CLSmatography-Success using Closed Loop for Pesticide Remediation

Attached are two photos of before and after test results.

The original sample (baseline) was a batch of distillate I made for a customer (who clearly doesn’t know how to grow). You can see it tested positive for 8 pesticides. LOQ means it tested positive but under the limit of quantification (the machine can’t detect the amount). ULOQ means upper limit of quantification which is +10 PPM. You can see the legal limit in Michigan for myclobutanil is 0.2 ppm.

Next, I took a 20g sample of the failed distillate, put it into a pint sized mason jar, carefully squirted butane in there and capped it. I’d say I did about a 1:1 volume ratio. I let it dissolve for about a week (it didn’t need a week, it just took me a week to get to it).

After the week I put the mason jar in the freezer to keep it more stable for the next step. I then packed a 4”x8” stainless steel filter stack with a 5 micron sintered disk from BVV then 100g t5 on top of that, then 200g magnesol, 100 silica, 100 magsil pr, and lastly a whatman filter paper with a ring to hold it in place. Next, I took the mason jar out of the freezer and poured it into the filter stack right on top of the filter paper.

Using a little colder than room temperature butane I began to flush the distillate/butane solution through my CLS and into the collection bowl.

It wasn’t a quick process, but it works. 7 out of 8 pesticides including myclobutanil, paclobuzatrol, trifloxystrobin, and piperonyl butoxide were removed in the process.

I ran butane over my filter for about 1.5 hrs. Stopped to check and see if all the distillate filtered through and it hadn’t. When I pulled the top of the filter stack, half of my original solution still appeared to be in there and it was soupy still like when I first put the sample in the filter stack. I didn’t turn to a rock which is what I had expected due to the colder temperature.

I capped it again, poured more butane over the top and then stalled it for 25 minutes so the butane and distillate mix could solubility more before pushing through the filter. Then I flushed it for another 1 hr with butane continuously using my pump and heater and condensing coil. By that time the sample had made it all the way through into the collection bowl. All in all it was about 4 hour experiment.

To be honest, I didn’t do the best at measuring weight in and weight out so I’m not sure how much was lost, other then the pesticide weight; and that was the goal.

Just wanted to put my notes out to the community. I think you could run liters of distillate through this process if you did it right. Bigger filter stack (maybe a cone filter like ive seen on Bizzybee Instagram), warm distillate, warmer butane liquid/vapors and either a vacuum or nitrogen assist to get the flow speed right. Some Sight glasses would be great to incorporate for better visuals.

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You answered a question we have been throwing around for a while in the crc thread, I think @Shadownaught said he would give a free amount of magsli pr to the first person to show test results using magsli pr in a line close loop process

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Yeah he did say he would throw out some magsil pr to anyone who would test it, I think @FRESHcoastextracts deserves it! Amazing work!! Wow these filter media’s in butane are really gonna change the game!

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Nice, would of been good to weigh what came out to see what was lost from the 20g you started with.

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Very cool, I wonder if this technique would work using pentane pushed through a crc column with nitrogen.

Do think it was necessary to use 100g MagsilPR for just 20g of distillate?

At those rates it might not be economically feasible clean liters of distillate.

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I think he just wanted to see if it was even possible to remove these.

Now he can do more testing to see how much of each absorbent he needs and which pesticides they affect.

I bet you could get the close same results using just silica, youd just have to use more of it compared to the magsil PR. I personally like magsil pr though. I bet magsil pulls pesticides silica alone cant.

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How are you vaccing your system down with butane in it??

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I went high on the magsil to hopefully (which I did) prove that it works for remediation (assuming magsil was the key part). From there it’s time to dial it back and see how effective it is at a 1:1 ratio distillate to magsil. Problem for me and testing is that it takes 8 hrs round trip to drop off a sample and takes 14 days to get results back. Pain in the ass but worth the data. Wish I had quicker turn around times.

FCE

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Spot on.

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…very carefully…?

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Did you apply pressure to the headspace to increase flow rate?

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Yes I did.

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use a recovery pump or put a cold trap before your vac pump

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what is the question at hand here? @FRESHcoastextracts im confused how its in a CLS yet you take it out of a mason jar and pour the mason jar over your filters? yet its CLS? …….doesn’t make sense… as far as magsil PR in a CLS; why wouldn’t it work? just like any other media. when we had a 3foot 6" chromo column of magsil PR it took out just about everything

That explains nothing lol

Same way you load material into a cls column, recap and vac

From what I’ve read, about 1:1 ratio, concentrate:magisil pr, is sufficient for remediation for traditional chromotography methods. I imagine it would be similar in a cls

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Won’t terps drag several pesticides with them
Future did a post about remediation only really working on first pass distillate and you needed to be sure you removed all terps

I’ll be loading some magsil-pr this week on a cls grabbing the last bit of my crc column today and we’re gonna give it a go I’ll let you guys know when it’s finished

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So is the conclusion that magsil pr will remove piperonyl butoxide? Just had a distillate run pop up for this and Pyrethrins. First time fail on a COA and the COA of the trim said it was good to go.

Things that dont even show up in high enough concentrations to have peaks on trim tests can be concentrated into above limit amounts quite easily …especially if lots of poorly treated trim yields a low amount of “crude oil”…less oil with more sprayed on the material it was yielded from :man_facepalming::pensive: