Waters SFE Clogging Issues


#1

So, via suggestion of a Waters tech, I’ve swapped the jackets on my extraction vessels. Initially it seemed to work wonders, we were getting super efficient extractions, as a result, higher yields.

Then the clogs started.

Seems like I can’t run a vessel more than once now without it clogging. Tried adjusting parameters some, to no avail so far. I’m tempted to just switch them back.

Any suggestions?


#2

@ExTek90
I worked with a 2x5L waters SFE for a couple of years, we used to get THCA clogs and such all the time. We had an EtOH cleaning protocol I can look for, but it was always a pain in the ass. Do you know where the clogs are? We used to get them around the ABPR and MBPRS, basically anywhere with a needle valve was am issue other than the manual valves off the vessels.

What change to the jackets did you make, also who is the tech?

Honestly at the end of the day we just stopped running SFE all together, I found it to be expensive and a headache.


#3

I’m thinking the clogs are indeed THCA based on the fact that there’s a bit of crystals in a ring right around the filter on the cap. It’s in the lines before and after the ABPR as well as in MBPR1.

I’ve done EtOH cleaning runs on them a few times, as well as dry cleaning runs. The dry runs get it all pushed through, but, I’m sacrificing a bunch of throughput time.

I’d rather not mention the tech’s name just because I’m not sure they’d be ok with the info being aired on the net. The change was moving them from the bottom to the top of the vessel, the idea was that the CO2 comes in from bottom to top, and some phase change near the top was making the extraction less efficient.


#4

@ExTek90
Good call on the tech, I got the same advice and ended up with the same problem haha. I also used to see crystals on the frits and around the area where the outlet line meets the top endcap.

I won’t ask your method parameters, but what is your current throughput at?


#5

The waters machines were not designed for THCA, so getting crystalline solids to flow through those small tubes might always be a problem. A heatgun can help things get moving when they get stuck.


#6

@jugglingjesus agreed, I found the ID on the lines was never adequate. Maybe it was my unit, but it always seemed like Waters engineers loved 90* angles too…


#7

I run one of these and you’re right, they are a bunch of trouble. Have you had the waters tech come out to your facility? Do you have the recycler? I run mine that way with the CO2 coming in from the bottom and out of the top into the ABPR. Some of the steps we used to help alleviate clogging was to run the material column at 50c. We shortened the lines from the top of the column to the switch box before the ABPR as well as placing some foam insulation around the lines from the top of the column to the ABPR. We had waters come out and service our ABPR which wasn’t working 100%. We clean the metal filters (waters called them frits) on top of the material column at least once a week. We try to keep it running too. we’ve done overnights and 24 hour runs. At the end of the day the waters machine just isn’t worth the time and effort.


#8

@thehashmob at one point we had a waters tech at our facility every other week


#9

lol. I about spit out my milk. I would have too, if they weren’t so far from me.


#10

I was getting around 12% final product yield at a rate of 3 lbs in 6 hours.

The batches with it switched are averaging 14.5% final, but it’s taking me almost twice as lomg, as I can’t get it to successfully run overnight.

@thehashmob I have a recycler, using the heat gun usually works, I sometimes have to take a line off and push some alcohol through to clear it with the heat gun. I clean the frits or filters (whatever) after every 2-3 runs, or in between strains.

Edit: Yes, had a tech out a few times. Seems none of them know much of anything about running cannabis through the things, so it always just ended up being cleaning visits. I can and have done every type of maintenance on the machines except for taking apart the recycler. I’d be surprised if Waters wouldn’t hire me at this point. I likely know more about running the thing then half their techs.


#11

Reasonable, however, I ran the things for almost 6 months with zero clogs. Wasn’t until the heat jacket switch that I even saw crystals. We were definitely pulling THCA before, had to decarb everything.


#12

Oh yea, the techs do not know anything about running cannabis, if they did there wouldn’t be 1/16th inch lines on the thing. The last time I had a tech out I made him collect out of the first collector, you know the one that shoots out like a missile. The vessel he was collecting into went flying out of his hand and he got moderately covered in hash. :grin: Good times, good times. I also try to bleed my recycler once a day as stuff can collect on that filter after the recycler. I do not run my material column any higher than 200 Bar either, in am effort to not pull as many undesirables. Has anyone tested that white powder crystal stuff? I’m not 100% convinced it’s THCa, since I cannot dissolve it into ethanol or iso.


#13

I’ve been collecting bits of the crystals, don’t have a .5g to send in though, maybe .2g.

That’s hilarious about the CS1 pull. I’ve taken those ridiculous tubes off and found a way to get it out very smoothly, actually.

I was thinking about seeing if they’re water soluble, ever try that?


#14

I have not tried water, I will when I get some more. I don’t always get it to collect. Some strains seem to deposit more of it than others.


#15

Most people at Waters have little to no experience. I have had the pleasure of sitting down with John Mackay for a few hours, he has done extensive work with Cannabis SFE, though I don’t know how public he was about it before leaving Waters

We did some in house HPLC on the stuff, sometimes THCA would turn up, other times not. We always just cleaned it and dumped it unless something extra special turned up.

@ExTek90 How often do you check and clean the inlet filter between the recycler and the solanoid? I found sonication of the filter to be useful as well, but if you’re not experiencing pump starvation then it’s probably not a problem


#16

I clean it whenever the pump starves, which isn’t very often. I always just clean it with acetone and dry it very properly.

I had heard John knew a bunch about it, but, I never got to meet him personally.

@Phytoalchemy What was it that was “extra special” turning up? If I may ask?


#17

He does a lot of work with terpenes and I believe has his own analytical and consulting firm. Very brilliant guy, and very humble for a Ph.D He is on my “lifeline” list of contacts for extremely difficult problems to tackle.


#18

@ExTek90 I’ve seen fairly decent precipitation of THCA in the cyclones, can’t speak on what pressures/temps we ran, but lets say they were geared towards terpene pulls.

@thehashmob I was training a tech on the waters and warned her about CS1 and to open it slowly, she…didnt quite do it slowly enough. Those loud pops and spurts on CS1 are always reliable for a good laugh.

We tossed the default collection tubes for the cyclones early on and just blasted right into stainless beakers from the valves


#19

Super interesting, I wouldn’t expect parameters, although I’m not entirely sure why they’re still considered proprietary.

I’ve heard rumors of a tech that would intentionally clog their MBPR1 in order to crash out THCA into CS1. He would then have to take the cap off and scrape, then wash 'em, but, I hear it worked pretty well.


#20

@ExTek90 That particular company is pretty strict on NDA, my personal project is pretty transparent and I always share what I can.

I wonder if that tech you heard about was me…

Edit: blocking CS1 wouldn’t be exactly how I did it, but eerily similar