Whats up Future.
Have been reading for months and finally signed up for an account. Just want to thank everyone for all the awesome info being shared regarding SPD.
With all the threads and pointers, I was able to pull the trigger on my first run. I know there are many threads similar to this but I am in the middle of my first pass ever and experiencing something that I have not come across before. Hoping for some guidance.
Followed a GLG SOP and got everything Decarbed and through the first couple steps. Currently at 125* Mantle but my vapor temp is stagnant and not changing at all. As I understand I should be seeing fluctuation as I ramp up mantle temp. Is my thermo incorrect? Pictures attached.
What size system, how much crude, and what pump. Vac looks a little high. You shouldn’t see notable rise in head temp until minimum 150°c on the mantle, depending on vac depth.
5L. 450G crude. Welch CRV16. Have been able to pull 380 micron on an empty system.
Adjusted thermo and vac dropped to 780 and vapor temp is climbing again.But really curious as to what I was pulling through into the receiving flask. Still at a slow drip.
You probably still have a leak. Also 450g is a light load for a 5l. I’d wait until you get to 140-145°c on the mantle and get most the volatiles out. Hopefully your vac will drop. What’s in your cold trap?
Wanted to start small to avoid any unexpected hiccups/burping. Should I be seeing material in reciving flask with 130* mantle and 5-10* vapor temp? Cold trap is an immersion chiller with isypropyl.
Vac is still dropping 686 currently.
I’m on a 1st pass as well. I’m at 137°c on mantle, and head temp is 30°c. I’m rocking 2l ai glass and 1075g crude. I’m running a welch 1400 for the shit until I get to 160°c and switch to my alcatel.
Your not quite to heads yet. Hold out on swapping flasks until you see goodies coming over. Should be around 190-220°c depending on vac level. More vac requires less heat. With the amount of crude and vac, you’ll probably be around 200°c before goodies arrive. Once you get up to 150-165°c on the head pay attention.
Might be roasting your vac oil. Can you get a reading on the cold trap?
Cold Trap is at -5C. vac oil seems good. No smell or smoke. I’m hesitant to raise the mantle temp more because my vapor temp is still so low and not moving up as ive seen in other runs. Could condensation on thermo cause inaccurate read?
You need your cold trap way colder. Use dry ice and acetone, that holds -78°c as long as you keep it full. The vapor you cant see is going straight into your pump oil. Run your ballast open until after heads.
Also your vapor temp won’t rise until you’re distilling heavier compounds with higher boiling points. Just keep your cold trap as cold as possible, keep your gas ballast open until around 180°c on the mantle, and wait lol.
Thanks for the input man. Sounds like your first run is going much smoother.
going to try dry ice in the cold trap next run. I opened the ballast and smoke/vapor came pouring out of the exhaust tube. Do you think thats toxic?
I think the thermo reading in the head is all wacky, so I will be going off mantle temp and appearance for the rest of the run. Plan on slowly ramping to 200 on mantle and watching for reaction. Vacuum is holding between 550-600 now. any other thoughts?
Try and get -200 microns if possible. Find leak or change vac oil
Sorry bro, been on the phone for the past hour and change. Ain’t my first rodeo lol. I’m trying to get you advice on your specific run.
Your vac is way of
Your head is to cold
You need to insulate it or better yet heat it with a heat gun
Any reflux gooing on ?
At 500 mic expect a 210c in the head and 240c on the mantel before you see mains
Yep. Going to re-evaluate all joints and change oil before next run. At least I learned something.
No worries! Your advice so far has been spot on and I cant tell you how much I appreciate it.
I think the thermo in the head not working properly is kinda forcing this to fail. Posted a few pics above.
Blue is azulene
Green is chylorphyl (need to winterize better).