Acetone Micro Extraction R&D

Bump.

New gig. Need to figure this out for Rec/METRC in a hydrocarbon lab.

With hemp nobody cares about 10-20g grabbed from here/there/everywhere being extracted and sent off for testing, but under METRC everything needs documented.

I can certainly destroy samples for testing, either internal or external, and document that destruction. Trick is gonna be setting up the micro-extractions in a safe and repeatable fashion.

We’re gonna be using hydrocarbons, probably straight n-butane to start, but machine is spec’ed for 70/30.

The (rather thin) survey from once upon a time (above) suggests that using our extraction solvent as our test solvent is the preferred route…but that glass tube on my dashboard isn’t gonna cut it.

Nor do I really want to reuse the solvent.

Has anyone formalized a micro-butane extraction on their incoming biomass in a regulated environment?

How exactly are you playing/documenting that?

How about screening with a different solvent? (Has it ever led you astray?)

I’d test with the solvent you run with first and foremost. Maybe run a couple other micro extractions with other solvents to see if you can concentrate any nasties that may be present that your normal solvent doesn’t extract so well. More data = more better

Maybe consider something close in properties as your bulk extraction solvent. If you sre using butane/propane maybe try pentane for your incoming biomass extraction.

Maybe create a new item in Metrc called “QC Sample (biomass)” And just manifest to a testing lab per usual

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I’ve proposed a tiny (10gram) CLS with a controlled leak on the “recovery” tank. whereby the “recovered” solvent is actually bled off to atmosphere over an extended period of time. what I haven’t done is contact my 3rd party engineer (just did that) to figure out how we can get that sort of noise past the fire marshal.

what I’d really like is a add-on to the Luna (or any certified rig) that formalized this process for all.

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Adjust and waste after extraction in METRC.

Edit: maybe only testing labs can do this, there’s a dialog box that says “Testing lab use only”.

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yeah, that sounds like a safer option, and certainly an easier one to get past the AHJ should the question ever arise. probably can’t get much closer to butane than pentane as far as “who’s coming for the ride”…but I do worry about the (potential) differences in extraction efficiency if I stray from my production solvent.

pretty sure I can also document destroyed for “in-house QC”…never tried flying the Organoleptics: In House QC? METRC designation, but I do feel it’s an important piece of getting this job done right.

I’m wondering about using a 20lb “recovery” tank for the itty bitty CLS, and then taking the potentially contaminated solvent off-site to power one of these (whoops, I mean; “safely incinerate”).

EDIT: although using river rocks here doesn’t sit well with me… it was just a random example of the concept. I’ve made decent cutting edges by heating river rocks…

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why not just recovery pump your miniscule solvent pool?

blast using a <1in x 1in spool into a 3inch sight collection.

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Because I don’t want to use (potentially) contaminated solvent again.

Lots of small runs pumped/recovered into a 20lb tank that is safely flared off at another location would certainly fit the bill. So long as nobody looked too hard at the “disposal” plan.

Plenty of trs-21s collecting dust that could manage the “recovery for disposal”

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It’s been a while since I was on the METRC user group…but I’m reasonably sure I can take my samples, create an appropriate package, and either manifest it to the third party lab or document that it was analyzed in house.

If they haven’t wrapped their heads around that concept yet, they will need to be educated. I was just hoping to find someone who had already formalized this ritual and had the pipeline documented in metrc friendly terms.

Regulators certainly have no business telling me that I can’t do pilot extractions and test them in house before purchasing or processing a batch/lot.

Nor can they legitimately argue that huffing the product to determine marketability is off the table.

Only that I must track the cannabis that goes in the tube…

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@RogueSky has apparently mulled this over in the past…

Ha!! @cyclopath , I knew you’d suck me into this after we chatted!! :wink: I’m not a chemist… just a dumb engineer, so I can’t speak to the chemicals used, but I did develop a design for a micro extractor a few years ago for the very purpose of sample testing a few grams. We shelved it because we got busy, but was a fun project.

The original one was for butane, but it’s functionally simpler to run ethanol or acetone. The idea was pretty simple. Have a separate cylinder filled with butane (cryo or not), or a liquid of your choice, then do a nitrogen push through the biomass tube and into the collection cup. Provide some light heat to the collection cup and vapor off the solvent to atmosphere. Not much to vent off and it’s not worth the cost for recovery, especially if the solvent could get fouled. There’s obviously more bits to make this work, but the concept is a simple one. As long as it’s used in a controlled environment like a C1D1 or under a flammable fume hood, it’ll fly with the AHJ and it’s covered with the peer review report.

If there is interest, we could pull a system together, but will have to wait until we get through Vegas next week. I’ve always thought there is real value to having a system like this out in the wild and I’m happy to see people poking around the idea.

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lol I think know which lab. They have… billboards, and cheap stinky distillate.

Once upon a time, i used to do micro extractions by stuffing a small copper tube with ~1g of biomass, and injecting canned butane through into a tared 40ml vial. Then i would let the butane evaporate and weigh what remained, and test it. I did all this inside a fume hood.

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This topic intrigues me. I do “micro extraction” of incoming source material by doing like described by other users as “a pinch here a pinch there a pinch everywhere!”. Solvent of choice is Acetone. To me it was:

*Source Material
*Beaker
*Pyrex Dish
*Coffee Filter
*Rubber band
*Hot plate
*Fume Hood
*PPE

After acetone evaporated, oil would get placed inside sample jars and labeled for testing. What’s interesting to me is how sometimes our R&D tests would come clean, but when extracted via closed loop hydrocarbons i have seen a test or two pop up hot for pesticides upon getting final COA. So, reading from some of your guy’s experience it might have been I didn’t use the original solvent of extraction, which in my case is butane.

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Better to do a quick turkey baster sized open blast imo

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Except for the part where I need to document it in metrc, and would prefer to be able to point at a process the AHJ would approve should some bean counter decide to question the hundreds of “micro-extraction for in-house QC” they’ve never encountered before.

Not a necessity, just a preference…

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Would a “micro extraction SOP” work if you’re using the same solvent volumes and weight of source material for the batches being tested? Just deduct the sample weights from batch ID and add to metrc?

I’m sure people have squirted more volumes of Gas in a booth before. Get a 2 x 12 spool and pretend it’s your mol sieve

Aren’t you allowed to take a gram out of every batch as a “QC sample”?

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getting an extract sample large enough to send out for third party testing will likely take 10g, but yeah there should be no problem with taking samples so long as they are documented as such and actually extracted.

assuming they are appropriately documented, and anyone wishes to follow up, I’d like an extraction SOP that doesn’t read as open blasting in the booth.

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