First successful distillate "with a smell"

My first successful distilate … it s a bit smelly but n think was due to my heater over shooting to 322deg…
So i have taken B-pinene and used this as my green solvent, solvent was @ -18degc but the material was room temp, mixed both in a bottle shaking vigorously for a minute or 2, then drained …for my equipment, i am using ss316 2" chamber 200mm height, with 2mm ceramic balls about 30mm full at bottom… overhead is 1/2" pipe going to 1/4" coiled ss316 pipe to ss316 collection pot… i start off with bottom temp between 96 and 101, and remove b-pinene and other lights and volatalities round about pinenes bp… my vacuum was between 46-36mbarA , i run it until my overhead temp and pressure goes down … then i remove heat , the let it cool down for a day with vacuum not yet vented… next day i retrieved my yellow/orange overhead moslty pinene(solvent) but lost half of my solvent? But suspect it is lodged in plant material??.. i then started my vacuum again to reach a vacuum of 3mbar, started the heater set at 250degC, as it was heating ,my vac went to full vacuum for a moment , and went back to idling between 3and4… my heater temp was reacting slow so my heater overshot to 322deg , after adjusting i managed to get it to control between 250 and 290, my overhead temp ran at 89-90(not true reading because my temp is mounted on the outside overhead pipe . will fix my temp control issue and overhead temp accuracy for next run… my over head is a beautiful color but it has a foulish smell to it … ? Maybe the temp that overshot? But anywayz this is my first post and first successful run thanks to this site…


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Can you post pictures of your setup?

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wow that look gnarly! i wanna see the still!

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Yes i will def. Share pictures , later today

Show.the.still.

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So here i have a pic of my still with heat-tracing element coiled around it , like i said i will remember to take photos later today.

I have not had the chance to play with glass sets because i have easier access to stainless steel than glass.
Advantages in my opinion is that i can also build and break it into pieces make modifications, my pressure can go well above 7000kpa (critical co2)or hp steam generation to purge clean system without disasemmbling it … also durability is amazing and temp ratings are way above what is needed, only drawback is or was , is the fact that i cannot see wat is physically happening inside the column like glass, but it made me learn much more about the processes seeing that i had to rely only on my pressure and temps to tel me what is happening, i had loads of failures and loads of bud gone to waste … but definitely worth the learning curve.

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Oh and by the way little more about myself… im a instrument artisan in south africa working for a refining company , so the intel is beneficial for what i am doing as i work to maintain measuring and controlling devices in the plant full of distilling columns arranged in trains to extract solvents from crude minerals…

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A fraction finder may help you out greatly for running “blind”.

Thumbs up for your achievement :+1:
As for the scent it s very common to have a faul scent on the first pass
Second pass should take care of that
As for control are you having good vacuum readings ? Digital ?
I to work a lot on stainless and I am pretty sure some sightglass can be implemented on the receiving side
The boiling side might indeed be harder to implement but I am having no isseus
Using tuffsteel gaskets by rubberfab
Rated till 280C
As for sight glass gaskets they make them Costum to your specifications
As for heat transfer if the coil
I made the coil from copper and then filled all the gaps with soldering silver/tin wich fuses pretty well on stailessteel giving a way better heat transfer making it more likely possible to
Use the temp of your cooling/heating fluid
the way a glass distilled uses his mantel temp
All in all nifty solution

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I do have some ideas for the recieving flask , but as i have failed alot of times and mostly it was because of tiny leaks , so i basically i try to have as little gaskets and noints as possible , yes my vacuum is good , my digital gauge , when starting my highboiling temp for distillate at 270, my pressure is at 4mbar jumping to 5, i will definitely do another run soon so that i can have my overhead temp actually inside the head and not only on the outside …

I wil definitely read on about this fraction finder,thanks

Uhhhhh. There a bunch of issues. Post image of the spd setup.

You are literally fighting the tide doing everything you can to complicate the process a s possibly even waste time doing it. Spd should be setup in a perticular way and the temperature issues you are having are a direct result of the loss of control over the process.

Yes and that was exactly what i realised, and modified it to be a simple fractioning column packing material is 2mm ceramic balls barely quarter filled,i ended up using a T head for the column letting it tilt giving me a nice internal reflux,my temp probe is put in deep enough to be at the junction, my overhead stays half inch then goes to a expansion chamber (helps alot collecting my overhead high temps and draining my light that boiled off at first , so basically i run my batches and collect my lights in the bottom flask and my viscous liquid gets golected in upper chamber(expansion chamber) also helps putting vacuum area to the overheads and collecting area… i also adde a 1/8" pipe at the top to be able to suck up my solution (terpene as solvent) … so i do not have temp issues, i had , that is why i got myself a temperature robe to be inserted to my overheads. This is my first sucsesful run … i had thousands of other runs i started of distilling terpenes off , but never had a vacuum until recently… now my adventures begin … you see? What do you think i can change or do else? This is exactly why i joined this community.