No Heat No Vaccum

Thank you! I’m a hobbyist and supplementary revenue stream for the BM massive growers I work for. Once I’ve built the funds, I’ll probably build out a separate facility for all this for my buddies. It started with unlimited trim, make something worth money lol. I try it all, even crap they send me will just get turned into coconut oil extract for edibles. They really like to have concentrates/diamonds and sauce to match their flower market. It helps their sales. But their game is top notch flower in a BM state. Anything I do for them is bonus. For them and me.

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Sorry, I’m pretty careful with pictures. I can’t find any on my phone right now, but I have some lemon haze finishing up along with some Go, zkittles, and FF. Still need to process some BI and GG. I’ll post pics with my chromatograms in the next week or so.

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I’d be curious to see if the test results match your nose tests. I’ve had some really fragrant extracts that come back with low terpene %

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I’m ready to see the results too. I had to let someone else switch out the column on the GCMS to run there samples. They should be done before the weekend is over and I can change the column and quantify. I go off of smell, but also flavor. Then the main reason for my belief is just longevity of my EtOH, compared to my prior work. It takes tremendously longer, more material run to accumulate enough terps in the OH to tell they are in there. I also think alot of terps get missed by labs. I think most use FID instead of mass spec, so they have to have a tremendous number of terp samples to really account for them all.

How many different terps is your lab testing for?

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How do you get hot nitrogen?

I agree for sweeping but not for sparging liquids dry before certain reactions I find nitrogen does a better job any chemist to give an explanation ?

Here’s what our labs test for:

What if we did that… under vacuum though @tweedledew this might be getting closer to what I just brought back up the other day in the other thread.

That’s a decent swath, but a lot of labs you look up will do 35 or more, out of over 100 total that can be found. The key is using a good mass spec as the detector. FID requires standards. I completely volunteer that technically the MS requires standards as well, but you have giant databases that identify all the components, known or not. I changed the column today. I will run some samples in the next couple of days. Terps in finished product as well as recovered EtOH.

Looking forward to seeing the results

Been pumped down for 24 now. The N2 level is finally ok. Got the autosampler running…

So after recovering 50 L of EtOH, it is still greater than 94% ethanol and I only started with ~95%. I have changed the scan parameters to help bring up the signal from the heavier terpenes. The lower/smaller terpenes are at less than one percent limonene and similar sized. All the smaller fragments from these and ethanol make it harder for the MS to match the higher terpenes with high confidence. Also using library identified terps gave me 7% in my extract, but again I’ll be implementing a solvent delay or changing the range of the MS to get more complete look. Pretty Spectra to follow.

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7% terps in your extract is higher than anything I’ve ever produced. So youre not using a rotovap for any solvent recovery? Just your oscillator?

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Yep oscillator and flowing gas. The flowing gas is going to act like a small vacuum and the oscillators as the rotating action of a roto-vap. I am fairly positive this can
not compete on speed with a roto vap, but I don’t think it’s tremendously longer at the 20-50L scale. I’ve seen people go at really low temps in the rotovap, not sure what kind of times came with that but they were retaining more terps as well.

Do you have specific temps for “low” temp on rotovap?

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36C is a good limit. It slows it down alot but everytime i take my time at 36C it comes out crystallizing, so thats low enough to retain the acids and maybe not low enough for the terps.

Id be curious to see how this tek would work directly after a FFE. U should only have a couple seconds in the FFE to strip 80%+ of the solvent off. Then place in the oscillator and gas sweep until its gone. I think that would be the best of both worlds

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What %terps are you retaining in your final extract if your rotovaping at 36C? over 4% terps?

Most guys I follow on rotovaps are 30-35c, 36c seems perfectly fine to me. I don’t temp control, so some summer days when I’m not home are definitely 36c. My personal experience is full vac will leave you with 2-3% less total terps than something like I’m describing or a rotovap between 30-35c without a full vacuum.

Im curious to know if the higher terp retention is solely because of the termpeature vs the flowing gas. Thoughts?

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I believe it is entirely temp related. You can see the heavier terps sink, while the lighter ones look like leopard spots on the surface. Any vacuum would pull those on top for sure. For me the flowing gas is to force the pace of evaporation, while the temp is keeping more terps.

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