After Months of Reading, First SPD Run!

cbd

#1

After months of reading about distillation on this forum and weeks of waiting for parts to piece my first rig together, it looks like everything is ready to go in the morning! :grin: I did a dry vacuum test and only achieved 37 microns, with 4 microns at the pump when blanked off. Though not bad, I was expecting a lower vac given the k25 hoses and all glass being Chemglass, LS, and Goldleaf. All glass to glass joints have PTFE sleeves with a smidge of Krytox vacuum grease. Thermocoupler adapters on head and BF are Chemglass PTFE also with a bit of grease (no sleeve). Steel keck clamps all around except for the cold trap. PTFE GL18 to KF 25 adapters on the cold trap and cow. Fiberglass rope on top, and I plan on breaking out the space blankets as well for the BF, head, and condenser.

A few things I’m a little concerned with are my lack of bleed valve for vacuum and condenser hoses. Have a valve that can control how fast the pump pulls, but I can’t actually bleed it once it’s pulled. I’m also using a heating circulator that gets up to 100c. I’m planning on running the condenser at 90c. I’d run hotter, but water boils at 92c in my neck of the woods. Which brings me to my second concern, hoses. After a test run, this vinyl hose is getting scary soft at 80c. Thinking of picking up 5/16” radiator hosing while I’m out grabbing dry ice. Is there a better option than that?

Here are some photos of the setup. Promise I’m not a slob, the mess of wrappers and such are getting cleaned up before starting :flushed:.


#2

Yeah silicone/heat resistant tubing is probably a better bet for you.

I use a welding blanket for my insulation on the BF.

Looks good! You’ll nail it. My setup is way worse and I produce great product :wink:


#3

Rock and roll buddy yust keep a kf flange loose but atached When starting to pull vacuum while oil is reaching around 120C
So You can release vacuum If neccesary
If all go s Well You thighten
:+1:


#4

think im gonna have to copy your set up a bit with the wide bore trap and with the cow kf adapter…great vac level…looks like your a go for today…good luck


#5

Thanks guys! @Killa12345 weren’t you getting like 11 microns with your setup? I remember being blown away at you getting that low with GL lines and china glass. Think I could find silicone hose in town at like a Home Depot? Autozone didn’t have it, omw to grab dry ice now. Might have to stick with vinyl for this run and just stay around 80c…


#6

I only got to 87 microns. You all are killing me with your set ups. Getting a serious case of jealousy. Lol.

Looking forward to the show brother.


#7

looking good man!


#8

Preheated the crude in the vac oven over night at 25”Hg and 70c. Poured into the BF, cranked vac to 1300 microns and have a bunch of boiling. I’m assuming it’s residual solvent. Getting condensation on the cold trap, gonna let it rest there for a bit and let it calm down before turning on heat (stir bar is at 1400 rpm). Probably going to break vac and empty cold trap flask before proceeding.


#9

No vortex at this spin speed with this 1”x3/8” stir bar. Should I be concerned?


#10

No not at all viscosity Will lower the hoter iT gets :grinning:


#11

2 hours in. SV 180. PV 170. Stir 1500. Mantle 137. BF 84.7. Head 28.5. Vac 47 microns. Took it up super slow to ensure no boilover. Still steady boil. So far so good.


#12

Bf temp now at 123 and vac jumped to 57 microns. Nothing in the head yet.


#13

Like reading posts on FB. Rock on and keep us posted :+1::grinning:


#14

First of the heads at 157.9c in BF. Head is at 47.7. :grin:


#15

Nice one, I probably run less vacuum than you. I think my lighter drips are done by 180bf, then usually get through the heavier heads and into the hearts by 208bf.


#16

Great to know! Thanks, I was actually scouting the search engine here looking for guidance on that, lol. I’m at 50 microns right now. 57 head, 170 BF, 221 mantle, and 1700 stir speed. Slow drip so far.


#17

I set my stir bar speed at a way lower spot, as long as it prevents bubbling over/popping then that’s all it needs to do.

I always set it to 420 :stuck_out_tongue_winking_eye:


#18

Ahh, maybe I’ll stow her down a bit the. I was trying to compensate for the fact it’s only 1” (:smirk:) but I’ll see what happens if I slow it down some.


#19

Looks like a green fraction coming through. 48 microns, bf 175, head 73. Just slowed down stir to 900.


#20

180c should boil off all the garbage (residual solvent, h20, terps). 200c is where the magic happens

Been washing and filtering 50lbs (25gallonsl the last 9 hrs