Hi guys, I’ve read for many moons, and either need someone to walk me through the Sulfur method or to sell and walk through a useful method. Have a Reverse Phase flash system, so can purify if need be. Please DM details
What’s the main issue that you’re having
Mostly that I don’t have time to conduct a long period of R&D, so before I attempt the Sulfur SOP, I’d like to talk to someone that’s done it- I’m pretty good with a D8 SOP I’ve been refining for a while now, but have never worked with Sulfur. The heat + oxidation (possibly with UV) seems like it’ll be weeks before I find out what the outcomes will be for various attempts. Just need some guidance is all before I try these procedures
1 Like
That sop is stupid frustrating and doesn’t even begin to really explain shit and you’ll have to modify the hell out of it to get it to work. Don’t put the gas trap on dry ice, it’ll freeze solid and then the hydrogen sulfide won’t go through the solution that’s supposed to make it inert. (Spoiler alert it doesn’t do shit anyway) gotta use a fume hood for sure and you’ll want to run the reaction til it’s done evolving hydrogen sulphide and then a bit longer. It stinks like egg farts, and It’s for sure not gonna be done in whatever arbitrary amount of time they claim in the sop. Half the shit in the items needed portion of the sop is shit you won’t use, or at least won’t be referenced leaving you to research what it’s use could be or make an educated guess, in reality it’s been swapped for something else. When done the “chromatography” referenced is just filtration and is poorly explained, varying polarities to separate fractions aren’t really even discussed. The distillation temps are off like a mother fucker. Copper did very little to remediate the sulphur smell but did help when I soaked the copper wool in the Cbn crude with ethanol just not much. Best result was packing the head of my spd with copper wool after attempting to soak it in ethanol, turned copper black in both instances. That fucking smell tho, it doesn’t get better. All in all it’s a convoluted asswipe of an SOP and there’s better ways to skin a cat. Someone put the time and effort in to write it and for that I’m appreciative and glad I got the learning experience but it’s certainly not an operating procedure I would call standard as it doesn’t provide something easily used. If you don’t have the time for r&d you don’t have time to fuck with that non standardized operating procedure.
tldr; it did make cbn, That was a beautiful red color with amazing clarity, it just wasn’t easy, took a couple tries and smells like shit the entire time. Was decently high yielding and overall it did work but that doesn’t mean it’s a good method for production.
At one point I had a jar of cbn crude break in the floorboard of my car. RIP FLOOR MATS, you will be missed.
5 Likes
sounds like you’re just the guy to rewrite it! And sell it for money!
2 Likes
Yeesh I wish I saw this a few weeks ago. We did an attempt with crude CBD originally, and while had some conversion it was piss poor.
For example here’s the results using SOP as is.
Input material-Crude CBD oil
CBD-55%
THC-3.23%
CBN-0.87%
After:
CBD-0.96%
THC-0.15%
CBN-5.89%
So glad we started with a kilo on the first test (lol)
Did another run, but small scaler scale of like 200g input material of 1st pass distillate.
Before:
CBD-65%
THC-3.76%
CBN-1.05%
After:
CBD-2.01%
THC-0.75%
CBN-6.8%
As for the garbage smells and end product we aren’t too concerned because we have flash chroma that (hopefully and thankfully) we can use for purification. But those yields are pisssssss pooooor. Our second run is still setup so I just turned the heat back on and since it’s waste at this point anyway are going to cook it a lot longer to see if that has any better results cause fuck it.
Have any starting temp/time ideas? I don’t think I’m going to try that SOP, and we have ridiculous amounts of lovely CBDa Oil to ruin
Start with d8 and look into dehydrogenation, that’s really the answer. There are various methods for dehydrogenation that can be applied here. Look into and learn about stoichiometry. It will change the game for you.
1 Like
Im about to test longer time now. The biggest noticing difference on the previous runs was after H2S gas was done being produced, was a steam/smoke in the flask rolling around. I was actually afraid we went too long. There only big difference in our two runs was the amount of sulphur used. In the first one we went over the 2:1 ratio as the SOP said the reactions work from 2-10:1, on the second we were right on with the 2:1.
The second one I just heated and letting it go for probably 3 hours (again this is only 200g) to observe changes. Ill update this post with my results
First hour is up, results are:
CBD-2.9226% (increase is interesting)
THC-0.71%
CBN-7.00%
Second Hour
CBD-2.85
THC-0.59
CBN-6.15
Third hour
CBD-2.7%
THC-0.5%
CBN-6.01%
I would not call it a change, significantly anyway with the increased time.
@DUMPSTERFIREOG It would be great to start with D8, but because we are not in a full legal state we do not feel comfortable converting cbd to that first. I’m aware there are other, maybe more efficient methods, but sometimes those other methods are not conducive for others for various reasons. I’d equate it to trying to go on a cross country trip. Sure, an RV would be the way to go… but some people cant afford/drive the RV so you have to make due with other methods. You mention it was decently high yielding and did work but sounds you moved away from that method. If there are any bones you could toss out that would be greatly appreciative (for many people).
I understand that completely but you’re stabbing in the dark with a knife with these methods, which is why I mentioned stoichiometry because then you can at least be certain of what you’re doing and what the potential outcome might be. If you absolutely have to start with cbd you should be using isolate, I haven’t found that the method of using sulphur converts the cbd to thc to then become cbn. If this were the case we’d see large amounts of thc converted instead of just unknowns. I’ve found great success using d8 to cbn and even that success was more about how well I was cleaning it up after the fact. I think you have a long road ahead of you if you’re trying to convert cbd distillate or crude into high yielding cbn successfully using the sulphur method. I’m sorry I can’t give you a better bone but thc is what you really need to be using.
Thanks for that added info. and I agree with you. It was very surprising to see how much of the THC dropped in terms of magnitude compared to the CBD. But the other fact of the matter is, what happened to the CBD. Back to research it is for that, and well now… so is adjusting the Ph. and times
I’ve got some poorly converted stuff I could redeem the value of with a method like that- I don’t have a great plan for separating from unknown isomers, but if could convert the D8, it could be salvageable because I can purify via flash chromatography and distillation. I haven’t tried any other solvent systems with the flash system besides methanol and water (to separate the D8 from all its evil twins), which I believe with enough tinkering could work, but I’d rather skip that and try to save the 65% marketable cannabinoids by cyclization into CBN to make up the loss. Care to extrapolate? Perhaps a consult?
methanol and water could maybe work for C18 (extremely cost exhausting), I would believe there are better systems. Some separations can be done on regular silica too, see pamphlet from Biotage. However, if you have shitty stuff and want to “redeem it”, you usually turn shitty stuff into even shittier stuff and loose lot of consumables and time. That’s my experience. Although it would really help to know the actual composition of your material that needs to be redeemed. Do you have at least TLC of your mixture? What method are you intending for the transformation?