Wiped Film Parameters

thin-film
wfe

#42

As a rule of thumb the best way I have found to dial in potency is this method.

You take the amount of time to run your batch that came out lower than expected in seperation and double it. If it took an hour to distill the product then figure out what temp settings and procedures are needed to make the run in two hours.

The potency is almost assuredly going to be different and likely much higher. This is just a rule of thumb I have used and it dials it in pretty well. Once you find the very lowest temp possible to still run then you have a definite data point to work from that I call dead slow. Then the equation is about how long you are willing to wait. 10-15% faster than dead slow is about where I set my stuff and get minimal contamination.


#43

I am still working on perfecting this SOP as i will get a little smell to the distillate or some swirls occasionally, but here is a rough draft of it right now that i am achieving 93-96% THC regularly with. This method does for some reason unknown to me yet (and when contacted Pope, none of their engineers could figure it out either?) but during devolatization you will see terps flow down into where your THC fraction would normally go. I have a bucket that i just dispose of them in. Maybe someone can offer some thoughts as to why this happens, and the deeper the vac, the more it happens…

Winterize crude, 1 room temp pass after 4+ hours of sitting in 15:1 ethanol and then chilled to -80c. Maintain -40c or lower while filtering.

Recover your ethanol, i run mine around 68c @ 125rpm. Pour crude into induction pot w/ induction burner. Depending on how much crude volume, use a larger pot incase of muffin-ing. Set aside until your Pope and chillers are completely chilled and ready to be ran:

Setting up the 2" Pope:
I run two external condensers w/ polyscience chillers on mine, both at -20c.
140c for your first pass on the main body.
I have my feed flask wrap set to 110c.
Internal condenser set to 69c.
On my vacuum I have the swagelok setup to control vacuum, so what i do is leave it open and spin it open as far as it can be, so that once started it will not immediately begin trying to achieve a deep vacuum.

Once all parameters are in place, chillers are chilled then i begin heating my crude up. Induction burner set to 320f, put your safety glasses and lab coat/gloves on and have a whisk. Whisking constantly, bring crude solution to 140c. Depending on how much ethanol you have remaining, the material may muffin if you let is sit without whisking for too long. I bring the crude to 140-150c using a laser thermometer. Now, at this part it can be a little tricky and you will learn over time, but as you start to near 110c you should pay attention to how “foamy” the material is being and you may want to turn the temp down on the induction burner to let it idle at that temperature for a little bit until it starts to “foam” less. You will want to do this under a hood preferably, or at least with a fan pointed over the top of the pot to pull the smoking terpenes out of the pot and away from you and plenty of fresh air circulation. It can definitely get a bit smokey. By the time you hit 140c, you will want your material to have little foam on the top and not very volatile.

Once ready, i pour into the feed flask, cap it and turn the pump on.

Depending on how “foamy” the material is and how much you are loading in there, you will need to watch carefully as it may try to muffin. Flick your vacuum on/off if needed. I usually start around 50torr and gradually work my way down until the vacuum is fully closed and leave it around 2-3torr to degas for a few minutes. Once the material has calmed down a bit, close your vac and let it begin getting deep as it can go.

At this point, I let the material sit in the feed flask for an hour or two to degas as much as possible before opening it up to run. I can usually achieve 40-70mtorr and the material will show little activity up top in the feed flask. From there, I turn the wipers on to 50-60, and let it begin a semi-rapid drip. Usually around 150-200g/hr drip rate.

Once it’s done, remove your flasks. I pop my crude flask into an oven @ 120f to keep it warm. I then wash some ethanol through the system to clean it out, set my body temperature to 179c and let it dry. Once mostly dry, I put two flasks on real quick and put it under vacuum to remove any excess gas or residual ethanol.

Reload your crude material into the feed flask, all other parameters are the same except the main body is now at 179c. I however do not run my system at this point deep as it can go any longer. Using the swagelok attachment, i will actually decrease the vac to around 450-500mtorr. From here, the wipers go to 80 and same flow rate as before, medium to semi-rapid drip, approx 150-200g/hr.

If you have done it perfectly, your material should be completely still in the feed flask w/ no volatility happening. If so, you’ve done it correctly and you can open the drip to a steady stream, around 350g/hr w/ no potency or yield loss.


#44

At the point you begin to see your THC stream coming down, watch it and from there you can adjust the parameters to fit your material. If you want a little lighter color, decrease your temperature down to 178c or try letting off some vac.

You can increase yield w/ decreasing potency as you adjust the temperature. For example, I ran did 3 runs w/ 179c, 180c, and 181c and as my yield increased from 54%-67% at the highest temperature, my THC levels went from 96.3% @ 179c, down to 93% @ 181c.

If you are seeing swirls inside your distillate, you didn’t remove all the volatiles prior to distilling the thc. Try re-running the material again before proceeding with the entire run, or re-distill the THC distillate to remove.


#45

Fantastic reply! Many thanks, will definitely be experimenting with these parameters.


#46

Excellent SOP! Heating of the crude in the flask with vacuum allows for lower heat wrap temp. Faster decarb when necessary. I have not run double external condensers on a 2" system; only single @ -20C and cold trap with -60C stinger chiller or dry ice. I would think that this tandem setup you are utilizing would further eliminate terps from entering the main. I have seen it happen with an Agilent dry scroll that was almost too powerful for the system; I was doing more throttling than one should. Pope could not answer me as well. Side note: When vacuuming down, are you opening up then closing the bulbs on the end of each stopcock? (Feed Top, Feed Flask, Cold Trap). While they still have a lot to learn; is one of the most useful tricks Pope engineers taught me.


#47

Also to note, if properly done in the pot you can fill the feed flask to 1800ml immediately w/ little worry about it boiling up. Carbon scrub can also be utilized. While I agree that Cbleach is a fantastic product for SPD, i have not had success with it in the Pope. Filtered through silicate twice, but crude becomes very reactive and several runs are needed to to fully extract all THC. I would like to one day experiment more with it though to see if I can get it to work.


#48

It sounds like you aren’t doing a full decarb before running? Pope doesn’t recommend a full decarb of the material? Interesting that you don’t go to full vac depth for best purity. I had some of my best (highest THC% runs) on a VTA when I was having vacuum “problems” and not feeding at full speed (i.e., much less than 1L/hr).


#49

We are using bho made from dry trim, winterized in etoh:

After etoh recovery, we do a decarb/devol in the roto (90+c) 50 torr.

Using a 2" pope, we do a first pass at around 105/50c (evaporator/internal condenser) and run it around 1 torr. ~350ml/hr @ 35%

My second pass parameters are as follows:

Evap 148-155c
Int cond 98c
External condenser 0-10c
35% speed
~250ml/hr
Vac usually settles out at 50-100mt

We’re getting 96-97% product. no swirls, electric yellow color.

I’ve had to adjust evaporator temps based on what I was running, however. This is just the process we use on our in house material of known quality. This doesn’t work for all material.

The pic doesn’t do it justice, always looks darker than it does in person.


Chiller solution
#50

Had to run clean up on some distillate made on an spd and my evaporator temps were way lower and I still didn’t achieve the best color, but it was better than it was when I got it. Got about 80% return.

Had to run this at 135c/98c and 50-100mt to keep the red streaks out.


Before


After

No swirls, and it’ll look fine in cartridges/buckets. No word on potency yet, but I’d say we’re in the middle 90s.


#51


This is a test result from our cart disty (made with the 148-155/98 sop) dosed with 3.5% terps.


#52

Yup, very good point! One has to purge the backsides of all the stopcocks!!!


#53

Thank you! Nice work, color’s fantastic on that final pass

Below is an image for those of you wondering what the “Backside of the stopcock” is.
(I know, it sounds dirty)


#54

That reminds me! The stopcock on the cold trap is also a good spot to isolate anything that may collect there. I purge the backside, then turn it so the hole is sideways. If I get a few troublesome terps that are ruining my vac stability (sometimes it only takes a few drops) I can drain them to the backside of the stopcock and isolate them from the system.


#55

I hate that stopcock with all my heart. Can’t believe it took Pope this long to finally update that.


#56

I can agree on that. The problem is that it’s the closest one to the pump, and has the most volatiles sitting right on top of it. Secondary cold trap might mitigate the impact.


#57

leave the valve open and run tubing to glass adaptor with a flask off that stopcock and some dry ice, it will remove all the volatiles out of the system and stop fucking up the vac.


#58

Not a bad Idea! I’ll have to try that. :ok_hand:t4:


#59

Any one know of what solution to use in my whiped film for the chiller and heaters? I’ve herd for chillers use iso but I’m sure there is something better anyone can help me out?


#60

Syltherm

https://www.dow.com/en-us/products/sylthermsiliconefluids#sort=%40gtitle%20ascending


Chiller solution
#61

Thanks. What’s the cost and where would I buy it should we just google it?