is to not extract it in the first place.

To do that I drop the extraction temperature below -50C using either dry ice or LN2. That allows a longer wash while minimizing dissolving the l molecules longer than the C-22 cannabinoids that we are targeting, like C-40 carotene and C-55 chlorophyll and pheophytin.
At what point are you adding the dry ice? Before and during the wash?
 

Fadedawg

Well-Known Member
I freeze my material in a -18C/0F freezer and put the dry ice into the alcohol to cool it down before and during extraction.

With LPG I run it through heat exchangers that are either in an alcohol/dry ice bath, or through a counter flow heat exchanger with LN2 on the cold side.
 
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