First time running a short path distillation setup. Comments and Suggestions Please!

diy
distillate

#61

:+1::grinning::poop::star:️:boom: Good job and No worrys If My time calculations are about i don t expect more than 5% CBN [quote=“Killa12345, post:59, topic:5927”]
up.
[/quote]


#62

Thanks for everyone’s help. I’ll make a little wrap up and what I learned in the morning. Definitely a learning experience. It would have been much longer for me to try this if not for the community here. You all gave me the confidence and the knowledge to pull this off today. Thanks to everyone that lent a hand here or any of the other spd beginner threads.

Thanks from the bottom of my :heart:️! Seriously you all a great! Have a wonderful Friday and weekend!

First pic is the tails second pic is the body


#63

So let wrap this up on what i learned. I hope the failures shown in this thread will help out members in the future so im going to list a bunch of stuff i wish i would have done differently or learned throughout the process! This list wont be in any particular order just spitting out the thoughts as i have them and will update this post as i think of more!

Pre-run thoughts

  • I think the first and foremost thing i would have changed is my fear for the process. While the process could look daunting at first. It merely a process where you watch a “number” which is the head temperture. And change the receiving flask when you short path head hits a point.

I think the fear comes from the amount of concentrates or raw material one run can take. Usually it takes thousands to tens of thousands worth of raw concentrates just to run. That can be a pretty scary bet for some.

  • Next is the notion that Chinese glass cant do this properly nor get down or maintain an adequate vacuum. I understand that i see some peoples process down in the single digit micron range. I cant recall seeing a person using GL fittings getting that low on first pass though. People have been using chinese glass for decades. Maybe not in the cannabis industry but in just about every other industry. I feel like if i really had a bit of time and a tank of helium. I really could have pin pointed my leak or problem and got my system below 87 microns. This was just rushing. Literally i spent absolutly NO TIME trying to fix this. Once i saw my system empty was under 100 microns. I stopped right there knowing id be starting much lower than i see people start.

I feel as cannabis users…we are inherently a bit lazy. Im the laziest piece of work there is…If there is a “work smarter not harder option” the cannabis user usually picks that option…Why…why else so they have more time to dab! LOL

  • While we are on the subject of vacuum. Find an adequate vacuum pump for your application THEN buy 2 sizes up. LOL This might have help me achieve that low vacuum. Yes, my vacuum pump might have been overkill for my system but it made the job super easy and i bought my pump USED. Flushed per the directions in this thread and my pump was pulling to ultimate vacuum
  • While we are still on Vacuum…buy a real vac gauge. How the hell are you going to know you have a leak or are even capable of distilling cannabis with a possible high vac level if you dont know the vac level to begin with. Really i cant even understand how people get around this. This was probably my biggest confidence is my system was under 100 microns which i see a lot of people start in the 200-300.

  • Next dont buy shitty lab stands like i did. My lab stands sucked and i had a fear of my cheap $500 glass set up was going to fall.

  • While we are on dont buy stuff…dont go stupid overboard like i did. I fucking bought every single filtering aid i read on this site. I was taking 2+ year old material that was improperly stored and trying to make gold out of it…LOL That dont happen. Filtering aids are going to help filter. They will not turn water into wine. This could have saved me a few 100.

Not to mention i bought 3x identical vacuum pumps…musta been stupid high that night and thought “what a wonderful idea…lets just buy 3x of them cause they are a great deal, what happens if i wreck on the first run?”

The 7l heating and cooling circulator MIGHT be on that list too, but i dont know if a pool pump would circulate 80c water like my circulator did yesterday…so this might be good, but i could have just bought a HOT WATER one for half price. I bought mine only for $800 shipped and i think it will come in handy for my CLS as well

  • Find a way to vent your vacuum pump outside. This is another must do!

  • I bought a fancy kangaroo traceable thermometer but it just gave me issues. the $3 cheap mercury head thermometer worked and was my origanal source of vacuum leak was the kangaroo thermometer adapter. Once i change the thermometer for a thicker mercury one. My vac levels got sub 100. Sometimes cheaper is better.

During Run

  • This is probably the most important detail. DO NOT WALK AWAY FROM YOUR SHORT PATH FOR THE FIRST HOUR OR SO. This is how my round 1 ended. i literally turned on the vacuum walked over toward my dab rig for a hit and BAM! OIL IN MY HEAD ALL THE WAY THREW TO MY RECEIVING FLASK! Literally under 10 seconds. This would have saved me a ton of time and frustration yesterday. i didnt realize how fast a problem or error can happen.

  • If this is your first time. You might want a vacuum vent valve close and handy. Even though i had one. The first time i didnt realize how fast a problem can happen. When i read Summits Short Path SOP. I wondered why you want certain vac levels at certain temps. This is to prevent your oil boiling over into your short path head if your like me and unsure of what impurities still lurk in your oil. You will need to throttle your vacuum till around 100c if you suck at decarbing and dewaxing like i apparently do…Even though i followed the GLG decarbing SOP and added time to that on top of whats stated.

  • I had fiberglass rope around my BF when i started. Ive never seen even what happens. This was a mistake. Once i learned what to look for when my BF is boiling over…I was able cover the rest of my BF with Aluminum foil for the rest of the run. Even though this is counter productive and your probably gonna lose a % of THC to CBN. Your learning. This isnt gonna go perfect first run…Its a bumpy road ahead.

  • Run slow. And when i say that. I mean once you get past 140C only raise your mantle temps buy 10C a time and chase your mantle up to the thc BP. This really dont take long. I looked back at my notes from yesterday. I started round 2 at 10:45am by 12pm. My head temp was 130C i saw a sudden and real sudden thicking of the concentrate coming from the head and knew i was close to the THC. By 12:15, I was on the THC(first time my short path head broke 155C). And at 12:30 i rotated my flasks to the body flask. It doesnt take long to get there. It takes long to collect. So dont rush!

I had my condenser on 30C till i saw that change at 130C on the head temp…then i raised my condenser to 50C which i felt was too cold still. My short path head kept clogging with oil. so i eventually raised it to 80C. This is where a heat gun is almost essential for me at least with chinese glass. i dont know if everyone experience the clogging but it was a pain in my ass all day until roguelab’s tip of the day! After this. my run when ultra smooth.

  • Heres another tip. Test your condense fittings before you run. I noticed one of my fittings was leaking. I was able to catch it quick because after my round 1 fuck up…i didnt take my eyes of this apparatus for hours after. I was able to wrap it with a paper towel which worked till the end of the run.

  • Heres another thing i had a big fear of. Turning the cow to different receiving flask. I kept reading what summit said about this and how unsafe it was. By the way he was talking, i thought this was going to have major resistance and hard to more…NOT AT ALL This is a greased joint that moved super easy and one of my biggest fears was stupid!

  • It was a bit hard for me to see the red when i happened. I might have switch my flask a tad bit premature but once the head temperature hit 170C or so. The color was noticeably red, and i was happy i had switched earlier.

Post run

  • Buy a Ultrasonic cleaner. A large one. I bought a 30L one think it was super overkill. It wasnt. There was nothing i wanted to less then clean all this glassware after running for so many hours. Its was so easy to rinse most of the stuff out with acetone…then throw it in the ultrasonic cleaner with alconox. This was so worth the $250 i paid… I would have just about paid someone $100 to clean up after me yesterday…but this made the job super simple and my glass ware looks spotless.

  • Probably not needed but it came in handy was a nice lab drying rack. I got mine off amazon for $90 and it made drying my now clean glass and keeping it very organized.

  • Splurge for some kem wipes. I didnt and i really didnt like using a lint free paper towel and acetone. They arent expensive and first on the purchase list for me.

Ill update this as i think of more things i learned. This should help out an of our begnneers like me and hit me up if you need help…the people here helped me…time to pay it forward! thanks for viewing ask all you want.


SPD sop
#64

Thanks for this detailed walkthrough, can’t wait to tackle this beast next, haha wanna sell one of those extra vac pumps?
The problem I see with American glass is they think it’s made of solid gold and sell it as such…


#65

Isnt he silly?
Good run, and nice write up. It definatly sounds like you learned alot. Now time for the 2nd pass!
You will want to wipe out any ground glass joints that had grease with hexanes, not too much cuts that grease.:love_you_gesture::sunglasses:


#66

I lost count of the times I had to deal with this sort of thing. For me I really make sure the decarbing is done if at all possible before it goes under vacuum. I also have a vent valve that will not break vacuum if the pump is running. The valve is electronic and if the switch is momentarily pressed the valve just bumps open briefly. What a great asset when dealing with first run stuff that can bump up like that.

The trick is all in attitude really. This stuff pisses me off when I have to deal with it but honestly it does not take that much to restart. Having any sort of leakback valve for initial pull down sure has helped me but my stuff is obviously coping with a bit different scenario.


#67

I find a variac gives me the best temperature control and the most even heating, far above a PID which is above a dimmer. A guy from california is selling a good variac for 38$ shipped, I got his 46$ version (10amp).


Distillation controllers with both temperature and power control
#68

thats cheap for a variac, got a link? I wouldent mind picking up one. The advantage of the pid is the automation, if you walked away from a variac you could have a run away distillation.


#69

:blush: You made my day…

Yes, a 10 amp Variac will do, but I still recommend splurging on a 20 amp because sooner or later you or someone else will use it to control a motor, and for that purpose you should have one rated for double the device power you’re trying to control.

Variac page at eBay:
https://www.ebay.com/sch/i.html?_from=R40&_trksid=p2380057.m570.l1313.TR12.TRC2.A0.H0.Xvariac.TRS0&_nkw=variac&_sacat=0

Brand new 20 amp Variac for $72.95 with free shipping:
https://www.ebay.com/itm/Auto-Variac-Transformer-AC-Metered-Variable-Voltage-Regulator-0-130v-20Amp-2KVA/323013011922?hash=item4b351369d2:g:cegAAOSwZFdaYWnj:rk:2:pf:1

For smooth boiling/distilling you should have precise power regulation, but to just hold a liquid beneath it’s boiling point a PID controller rules.

I’m dumping for free all my stuff, controllers, solvent stash, everything related to cannabis down to my Mobius Matrix bubbler due to my big brother kicking me out of the house that was supposed to be mine to live in until I die, and I can’t afford the rent somewhere on my measly Social Security check. If someone with a lab in Southern California would take all of my stuff, AND offer me either a little something each month under the table for whatever services I can offer, just enough so I can afford rent, or provide me a room, I would greatly appreciate it. I have until January 1st to get out, or the cops will be at my door, and I’ll be on the street or in a board and care. I’m old, but responsible when called upon, surely someone could use me to monitor an SPD unit during a night shift, wash the glassware or do something no one wants to do for cheap. I made tentative arrangements with some youngsters from Orange County a couple of days ago to take everything, but I don’t think they are a perfect match for what I’ve got, and I’ll still be homeless. I’ve contributed every resource I have for free for the last six years until I’m broke, anyone who’s followed me at Toke City and ICMAG Forums knows of my work, please, I’m begging to go on contributing and have a little life until I really need to be cared for. Thanks brothers and sisters for the friendship, much love, John Schuyler in Sun City (I’m from LA --> Orange County and absolutely would like to return to one or the other) Picture of me being served a HUGE masala dosa in Little India Cerritos, yes I’ve been ‘dosed,’ many a time… I’ve let my hair grow out since that pic, I’m back to looking like a hippie.

Here’s a list of some of the stuff I’ve got:

My cache of solvents that I bought to prove they were readily available to anyone, they’re untouched since I posted up about each purchase, my mom’s hope chest is full of the liter bottles and four liter jugs, nifty stuff.
Solvent list:
https://www.icmag.com/ic/showpost.php?p=7933632&postcount=162

Cases of surplus butane refills I purchased doing the mystery oil testing - includes a full tank of butane minus what I used for the test.

Stock pot vac chamber, silicone heat mats and controllers, the distillation equipment and controllers I’ve been experimenting with etc…

Iso 3, never unpacked

Authentic Pyrex scientific glassware containers, other glassware… test tubes/watch glasses/pipettes etc. - all new.

Cannabis and lab science reference books.

A classic Mobius Matrix bubbler in perfect condition with accessories, nails etc…

Soldering iron dab station (heavily used but functional) with extra replacement pieces.

I have a lot of tools, digital variable speed Dremel tool with all the accessories to make it into a drill press, miller, etc., mechanic’s tools, electronics equipment, soldering irons, heat gun, nice selection of 3M heat shrink tubing etc. but I’ve yet to decide whether to somehow hang on to these or give them away - if someone would really would appreciate them- it’s theirs.






Cannabis Alchemy Extraction Method vs. Modern Etoh Extraction Methods
#70

Do you turn the mantle temp all the way up, then use the variac yo adjust temp at desired spot?

And wtf is that in the last pic? Looks like an epic taquito


#71

This is really sad @SkyHighLer. I really hope someone in the southern california area can find something for you to do in this industry.

Never been on Tokecity but ive followed your work for a very long time on Icmag. I believe your work on butane alone should warrant you a place in this industry.

Really saddens me to hear of this. I think we need to move this to its own thread so it can get more eyes from the members here. Maybe we can create a gofund me page for you cause it seems like you need a hand and its even shittier that your considering giving away all your stuff. This kinda reminds me of a situation i went threw 15 years ago. My son’s mother just passed away in a car accident, i was in my late 20’s finishing up 2 masters degrees, raising a kid by myself. I had to make a choice…i had a certain amount of money; no job. I had to pay off my last semester of college or pay the rest of my house lease off. Could dont both… I literally had to sell every last possession of mine to be able to rent a room and finish of grad school. Me and my son lived in this rented room for 6 months before i could find a job. It was a big turning point in the way i lived my life.

i know what its like to lose every single possession in order to make it one more month. It was the most depresing time in my life. In one hand i was trying to better myself with education…the other i was going broke and homeless.

@sidco and @Future is there anyway we can move these last few post to its own thread with hopes of getting our brother @SkyHighLer some help! maybe the brain collective can think of something better than my gofund me idea??


#72

@SkyHighLer

Wish I could fly you out to detroit for a day or 2. I’d prefer to pay for experience vs me stressing running my spd.


#73

Here’s a picture of the inside of a Chinese stirrer/mantle someone sent me with a similar question.

The first obvious problem is the circuitry for the stirrer and mantle so co-joined you can’t simply go in and separate them. My suggestion was to disconnect the leads to the mantle, and bring out a new pair you can plug directly into the Variac.

If you have a built in PID controller, you can’t go in and bring leads to the outside to insert the Variac between the controller output and the mantle, the solid state output device(s) of the controller will go crazy trying to rapidly throw the Variac impedance. I tried it, fortunately my SS relay recovered, this lead me to the PID or ON/OFF or Limit controller firing a mechanical relay I could feed the output from the Variac through.

Here’s a few pics, Kill-A-Watt power meter --> Variac --> Auber SYL-1512A controller with mechanical relay --> heater



The Variac connected directly to the mantle will work just fine as gonzo stated, having a ON/OFF or Limit control to ensure the temperature doesn’t creep up while you’re not looking is the point of the temp controller.

The best way to go is with a Auber DSPR220 or DSPR400 distillation controller that drives the mantle at whatever wattage you choose, and then drops the wattage to a level of your choosing at a temperature of your choosing to start the actual distillation and maintain the speed (level of boil) just where you want it. At that point, you can step in if you want and set up the controller to lock the temp in like a rock with the trick I came up with that is posted up in the Advanced Distillation thread I have up.

(A dosa is a giant crepe made with rice and urad dal flour, a South Indian form of bread, it is rolled/filled something like a burrito with a spicy potato mash - always served whether plain or with stuffing with a thin dipping soup called sambar, personally I prefer North Indian dishes served with fried bread called puris. Find your local Indian community and look for what is called an all vegetarian sweet shop, they’ll also have salty savories and quick snacks like dosas, go in stoned with an empty stomach and eat like you’re the Chief)


#74

Skyhighler beat me to it :slight_smile: I was thinking about using the Variac with the PID but it is so easy to dial in a temp with the Variac that runaway doesn’t really seem like an issue. I guess I could use the PID in on/off mode as a ‘fail safe.’

I’m thinking about ordering a bigger heating mantle liner from deschem and then making my own heating mantle that is big enough to cover more of my reaction chamber. I hate how the top of the damn thing is always cooler.

@SkyHighLer Don’t give all your stuff up, yet, things can change quickly and you never know what opportunities might come up. Sell some of it if you need to or trade it around to take care of business but no need to make hasty decisions in the face of tough news.

As for the chinese mantle I would cut the leads that go into the heating mantle liner and run new leads to the variac personally. As mentioned you cannot simply plug it in because it would mess up the circuit and the stirrer. The problem with PID is that it is lazy and the programming tends to prefer shorter but stronger bursts of heat (minimal input) in order to maintain the temperature. I prefer lower but longer (more gentle) heat. On my first run I noticed some carmelized something or some residue on the bottom of the RBF that I was sure probably came from hot spots or high intensity heat when the mantle was working to keep up with vacuum coldness. After that I used the PID with a dimmer and burnt out the dimmer on my 2nd run :slight_smile: Now I use the variac and it is killer!


#75

Thanks for this writeup, I’m trying to get my SPD system up and running and this has been a huge help.

What is the product name for the apparatus that the vacuum gauge is inserted into?


#76

It’s a kf25 to 1/8” female npt adapter.

And glad it’s been a help. Feel free to ask any questions needed and I’ll try to get back with you as soon as possible.


#77

Is there a reason you went with the 4 way KF25 fitting as opposed to something like this https://www.ebay.com/p/Adaptive-Tee-Adapter-Kf25-X-1-8-FNPT-Fit-Most-Vacuum-Gauge-NPT/22024020465?iid=223155521318&chn=ps

Also what type of rubber tubing is that?


#78

That was the exact adapter I originally wanted but they were outta stock at the time. But after I set everything up I’m kinda glad I set it up with the 4way kf25.

I wanted a way to break vacuum because I had planned to move to a single cow system eventually and knew I needed a way to break vacuum to switch cows and receiving flasks.

I really spent a lot of time thinking about the vacuum setup. It was very expensive this way but it left me future expansion.

I knew I wanted a close off valve for the pump, vacuum vent valve, spot for my bullseye. This was how I configured it to meet my needs. I’m sure people can improve on my layout.

The rubber hose is a high vacuum rubber hose. Here is the link.


#79

I had some rubber hose similar to that and my vacuum pump didn’t collapse it but did compress it in a few spots. Deschem sells the 15mm OD which is what I used but I am switching to some stuff from ideal vac that is really thick (seems much more thick then they said).

The little one is the deschem and the big one is ideal vac.


#80

Need to go full bore . Those hoses IMO don’t work