Dual Phantom Peaks (With chromatogram)

Hello everyone! Im looking to see if anyone has had this problem or something similar in the past. I believe it is an isomerization issue (see below) . Here is some backstory:

I recently was told by my testing lab (MCR) that the distillate I sent out for cannabinoid testing had a high phantom peak around the 8.8 and 9 minute mark. The testing was done with a HPLC and test was duplicated with a second HPLC to confirm. I was told they believe that it is delta 10/10a based on a standard they got once. With no standard they said it would be hard to quantify or deturmine if or how much D10 is in there. They roughly estimated 5-20%. The peak does come over where THCA should be.

Does anyone know what reaction is happening? The two peaks show up in our old test results but as much smaller peaks. I do notice that the CBN levels do increase in my tail fraction compared to my head fraction but that also could be the effect of the hot condenser tec. (@anon42519203 please correct me if im wrong). I have sent samples of decarbed crude to the lab to see if this phantom peak is in the source oil.

Any help would be much appreciated!

-Franz

2 Likes

@kcalabs

6 Likes

Thank you! I just called them and one of their head scientist was able to help take my question and provided an email to chat.

3 Likes

@Kingofthekush420

Any more insight by seeing the graph? Thanks as always for the help

@phenethylamine1
I saw you posted this and was wondering if it could pertain to my problem. I checked the pH of my ethanol solution (190 proof) and it was 6.5-7 according to my indicator so I dont think its a issue with a base contamination.

Are you running any media in the flask?

2 Likes

I am filtering using AC and DE but I have a second filter into my rotovap to make sure no DE or AC particles get in the flask. Have you seen these two peaks before using media in the flask?

I had the opportunity to briefly chat with Ryan at @kcalabs. They are science-forward, qualified and ethical as a company. Their testing is leaps and bounds ahead of any competition. There’s a reason that so many people respect them as a company.

3 Likes

Cbc most likely.

2 Likes

Depending on your process methods its probably a degradation due to heat and time reaction. Like say an spd at low heat for long periods of time

1 Like

@AgTonik thanks for the kind words. We should use this comment as a testimonial somewhere.

2 Likes

Thank you for your input! Here is the cannabinoid test result from MCR (see below). I thought it would of been CBC too but according to the HPLC programming the CBC peak is slightly after the dual phantom peaks and 0.2%. I do understand that there is some isomerization becuase of the 1.7% D8 and 1.4% CBN. My total run times is maximum of 6 hours at the longest for the main body. I have a 12L Lab Society G2 SPD. How long does your 20L SPD take for the main body?

1 Like

It should be noted that I have distilled 90%+ THC with the same setup, vacuum levels, and run time. Only thing different with this run is low quality starting materials aka low quality biomass.

My lab society 22 liter would take over 24 hours to clear and I never had problems like this

The fact there’s cbn and D8 means there’s something going on, you won’t make d8 without something in the flask even at 1.4%

1 Like

First pass main body on a 20L, 2.5hrs… its a whole other monster though.

Ya potentially the starting material needs preprocessing then. Ethanol extract can pull alot of water soluble compounds, acids potentially can do all sorts of things. Id run it through a few low pH washes, removal all water as best i can, magsil run it all. 80cu in per 2L of product… then one low pH wash, and 2 neutral washes… then go in for that pass.

2 Likes

How do you achieve flow rates of 4L per hour? Im hitting 1L per hour without counting the time for my heads or tails fraction.

Have you ever seen this type of dual peaks before CBC? The size of the first phantom peak compared to the second always seems to be the same ratio. Also have you seen delta 10,10a peaks?

1 Like

Something going on meaning filter media or something meaning an acid or base?

Either or, there’s definetly something in there causing this

Its not due to time/heat/low vacuum like a few have told you

I still suggest sending a small sample to @kcalabs, ive spent time on the phone with Ryan there and dudes the shit (pardon my french)

The fact there willing to help with R and D on unknowns is the reason there the best, all the other labs just want to be paid and get the test done. KCA goes the extra mile

3 Likes

The new heads i designed, especially the one with the halo condenser. The opening is super wide and the head is short. The entire principle of the design is to help you go faster. The 150mm i clocked at 6L/hr on the slow setting… hut it takes a while to get to max temp and all the settings correct. But once its rolling its done super quick

2 Likes

6L/hr is nuts :ok_hand:

2 Likes