Beginner SPD questions/first run.

[Fullmeltalchemist]

Hello!
I’ve been lurking here for about 2 months studying up and reading all the threads I can, but specifically regarding etoh extraction and SPD. I’ve found it to be both enlightening and entertaining to follow along while the community helps out those with less experience. It’s actually quite refreshing to witness in a time where there is so much discord on the interwebs. My hat’s off to you all.

This journey for me all started out with my girlfriend wanting to grow hemp this past spring as she’s into plants and tinctures. She grew a couple hundred plants of some great quality flower and has supplied a few dispensaries around our area as well as a few out of state. It’s by no means a big business, or even profitable at this point. We both still have dayjobs. Really, it’s just funding our hobbies. I come from a field engineer background so I’ve been tasked with both the R&D as well as building whatever we need on a fairly tight budget. All in all it’s been pretty fun, albeit challenging at times, and as a bonus we’ve gotten the added benefit of supplying organic, well tended to, clean medicine to friends and family. The goal here is to take what we’ve already done a few steps further.

So, in the recent past we’ve done rosin, winterization, basic cold etoh extraction, etoh distillation and filtering. My current plan is to go through with the whole process beginning with something resembling bucket tek with -60c ethonol cooled via dry ice and ending with distillation.

For gear I currently have:
A full set of 14/20 fractional distillation glass.
Full set of 24/40 SPD glass, 500ml BF
500ml digital mantle
A small 3CFM pump
HFS 12CFM vacuum pump (supposedly hits 15 microns)
A vac gauge that only hits -30hg
500ml Buchner funnel
A finger style cold trap (will be cooling in a dry ice jacket)
Heatgun
Digital temp gauge

Things I plan on getting:
Thermocouple
Vairiac
Wattage meter
Better vac gauge
A different/another cold trap
Full bore vac lines and an Alcatel 2021i pump
T-5 and AC

I have about $150 to spend on this project for the next two weeks unless we sell some flower in the meantime.

I actually totally spaced on a 10/18 thermometer adapter. Could I use a rubber stopper or is that not recommend? They don’t have them on Amazon prime and it would take at least a week to get here. Any fixes?

Now for the questions. First, temps. What is the condenser temp supposed to be? I was under the impression that it was supposed to be cold, but I’m seeing some information that conflicts with that. Is around 80 c the target temp for the condenser? My understanding of the idea is that the BF is meant to vaporize the target compound, the head temp is meant to further that vaporization a bit under the BP of the target compound until the bend of the head where it is then cooled by the condenser. Is that all correct? Is the 80c condenser temp meant to keep the compound in liquid form until it reaches the recieving flasks? Further, would a super chilled condenser work if one was distilling off terps or etoh off a crude+etoh solution? Being that I don’t currently have a rotovap or a countertop distiller I’m planning on distilling my etoh via SPD with the 24/40 glass and the small vac pump.

Do you guys think I should give it a go? Or, what is the most important thing I can purchase under $150 that will aid in my success?

I can post pics of my setup and runs later.

I’d appreciate any tips, pointers or criticisms!

[Concentrated_humbold]

A vac gauge, cps has one that works just fine for 150 or less.

[noname]

i used silicone to secure my thermometer cause i didn’t have a adapter too.

i made my condenser cold for the heads / volatiles then crank the heat up for the mains.
i set mine to 85c for the rest of it.

im sure you can distill the etoh in your spd. iv never done it before.

post some pics of your setup

[Fullmeltalchemist]

Turns out that my mantel does 20c above room temp at it’s lowest setting. And it’s a bit touchy at it’s lowest settings. I distilled off the etoh in the SPD by just taking the vac hose off the cow. For a thermocouple workaround I took a piece of aluminum foil and wrapped it around a thermometer probe and stuck the foil under the BF. Seemed to work pretty well, I could at least get a reading of what the mantle was at.

I ended up using a dropper head for my thermometer hole at the top. It should work to stick my thermometer through it in the future, we’ll see.

[noname]

why would you put the thermometer under the boiling flask? what are you using to read your head temps?

[Fullmeltalchemist]

I only distilled off the ethonol so far, so I didn’t really need head temps.

[Fullmeltalchemist]

I found that getting a reading of what the mantle was at itself was helpful since the thermometer in the BF only reads at 78 when distilling etoh. Being that it’s a new tool for me and I was unsure if it’s stable, I wanted to read the actual (or as close as I could get with foil) temp of the mantle. Turned out to work really well since I could go up over 100c mantle temps and get a pretty solid flow of distilled etoh

[noname]

ok cool your ready to distill now then

[Fullmeltalchemist]

Yep! I only have ~20ml of crude right now though. I need to go grab more dry ice and extract/distill some more this evening.

[Demontrich]

20ml crude should net 12g disty.

[square_root_pharms]

I think there’s a few ppl on the board that have stated you get better mantle heat controller and less overshoot when putting your thermocouple between glass and mantle. Maybe @cyclopath I can’t remember now. It may have even been @Beaker but sadly he is no longer with us.

[Fullmeltalchemist]

Last night I was distilling off some etoh and witnessed that overshoot. I have a thermocouple on the way here.

Also, it seemed as though a variac would smooth out the temp control.

My next purchase will be a panda. I don’t like wasting any ethonol. I put the spent biomass in a mesh bag and squeezed it out the excess in a press, but that stuff came out really green, and I couldn’t collect all of it. So, I think a panda is in order.

At this scale it’s going to take me a while to get up to 250g of crude to distill, so I’ll probably put the vacuum gauge on hold for the time being. I checked out that COS that @Concentrated_humbold mentioned and it seems like it will due.

While distilling off etoh, is it beneficial to do it under a vacuum to reduce oxidation of the cannabinoids? While I was watching it boil last night it dawned on me that by not having it under vac it is being exposed to oxygen. What effect does this have on the CBD?

[Concentrated_humbold]

If it nust a small amount id do it no vac, it wont take much to remove a few 20mls. So your gonna decarb in the spd.

[Fullmeltalchemist]

It’s a bit more then 20ml. More like a liter. It takes about an hour to do 500ml.

I’m chilling some flower and etoh right now and will be extracting again later.

My t1 and t5 will be here soon so I’ll probably wait in that. Or can I just dilute my crude and run it through filtration again? It seems like somewhat of a waste if time but I have the weekend off and a good book so whatever.

[cyclopath]

@Fullmeltalchemist

I have a thermocouple on the way here.

A bare thermocouple like this would be your best bet…

(No idea why that was in my carry on )

[Fullmeltalchemist]

I’ll most likely get that hooked up tonight. I’m in the middle of extracting at the moment and just found out how to bookmark posts a day ago so I didn’t save that thread. I’ll post it when I search.

The thermometer gun is a great help with extraction.

[Fullmeltalchemist]

I haven’t reread through it all but this may be the thread about installing the thermocouple.

Cheap mantle thermo-probe fix?

@midsfactory: Continuing the discussion from How much is left in your boiling flask?: ouch. as a one off, replacing that probe that came with it with one that sat between the flask and the mantle might be more work than it’s worth. as a community project, where dozens of these things could be re-hab’ed it might be worthwhile. my guess is they’re using a k-type thermocouple (but that is just a guess). You probably don’t have a half dozen PID controllers lying around like I do, so hooking th…

[cyclopath]

@Fullmeltalchemist

Last night I was distilling off some etoh and witnessed that overshoot.

Have you tried the “auto-tune” function on your controller?

I’ve had success with it in the past. Not sure how to enable it on that mantle.

You want to tune with your process fluid, or close to it. So if you tune for ethanol distillation you’ll want to retune later.

[Fullmeltalchemist]

The manual has no mention of any sort of automation. By holding the set button I can bring up a variety of parameters “a” “r” “c” etc. I haven’t a clue what those mean though.

[Fullmeltalchemist]

Alright. I hooked up the thermocouple to my temp gun. So for now the reading on the mantle is only relative. It’s about a 20 degree difference. My vac still says -30 and I have a rubber stopper in my head with a probe in it. It’s all…kinda working. We’ll see.