BreakingDabs Distillation Tek

I started out in distillation with next to no training, I had no idea instagram had so much info and so many people conversing on the subjects. The same goes for co2 extraction which was my previous role in the industry before SPD. So I worked many many ideas over on just running a short path efficiently to go from sludge to gold in 2 passes or less. I knew three passes caused serious amounts of degradation for me based on testing so I knew it needed to be done in less runs.

Because of this I’ve mever really gotten up to speed using preprocessing methods. The only one I really spent time on was carbon scrubs in etoh or ISO. I wrote a small article of the use of an ultrasonic bath to help speed up the process of mixing and filtering through the carbon in the solution.

For any material these days if it isn’t ethanol wash or acetone wash… I don’t bother with preprocessing. I use condenser techniques and very low vac depth techniques to removes unwanted fractions.

On first pass my apparatus typically is very long and efficient with cooling capacities. The reason for this is I typically will ramp up the temp and stir bar very quickly to 150C and then slowly work my way closer to the heavier fractions. As I do this I can soak a pump very quickly with solvents and volatiles… so the longer the chain the better.

My chain of pieces usually goes:

Boiling flask
3 way adapter 105 bend (also know as a Head) used to capture the main body in a rotational section attached to the end of the actual head
Liebig condenser (or similar)
3 way adapter 75 bend (receiving via the side port.)
Dewar cold trap (or HE Friedrich currently)
Second dewar cold trap,
And sometimes 3rd dewar cold trap.

The temperatures of the Liebig and any condensers beyond that is set to the lowest temp my chiller will go… which is typically -23C

The head condenser I either keep at the same temp as my boiling flask as I scale or just below it.

When I reach my heads fraction I immediately slow down the process, I preset the BF temp 5C below current, turn down my stir bar and begin bringing up my head condenser temp to 155C. Once I am at about 135C on the condenser or more I allow the heads to start leaving the column. I do this by increasing my stir bar speed. Stir bar speed can purify a fraction ascending and give and extra umph behind the fraction to allow it to exit the port. I’ll typically set my Liebig to 10C at this point.

Typically I’ll watch for the haziness in the head and condenser to change. As well as at 155C not much of the heads should be condensing in the head condenser. It should be really condensings after the condenser and dripping into the Liebig.

I allow this fraction to continue until I see an appreciable amount of clear building in the head condenser at these temps. Then I will spin down the main body receiving flask andbump up my boiling flask temp so that I push faster through the head condenser.

There are a few tricks to the head being this hot. Pushing heads past the drop off is not easy to nail down the proper proceedure because it’s different every time. Sometimes I lower the head condenser temp because I’m seeing main body recondense on the other side, other times I bump the boiling flask temp or stir bar up more to speed it up so that the heads makes it to the other side of the boiling flask… and sometimes but rarely, I go above 155C to push junk across.

If you run so fast that 155C is too hot and main body is making it into the Liebig… then turn down the temp. But for the ultimate separation. 155C should be used and aiming at proper fraction removal prior to main body is important.

Second pass is similar but much smaller and quicker.

Setup is as follows:

Boiling flask
Drop down 3 way
Vertical 3 way
Dewar cold trap

The reason for this is that if the first hot condenser was done right… there are no volatiles and the material already has a consistency that’s like glass to the touch.

… but I’ve never found first pass satisfactory to me… so I do a second pass

I start by evacuating the entire system. I turn nothing on except the pump. I check all fittings to make sure they’re perfect with no leaks.
Then I walk away for an hour.

When I come back the vac is usually below 4 micron.

I then begin scaling temps and get the stir bar going as fast as possible as soon as possible. When I reach 140C on the Bf… I slow down my ramp up. Set my condenser to 155C and pull a very very tight heads fraction, typically it’s green for me. I allow this to collect and slowly drag out off the Summit key. Then when it’s completely I’ll go for main body. I again aim for any heads to make it past but I never turn my head condenser temp down on this run. I aim for the speed and temp that gets just the main body to fall. You can tell based on the color and clarity of what makes it to the liebig. When I know the heads are completely done, like ultra positive, I’ll drop the head condenser to 100C and push a bit harder on the BF temp. To capture main body quickly.

As I reach tails (I can tell based on captured quantity) I start to lower my bf temp to starve off the tails as long as possible. If you do this long enough and precise enough the boiling flask will turn yellow and there may only be 50ml in there. But it’s a pain. So typically I end it sooner and capture tails.


Do you have a range of stir speeds we should be shooting for with the aforementioned SOP? Also, which stir bar do you prefer?


:man_shrugging: Sure


Should I wait to answer the stir bar and speed when it’s changed to a different post ?


Your tek is super valuable info, id like it to have its own topic so that more people can see it :slight_smile: I flagged it for @sidco to move it. go ahead and respond to stir bar speed and Ill have him move it over as well


Please attach a list of all vacuum fittings and grease used as well, I can’t get my wholes system under 50 microns.


did u try finding the cause of the leak with helium?


I use apiezon, I was a huge fan of the lvp before krytox stopped making it. The apiezon is right up there and I couldn’t tell you which is better but I have zero issues with the apiezon 501.

As far as fittings I use standard kf-25 seals, quick detach clamps and most of my fittings are originally from Cacejen Vacuum. If you can think of it they can make it. I currently have a manifold being made through them for my personal system. It matches a lot of current gear from Summit so we’re going to probably market it towards that idea if anyone wants to copy my system design. I make nothing off the concept but I figured since it’s going to be featured soon in videos… may as well offer it so people can play.

The manifold will allow up to 4 pumps be independently connected as well as a gauge in a safe spot away from the vapor path (yes you can get useful accurate readings without throwing a gauge in a bunch of junk.) the whole assembly with also button right up with the new Summit traps. I opted for this concept due to the limitations of the new Summit downpipe.

My setup has evolved and seems to evolve every single run so I can’t nail down exact parts as I’m always trying new things.

General rule of thumb for me, complex long change of traps on first pass,
simple barebones second pass but extremely tight tolerances.


Very impressive!


As for stir bar speed. The general rule of thumb for me is faster is better and here’s why.

Not only does it allow the material that is boiling to be as close to the same temp throughout as possible. It also keeps the column “action” consistent. Popping and bubbles in the flask can cause contaminated to climb the column so the earlier you get it up to speed the better.

But there’s a system, generally there are 3 zones of fractions. 75-100C 120-145C and 170-190C on first pass. Most of this note will be about first pass because second pass is a no brainer if you know how to scale temps correctly as well as make sure everything’s perfect. I can go over that later.

Generally I watch my vac gauge. I always put my gauge close to my pump. A lot of people like to say that’s not accurate… well neither is at the top of the column… or after the cow… or before the cold trap… because they give an accurate reading of the area… but regardless where you put it once you get used to the readings you should see it becomes habit. I put mine close to the pump to avoid ruining it with constant vapor interaction. I’ve seen as high as 5000micon while at 130C on the flask. I did not decarb but I cranked my stir bar when it finally was able to move faster and the burst of vapor caused my gauge to skyrocket. While turning this up caused my pump to work hard the good thing about an Edwards 30… is it could handle it via the cfm… a wide bore setup is much much different then tubing. There’s no hold up. What happens in the flask is seen within 3 seconds at the pump gauge… 3 seconds sounds like a long time… but it’s only enough to say I turn the stir bar up by 500 rpms and within 3 seconds my vac gauge is scaling up as well… granted tubes do see the change but not as severe… it’s just faster. Turbulence is a bitch. Cows and tubing create huge amount of turbulence.

I use the biggest polygon egg I can fit in the flask without it having spinning issues. This means 3.5” in a 20L or 3” in a 10 or 5L and even the new Little green one I got in the 2L system… the reason being is even if they don’t hit 2500 rpms… the size of them flings material all over the flask and keeps a roaring boil. This benefits because cannabinoids are extremely viscous, the viscosity creates cohesive properties that trap lower boilers… the only way to really get everything out is to thin it out over and over. The bigger the better.

I generally test every stir bar in an empty flask before running it. Just to double check. I check slow speeds. (The green one doesn’t like slow speeds at all) and I check the ultimate rpm of the bar with no obstruction. Generally I take that number and take about 80% from it and expect that’s it’s ultimate speed with material surrounding it. And even then typically will scale up by 100 rpms as I get close to that number. Just to double check and not create unsettling oscillations based on ramping within the electronics.

So to me… bigger is better, ramp ASAP and by heads, make sure it will remain perfectly constant the whole run. If you’re set so high that it falls off it’s flight path over and over. Don’t force it or you’re contaminating your fraction. I put a vid up on Ig recently of me distilling some etoh out of some first pass through a summit head… the etoh was coming out so quick it was dragging the disty up the column at 22C… part of the reason was I couldn’t turn the stir bar up anymore to allow it to come out at lower temps because of the viscosity of the oil at that temp.

Best bet is if you see main body try and climb and you shouldn’t be seeing it… turn your stir bar up… you’re probably trying to kick out a high quantity of a fraction at that temp and it needs help expressing itself quickly.

Also, always, if your pump is seeing a high value for Vacuum. It is seeing vapor… on first pass this is okay but should be kept to a minimum for a good Vacuum by main body. The reason is those volatiles in the vacuum oil that the pump just saw. Are going to constantly boil out and hold your vac depth high. I’ve been testing multiple pumps at the same time recently. Using a volatile pump to get me through the junk fractions then kicking on the precision pumps at the end to save their oil and ultimate vac from suffering.


A few points on leaks.

Gl connections are always going to leak. Period. The gasket is not secured properly (look at a kf-25 seal) and the materials are not proper, I have seen tons of melted gl connections on the backs of cows…

Silicone hose will leak constantly… as well as offgas (it has a smell doesn’t it) I’ve used it for high temp hosing for condensers… never again. The mineral oil diffused right through it and into the air… after the run I checked the hose… it looked perfectly fine but was weeping.

If you do not clean your joints right before you grease them with acetone you are subject to poor joint connections. As dumb as it sounds… atmospheric humidity can keep the grease from applying to a glass surface enough that it can cause fissures in the grease during a run.

I rotate nearly all of my joints (if I can’t… I can’t) while the system is degassing and during initial fractions to make sure any small fissure is taken care of and the system is tight. Not a lot, just like 1/4” turn is all at most. You’ll get used to the concept and it becomes second nature

Oring seals on clamped kf-25 fittings can age and die. If you’re bottoming out your clamp… chances are it’s because the oring is flat… this can mean toooons of vac difference.


Pump maintaince.

Know your pumps ultimate vac. Period.
Know your pumps ultimate vac. PERIOD.

If you take your vac gauge and Place it directly on the inlet of your pump with nothing else attached… clamp it down… and turn the pump on… the pump should hit the current ultimate vac within a minute at most.

If it’s not satisfactory then you have two options… throw the pump against the wall or change the oil. There’s a proper procedure for oil change.

If the vac depth is reasonable (I expect 2-3 micron at most out of my precision pumps)
Then open the ballast and walk away for an hour. If you can close the ballast after and hour and get thag same ultimate vac. Then the pump is clean… if not, dump and refill… it was an illusion pressure.

Vac oil runs at about 160F during normal operation. The temp is meant to keep the oil at a specific viscosity to get all the internals properly lubricated and keep the seal. When you open the ballast you are forcing air into the vanes. Which makes them work hard which heats the oil. Leaving it open for an hour or more over heats the oil… all this does is force anything trapped in the oil to express itself in the vanes, which causes back streaming to occur and change the reading of the vac depth.

Proper procedure for pump oil replacement

Check that vac depth is not acceptable

Blank off inlet to pump and open ballast.

Place in a well ventilated Place

Turn on pump and allow to run for 2 hours undisturbed

Turn off pump. Open fill cap for oil.

Open drain plug and drain oil into waste container.

Tip pump to remove particle sediment on the floor of the pump chamber.

Place back on fable and screw Drain plug back in.

Fill with oil. (This is a relative amount. If you are unsure the vac depth will be acceptable after this Drain and fill then only fill to the minimum line in the sight glass) ((technically if oil can be seen in the sight glass, the pump can run.))

Keep ballast open, close fill port for oil.

Turn pump back on, leave for 1 hour.

Come back, close ballast. Check ultimate vac. If acceptable, fill completely with oil to the max line (I prefer this on first pass because more oil means more saturation quantity it can sustain without vac depth issues at the end of run.
(For second pass I fill to the middle of the min and max… no need for any extra since there are/should be no more volatiles in this run)

If it’s not an acceptable vac depth… rinse and repeat.

In extreme cases, some pumps can be filled with solvent and allowed to sit for a day or so and then drained… this is not okay with all pumps and you need to check with professionals for what your pump can handle. I know e2m30s can handle ethanol… which I have filled a pump with ethanol and drained it a day later… ran some hot oil in it, drained that and refilled and had great success at rejuvenating the pump… it’s rarely necessary and best to just have a professional take a look at it… but things like that are possible.

Vac depth defines a lot about how fractions come out.


Vac depth can very much define a second pass. I’m not sure how many of you see an emerald green fraction on second pass heads… but if a system is brough below 10 micron on a wide bore setup (gl may work as well) and the temps are ramped so that this vac depth is never lost, stir speed at max asap… then when you get close to heads you go slow. The emerald green will appear and Drain off. This is 100% the cause of the smells in most disty… concentrated it is terrible, when allowed to sit in atmosphere over night it 99% of the time will turn red.

Once you reach the green in your condenser or collection cup at the top for those using the FC from Summit… do not change temps… and keep it constant for as long as that comes out.

As vac depth gets deeper, fraction temps get closer. So you can have a range of like 15C on main body when you have a looser vac depth. But at 10 micron and below that number becomes 5C difference can be huge change. It kind of works like a logarithmic scale. I’ve had the same experience with temps and pressures using co2 as a solvent.

Co2 as a solvent can have the same affect within 250 psi at 120F… but at -20C the difference is within 0.05F


As far as checking for leaks. If you don’t see a perfectly glossy seal with mild pressure and a slight twist… redo it no exceptions.

Helium is not necessary for good glass joints. And from what I’ve heard from people testing rotary vanes and kf-25 fittings, spraying a tiny amount of iso on a joint will be enough to see a change in vac if there is one. Helium can sometimes be undetectable because the change is so slight


But again… if it works for you. :man_shrugging: I’m happy for you.


Awesome explanation! Thanks for the write up. What type of hose do you recommend as I know exactly what you mean about the stank hoses, and they do get greasy to touch!

Currently I am exhausting through inline fan and out the poorly routed ductwork (already in place when I took over), but with such high ceilings I’m afraid pressure would be lacking for running a hose all the way up and through the roof to push out the oil mist and I know the ducting for this area is coated as I’ve seen random drips coming back down. Only route is through the brick wall at the back of the shop somehow as the only other way is through the front which would greet neighbors with stench, given these minimal options for exhausting and saving my lungs, what would you do?

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I also like the “twisting to seal the joints” tek.

I was informed by summit when they started distributing monocows, that twisting glass under deep vac was extremely dangerous and should not be done with their glass (at least 2 years ago)

But I abandoned that advice in the pursuit of chasing vacuum depth.


That was because at the time he suggested using no Grease… there was a concern at some point about safety with the use of krytox and DC was out of the question


You have to be careful attaching small hoses to the back end of your pump. It needs to be able to breathe or you’ll pop an internal seal. I believe that happened to Columbo twice in the same week. I could be wrong.

I’ve seen molecular sieves used.

They’re not cheap but they capture a lot. You can clean them by blanking them off at the inlet of your pump at the end of a run or with cold oil in your pump. Turning them on. An internal heater will heat up the beads causing the material to boil out and go in your pump oil. This can then be dumped as usual. But I don’t know how long it will take it to saturate.

I’ve also thought about taking one of the new Summit cold traps with the buttplug and rigging it up on the back end of the pump with some dry ice in it and see what I catch.

Cleaning your oil mist eliminator from time to time is also essential.


For those using a 24/40 setup, here’s a set of parts to do the shotgun condenser setup on the cheaper side. And to be honest. It’s all that’s really needed to start working in wide bore. From the outport side of the setup is a 24/40 to KF-25 adapter and some length of flexhose to a valve… always use a valve on a wide bore for first pass especially… the system degasses so quick that before you know it even decarbed material at room temp can muffin through your setup. Best to degas slowly and use temp and stir if necessary to get the material to settle.

A second cold trap can be implemented with the same parts and a little imagination. Only necessary for first pass.


For 29/42 setups. Just look up the initial cg-xxxx and you’ll find the respective 29/42 assembly parts.

Remember that as soon as heads really begins you’ll need to increase the “Liebig” condenser temp to 10-20C at least to get it to continue draining.