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Trying to improve my freeze precipitation technique - advice please!!

Dmt-74

Dmt-74

Esteemed member
Hi

This is what I have been doing so far:

1. Extract naphtha
2. Put it in the freezer in a Pyrex dish with a lid
3. Ditch the naphtha once I have crystals
4. Let the crystals dry
5. Collect them with a blade
6. Repeat the process with new naphtha

I would like to know if it's possible to leave the crystals in the dish once I have ditched the naphtha, then add the new naphtha from the next extraction and keep doing that over and over? The aim being to have once dish full of crystals at the end

Thanks
 
Dmt-74 said:
Hi

This is what I have been doing so far:

1. Extract naphtha
2. Put it in the freezer in a Pyrex dish with a lid
3. Ditch the naphtha once I have crystals
4. Let the crystals dry
5. Collect them with a blade
6. Repeat the process with new naphtha

I would like to know if it's possible to leave the crystals in the dish once I have ditched the naphtha, then add the new naphtha from the next extraction and keep doing that over and over? The aim being to have once dish full of crystals at the end

Thanks
Click to expand...
This one seems to have slipped under the radar - apologies!


Yes, you can add fresh naphtha pulls to the previous batch of crystals. The naphtha can also be reused for more pulls once you've freeze precipitated the product out of it.

"Ditching" the naphtha sounds incredibly wasteful. Maybe you didn't know how to articulate "decanted off and put to one side for later use"?
 
Yeah... save all the solvent you can. No sense in wasting what can be easily reused. Just put what you pour off into an airtight jar and keep it in the freezer. Make sure it is an airtight jar because the solvent can leech into your food if not.

Another idea: when you empty a small can of solvent, keep it and begin storing solvent that you want to save in it.

One love
 
PshhhUnreal said:
Why keep poured naphtha in freezer?
Click to expand...
Hello. Welcome.

My impression is that this will slow evaporation of the naphtha during storage, which is perhaps more relevant for people living in areas with consistently high summer temperatures. (And I see vm beat me to it on that point!)

One also ought to be aware that specialised spark-free refrigeration appliances exist for the purpose of storing volatile flammable solvents (particularly diethyl ether) in order to prevent vapour explosions. It would therefore be prudent to do some careful safety calculations before storing any given flammable solvent in a domestic fridge or freezer.
 
Thank you both. Not to bring attention to the obvious, I am new. First extraction last night. 1 more question. I followed a popular easy method from you tube. 12C water, 1C lye, 300G bark, shake, 3C (700ml) warm naphtha, flip 50x, sit 1 hour, then pull.
When I pulled naphtha layer after a little over one hour there was less than half so about 300ml is in freezer. Is this normal?
 
Voidmatrix said:
Sounds like there may be some solvent still in the soup. Did more float to the top?

One love?
Click to expand...
This could be another example of how it's generally better to go for a smaller extraction, especially if it's your first time, @PshhhUnreal. You'd be committing a lot less material to the process in case of mishaps, it's easier to handle and mix, and there's less volume and granular surface area for the solvent to get lost in.

The good news is, your subsequent pulls will recover the vast majority of any spice held up in the trapped naphtha. If your cup is a standard 8oz, 250 to 275mL kitchen that seems on the face of it to be a reasonable, but it still makes for a cumbersome (~3+L) amount of liquid to be handling. It may be an idea to carefully split it up into four or more smaller portions for the subsequent pulls. Mixing and separation of the naphtha should be more straightforward that way.
 
No layer of paydirt today. Here’s where I’m at after one pull. Small jar is fresh 3 fresh cups of naptha, but it’s same amount I put into soup, as you can see… much less came out.
Moving forward what should I do with this soup?
Separate into 32oz jars, then add naptha?
Do I stir before adding naptha?
After adding naptha do I just flip upside down 50x again?
How long is okay to let keep naptha in soup before extracting?
After extracting naptha into sealed glass does it matter how long till I freeze?
I know I’m kinda all over the place, any suggestions would be greatly appreciated.
 
Meanwhile, you need to think very carefully before decanting any amount of caustic, flammable sludge. If you can't write out a step-by-step plan of action it's probably better not to do it, and just to stick with dealing with the big extraction.

That said, it depends to an extent what equipment you have available. First and foremost would be eye protection. It would be OK to leave the soup for a day or two if you needed to sort out supplies but at some point the may start to weaken the glass it's in.
 
Good looking out on the pic🤙🏼
I watched imakeDMT EZ Base Extraction
on YouTube. That’s my level of preparation and equipment. I do have safety equipment. Doing in garage, no open flames. My goal is to get highest yield in timely manner with supplies I have.
How do I get that “lost” or “trapped” naptha back?
And at this point should I just keep filling big jar with naptha and doing the “50x” flips? And is 1 hour long enough to wait to extract?
Much appreciated
 
Like I mentioned in a previous post, you'll recover much of the trapped "material of interest" just by doing three or four more pulls.
Transform said:
The good news is, your subsequent pulls will recover the vast majority of any spice held up in the trapped naphtha.
Click to expand...

Rather than turning it end-over-end, it's better to make more of a rolling/tumbling action as though the ends of the jar were bicycle pedals. The object is to maximise contact between the naphtha and base soup phases while avoiding making an emulsion.

Since you were able to recover some of the first pull, we can infer that subsequent pulls should come back out as the full volume - if you think about it, the 'gaps' where the missing naphtha went will have been filled up already.

Imo you'll get away with a far shorter mixing time - much of the DMT will have migrated into the occluded naphtha already and be far easier to pick up.
 
PshhhUnreal said:
Sorry one more, my soup PH is 11
Do I need to increase?
How?
Click to expand...
That's a bit low - pushing it up with the cautious addition of more lye may even cause some of your lost naphtha to reappear.

Do NOT add too much at once!! The subsequent heating is capable of cracking some glassware. Good-quality, reasonably new borosilicate glass should be sturdy enough, however.
 
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