Lolz, I took all my lab notes with an iPad as video. Then I posted them on YouTube. 28 vids showing all this stuff including DCVC chromatography, boiling points and info, and the horizontal distillation configuration. then… Youtube informed me I was violating their drug policy. All my vids voilate it it seems but it took tens of thousands of views for them to determine this lol. So sorry about no visual data because the vids got erased. They were just lab note stuff spur of the moment but it did show how to obtain absolute purities and two of them were dedicated to demonstrating visually the boiling points I will describe here.
Determining boiling points is a subjective assesment in a way at these pressures. My typical run once it reaches the cannabinoid are carried out at ¾ of one micron as measured by a Pirani style vacuum sensor. This of course is not achievable until all of the terpenes have been separated first because you really can’t pull down to ¾ of a micron during a boil when terpenes are still present in the compound. In fact the way I know to clean the cold finger and reinstall it to catch cannabinoids is by watching the pressure. As the pressure ticks down micron by micron it is an indication that the terpenes are being depleted from the puddle. Once below about 2 microns I pull the cold finger and clean with acetone and dry it. Then it is replaced and begins catching cannabinoid. Pressure tells me everything in my rigs.
My methodology first was to measure the boiling flask “head” temp in my horizontal configuration with a thermometer inside a double neck flask suspended over the puddle. Cannabinoid began to flow into the receiving bulb at 132C. However there is significant boiling that occurs before flow begins.
So then I switched to my cryogenic sublimation apparatus. With this apparatus I can look straight down on the boiling puddle and see the bottom of the cold finger suspended about an inch or so above the puddle. Temp sensor is placed outside the glass under the puddle. I run a batch every month for myself, sometimes two (I scrape the oil from my bong and vaporizer and run it again sometimes). I observe the boiling points routinely and based on this chart set my cryogenic sublimation apparatus temp to dial in the compound.
For “boiling” I considered the temperature at which THC begins to accumulate noticably on the bottom of the cold finger in the sublimator to be the boiling point. This begins at about 120C when the pressure is displayed as 3/4 of a micron. It will take a long time to run a batch at just 120C so I typically shoot for about 135C which can run the entire batch in about 30 minutes or so. I do not journal or any such thing and only seek to share info. I am very adept at isolating pure D9 THC in my home lab and my data is from observation. Pubchem provided one of the points for D9 THC which they list as 200C at 20 microns. I used their data point from 20 microns which fits the curve. I do not know how they arrived at their data.
I observe these temps routinely on a monthly basis. The problem I have using a sublimator for final refinement is temp control is critical for absolute purity. At 120C the compound is very pure as it deposits slowly on the cold finger. At 135C the product is still very pure but will include trace contaminates from the higher boiling compounds. At 150C the compound begins to darken up considerably and much of the higher boiling contaminate then gets deposited making it brown and dark instead of pale and yellow. Higher temps start to add even more contamination because the smoke point can be reached above about 165C and then foul flavors and smoke particulate are added to the compound.
Other than the two observed data points the rest of the points are computed based on the two observed points; my own observations at ¾ micron and Pubchem tech data listing boiling point they measured at 20 microns for Dronabil (the pharmaceutical equivelent of D9 THC).The chart and the computations are considered crude estimates other than the observed points but even as a crude chart it is the best tool available to compute such things.
Thank you for offering to host but if I transferred a video to you guys showing any of my labs I would just send it along as a gift for your use without restriction instead of fiddling with mirror sites and such and worrying about ownership lolz.
The nice thing about a video purge is that my labs are not scripted at all except that before I begin doing something I often arrange the gear in a way for a good camera angle. Mostly though I just grab up the iPad and get pictures that look interesting to me. So the vids that I took down from Youtube and that they took down we’re from older runs. Most labs reveal things to me that can be done better so really what I intended to show as a retired engineer is not just the technical details but also document how an engineering project evolves in an R&D mode. For me it evolves with a general vision in mind but the details get worked out by just doing it and see what works and what doesn’t then altering concept and repeat.
All my old vids all had technical errors and some even overtly blatant errors left in on purpose to show the progression of problem solving. I did not envision the videos themselves being of real value but was hopeful my fellows in industry could glean useful info from them. It is nice to see old blunders go away even when ready for the pot shot criticisms of those who could not see the obvious concept being deployed as I just described. The hit and run marijuanna experts made me almost immediately terminate all lines of communications from my posts because my doctor has placed me an a bullshit limited diet. It stopped being fun to post because I had to disable comments and block email from folks who for some reason painted me as a target. I have even gotten strange “flame” posts from at least one known supplier of distillation gear who themselves seem to have a dyslexic website in which virtually every procedure they describe that even comes close to my stuff is incomplete stopping abruptly mid SOP, has a complete lack of visual info (text only), and frankly when scrutinizing left me confused as to what exactly they were trying to communicate.
So it is kind of nice to have got rid of the vids because I ended up distracted from impolite posts instead of working towards my next goal, but also there are better ways to do some of the things I made vids of now for me. For the record I am absolutely progressing toward a highly specific goal and the credentials I have claimed is a clue to where this is all going but refinement of process as an SOP in itself is being employed in a manner I am experienced in. Mostly I enjoy sharing but the nuggets of info back from even casual comments all add up.
A vid request for DCVC run is no problem for me to do really and I would not mind just gifting it to your blog for whatever use you see fit. I owe everything I know to those who came before me in this world. For my own sense of spiritual completeness I do not need to pay back those who came before and gifted me schools to go to, roads to drive, and clean water to drink. I would much rather pay the gift forward so those coming along after have a good life too. A ripple grows into a wave. Let me see what I can come up with?
Let’s get some videos up for sure, I’ve tried robbing my OTSS chunks, then washing and decarbbed under vac, ended up with some really clean beautiful stuff, gonna give another go soon.
@Soxhlet mentioned this while helping me, he’s been freaking awesome to me!!!
@Beaker, firstly thank you for the abundance of information you have/are sharing with the community!
Secondly, the profile pic of a dogs nuts… hilarious!
Thirdly, I would love to see some vids of your preferred distillation apparatus in action! With your knowledge and experience of distillation perhaps there is an SOP that could be developed for first timers looking to try distillation?
Those are dog nuts??? Wow. That explains a lot. That is Houdin! I have a Tegan too but she prefers more discretion when snoozing…
I am not the one that has experience creating an SOP and I would drive you nuts how much I change up all the time in procedure. I explained once before somewhere I am in R&D mode and have been these few years figuring out a general flow from micro process to micro process that is least complex, least cleanup and loss, and obviously purified med. I am not there yet enough to really be the SOP sort of guy imo. Plus I am pretty flaky…
I know precisely what you are talking about and it is the reason I share online. Because when I started this even such fundamental information as the accurate boiling temp of the compound was not even known. There was much speculation of course but damn little visual evidence to verify anything. My payback is the information nuggets that ALWAYS pay back big time even if it is from a post that tends to flame or unfairly scrutinize. I have found that putting out effort always seems in some way to rebound back and so in this way is selfish. Humans do stink and make messes and stuff but I like them and want to help them out I guess so I post things I would want to have had posted for me.
The owners of this blog are the SOP folks and understand that realm far better than most imo. I support your idea and would gladly assist for a micro SOP for beginners to distill personal quantities. I suspect the best one to solicit would be @Future. Just to prove there is a dog attached to the nuts here are both!
I would talk about you if I could!.. but all I know (don’t actually know just assume) about you is that your a passionate and curious cannabis enthusiast who has the right attitude of sharing and helping people.
It sucks that people such as your self, who have nothing but good intentions, get torn apart on the internet for sharing helpful info. But that is the way of the world these days unfortunately haters will always hate and jealous people will try and pull you down but keep moving forward and you will always come out on top. Atleast on this forum I would like to think that people will not tear apart your flaws if you do share videos. It seems that most people here understand that we are all dabbling in relatively uncharted territory and are all doing our best to learn and contribute to the wealth of knowledge about the chemistry of our favourite flowers.
I am excited to see where your R&D leads you! I have seen you drop a few hints around the place about what your working towards and I can only assume it’s a scalable and potentially automated distillation apparatus. I am a big fan of chemistry and engineering so am very intrigued to see how you or others approach the challenge of commercial scale distillation automation…if that is infact what you are trying to achieve, I’m just throwing out a guess.
Thanks for the kind words. Please let me offer you another possibility in the spirit of “think tank” talk only (this is not a hint lolz) let me ask you this about your the idea you pose above.
Would it be more of a challenge and potentially more useful to the general population to design a perfect large scale commercial operation capable of producing pure medicine for sale,
OR
Would it be more of a challenge to design a hand held unit that could take crude extract and produce pure THC for the patient from a 120VAC socket in under ten minutes and with no particular technical expertise required?
Option one large scale has economies of scale to benefit from in producing, storing, shipping, and delivering pure med.
Option two would have the benefit of no cost to store and maintain pure med other than the existing supply chain (dispensaries and processes already in place).
Which one would you pursue as an engineering effort?
Very interesting question and I believe the answer will hinge on what goal is trying to be achieved. If the driving force is making money then commercial production would be choice. Although I am not a huge fan of money and what it does to people. I personally think that a portable device that can be used by anyone would be a much more desirable goal to pursue. Mainly because this will help educate and spread awareness to many many people that would otherwise have no idea about the concepts of distillation. I believe that the benefits of educating a large population of people far outweighs the benefits of making yourself rich.
Ebizzle is the shizzle. Like half my equip comes from there because I live in an location where I can’t exactly walk in to a lab supply store for my needs
@Beaker your posts are some of the best on here, don’t stop. And the haters comments and your sarcastic dry humorous remarks are some of the best parts to read as time consumming as they must be. To answer your question I believe #2 would be more of a challenge. #1 has already been done to some extent. And has not benefited the gen pop in a significant way.
Right now people have to rely on test results from dispensaries or their buddies word both have proved unreliable when it comes to actual THC content. People including myself would rather do it themselves if it was easy enough to understand…with legalization polling strong everywhere, more and more people will be growing their own flower. When it comes down to it we all just want control, over everything. No one wants to rely on anyone for anything. #1 just helps the rich get richer, most who have nothing to do with the cannabis culture and decades of activism leading up to where we are now. #2 could actually be night average Joe consumer.
Can we dream bigger like a hand-held that turns flower/plant matter into pure thc. If hand held is too small, countertop coffee maker size works for me if your taking orders.
That last line makes me think of a shop that converts fresh nugs into dabs right in front of you like making your coffee. Even better if they do dabs and coffee at the same time, one stop breakfast shop
When I was in grade school nobody in our family in Oregon owned a microwave oven. Back then it took a bare minimum of thirty minutes as a practical matter to turn a potato from weapon use only (long story) into something cooked that I could eat. For that kind of speed, thirty minutes, I am not counting the cleanup. Ovens are no clean up but take very long to warm up and so forth.
Now fast forward to today. I personally cannot recall ever owning a microwave and I do not now. I have used them though of course and now a spud can be degraded to non lethal and edible hot and yummy in about two minutes? I could be wrong because my lab does not employ microwave energy… but do you see my point?
It might seem outrageous in this moment to imagine popping a bud into a unit and setting a knob and in two minutes have it produce for you absolutely pure D9 THC or CBD or ??? but only because the arrow of time is presented as an asymmetry in our existence from our own individual relative perspectives.
haters will always hate and jealous people will try and pull you down but keep moving forward and you will always come out on top. Atleast on this forum I would like to think that people will not tear apart your flaws if you do share videos. It seems that most people here understand that we are all dabbling in relatively uncharted territory and are all doing our best to learn and contribute to the wealth of knowledge about the chemistry of our favourite flowers.
