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Freeze precip, something wrong here? Options
 
Donald
#1 Posted : 1/4/2012 12:23:19 PM

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Hi there everyone,

I've been reading tips and STB teks here for quite some time and finally decided to try an extraction myself. I have pretty much followed the Noman's tek. I started off by adding some white vinegar to 50g of powdered mhrb as suggested in some tips to increase yield. Then I added about 1300ml of water and 50g lye. I let this bark soup stand for about 10h. I did the first two pulls with 20ml of unheated naphtha and put them in the freezer to sit overnight at -26C.

Next morning I saw this cloudy-like thing floating in the solvent. I put a coffee filter on other jar and poured these 2 solvent jars through it to catch the cloudy-like thing that was floating there. There wasn't really anything stuck to the bottom or sides of the solvent jars. I let the coffee filter dry for a while and picked the powder up there. Did I do something wrong here or is ~40mg of this powder the final result of my first 2 pulls? Surprised

I did next two pulls with heated bark solution and naphtha and let them sit in freezer for 24h. I just went to check how are they looking but it's pretty much the same as last time. My freezer for some reason had went to -18C but I don't know if that matters. I didn't pick them up yet because the first pulls looked the same and I'm not sure if everything is correct here.

Thanks in advance,
Donald
 

Live plants. Sustainable, ethically sourced, native American owned.
 
endlessness
#2 Posted : 1/4/2012 12:26:40 PM

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How well did you mix each pull? Did you do many cycles of mixing/letting stand before pulling? Is your mimosa from reputable supplier?

Maybe evap your naphtha to a quarter of the amount and freeze again (and next pulls, already freeze half or 3/4 of it and put in the freezer)

Also, check this out:

https://wiki.dmt-nexus.m....27s_my_snow_globe.27.3F
 
Donald
#3 Posted : 1/4/2012 12:38:26 PM

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Thanks for quick response. I rolled the bark solution + solvent around in the bottle and turned it from end to end for about 1-2 minutes and then let it sit for a while. I repeated this four times before pulling the solvent out. Is it supposed to noticeably change it's colour? For me it looked quite bright when I pulled it out. Also am I supposed to see all the spice stuck to the sides and bottom of the jar after freeze precip rather than floating in the solvent? I'll try to evaporate them a bit even though I used quite small amount of solvent as suggested for easier freeze precip.
 
amvitamine
#4 Posted : 1/4/2012 5:42:29 PM

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In my experience you need to let the solvent sit for a few hours at least to get the best pulls. I let my solvent sit for about 10 hours. Pulling it out after 20 minutes just won't do it.
Also with 50 mg of bark I would use around 50 ml of solvent.
Another tip is when you pour the solvent in your coffee filter you can put your mouth over the filter, sealing it with your cheeks and gently blow. This way you create a pressure in the filter and you quickly blow through all the solvent so it doesn't get a chance to warm up and redissolve crystals
 
Donald
#5 Posted : 1/12/2012 3:46:20 PM

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I did two more pulls and took my two earlier ones out of the freezer and let these four containers sit in my garage for about 3 days to evaporate a bit. They evaporated to about 1/3 of the original volume and I put them to freezer for 24h.

This time I finally got some crystals over there. They're quite yellowish so I guess I'll attempt the sodium carbonate wash. They weight about 180mg according to my scale. I still have the mhrb mixture sitting in my room so I think I'll be doing a few more pulls as well.

There wasn't much stuck to the sides of the containers but rather 1-2 of these bigger thingys in each of them. Here's a few pictures:
Donald attached the following image(s):
IMAG0163.jpg (1,033kb) downloaded 77 time(s).
IMAG0165.jpg (984kb) downloaded 77 time(s).
 
MooshyPeaches
#6 Posted : 1/12/2012 6:17:57 PM

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definitely have some plant oils in there. did your first pulls come out white? i find as you do more pulls it goes from pure white --> yellow tinge.

50g lye 50g mhrb should be working fine for you. add in naptha and mix it around like you said you did before, maybe let it sit for 1-2 hours and mix again, although i think once the layers separate your good to go.

swim pulls with 60-80 ml of naptha and has no problem freeze precipitating pure white globes. make sure as soon as it comes out of the freezer you pour it through your coffee filter as fast as possible. Also some of the dmt will be caught on the sides/ bottom of your jar so use a knife to scrape it all loose before you go pouring it out.

if you continue getting yellow crystals try adding more lye to your mixture and let it settle before next naptha pull, goodluck =]
 
Donald
#7 Posted : 1/12/2012 7:05:51 PM

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MooshyPeaches wrote:
definitely have some plant oils in there. did your first pulls come out white? i find as you do more pulls it goes from pure white --> yellow tinge.

50g lye 50g mhrb should be working fine for you. add in naptha and mix it around like you said you did before, maybe let it sit for 1-2 hours and mix again, although i think once the layers separate your good to go.

swim pulls with 60-80 ml of naptha and has no problem freeze precipitating pure white globes. make sure as soon as it comes out of the freezer you pour it through your coffee filter as fast as possible. Also some of the dmt will be caught on the sides/ bottom of your jar so use a knife to scrape it all loose before you go pouring it out.

if you continue getting yellow crystals try adding more lye to your mixture and let it settle before next naptha pull, goodluck =]


My first two pulls were white but I didn't evaporate it before freezing back then and I got extremely low yield. For these 4 pulls I shaked and mixed a lot harder while pulling. Should the naphtha change colour after mixing and pulling it out? Also is it normal that the layers separate relatively quick? I mixed these four pulls as hard as I could and the layers separated in just a few minutes in water bath.

As swiy uses 60-80 ml naphtha, do they evaporate it at all before freeze precipitating? And am I able to get these oily crystals washed with sodium carbonate or what should I do with them?

Thank you
 
Donald
#8 Posted : 1/16/2012 9:40:03 PM

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Does anyone have any tips or answers on my questions above?^
 
 
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