Butane in the terps

Heyo I’ve come across a problem where the regulations in my state are pretty strict about butane in any concentrate form and my vape pens are failing.

When we create our Liquid Live Resin pens, our tests fail after the Liquid Live crude is recombined with terps.
We do send it (the crude after decarb) out for testing prior to the recombination which it shows having NQL/ ND of Butane or any solvent for that matter.

Then our vapes after being filled are failing for butane at around 54 PPB.
ya my state is dumb with its ppm/ppb but I cant change that, though I have been trying.

For our decarb process, we use a casacade vac oven set to 85 C pulling vac down to 12.7 tor while having a cold trap to capture the terps ( -50 cascade Chiller/ Maxtrap 105) this goes for about 3-5 days depending on the batch size.

What i am assuming is happening (mind you my company has no money to test the terps to see if they are the culprit ) is that in the cold trap as the crude is decarbing and off gassing, leftover butane is turning into a liquid and being “traped” in the terps.
My terps are kept a room temp and we do agitate them with a stir bar

( I honestly dont know why they agitate the terps before adding them to distillate, this was set up here before I arrived in this lab, its a questions I’ve been meaning to look up as well).

So my cannabis sleuths, what do we think is the problem/ solution?

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This problem is something I had for a while, and I know this doesn’t help because it’s a extra cost but I called summit research and they had a machine that separated the terps and the butane laden sauces. I haven’t had a problem since and I can toll out and refine there as well really quick. Also all the color is removed. I know it doesn’t help knowing other hardware can be bought to solve this but you are looking at a couple molecules that are trapped and won’t come out as easily.

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Other things can get caught in the cold trap - yeah? But you can still off-gas what’s trapped in the trap at lower temperatures, if you wanted.

I also heard you can do this with a centrifuge - although I have never tried that. I always just went with agitation at room temperature. But that’s just me.

Also - at the PPB level - make sure that where you are mixing and filling your carts have separate air than where everything else is happening. I know some people do silly things like prop doors open and such.

Solvents can settle in places that you least expect it - where your LEL detector isn’t noticing them but they are still there and then they contaminate your other stuff.

If they don’t want to test their raw materials - then they can’t be mad about failures. Or they can - but they shouldn’t be. Garbage in Garbage out.

Doing some tests now, will help you know just how much is present - and that will help you determine how much still needs to be removed.

And if you find that your terps don’t have any solvent in them - then you know its cross contamination from your facility air and you can fix that instead. :wink:

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Yeah, there is definitely detectable butane throughout our facility. Going outside to get a “blank” makes that quite clear.

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Lots of good advice here, where are you at that requires such low levels of residual solvents?

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I shall try the centrifuge! any idea with parameters for temp? id set it to 35 C to see if it works.
I did get cleared to test 2 of our 30 strains of terps.

For clarity, before our terps are mixed in with our distillate/Liquid Live Resin, it is spun on a hot plate with the temp off and done for 15 mins before we add it to the hot ( around 70 C) distillate that is also on a second hot plate (set to 70 C ) with a stir rod spinning.
this mixture is spun for 15 mins at 70 C. We check the weight of it after we combine, and then again after it mixes/ homogenizes to see if we lost terps due to the heat. Thankfully we have notice no lost terps so far.
My failure rate for butane in my vapes is very low though. Like its happened only 3 times in 2 years out of millions of carts.
hence why they dont see the need to test the terps.

I do have ventilation box (instead of a vent hood) I could start formulation of the liquid live in there to see if it is an environment contamination.

Thank you, both the centrifuge and ventilation box idea will be used and see if anything come from it.

I could contaminate my terps with butane prior to trying out the centrifuge idea to see if that works. could use the two tests for testing the control to make sure its contaminated, and the second sample being tested is the terps after its been spun. :thinking:

IF its the environment and air duct work, i doubt my company will do anything to fix it. thats the worst part. Hence why im hopeful of implementation of a method during formulation as a preventive measure.

how Butane survives being trapped in the terps that is exposed to heat for that long is baffling.
We also extract with a propane/butane mix and have never failed for propane, only butane.

Good Olde Commonwealth of Massivetwoshits

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A vent box should help, flush it first. And giving the extractor some distance.

I do my stuff at room temp when working with terps - so like 20-25C not 35C. But that doesn’t mean higher wouldn’t work.

If its happening sporadically you might also reach out to the testing facility about laboratory investigations for an out of trend incident.

Shouldn’t be like - nothing is happening and then you change nothing and something happens. I mean it does happen, but usually its because something is different but you don’t realize its different.

let us know how the experiments go.

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Good fuckin’ luck. Better off getting into the squishing game.

Confused.

Are you calling your decarbed crude “distillate” here?

What is it you’re calling “terps”?
Or “crude” for that matter?

Not that semantics or terminology is gonna change the physics / chemistry, but it does make it harder to know exactly what’s going on and help.

If your “terps” are “all the liquid we get in our cold trap during decarb”, then yeah, that may be the source of your residual solvent.

15min at rm temp?!?

Maybe try 20min…and zero

Have you asked?

Perhaps the person that developed the SOP understood the possibility of residual butane at -50C ??

…and added this step to mitigate that possibility, as suggested by @Cassin

I’d suggest higher temps (than the -50C for three-five days)…rm temp isn’t horrible, but you might consider longer or under vac (15min, 15-20” Hg?).


Ref: Propane Butane Mixture - Evaporation Pressure

Suggests to me that yeah, you are catching some butane along with the volatiles you’re after, and you should perform a data informed purge (3rd party if you have no in house analytics).

$2k will get you a critter capable of informing your purge….

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To Clarify,
We take our decarbed crude ( could be Liquid Live Rosin/Resin or distillate) and test it before we add any terps to formulate into vapes. depending on the input, my output is a different sku.

I call everything decarb crude in the lab prior to the final steps. we dont use distillate but we do have a still and everything besides the Liquid Live Resin is put through the still.
Mostly all my crude could be called distillate as well.

I hope that clears up any confusion with the terms decarb crude, distillate, or crude.

The terps are the liquid we get from our cold trap. and that is where I suspected the culprit to be of where the contamination happens.
after we collect the terps they are spun in a beaker for 15 mins.

the only time the terps are exposed to heat is when its combined with the hot input (ie: crude/ distillate/ liquid live resin) and that goes for 15 mins at 70 C.

I have asked. My staff has no idea as the previous people who set this up have been gone for years.

but thank you for the responding !
This is all helpful and I will report back what I can.

I will do my best in my next post to properly communicate what I did and I am doing to help mitigate this problem.

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I run a lab, we do solventless as well.

Had this same issue. Butane was getting trapped in the terps. Left them at room temp for an hour and then in the centrifuge for 45 minutes. Never had another issue

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Your naming conventions seem designed to obsfucate rather than educate…

Is the goal to make your SOPs unusable outside said lab?

IMO running a lab should involve training others, I would argue that using non-standard terminology does those you train a disfavor.

Imagine if the technician that developed the SOP you’re following had documented it appropriately…and explicitly stated WHY they off gassed the cold trap condensate?

You would have immediately known you needed to lengthen that off gassing…

Close. I would suggest that “butane is being trapped (condensed) ALONG with the terps”…is the more correct way to look at/communicate the phenomenon.

This is occurring in the cold trap, they don’t actually get stuck in the condensate (once removed from -50C)

Undisturbed or agitated for that hr?

What benefit do you see in spinning your cold trap condensate?

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Failures at 54 ppb butane got me to look up rules and regs in Mass. I believe the following links apply.

Found an “Interim - Not Final” doc from 2016/2018 that gave upper limits for residual hydrocarbons at 1 mg/kg (1 ppm).

https://www.mass.gov/doc/exhibit-7-concentration-limits-for-residual-solvents-0/download

Found a more current version of same Exhibits 7(a) and 7(b) dated 2021 that increased the tolerance to 12 ppm.

https://masscannabiscontrol.com/wp-content/uploads/2021/06/202105_Exhibits_7a_7b.pdf

IMO, 12 ppm is still unnecessarilly restrictive, but is a lot more workable than failure at ppb levels.

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edited as I did not read the message! Sorry Cyclopath my bad for not reading fully

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Wow!

Yeah, glad that’s not the field I have to play on….

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Get a planetary mixer form @Lincoln20XX

Guys a total cunt but can get these

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I’m gonna let your own words be a response to that undeserved slur…

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Thanks this was a moment of healing the whole community needed.

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