Unknown White Powder Isolated from THCa Crystal Growing

Hash and Stuff Crystallization
1

I’m hoping the infinite wisdom that is F4200 could help me elucidate an unknown, beautifully fine, white powder that I have been reliably isolating while attempting to access THCa crystals from ethanol extract. Please let me know if you have any thoughts on what this material might be, I’d really appreciate the discussion! Information is below:

You’re going to ask me what I did, unfortunately I’m held to NDAs, but I can say this was a basic–>acidic then buffered work-up which then involves jartek to crash out THCa. Most of the time it works, but ~30% of the time I get the white powder shown below.

I would LOVE to have 1H 13C NMR data, hplc, mass spec data on this powder but I cannot get it to dissolve.

Solvents it is insoluble in: EtOH, MeOH, toluene, benzene, DMF, THF, DCM, CHCl3, methyl tert butyl ether, diethyl ether, ethyl acetate, acetone, water, hexanes, heptanes, pentane (including heating, and sonication in all of these solvents)

Melting point: >250 C, that’s as high as my melting point apparatus gets and it was still going strong

Alternate Characterization: IR and MS I don’t have access to currently, but I am working on getting this done. Solid state NMR is a possibility as well, but again waiting for some resources. My current theory is some kind of polymer based on the structural durability and insolubility of this material. Perhaps GPC could be enlightening, but I have to brush up on my science behind polymers.

Has anyone else encountered or had any luck deciphering this problem? I can’t wait to hear from the minds of the best!

Mystery Powder 1
Mystery Powder 13968×2976 1.36 MB
Mystery powder 2
Mystery powder 23968×2976 1.5 MB

5 Likes
2

What’s the ratio of input material to white powder output?

3

Is it soluble in either acidic or basic water?

4

30 g input extract; 7-12 g white powder

5

It is not. I forgot to include 1 M and 6 M NaOH, acetic acid, 1M and 6 M HCl in the original post. I will update if I can, new here, unsure if I can edit this. I will be seeing what happens in sulfuric acid this afternoon.

6

At that ratio i wouldn’t think there’s a lot of possibilities beyond cannabinoids or isomers of the original cannabinoids. Wax, lipids, sugars, even clay contamination, wouldn’t show up in those quantities. Seen your update on acid additions, going with isomer.

7

I would love it to be an isomer! But I have not come across any literature or hands-on experience of an isomer that would be so insoluble. It would certainly be interesting. Thanks for your responses!

1 Like
8

If it is a polymer, then probably an IR spectrum and DSC would be a good place to start. GPC only works when you can dissolve it in something. My MS was concentrated in polymer chemistry.

1 Like
9

I totally forgot about DSC! That’s a great idea and I certainly know a colleague with one. Thank you. I will pursue this. I really hope to get this sorted and I will update with results if it proves interesting!

1 Like
10

If you have a university near you they may be willing to assist. IR via ATR should be really easy to get a good scan on.

1 Like
11

Absolutely. It is in the works to get myself a quick 10 minutes on one haha.

12

My apologies if this is the wrong thread but it was the only spot I could find for mystery white powders found.

We have found a similar substance in our oil mist filter. It is a putrid smelling, material that was flaky , and is not soluble in etOH . I’m not sure what it is, and haven’t been able to find any luck on what it is from my colleagues.

In the picture I sprayed etoh in the flask to see if any dissolved.

image
image874×1624 247 KB

1 Like
13

How does it taste? Have you smoked any?

don’t do this

1 Like
14

Haha that seems to be everyone’s first answer

One guy mentioned d12 but I’m really just at a loss

15

I think d12 is that band with Eminem in it. D10?

14 Likes
16

100%

By adding that in, I was getting at I’m not getting very helpful advice. Im going to see if I can r&d it at our local testing facility for better idea

17

Soluble in water?

18

yes it is water soluble

19

If you have been stripping terpenes with the pump that would account for a bad odor, I am lost on what the material would be. Have any more information? what is the pump used with?

20

Ive seen buildup on extractor parts that looks like this only from certain biomass.

Kind of a fine plastic. Smoked it and it tasted like plastic poison. Could it be pesticides?