Aloha all. I am new here so a brief introduction and then my questions.
I have been in the cannabis industry in NorCal for several years and before that I worked as a lab tech for a biotech company straight our of uni. I have worked for extraction labs before but am just now embarking on the SPD road on my own and I have lots of questions. So…
I recently made a batch of cryo alcohol crude with some new material I obtained and it came out quite runny and during decarb it formed waxy globs as well as a hard crust on the bottom of the container and on top of the crude that reminded me of caramelized sugar. I have made crude tons of times before and never had this happen.
What could have gone wrong? I did everything as normal with one exception. My thermometer seems to have been out of calibration and may have been telling me the extraction temps were colder than they actually were. Still, I have made RSO at room temp and never seen this happen.
I am wondering what the best oil would be for running a Welch 1400 on a 2L rig. Since I am a beginner should I go ahead and buy the proprietary Welch oil or would any 19 or 20 grade pump oil be fine? I am trying to minimize potential sources of failure for my first run when the equipment arrives.
Would the Welch 1400 definitely be sufficient for a 2L? It’s used but the guy who sold it had a pic on ebay of it pulling ultimate vacuum down to 1 micron. The guys I used to work with had big Edwards direct drive pumps.
Thank you to any one who has some answers! I am excited to be embarking into this world.
When the distillate stops dripping and starts to run thick, does that definitely mean I am on my main body? Some one I worked with told me once that just because I am getting honey does not mean I am pulling only main body and I should watch for red and blue colors to appear which I am assuming must be plant pigments.
Has any one tried filtering particulate from fresh alcohol extract by simply hooking up a series of inline capsule filters and running it from one barrel to another with a peristaltic pump? That’s how I used to sterilize fresh cell culture media back in the day and it seems like it would be hella faster than using vacuum filtration.
I had an idea to extract with room temp alcohol and then concentrate it in the roto down to 1 or 2 buckets and winterize at -50C because it seems that would be easier/faster than using dry ice to keep a huge barrel at -50 for 2 hours for extraction. That much dry ice gets expensive.
A lot of your questions can be answered if you search for people’s spd threads there’s a bunch Out there. Off the top of my head I know of @Demontrich@coppertop and @Killa12345
I don’t have time right now to go over all of your questions in detail, but I will say it sounds like you have water solubles in your extract. That can be remediated by either doing a liquid-liquid extraction with heptane and water or simply filtering over a healthy cake of T5 bleaching clay. If you do the LLE, I suggest recovering all of your ethanol and dissolve the extract in methanol as it’s likely going to be cost prohibitive to try to recover your alcohol and tossing that much food grade etoh is going to be expensive as well.
As for the pump, it’s generally recommended around here to use the special Welch oil with the Welch 1400. That’s why I opted for the Alcatel 2021. Got a refurbished one pulling 3 microns for a little over $1,000 after shipping, but there are cheaper options if you want to take a risk on a used pump that hasn’t been rebuilt (which most folks here have had good luck with so far). Either one should be adequate for a 2L system though.
To determine what fraction you are in, your head temp probe is going to be your best friend along with visual cues. You’ll be able to find a bunch of other threads on this site going into detail on what temp exactly most people find their main body to start coming across, but in general 160-170c head temp is where most people switch to the mains. This is assuming your vacuum level is sub 100 microns. In my experience, switching from heads to main is pretty intuitive after your first run. It’s switching from mains to tails where most people have problems deciding when to switch over.
I’m digging your filtration idea. I think I remember someone doing that, but I can’t remember who it was or where to find that post. I think it would be worth experimenting with and letting us know the results. Right now I’m pushing everything through a 5 micron stainless sintered filter at 60 PSI. While it’s much faster than vacuum, it’s still painfully slow for my scale. I eventually would like to pick up a dedicated centrifuge for particulate filtration as I think that’s going to be the fastest method.
I have moved over to room temp extractions myself. You’ll see arguments all day on this forum between folks who swear by skipping winterization with ultra cold ethanol and folks who swear that winterization is still necessary with cold etoh extraction. I personally fall into the latter camp. Just know that in addition to more waxes and fats, you’ll also be pulling a lot more pigments and water solubles with room temp etoh. There are some steps I follow in my own SOP to remediate that issue, but I eventually plan on moving away from ethanol extraction entirely in favor of heptane extraction because fats and waxes are so much easier to remove than pigments. But that’s a whole other ball of wax you can learn more about in other threads around here. Just make sure to pay close attention to the exact ratio of ethanol to extract when you go to winterize. So rather than ballparking it, I would just remove all ethanol, then add ethanol (or methanol) back to the extract to achieve a 6:1 ratio before winterizing.
Wow… I guess my “quick response” turned into way more detail than I thought I had time for.
Same, amigo. But these new state regs finally got a fire under my partner’s ass to look for some much needed capital and it looks like we have some promising leads to get a good fuge and more than 4 figures in the bank account, so I’m hoping that won’t be an issue for much longer. In the meantime, I’m considering putting together a couple of 8”x24” spools and pumping heptane through biomass loaded in a sock. It’s cheap enough to not worry about lost solvent too much, just gotta throw the spent stuff on a tarp outside to dry. Which shouldn’t be a problem with the 100 degree days and 10% humidity we’ve been having lately.
I’ve found it to be my favorite ratio balancing filtration speed and ability to precipitate fats. Ymmv, so I encourage you to play around with different ratios and see what works best for you, but in my opinion, the conventional 10:1 ratio is dogshit if your goal is to remove as much wax as possible.
Oh, and that’s for both. I haven’t had a room temp winterization that didn’t give me even more fats after freezing yet. My end goal is always to get a finished product from a single distillation run since that’s my current biggest bottleneck for processing, so I’ve gotta be super anal about my pre-processing.
Thank you for the detailed reply. What happens if I just load it up and try to distill it as it is? Is it just harder or impossible? I considered doing a hexane/water wash to remove the water solubles. It’s the only method I have used before and I have only done it with first pass disty, not with crude. I will look into your other recommendations. I did manage to increase the viscosity a bit by heating it to 155 under vacuum for about an hour. It foamed like mad in the beginning.
I got a Welch 1400 (not rebuilt) and went with Inland 19 on account of the price. I just did my first dry cold vac test and got to 16 microns. No idea what that will mean when there is an active distillation going though.
I plan on trying the pump/capsule filter method for filtration as soon as I can afford the equipment. I envision having extraction buckets in a -50 freezer and just pumping straight from those. My only concern would be saturating the filters with particulate and getting pressure build up. I have seen filtration setups like this literally explode and splatter an entire room (and the operator) with media. lol
U ever try hexane soxhlet to make crude I did that with a 150c decarb n volatile cook off not winterized even and barely had any Terpene fraction single pass and it looked and smoked absolutely amazing. I went through like 4 other methods so far the hexane in a soxhlet gave me the easiest time least amount of work and best results second best results were 10 room temp hexane wash and celite545 and carbon scrub after room temp methonal winterize then LLE washing with methonal to pull terpenes. If you do hexane soxhlet watch the residence time in boiling flask so be sure to exchange extract in boiling flask with fresh hexane n roto crude
If you can avoid a cryo method its beneficial cryo costs a lot more to use in your process if your savvy at handling chemicals room temp methonal winterize is a huge savings in time money and effort
The welch pulls less than 1cfm so when you can upgrade for fastwr runs. The stuff on the bottom is probaby particles that didnt fimter out. Do everything like normal but scrape those out and let tbem sit in a lil etho and see what happens
Today, an experiment of 10g flower went thru QWET. About 6 ounces of absolute ethanol did the wash. Dry ice was used to super cool all materials including bud, containers, etc. Seemed fine as the solution through a coffee filter was very clear.
Assuming most of the fats, lipids, and waxes were caught up in the washed flower and filter. However, a second and third filtering through Whatman #1 filter captured a bit more.
