Theres a theory that Phoschek fire retardant used on wildfires has contaminated a huge amount of outdoor flower in places like NorCal.
I would assume that even though the contaminant is water soluble, it makes its way through extraction when unaccounted for. Doing a brine wash on crude may help…anything to remove potential catalysts before distillation.
Well I’m glad that could be the issue, and that I also have a 5L BF to use. Does suck that this material had such a low % but thats how you learn.
I have done multiple runs in this setup, however this was the largest and hottest we have ever done and the last batch that came back at 60% was the second largest. Our best test results (90%) was when we ran less than 3L in the 12 with a single pass and a fully packed head of 8mm rashig rings.
We will be doing another few run here in the coming weeks, we just need to stock crude first.
Our vac never gets above 100microns, we decarb the plant material so there is hardly any popping to deal with. This run was at 35microns 90% of the time and only hit 75microns pulling some residual ethanol. We wrap the head in foil and fire rope but it was still 30 degrees lower, we can usually get 20 degrees lower, however it requires some heat guns.
Our stir bar is constantly loosing magnetism- we can only get it up to 70 (on the lab society spin controller) even when there is nothing only the tails fraction left in the BF. We usually have a half ass toilet whirlpool going on.
How else can i speed up our system?
We do not have the ability to do a “full bore” setup yet… unless its absolutely needed?
Someone wins $10 hahaha
Change your stir bar, bigger and stronger is better, it makes a HUGE DIFFERENCE in speed and fractional separations
We have an indoor facility what catalyst could it be?
Could it be an ammonia production of bacteria in the soil of your plants?
Your runs dont seem that far off except taking a long time, but ive had runs take 24hrs and not have isomer issues…
But the general rule of thumb, low and slow is good color but bad test results… its a trade off… youre going to have to do alot of test runs to figure it out, id get a 2L version of what you have and try stuff like heptane washes and whatnot… if its a isomer issue due to heat and time a 2L would prove that, if you still see the peak… then it could be something else.
Check your plants though, im not a grower so i dont know much about what that type of thing could be. Relating to them…
Just curious about something. I use a BR spinning band to do my distillation and I was told that I should not allow vortexing to happen in the boiling flask. Is this true, or bad information? Generally I have my stir bar at 30,000RPM and it creates a very small vortex, but definitely not “bigger/stronger”.
Thank you for the help.
Unfortunately, I can’t show any R&D test results I have because of my confidentiality agreement. I developed the methods on my own though, so I have all the rights to what I came up with.
How are you accurately measuring the PH? Titration?
are you speaking of this: Diammonium Hydrogen Phosphate. I see it as a catalyst, but I don’t think it can do the kind of rearrangement we are talking about at the 100-200C range. Or am i missing something?
there are other catalytic ingredients in Phos-Chek besides the ammonium phosphates.
30000 rpm a magnet stirrer thats more than a homoginiser are You sure
Just currious
If you read the literature, d10 creation is a base catalyzed reaction. Refluxing with acid catalysis will reisomerize double bonds. The benzylic cation is theoretically the most stable carbocation but I haven’t researched the mechanism. Haven’t tried the experiment, but I should. The lit uses sulfuric acid, Lewis acids, toluene sulfonic acids. Btw, We see two peaks by GC in our “d10”. The d10 I was given, 80% pure by 1H-NMR, had the same two peaks.
I didn’t see the 1H-NMR, I can ask to get a copy and see.
We know from another source that the MS data shows the peaks to have the same mass as d9 etc. I haven’t seen the splitting patterns. I’ll request a copy.
That was a typo, its 3000 RPM
How do you clean your glassware? Are the plants the same genetics?
