My first attempt at Sauce Tek and CRC is a fail. I’m hoping to pick your brains about where I went wrong and the best way to go about fixing it. Sorry for the long post, I have to explain my process so you guys can try to see what I did wrong. Solvent not cold enough, CRC media/pack job, too much material to media ratio, not enough solvent to weed ratio, didn’t wet the CRC with solvent, pour out with too much/ too little residual butane, I made many mistakes…
I packed the CRC column based on a friend’s SOP then got the bright idea to modify it because I had some trace pesticides. I have a 4" x 8" CRC column I made myself from BVV parts. It has a 2 um sintered disk at the bottom, then I put filter paper on top of the disk to help with cleaning.
Top to Bottom:
280 g Silica
100 g Florisil
100 g T41
300 g Bentonite
200 g Charcoal
60 g Diatomaceous Earth
1040 total grams of media
I packed each layer with a stainless steel column packer. On a scale, about 50kg of pressure pack job, although the coal and T41 were super fine and hard to pack. I packed the column by sucking full vacuum when I purged the system prior to starting. Did this dry.
The CRC is in between my material columns and collection pot, with a Swagelok ball valve on both sides.
Then, trying to follow the OTS Sauce Tek as close as possible with my Precision X10MSE
which doesn’t have jacketed material columns and my chiller only goes to -37C, I proceeded to blast some top shelf fresh frozen Sunday driver. 100% n-butane, no blend. I had 40lbs of material, pre packed in column socks in the freezer overnight (about 18 hours). Freezer gets close to -40C. Columns hold about 9lbs of frozen material each. I chilled my solvent tank down the maximum it will go with my chiller, -38C and blasted all 40lbs of chilled solvent across the 9lbs in the material column. It took approximately 35-40 minutes to drain through the CRC. First run looked water clear going into the collection pot. I should have poured it out into it’s own jar, but I kept going because I wanted all 40 lbs run to produce one homogeneous batch of concentrate. Figured I’d pour it all out at once because its difficult to remove and replace the collection bowl by myself. I did not wet the CRC, I opened ball valve super slow and tried to be gentle until I achieved full flow (super slow)
I distilled the butane back with collection pot at 20C and when my solvent was fully recovered and chilled back down to -38C, I repacked another 9 lbs of frozen material without changing the CRC media. It took about 45 minutes to drain through the CRC the second time. I noticed some color in the collection pot after the second run but didn’t look too dark. I put a total of two x 9lb socks through the initial 1040 g of filter media.
I changed the media in the CRC, same pack job and layering and continued as above, three more socks, through the CRC totaling 22 lbs of fresh frozen blasted through the second CRC pack of 1040g of media. Near the end of the transfer through CRC, I was using 100 psi of N2 just to make solvent move, 30 psi was no flow whatsoever.
Following Sauce Tek as close as possible, I tried to eyeball “about 1lb of solvent” and poured out of the collection pot straight into mason jars. I was really disappointed with the color immediately because it looked like the sample run I did with no CRC. I put the jars in a dry ice/iso bath for two days. Out of the freezer the butane solution was frozen solid. I couldn’t tell what it was at first, left on the counter at room temp for four hours then it looked like this when it went into the oven with lids tight:
It’s in the oven now, after three days, I have small size crystals forming in only two of the three jars. The one with no crystallization was filled about 1/2 way, the two with crystillization were filled about 2/3 or more.
What to do with this dark resin? Thinking I should redissolve this in the material column with more butane and push through the CRC again to lighten it up? Or should I dissolve it in a liquid solvent and suck it through the Hochstrom filter with some media?
Should I just leave it and let it crystallize? It does have killer terpene retention, tastes great. Gassy with a subtle fruit finish.
This is most likely what I will get if I do nothing. This is from my test run with no CRC, it looks decent to me, but it looks dark in a jar or spread out on a sheet:
All I did to make these was blast at -38C, no CRC, distill at +30C to thick syrup, then pour straight into jar. I added about 1/2" of distilled butane straight on top of the resin and put the lid on tight and straight into the oven at 80F 3-4 weeks.
I need that bright yellow color; the buyers care more about color than taste in my neck of the woods. Can anyone advise me how to improve the CRC/Sauce Tek with my current setup or clean up the dark resin I have in the oven? I’ve been reading a lot about W1 in the CRC. Everybody raves about it on the CRC thread. Thinking I better get some before I try CRC again?