Personal size SOP, active, N2 push

Hash and Stuff Extraction
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I’ve been running micro (1-2oz) runs in a passive closed loop for years now. Using powders inline I’ve managed to improve my shatters from orange to yellow to pink and clear. Now I’ve managed to step up my game up to a 1-pound capable system with nitrogen push and active recovery. With all of the professionals on this board I’d really appreciate experienced input on my SOP wherever possible.

Purpose:
Personal 1/2lb runs with terp sugar as product
No need for diamonds, no desire for live terps
Just golden to clear tasty sugar with zero chlorophyll

Equipment:
Small N2 tank with gauge-regulator
–¼ JIC HVAC from regulator to tank vapor in
6-liter green Mastercool solvent tank w 5lbs distilled n-butane
–¼ JIC SS/Teflon from tank liquid out to column top
1/2lb jacketed column (1.5”x3’)
–½” steel wool puck
–fresh dry/desiccated material
–½” steel wool puck
–qualitative filter paper
100-micron SS gasket as filter support
Inline CRC
–Plastic cup filters
–Activated Charcoal T1
–Pure-Flo Perform 6000 (activated bentonite 2.5pH)
Cryo-rated Ball Valve
6” extractor lid w/ 6” spool and 6” base, not jacketed
–¼ JIC HVAC out to vac pump & bleed line, other ¼ JIC SS out to recovery pump
TRS-21 pump w upgraded gaskets
–¼ JIC SS out to Mastercool dryer can
Condensing coil in SS can, with iso/di slurry
–¼ JIC SS/Teflon from condenser out to tank vapor in
Second 6-liter Mastercool recovery tank empty and at full vacuum
handful of dry ice on top of tank

Prep Process:
Single-source organic frosty fluff grown to 50% amber trichs for a heavy stone
Branches hang in dark at 60%RH/65F for 7-14d, no direct fan, dehum only
Buck into 1/2gal Masons and burp until stable at 55-60%RH, seal, use soon as possible
Place jars in desiccator for 1 week before use, drop below 30%RH
(terps hurt my nose/eyes so I don’t want “live”, and dry trichs don’t stick to gloves)
Coarsely crumble handfuls of dry material into column hopper and pack w dowel
Load CRC cup with 25g Bentonite and 10g Charcoal, coffee filter and steel wool puck on top
Put CRC in vacuum chamber on high heat and high vac (<100 microns) for 1 hour
Freeze the solvent tank in a regular freezer (no big freezer, no deep-freeze)
Assemble extractor setup and vacuum
–Close extractor valve on recovery-pump side of system at 0PSI (pump doesn’t like vacuum)
–Continue to vac the extractor and lines down (how deep so as not to lose all the terps?)
Hand purge the nitrogen push line at the tank vapor inlet valve to remove any air

Run Process:
Confirm system under vacuum or vac down and close valve, remove vac, close all other valves and attach purge line where vac was
Fill column jacket with dry ice, set extractor base in SS pot of dry ice, handful on recovery tank, coil in slurry
Open solvent tank vapor valve enough to flow
Slowly open N2 regulator to 45PSI to charge solvent tank
Slowly open solvent liquid valve all the way
Slowly open valve at top of column
Wait 5 minutes for soak time, then slowly crack dump valve to start flow into base
Continue to flow slowly into base until N2 pushes through (fog) or base pressure equalizes
–If N2 fog appears, close valve at top of column, dump valve, solvent tank valves and close regulator
–If base pressure equalizes and liquid stops, slowly open base bleed valve to purge N2 below 20PSI
After all solvent has been transferred and is <25F bleed extractor base down to 0PSI
Remove base from SS pot of dry ice, and turn on base warmer
Slowly open ¼ JIC to recovery pump
Turn on recovery pump
Slowly open recovery tank vapor valve
Monitor base viewport for solvent to evaporate to desired pour volume
Turn off base heater, close all valves, turn off recovery pump
Open base purge valve to vent all pressure
Turn on air circulator fan in preparation to vent fumes
Open triclamp on base and remove bottom spool, rest extractor lip on silicone mat
Remove spool gasket, paper towel the edge to remove any drops of water or condensation
Paper towel the outside of the spool too, then pour into appropriate container for finishing process

Finishing Process (Terp Sugar):
Leave 1lb butane in the base
Pour into an ice-cold Pyrex round container
Set Pyrex into vacuum chamber
Turn heat on low (85F) and allow butane to purge through vent line
When oil is consistency of honey, agitate and/or seed, increase heat to medium (100F) and wait overnight, still no vac
Terp sugar should develop, scrape together and mix, turn heat to low, full vac purge for at least an hour.
Remove product to a sealable glass jar, and sample immediately!

Cleanup Process:
Move purge line from extractor base to column top, vent pressure and residual solvent vapor
Leave system venting through purge line overnight until all equipment is room temperature
Disassemble and clean

??? QUESTIONS ???
Any changes to my hanging, drying and jarring process?
How much bentonite and carbon, in the CRC (if at all) and which on top?
–1, 2 and 3 year old cured “stash grade” nugs stored airtight in mason jars
–1 month old or less, freshly dried, super stinky frosty fluffy stuff
How deep do you vacuum your material column down to, so you don’t lose all flavor?
Can my terp sugar process be improved?

Any other suggestions are highly appreciated.

-Spock

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Sketch

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Thanks for the input. I could dry ice the solvent tank for an hour while the column chills, instead of using the freezer. Less sketchy. Would the solvent then need to be injected through a coil in slurry to get cold enough or is a lab freezer the right move (is there a suggested model, like AccuCold)?

Anything else need improvement?

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I liked the write up. Not trying to criteque so much but I do have a question.

This is your inline dryer for moisture?

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Yes, it’s my dryer. I get my material very dry before packing, so I expect the dryer to do very little, but it’s there as a best practice.

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pretty solid process man! keeping solvent in a reg freezer isn’t the best but I’d be lying if I said I never did it… freezers rated for butane storage are fucking expensive.

small things that probably won’t yield much change to your final product, but -

as deep as possible. you don’t want any air in your system. you won’t sacrifice terps by pulling a full vac on the system. don’t let the vac sit there and suck on it any longer than it needs to, but do get it as close to -29inHg as you can.

vac down, close all valves, remove vac*. disconnecting the vac before closing valves may affect the depth of your vac. assuming your whole system is at a full vac and there are 0 chances of leaks, I guess it’s irrelevant. but, just best practice ime.

case by case, man. there isn’t really a one size fits all for CRC, other than the granulated stuff like CRX/CRY (which does work pretty well, and way less of a pain in the ass than powders). but if you’re using specific medias and ratios, it’s all about your starting material and what exactly you’re trying to remove. no issue with your current T1/bentonite set up.

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@ZizzleB
Doh! I do valve off the vac pump as soon as I’m at full vac and before shutting off the pump. I went back and added that to the post.

Thanks much for the input! :vulcan_salute:

1 Like
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One last run through the micro still to check processes and powder ratios before loading the pounder. Looks like tasty slurpy goodness!
I modified the sugar tek to include a slight whipping of the oil after it sits at low temp for an hour at no vac, plus dropping in a few seed crystals, then low heat overnight until sugar set. Scrape sugar chunks and sauce together to mix, then purge under full vac for at least an hour.

IMG_7495
IMG_74951920×1440 126 KB

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do you have a vacuum gauge? ideally you’d just pull down to your ultimate vacuum, release vac, stir, and repeat. longer single pulls don’t do as much

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Yes, I have a digital micron gauge and can get down to single digits if needed. I’ll try your method of multiple quicker pulls and stirs instead of the hour long pull just sitting.
LL&P
:vulcan_salute:

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Question:
On the recovery side of my setup, because the TRS21 doesn’t support <0PSI, I can’t fully vac all the O2 from my lines and components. Instead of purging N2 off the frozen collection base I think it makes more sense to purge N2 through the recovery pump, condensation coil, and downstream lines, to vent the N2 just before the recovery solvent tank. This would flush out any O2, prime the recovery side of my system with inert N2, and any little bit of butane vapor that might pass through will condense in my slurried coil. My recovery solvent tank has been pumped to vacuum, and I’d rather not vent/purge through the tank to minimize any N2 entry and increased headspace pressure.

Is this logical?

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Do you have a vacuum pump for your vacuum chamber?

I did see you have some sort of electrically powered base warmer? That seems a bit dicey.

As far as CRC powders go, most manufacturers are recommending between 1-4oz of powdered adsorbent or 4-8oz of granular adsorbent per lb of material or 1 oz of crude oil depending on the filter media in question and quality of your input material.

For fresh, high quality material you might only need 1-2 oz of powders or 2-4 oz of granular, where for medium quality you’re looking at 2-3 and 4-6 oz respectively and for older or low quality material you may need as much as 3-4 and 6-8 respectively. All per lb of material.

If you are working with good material using such a blunt adsorbent as Perform6000 is going to impact your aroma and flavor profile, which you said doesn’t matter to you, but if you decide you want to retain the original glory of your material you might want to switch to a blend.

I also didn’t see any mention of what vessel you are using for filtration. Maybe a touch more information regarding that portion of your build would help.

If you want to shoot the shit and get some free filter media visit us at gcffiltration.com or give us a call at (619) 913-2770. You’re definitely on the right track, though.

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Thank you GCF,

I run an Edwards E2M2 on my vacuum chamber and monitor with a digital micron gauge.

Filtration is done with an AFS 2”x6” inline CRC in between my material column and my dump valve. I use 25u paper on top of my 100u screen-gaskets, with one right below the material column and another below the CRC. The AFS CRC uses the drop-in cups with 25u paper molded into the bottoms.

That’s good info on the media amounts. My run gave a nice clear-yellow product using 25g of carbon and 25g bentonite with 165g input, but I think yield could have been better. Next time I’ll reduce the powders by 50% and see if the yield improves while quality maintains.

…and I replaced the base warmer with a warm water pot, and try to keep water temps below 80F to preserve flavors.

:vulcan_salute:

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