Its likely you have a lot of very very tiny particles of celite contaminating your extract.
How do you go about setting your celite filter bed in the buchner?
Sorry I wrote up a whole explanation but the site wouldn’t load it.
I made a slurry and pulled vac on it for 10min. It was poured on top of a filter paper then I put another filter paper ontop of the slurry for when I poured the AC/C545 mixed into the crude which was dissolved 5:1 in etho
What micron are your filter papers? And did you aquire your celite from a source that can verify it was produced to exacting standards like Sigma/Millipore?
What you can try to do is re dissolve the extract and add a small amount of bentonite to the solution and allow it to sit for a while. If there are any particles making it through your filter bed the bentonite will cause the particles to aggregate into larger masses of particles. The concept is referred to as flocculation.
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I think where youbwent wrong is by mixing the activated carbon along with your celite. They have different functions. Celite is a filter aid and should be the lowest powder in the stack because its purpose is to catch the other small particles from the other powders.
The last pic u posted looks like activated carbon is contaminating the crude.
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Regarding the pictures.
The picture with the 2 labeled jars is after the filtration.
The other 2 pictures are what it looked like when dissolved in etho before adding the AC and Celite.
Are you opposed to using hydrocarbons?
Not at all.
It was extracted with butane.
Why not incorporate a pass thru silica gel with your crude dissolved in heptane?
That would allow you to utilize your current equipment and not have to buy anything other than solvent. It would also remove a significant amount of the pigment compounds that give crude its spectrum of color.
Ill get some heptane and silica and give it a try next time. but this was a freak run, ive never gotten such bad results.
I am looking to put a C545 filter stack inline in my CLS. hopefully do a good scrub from inital extraction.
Or should I rather use Bentonite?
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Celite doesnt scrub the solution in the same way as the bleaching clays, carbon, silica, magsil, or polymeric adsorbents. Celite is just for physical filtration of solid particles. I like to put down a layer of sand on top of the first filter paper and then just add bentonite on top of that.
I got my celite from sigma and its honestly been a pain in the ass trying to keep celite out of my finished product when its the first powder to touch the filter paper. Such a pain in the ass that i dont even use it in my stack anymore.
Bentonite seems to do a good enough job of filtering out the fine particles if you make a proper slurry to set your filter cake.
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Ahh ok, so then ill rather try get some bentonite and some silica.
I only have a 1.5" column. so my filter stacks are very small. Keeping it simple which 2 solutions would you put into small filter stacks? I’ll put 2 x 1.5 stacks inline under my material column, but what do I put into either?
The one thing I’m worried about is if there will be enough pressure to push it right through. I don’t have N2 at the moment. But I do have a spare empty tank.
I would say if you already have a screened gasket for your 1.5" column then you should go with a 2" layer of sand and then slurry pack your bentonite on top of that.
Pressure assist doesnt work very well with condensable gasses.
https://www.mrwa.com/WaterWorksMnl/Chapter%2012%20Coagulation.pdf
Chapter 12 Coagulation.pdf (918.3 KB)
Edit: The paper deals with aqueous solutions but the information is applicable to other solvents, although it seems to be to a lesser degree. I dont get the large flocs like those that are shown in a lot of pictures but maybe thats because im not coagulating shit like algae but the bentonite does have an effect on the coagulation of waxes from solution during winterization.
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Forgot to mention that under normal conditions a solution of ethanol/methanol has trouble facilitating the adsorption of the pigment compounds in crude onto bentonite or silica gel, I dont know why this is the case for sure but my uneducated guess is that when alcohol is used as the solvent the solution has a greater affinity for the pigment compounds than the bentonite or the silica gel and so they tend to stay in solution.
You will want to use a non polar solvent to dissolve your crude when passimg it through silica gel and bentonite. If you dont have a rotovap it would really make more sense for you to buy some pieces for your CLS so you can remediate color as you extract your material.
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I would rather remediate in my cls. But do I need a N2 tank?
I take it bentonite will be best to try use Inline?
Or should I also have C545 as the last layer in filtration.
Thank you for the tips man
I do have a roto.
It’s been a while since i seen stuff that dark lol. What is happening here could be a few things. I suggest you cover these before using the crc. These issuses will help a more efficient crc pass.
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Biomass prep - Water & dead leaves removed. Water in biomass isn’t fully removed.
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Extraction procedure- do you mind sharing how your filling? Top or bottom? Soak or passing?
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Equipment- Molecular sieve for dehydration, dewaxing column (Time?), no heat exchanger with inlet solvent line if the recovery tank isn’t getting chilled.
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Winterization- The filtering procedure is incorrect or you’re using the wrong filter. Whatman #1 with a single pass will have you’re extracts looking gold. The filter needs to be wet with the same solvent you’re using before pouring. Also freeze your funnel 15 minutes before filtration procedure. This will ensure a faster process flow.
Try to get down these problems taken care of before using the crc. The one x-factor that could be happening is a floral spray was used before harvesting or something contaminated your biomass
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So form 800g of material. I got 80g crude. after winterization it went down to ±50g. Then after using AC and Celite it went down to 22g.
Is this normal to have such loss?
The material from what I was told was a mango cheese which was a very dark plant. I told the custy to store all his trim in the freezer double bagged.
Does Lycopene or Anthocyanins get pulled out easier than chlorophyll? and especially from very fine trim?
Ok Juice. thank you for helping me get to the bottom of this.
1: material was very fine trim that was frozen after trimming.
2: I have a small 500g column (unjacketed) into a 6" x 12" collection. Solvent was cooled to -35c± on DI, I inject at the top with very little residual time just passing the material.
3:No dewax column, not molecular sieve. I chill the recovery tank on DI. Still running a basic setup.
4: Ill check what sizes I have exactly.
This is the first time ive ever seen things go this bad other than when i start extracting with iso.
so please help me understand what happened so i can tell my client why its was so bad.
That’s bad numbers. It’s better off being used as a paperweight lol. I never answered you earlier because I wanted you to do some more research. I know you were under pressure and the lesson I wanted you to have is learning under these circumstances. We all had too.
Biomass - Needs to be COMPLETELY dried of water. Get a dehydrator or use an oven. Don’t decarb its unnecessary.
-Water will freeze around your THC. This is making a lower yield.
-The biomass needs to be in a vacuum bag or we use to use pillow vacuum bags. (Tip: put a napkin inside of the vacuum seal port. This will stop any biomass from letting the seal be completely closed.)
- I used a refrigerator, not a freezer. If a leak is present in the bag, then you will have moisture.
Your solvent is circulating water from the previous runs of biomass. You ever had a stage 10 clinger and you finally let her score? That’s how wet it is lol.
- Get a molecular sieve and housing ASAP. Do some research and know exactly where to put it and what kind of molecular sieve to buy. I think its 3A but it been a while.
-You need to bottom fil. But this will be a few more upgrades. Get a ball sprayer hemispherical end cap for the meantime. This will help give a better-uniformed disruption of the solvent on top of your biomass and will increase your yields.
-Never let the solvent stay stagnant in the column. Its always moving. When it stops you’re collecting impurities.
It sounds like you’re going passive. Remember this More energy----> less energy. You don’t need n2 assist. All you need is energy to flow the correct way. You’re cooling off the Recovery tank and sending it to more energy (heat) so here comes the tricky part. How do you solve this? Don’t freeze your recovery tank. Just give it a good ole ice bath. Buy a condenser coil and place it between your recovery tank and inlet feed to your column. Use a dry ice/isobath. Part 2. How to get get it from the coil to the column? This is where you need a dewaxing column or freeze your column in the freezer. Make sure you wipe out the interior of the column before filling it with biomass after you take it out.
I’m attaching my oven tek for shatter. But I give a lot of tips on the CLS process also. Make sure you’re packing your columns correctly. This is vital for good yields. Excuse grammatical mistakes. I
Humidity doesn’t stand a chance. Oven tek
I have a favor to ask well sort of an experiment. Can you get a cryogenic freezer vacuum bag? Take the dried biomass and place it inside of this. Take the bag and dip it in your iso/dry ice container. I want to see if you can flash freeze the biomass. First, get your client happy and come back to this. If I was running my old CLS still I would try it.
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