Try distilling under strongly alkaline conditions with hydroxide or something. The more straight forward way would be to use a super base like butyllithium, but as a professor once told me, “you can usually get a reaction to go if you just get it hot enough”
8 Likes
Still waiting for the analytical evidence demonstrating that this is in fact d10.
4 Likes
That too is a good point. This whole delta-10 = CBC on chromatograms thing seems to be totally unsubstantiated
5 Likes
If you haven’t seen it already, watch the video in the thread below.
3 Likes
Is there a reference for this? Only way I know how to tell the difference in the alkenes would be a 13C DEPT experiment where secondary and quartenary carbons would be more obvious from primary and tertiary carbons.
2 Likes
This video started the whole delta 10 thing. What people fail to understand, is that d9-thc degradation to delta 10 HYPOTHESIZED at the end of the video. It is not proven, and it isn’t even a really solid hypothesis, just an educated guess by the guy in the video. Most people who aren’t formally trained scientifically seem to mistake a reasonable hypothesis for proven fact.
I have been repeating this point ad naseum on this forum, but I think it’s worth doing to get people to think critically as we continue our research and discovery about cannabinoid science as a community.
18 Likes
Right on my friend, right on.
@Kingofthekush420 the sample that @highestzen posted the NMR results for was not a product he created. Fusion Farms supplied the Delta 10 sample, and he assisted in purification process. Yes D10 has been created, yes it can be crystallized, yes the NMR tests have been performed and showed 89% Delta 10.
9 Likes
i can confirm this. when we first started seeing it on bad BR distillation runs we thought it was CBC. Careful analysis of the 200-400 spectrum and retention times show it is NOT CBC. We have not worked up the samples to purity, so I can not call it 10a, but i have done spike studies on the HPLC and spiking a sample of bad distillate with the “mystery” (probable 10a) peak give 2 peaks in the retention time window, showing that the unknown peak is NOT CBC, but something that eluets very close it on our method. A sloppy lab could easily call the peak CBC.
7 Likes
The guy behind this video is presenting next week at ACS in florida.
1 Like
All that shows is a mystery peak eluting near CBC, it doesn’t show it’s Delta 10. I’m wondering how people made that inference.
1 Like
i would imagine most people were using the starting material as the basis of the D10 hypothesis. if you’re starting with THCa or Delta 9, then I think creating a conversion to CBC in distillation would be very unlikely. There are also other ways to identify minor differences between the 2 cannabinoids. On both HPLC and GCMS.
I know when I used to do potency testing and i’d see very degraded distillate, I would always see at least three mystery peaks, none of which was D9 or D8 (which we had standards for). So there must be something else going on. Unfortunately correlating GCMS peaks to your HPLC peaks is difficult (and the ion spectra are very similar), and LCMS libraries for unknowns do not have these compounds either.
Here is a comparative chromatogram from back in 2015! The black is good distillate, while the light grey has “mystery peaks” and low potency.
Distillate Comparison.pdf (46.7 KB)
You’ll notice at least three big mystery peaks (and none of them are D8). The third one elutes close to CBC. The other two are total unknowns! I saw this over and over again and I never was able to identify the compounds in question, but it is definitely a more complex mix than D10 alone. In fact it’s possible none of it is D10 in my mind. I certainly can’t see why D10 would be the one co-eluting with CBC anymore than it being any of the other mystery peaks.
Also note the “CBC” peak is not even the largest one. I think people have focused on it because labs return that peak as CBC, while the others don’t even get reported and go invisible. But it does not appear to be the primary degradation product.
6 Likes
I think once we come up with methods to identify and quantify these isomers distillation is in for a rough time. I have a theory that practically all distillation is causing isomerization fro d9, initially to rotational isomers of d9 and eventually to positional ones.
Simple bioassay is enough to demonstrate the degradative effects of distillation. Try comparing the effects of thca crystal to high 80’s to low 90’s d9 distillate. For me and and many others they effects are not even close in intensity. I am sure someone will start putting 99+% d9 from either sfc or low pressure chromatography on the market someday, and that really will put the final nails in the coffin.
3 Likes
To be fair, I’ve never seen any of these isomers crop up with wiped film.
10 Likes
Yep, residence time matters for sure.
8 Likes
Yes, a single pass or 2 on wiped film does not seem to have the time x temp needed to cause the d9 to positional isomers, without catalyst present. But there are confirmational changes that might/probably be occuring at lower temps, that most labs can not currently detect. Also, it is very challenging to routinely achive d9 (not d9 plus d8) numbers in the 90’s with wiped film. Multiple passes, scrubing, and very low yields result. Every pass on the unit is another heat cycle, and I would be willing to bet that if one runs the same primary extract through a good spd and multipule wiped film passes to achive the same potency, we would start to see compatible degradation. Wiped film is a better method, but it lacks the purfication ablity of spd.
1 Like
Hi! Interesting discussion. I also see a myriad of mystery peaks from many distillates using GC or LC. With enough samples, some correlation of LC peaks to GC peaks seems possible although it may do little to identify the compound. The uv-vis spectra isn’t very informative. The industry needs more reputable standards.
1 Like
I dunno, in my experience every method of distillation is heavily dependent upon good filtering and scrubbing methods prior to distillation if you want to hit those high numbers. It doesn’t matter if it’s SPD, WF or SBD and of course yield goes down as purity goes up regardless of the distillation method. I have seen the same crude run through all three methods and each has it’s pros and cons. If you have low grade crude with lots of residue (the black tar left over in the pot flask) it has a negative effect on each of these distillation systems. For wiped film you just end up with extremely low yield because the tar doesn’t get hot enough in the short residence time to wrestle out a lot of the CBD. It acts somewhat like an azetrope so you end up with very low yields. For SPD and SBD the yields are still low with low grade crude but you can wrestle more from the tar. However, it will require a second pass because of the smoke that is generated from the tar. It contaminates your distillate as well as your vacuum pump oil.
So, ensuring you have high grade crude is imperative regardless of the method. Distillation can only do so much no matter what method is used. But wiped film is just as capable as the other methods if you know how to manage the system parameters properly. It’s just a little less tolerant of low grade crude and all that goes with that whether it’s compounds with low boiling points (volatiles) or higher boiling points (tar residue).
2 Likes
I can hit 99% total cannabinoids easy on a wiper everytime. A wiper has better seperation then an SPD for 2 reasons. 1 a wiper has way deeper vac and 2 your pulling vac on a thin film instead of a whole ball of material. It sounds to me like youre not running your wiper right
5 Likes