So far i have only made stinky but not too terrible looking first pass. it seemed my vacuum was not up to the task so I have upgraded my system and hope to clean up the first pass. Im pulling 50 microns on clean yellow jacket oil (welch 1400) and ive dripped acetone on all joints and have not seen a jump on the bullseye. I know dow grease isnt the best but it should work right, the system is sealed pretty tight as it is.
Thanks in advance for your feedback.
is it worth the potential vacuum leak to put a thermometer in the boiling flask, will head temps be enough
should i use the third cow to capture tails or leave them in the boiling flask, is rerunning tails worth it?
my thermometer adapter seems to have the worst seal in the system. i havent tried sanding yet but would teflon tape work in a pinch. I have some 24/40 ptfe sleeves but they seemed to leak more than the grease
Looks pretty good from what I see and understand. But, I’ll preface my comment with; I do not know everything.
I would ditch the b.f. thermo. Its causing you vac leaks. No point really in knowing the solution temp. unless you maybe try and blast it up in temps.
I ditched it and went to single neck boiling flask and get great results. I slowly ramp temps and watch the reactions. No reaction and I will ramp the temp. up a little to the next target temp.
Are you decarbing prior to a run?
In terms of grease that should work. I personally like a ptfe sleeve on the b.f., grease on the cow and ptfe tape on the receivers. I can achieve acceptable depths with this. But there are many ways…I just really dont like the grease
Its definatly my ineptitude with it. I get it everywhere and on everything.
In your photo your cold trap is empty. You plan on chilling that durring the run?
Sorry, one more thing after looking at your photo again.
Your condenser is not tubed up to anything? Cooling? Heating?
ive yet to fill the trap or finalize the condenser tubing. double checking everything planning on running tommorow, dry ice is kinda pricey . its second pass so its already been decarbed it just has that distillate stink. for heating its a 250 ml flask in a 1 L mantle i was planning on filling the void with fiberglass rope.
I was considering doing a single necked flask, I have some 1 L that would fit better was not sure if the pump was up to the volume though. 1 L Bf, 3x 50 ml flasks and 500 ml cold trap on a welch 1400?
I had no luck with Teflon sleeves they seemed to make my system leak more ive had first pass success with grease
I have a simple aquarium pump in a cooler for chiller/ heater I add boiling water as needed to keep it flowing
Do you use a vacuum gauge?
@AlexSiegel there’s a Bullseye in the bottom right corner of the pic with the cord going under the table (hopefully to a T at the pump)
a 4 way actually with 2 valves one for backfilling with co2. i planned to just stick a hose in my dry ice chest. I have access to argon too though its more expensive, not sure if its preferable.
N2 is my choice of inert gas for economic reasons. I use it for many things in the lab
I would suggest swapping out that clear tubing for thick rubber tubing. It is a little pricey (~$60 for 10’) but will hold much better vac and last much longer. Those pvc or vinyl hoses are one time use and are fairly porous and leak.
You might want to get a boiling flask that matches the size of your mantle. You’ll want a tight fit for good heat transfer. Then add a temperature controller, or at least add a thermometer in the boiling flask and control it with some kind of manual controller (maybe pictured on the left?)
Use thermowells instead of those leaky thermometer adapters. Thermowells are pretty much bullet proof and very reliable.
Insulate the top a lot.
ive got some nalgene 180 (the clear tubing on the right 3/8ths) however it dosent seem to fit on my gl adapters and with a hose clamp i was unable to get a good seal ( do gl barbs come in 10 mm?) , maybe i just need to really torque it down. (the red hose is silicone probably still porous though)
I have a temperature controller of sorts, its an old school controller that controls the on off cycle not really the temperature. ( is it preferable to have a thermometer at the mantle in in the BF) ive got enough thermometers i could do both)
https://www.amazon.com/Atlas-Scientific-PT-1000-Temperature-Thermowell/dp/B07KJJ5CTC/ref=zg_bs_9931461011_20?_encoding=UTF8&psc=1&refRID=KV0ACPVKDZN44CB0JBD4
would this work if i made a gasket out of RTV or something similar
The thermowell is a great idea thanks! im just not quite sure how to make it work with a 14/20 female joint , what seals the thermowell in place it seems many of them use npt threading do they come in standard joint sizes or would a fanged unit with a gasket on the outside work?
Dow grease does not work on temps that we short path. it will cause leaks and low THC percentages. I’ve gone through that journey myself. I currently use
It’s a bit expensive, but it lasts a long time. Some people say Krytox doesn’t work, but I have been using it for about a year with no issues in test results.
As for the stinkyness, you need to properly remove heads. go slow pulling as much as you can before the main fraction. If you need more help, carbon scrub that bitch. i dont find carbon necessary, but it helps
There is a DigiVac gauge in the photo
Yes I was responding to a comment not OP
ill check that grease out im hoping i can get by with this run using the dow grease, the spec sheet says its good to 200 C i thought our temps shouldnt get that high
go for it. my experience is it works, but you will get lower percentages
You’re distilling at 170-215c roughly, depending on vac level, you’re definitely pushing it. @lefties.cannabis is trying to save your ass. I’d listen to the advice given.
use ptfe, stainless will expand and break the joint, too much expansion.
Thanks all I really appreciate the feedback, ive ordered some krytox. In regards to the thermowell, i had a feeling steel and glass wouldn’t be ideal for that very reason. @Soxhlet are you suggesting i use a ptfe 14/20 adapter and a steel thermowell or an entirely PTFE thermowell, seems kind of overkill. it seems many of these are threaded which seem useless for this glass application, can you suggest any particular setup?
I wouldn’t make it entirely from ptfe, just the joint. Really the mantle is best controlled with the thermocouple directly in contact with the mantle. That way the pid controller that is controlling the heat has instant feedback. You ever put your feet up near a campfire with boots on? the soles of the shoes get so hot they can smoke before your feet start to feel the heat. Your mantle is in a similar situation. Eliminate the internal probe and your source of leak for a more accurate way to control heat imput.
Check this out: Looking for 4-pin plug to enable internal thermocouple in Chinese heating mantle
