New to SPD. Need tips for a successful run

Hash and Stuff Distillation
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Hey everyone! I recently started messing around with SPD of ethanol extract and oh boy was I overconfident in my chemistry knowledge. I had a little explosion due to high temp and I collected something but not sure if we got any THC in it. Any tips/pointers/suggestions are more than welcome. I explain the experiment parameters and equipment in detail under this paragraph. Thanks in advance future4200 community! :heartbeat:

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(Pictured here is our 2L setup, its the same setup except it has a 2L boiling flask)

Extraction
-Flower mixed with ethanol in digester
-Flower filtered out of solution
-Put crude in -86 freezer overnight
-Filter the crude extract
-Decarb/Solvent recovery

Equipment:
-5L boiling flask
-2XZ-2 stage rotary vane vacuum pump
-VMV-1 digital vacuum gauge

What happened during SPD:
-Used vacuum pump, over boiled so we switched to a weaker diaphragm pump
-Started up the heating mantle at 60 (all temps celsius) when it reached 50 increase to 140. -Once it reached 130, increase to 220.
-Got bright orange head fraction around 150ish
-Started getting darker orange/amber fraction around 180
-After that, clear colourless liquid around the 200s
-Head temp after starts dropping to 50- 60 from around 100
-Decide to increase temp to 240 since nothing more was happening
-We got impatient, bumped to 300 from 240
-Thick white cloud of smoke appeared at cold trap
-Pressure build up at rbf - explosion

Identified problems:
-Solution over boiling with vacuum
-No way to control/release vacuum if needed
-Not enough vacuum
-No acetone/iso at cold trap
-No insulation for rbf
-Very little/no stirring
-No heated water in condenser
-(Obviously) too high of a temp change

Thing to change for next run:
-Buy insulation rope, and better stir bar
-Buy a water heater?
-Be more patient
-Change positioning of vacuum gauge to be beside the vacuum pump instead of in the middle of setup

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First thing you should do is get a proper vacuum pump. But back up a minute… You say you had an explosion? What happened?

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What waS your vacuum meter reading this whole proces in microns ?

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Yeah I guess before buying a new vacuum pump make sure you have no vacuum leaks. Your problem sounds like a classic vacuum problem. Once you fix your vacuum problems you will start distilling the main body at about 170° - 180°

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Sounds like what happens when you release atmosphere back into the still above 180°. This will cause the flash point to decrease and a “explosion” to happen

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Being impatient can cause accidents and accidents can cause others and yourself to be harmed if shit hits the fan.

Be cautious and always practice safe etiquette.

Pictured was a late night and ready to rush home, I released vac and instantly the spd lit up with a bright purple light and lit the vapor cloud from bf to cold trap. It had looked like the cold trap had taken most of the burn up as well.

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You have about 5-10 major issues to correct if you want to be distilling without issues or held back in the future.

You should invest in proper pumps, one for up to mains and one for mains and beyond.

You need a breather valve setup.

You need valves on each pump.

You need to expand your bellows before use and only use as much as needed.

Eliminate the kf between the discharge and trap. Set gauge on pump where it’s cleaner and more effective for you.

Get short path away from the AC unit above it, this will cause temp issues on the glassware and head.

The temp unit should be nearly directly behind your short path with minimal hoses.

You need to purchase and aquire a proper lab stand setup, you are begging for a accident.

Absolutely get rid of the china valve. That whole setup is asking for issues if you ask me. Go direct and avoid the issues or leaks from unknown hardware abilities. Removal of those options will allow your short path skills to benefit from any side quest problems.

Get rid of the dangerous gl fittings and use acceptable hoses and hose clamps. Those gl fitting looked like accidents waiting to happen.

Also you need to avoid high temps on china glassware, they are known to ship with high soda lime content style glass that will literally implode on you. Keep it at 220-240 or below. Those temps can sometimes cross the edge of what china glass can handle.

I mean I can help you and give you advice but whoever sold you that package knew they were going to ruin your day, that’s is exactly not how short paths should be setup or ran, it will ruin your day like you’ve explained in your problems.

Hit me up I can forward you to free consultants that don’t charge for help.

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looks like most of these replies covered the big things… bigger/better vac pump (most important), valves/places to release the vac, patience, cold slurry for cold trap, and you’re definitely gonna need a stir bar in the BF…

but one of my biggest recommendations to new distillers is to make damn sure you are post-processing properly before distillation. make sure your filtration is adequate and you decarb completely. this will go a loooong way in making your distillation go smoothly.

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came here to say this as well. i think most of the thread has covered your blatant mistakes, (are you running a stir bar in there only thing i didn’t see but could have missed)

Crude and the process you used to make it is extremely important don’t skimp there, but then also like others said here don’t rush stuff it sucks and take a long times sometimes but its the nature of the beast. I really liked having a super fine vacuum adjustment valve on the line you can use to throttle the process in the early stages when you are still going through a lot of reaction. I haven’t run SPD in a 3+ years but god damn that made me anxious and have some flash backs at the thought of OP running the set up with no real vacuum control

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You just missed our distillation class in Oregon. Hit up @PharmExOregon and see if he can do a quick phone consult and maybe go over the class booklet with you.

I’m glad you’re here. Based on the people replying, you are in good hands. Stay safe!

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I would like to thank everyone who participates on F4200, especially those who take the time to help newbies, like myself. Between reading here, a couple videos, and $6-7K we now have an operational 10L SPD. We have partners that produce bulk distillate via autos and wipers but I wanted an in house process to distill our ethanol cleanup THC into disty.

Big thanks for the safety heads up regarding letting atmosphere in at distill temps. Never thought that was something that would be done purposefully, but I came from big industry where most vacuum distillations would go boom if you let in o2.

It’s not the best, it’s what I could afford… Yes, it still needs improvements…

Edit: The test results from the first runs just came back. Single pass 79/81% THC 85/86% total canna. Was hoping for a little better but I guess a second pass will provide more experience.

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Nice! There are a few upgrades I’d still recommend you make. One of them being a shut off valve for the pump.

Happy to get you setup with a vacuum valve. Also when that digivac dies or if you want another vac gauge I have a good recommendation.

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Love to see the progress! Setup is looking clean. I would recommend adding another K25 tube for the exhaust so its easy to clean.

also for the for my OCD put that flask on the middle of the jackstand under the little grippy pad haha

I have ran alot of those CRV pumps in the past make sure you flush the shit out of them after every run or between really rough fractions that are pulling nasty shit.

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I like to always move my temps in 5 degree increments or lower, give your BF some time to do what it needs to and adjust. This is where patience comes to play so heavy in proper distillations.

In my personal experience I have never made bigger jumps in temp than 10 degrees.

keep a log of every temp change. record notes. record vapor temp and other sensor temps and vacuum
data is king to progress and efficiency.

Patience and following this you will always give things the chance to work through their fraction.

Rush from only changing the temp 3 times with big swings, and you will co distill your heads and your main body every time.

Patience Patience Patience. even when the corporate hounds want it faster. they will be happier when you have a clear nice tasting product instead of rushing and bogging down yourself downstream. always fight the shit upstream.

Have a good day and be safe out there.

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@AlexSiegel thank you for the suggestion, I found a valve and shorter line and threw them on. BTW your SPD components look very nice and I really want to try a 2L or 5L setup when $,$$$ allows. What vacuum sensor would you recommend, if you don’t mind me asking?

@DetroitLove Thanks for the feedback, you are correct patience and documentation are so important with distillation. I was considering the KF25 stuff for exhaust but its a convoluted mess getting into our c1d1 penetration for exhaust, so silicone was chosen. My ocd messes with me when the jack is centered on the flask and the thermocouple meter falls off the stand pulling out the thermocouples from the head, lol. I have had great, IMO, success with the CRV pro pumps. I picked this one up new from classifieds here. Still on it’s initial oil fill with multiple 7L starting crude runs with volatile strip. I can get in the high 20s with no material, 40-60 main body, and end of mains low 30s microns. I warm up the pump with gas ballast 2, the everything else gas ballast 1, never no gas ballast. Are those micron numbers reasonable or should I attempt to get lower? Sure I could make huge jumps in temp or stir bar speed and get higher microns but as suggested, I go slow and watch microns. If they are low I speed up the temp increase a little. If they are high I slow down temp increase to decrease microns. Is that a reasonable approach, assuming no/minimal leaks?

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Thank you for the kind words, anytime you’re ready to discuss some upgrades I’m available. Just DM and we can get on a call.

In response to your run notes, those vacuum levels are great imo. However you shouldn’t slow the stir bar just to lower vacuum levels. Let the stir bar mix and the volatile fractions will quickly distill out, usually resulting in your vacuum sensor raising a bit. That’s normal and shouldn’t be avoided too aggressively

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Changing the pump oil will help get a lower vacuum and ideally pass THC faster at a lower temp. This should keep potency as high as possible.

I change my oil after every first pass and it always comes out smelling like volatile compounds. How often does everyone else change their’s?

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We change our pump oil after every distillation but we run a wiper with a way larger pump.

the pump your using is looking pretty new, let’s say you keep waiting a few runs to change the oil you will definitely notice a decline in vacuum over time.

Even changing it after every couple runs would be better than waiting 7.

Pump oil should be something you use a lot of it’s just the name of the game.

We usually empty ours after every run and then fill it with fresh oil, run it for a few hours dump it refill it again run it for a few hours and then leave another batch of fresh oil. Then again we have like 55 gallons of oil so we use it like no tomorrow.

I’m not expecting you to go this overboard but I would definitely recommend staying on top of changing the oil.

I like to leave my ballast open when flushing or when running lower boiling point fractions to allow some vapor to off gas from the pump.

Your doing great and it sounds like your really taking the right steps to be successful at what your doing.

Always here if you wanna message for questions :pray:t4:

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@DetroitLove and @Chewwie I will be changing the oil tomorrow before firing the still up, thanks! I was just being cheap and not seeing an increase in microns I figured push it as long as possible… I guess that does not make sense because any volatile that gets past traps is in the oil. I notice if I keep the dry ice slurry full in both traps, the microns decrease. I should probably buy some glass crystalizing dishes or similar to run dry ice or wet ice slurry to cool traps collection flasks. That would probably help keep volatiles in liquid state and out of pump oil.

What micron readings do most people get on volatile strip, mains, and the slowdown at end of mains? I searched and found talk of 55 micron, single digit micron levels which seem crazy to me without diffusion pump, then people with pump and vac issues in the hundreds to thousands on microns. As an engineer I get the fact that Clausius-Clapeyron equation is used to predict boiling point changes as pressure changes, in this case decreases really low (lets say 40 microns crv pro 16 vs 4 microns pump plus diffusion). Is that couple degree C decrease in boiling point really buying me a perceivable quality increase? If so I’m down to start looking for second hand diffusion pump, but if 40-60 microns at full speed main body 600-900ml/H is good, no need.

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yes you should…except insulated and not glass would be my recommendation.

If you’ve looked at that math and only see a couple of degrees between 40um and 4um, that is probably more insight that some folks will ever have :shushing_face:

Deeper vac actually decreases the boiling point differences, making fractional distillation more difficult not easier…

50um sounds like a respectable spot to be. 5 is arguably better, but only if it doesn’t break the bank to be there. Seems more about bragging rights than functionality to me.

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not necessarily, at least not if you use the gas ballast properly

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