Safety in your isomerization please

The resolution of their method is indeed very poor. :confused:
Even for normal CBD products, such method is not ok…

The method I employ with GC-FID lasts at least 17minutes. Main cannabinoids appear between 11 and 15 minutes, separated by at least 20 seconds from each others… and there you can see that there are even few more others next to the main ones, generally present at lower levels.

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Our method is 25 minutes.

cannabinoids start around 4 minutes and end around 15

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@Dr_Jebril and @thesk8nmidget
Can you both share a bit more about your methods? Would be nice if the world could come to a standardized testing

I wish i could go into it deeper, but I am not the one that made our method. I would be happy to share the chem station data with anyone that is interested though.

Analytical is not my strong suit, i know just enough to get by and i am happy to say im always within a few percent to pixis labs.

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I occasionally described my method in various post in this forum.
It is adapted from a method I found in forensics literature.

In my case I employ GC FID. In short:

  • 30 m HP-35MS capillary column
  • He as carrier gas
  • split injection
  • starting temp 80°C, ramp up to 180°C at 30°C/min, then up to 280°C at 10°C/min, then higher to 320°C in case of oil tinctures.

There are variable parameters than can be tuned.
The key is to have a slow enough temperature ramp in order to have a convenient separation, associated to a long enough column … but this extend the run time. A lot of commercial lab want to go fast.

I made the method to primarily look at flowers and tincture, and be able to discern most terps and cannabinoids in the same run.

@thesk8nmidget what kind of technique do you employ ?

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@cyclopath figured this would be interesting for you ^^

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may I ask which method you used.

I have tried my self the phosphoric acid in alcohol, poly in heptane and aqua sulfuric acid
isomerizations and did not find this.

I know if the acid is even in trace amounts I get this affect your talking about.

though I never test my shit to be honest as I don’t sell it nor have any interest in selling it.

I am also not after a pure compound and find the mix better for my use.

my washing procedures is the same as is used for mercury amalgums
three times bicarb water
three times salt water

twice distilled water

I dont dry as I dont want drying agent in my product should my filter not pick it up.

I use heptane or diethyl ether as the solvent.

don’t use ether if your not trained in its hazards you will blow your self up.

it could be some kind of sulfite or SO2 complex of the oxidized phenols in CBD.

that for sure will have you coughing like a modern day plague barer :no_smoking:

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It was zinc salts, I can only surmise either my CBD had some high boiling terpenes that didn’t fraction off properly, or that I didn’t rinse enough. But I also wouldn’t think that the acid would boil over :man_shrugging:t2: but I guess probably in trace amounts

zinc is a catalyst for all kinds of reaction on aromatic rings and alkenes.

dirty dirty route.

now it makes sense.

transition elements rarely give straight reactions from what ive seen.

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Analytical labs in this industry don’t want standardized testing because then it would become a race to the bottom for pricing.

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35 meter HP-35MS column? Was this custom cut from a longer column or do you have a 5 meter guard column on a 30 meter column?

That’s weird, my zinc chloride refluxes give pretty consistent yields. I’ve definitely never found myself unable to breathe after dabbing some.

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Was probably me fucking up a procedure or being lazy

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Which goes to show everyone how easy it is, even for a well accomplished, knowledgeable processor to make a mistake that could be fatal.

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30 meters.
It was another typo my bad.

To me the ZnCl2 route looks the very similar to the acidic clay, AC, acid methods.
I don’t think the reaction is straight in any case. But it seems that the amount of intermediates (from CBD to D8, including D9 in between, plus presumably two others) varies as a function of catalyst.

:joy::joy::joy::joy::joy::joy::joy::joy: