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question: how long to let precipitate

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moracca

Rising Star
Following Noman's tek, how long should you let the jars sit in the freezer? From reading the tek, it seems like you can just leave it overnight, but is it better to leave it for longer? I can see some crystals on the bottom of the jar, but not a lot... The naptha is still pretty cloudy, does that mean there is still more that has to precipitate out? Thanks
 
moracca said:
Following Noman's tek, how long should you let the jars sit in the freezer? From reading the tek, it seems like you can just leave it overnight, but is it better to leave it for longer? I can see some crystals on the bottom of the jar, but not a lot... The naptha is still pretty cloudy, does that mean there is still more that has to precipitate out? Thanks

Sounds like your freezer is not cold enough or there is way too much solvent. 24 hours should leave you with clear naphtha. I would let it sit another day or two. If it is still cloudy after another day you should evap some of the naphtha and try sticking it back in the freezer.

Telling us how much root bark you started with and how much solvent you used would be very helpful in troubleshooting your extraction.
 
oh sorry, it was 200g bark, pulls of about 250mL naptha. It very well could be that my freezer isn't cold enough -- I don't have a temperature dial in there, so I can't adjust it :( I took one of the jars out and filtered it, and then put the naptha back in to see if anything else precipitates. I'm not sure how much came from that filtering, its still drying, but I'll see what happens. Thanks for the help :)

EDIT: Ok, so I let it dry, and it turned out to be about 435mg BEFORE an ammonia wash. I'm sure I'll lose a lot of volume, but the crystals look pretty good and its a decent volume (i think) from one 250mL naptha pull
 
Don't do an ammonia wash!!!

You can loose up to 15% of your final product and most of that is perfectly good spice! A wash is really unnecessary unless your spice is extremely harsh to smoke or if it burns strongly when placed on your tounge.

The best wash I have come up with can be found here. It uses baking soda or washing soda (sodium carbonate) to wash the naphtha before recrystalizing.

Using this method there are minimal losses (2-5%) and it will help remove a small amount of the oils from your product.


Also it sounds like you are using way too much solvent. If you do use that much (and I know alot of teks call for an ungodly amount of naphtha) you will need to evaporate most of it down to about 50-100mL tops for 200g of bark. I will sometimes evap my solvent down until it starts clouding up at room temperature, then I now it is darn good and ready for the freezer.
 
i wish I had seen your post like 10 minutes ago... too late on the ammonia wash thing. no biggie tho, lesson learned. i was under the impression that the amount of product lost to an ammonia wash is not something you want to be smoking.

EDIT: on a side note, I am seeing around 330mg crystals after the ammonia wash
I think you are right about using too much naptha. After thinking about it tho, it was 200mL naptha per pull, not 250... dont know where I got that number from. I was following noman's tek, but I think i may scale the naptha back in the future to make it a bit easier
 
so did I misinterpret the tek or something? I thought step 4 says add 1mL for each g of bark in the jarn and that step gets repeated 3 or 4 times... I guess maybe it means that that 1mL/g should be split between all the naptha pulls? heh oopsies

i think this may elucidate some of the questions I had regarding what exactly makes up a "pull"... i was confused because you are really doing 3 or 4 pulls in a row... but i wasnt sure if each addition of naptha was a pull, or if the final combined result is a pull. It makes a lot more sense this way tho :p
 
moracca said:
so did I misinterpret the tek or something? I thought step 4 says add 1mL for each g of bark in the jarn and that step gets repeated 3 or 4 times... I guess maybe it means that that 1mL/g should be split between all the naptha pulls? heh oopsies

i think this may elucidate some of the questions I had regarding what exactly makes up a "pull"... i was confused because you are really doing 3 or 4 pulls in a row... but i wasnt sure if each addition of naptha was a pull, or if the final combined result is a pull. It makes a lot more sense this way tho :p
I had been doing it this way as well, but after reading quite a few posts on the forums I figured out it out. I now recycle my Naptha after each freeze precip. which yields a bit better in my experience as there is usually still some left in the solution.

Agitations through the final freeze precipitation of Naptha = a single pull. Hope this helps :d
 
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