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OfflineIgnorantOne
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Freeze Precip Question
    #25830515 - 02/22/19 06:24 PM (2 years, 7 days ago)

I have a question about the freeze precipitation end process for DMT extraction from ACRB. Already have the naps in the freezer and it has turned milky and have big chunks floating in.

What I had done was follow the ThickLight Tek and then EarthWalkers tek for the mini A/B, all went smoothly... except for spilling naps on myself. Those fucking jugs are a pain to pour out of. Either way, my question is "How long should I freeze precip my cleaned up product?". I have read 24-48 hours is ideal, if I do not disturb it won't the naps turn clear as the DMT crashes out to the bottom? Would that not be a better indicator or does it not gain clarity as the DMT drops out of the solution? I kept my defat naps in a separate jar as it contains alkaloids as well, I am sure I missed some, should I pour off the naps from my freeze jar into this? I'd assume that even freeze precipitation will not get everything unless I had a badass freezer.

I am not completely sure this is the right spot to post this but I do hope so.


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Re: Freeze Precip Question [Re: IgnorantOne]
    #25830549 - 02/22/19 06:46 PM (2 years, 7 days ago)

Quote:

IgnorantOne said:I have read 24-48 hours is ideal, if I do not disturb it won't the naps turn clear as the DMT crashes out to the bottom?



Yes, exactly. When it's transparent again it's done.
Any standard freezer should be cold enough.
I wouldn't combine your precipitating naphtha with your defat naphtha. You can reuse the precip naphtha for more pulls. I don't believe the defat naphtha would have any alkaloids in it, isn't that done before basing the material?
Be sure to wear gloves, sleeves, a mask and goggles while working with naphtha. I've started using a full face respirator and it's a very good investment in your health.


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OfflineIgnorantOne
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Re: Freeze Precip Question [Re: Icon]
    #25830570 - 02/22/19 06:55 PM (2 years, 7 days ago)

Awesome sauce. I was figuring that it would clear up as the solution began to empty of DMT. Yeah, I need more safety equipment, facemasks only get you so far and the gloves I have are really high rated but a bitch to work in as they are not the greatest fit.

I am curious, what do you do about the emulsion layer in your main jug? I have tried salting and, while it helped, I still have a good quarter inchish layer. My soup is a little over 2500ml.

As to your defat question, I acidify, base, pull, then clean the pulls in a mini a/b which I thought was the defat step. MAybe I am using the term incorrectly?


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Edited by IgnorantOne (02/22/19 06:56 PM)


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Re: Freeze Precip Question [Re: IgnorantOne]
    #25830685 - 02/22/19 07:58 PM (2 years, 7 days ago)

Quote:

IgnorantOne said:
I am curious, what do you do about the emulsion layer in your main jug? I have tried salting and, while it helped, I still have a good quarter inchish layer. My soup is a little over 2500ml.

As to your defat question, I acidify, base, pull, then clean the pulls in a mini a/b which I thought was the defat step. MAybe I am using the term incorrectly?



When I did wet teks I just waited for the emulsion to settle, didn't really have a solution. But I only do the q21q21 dry tek now. No emulsions or large volumes of soup to deal with.

I've never actually needed to do a defat but I think that refers to a step before adding your base, to pull out any non-polar, non-alkaloid gunk that might be in the material. I see your mini-a/b step as more of a re-crystallization, to purify the alkaloids themselves. You should be fine to mix that mini-a/b naphtha with your freeze-precip naphtha then. You're right it may have some alkaloids still in it if you evaporate.


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OfflineIgnorantOne
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Re: Freeze Precip Question [Re: Icon]
    #25830713 - 02/22/19 08:06 PM (2 years, 7 days ago)

Ok, thank you for the information. We shall see what this yields.


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OfflineIgnorantOne
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Re: Freeze Precip Question [Re: Icon]
    #25847053 - 03/02/19 06:34 AM (1 year, 11 months ago)

Sorry to necro this thread but I have another question. In your experience, does the root bark lose potency over time? 1 kilo was ran and resulted in .6, the bark is several years old though.


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Re: Freeze Precip Question [Re: IgnorantOne] * 1
    #25847244 - 03/02/19 10:00 AM (1 year, 11 months ago)

You should be able to yield 10-20g per kilo of MHRB. 0.6g is extremely low.
I've heard conflicting reports about aging bark. DMT is stored as a salt in the bark which is more stable than freebase and should last for years with the only degradation being the DMT oxidizing slightly. Anyway, you can convert the DMT Oxide back into freebase with the help of zinc during the aqeuous acid step of an A/B.

If the bark is legit and just really old to truly have oxidized, the zinc step should convert all the oxide back to freebase and allow your naphtha to pull it out (n-oxide does not dissolve in naphtha).

But since oxidation in the bark form is very slow, more likely something else was incorrect during the extraction. Maybe you didn't use enough solvent, or it wasn't hot enough to dissolve much DMT, or wasn't alkaline enough to freebase all the DMT, or the bark was very low quality. :shrug:


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OfflineIgnorantOne
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Re: Freeze Precip Question [Re: Icon] * 1
    #25848095 - 03/02/19 06:01 PM (1 year, 11 months ago)

I am using ACRB and not MHRB. I do not think we have access to MHRB in the states. At 1% yield, I should be looking at around 5g for every 500g. Hmmm, I am thinking either I am not doing enough pulls or not letting the naps get hot enough.

Use a hotplate magnetic stirrer instead of just swishing it around. Only been doing 3 pulls of around 200mg naps each time. Let the magnetic stirrer mix the two layers for a while, then let settle, and repeat that 4 or 5 times. What alkalinity do you shoot for? iirc my tester said mine was a hair under 13. Should I be saying fuck it and shoot for 14+?


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Edited by IgnorantOne (03/02/19 07:26 PM)


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Re: Freeze Precip Question [Re: IgnorantOne]
    #25848237 - 03/02/19 07:02 PM (1 year, 11 months ago)

If you got that key from an auction site vendor from AK awhile back, that might be the issue. I ran a key of that and got less than 2g of ok looking stuff, which is what should come off 100g or so. It was also basically bunk. At 1% you would get 10g per key.


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Re: Freeze Precip Question [Re: hummingbird] * 1
    #25848277 - 03/02/19 07:25 PM (1 year, 11 months ago)

Correction! I ran half a kilo... My bad, apparently I forgot how to do math for a moment.


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OfflineLogicaL ChaosM
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Re: Freeze Precip Question [Re: IgnorantOne]
    #25848999 - 03/03/19 03:26 AM (1 year, 11 months ago)

How much vinegar and NaOH did you use for that Kilo?


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Re: Freeze Precip Question [Re: LogicaL Chaos]
    #25849044 - 03/03/19 05:26 AM (1 year, 11 months ago)

For 500g I did three cooks using 1500ml water and 500ml White Vinegar each time. Cooked for about 6-8 hours in a crockpot on low (it would steam and reduce so it was not too low). The liquid was a PH of 2.6-3ish according to the meter. The three cooks were consolidated and reduced to a volume of 2500ml. When I based it I used 70-80g of lye and the soup turned almost black. The ph meter read 12.8ish at that point. I think that may be the upper limit of my ph meter as I added another 40-50g, making for a total of 120ish grams of lye, to the second 500g I just ran and it still would only read 12.8ish in the soup. I am thinking that maybe, just maybe, this magnetic stirrer sucks dick at actually mixing the naps and soup. I have to push it to 1400rpm to get the two layers to fully mix.

I did 3 pulls earlier and have it milky white in the freezer. Went back and decided to see if I could saturate another pull and of course I did. I am now on pull 5. The naps is saturating to the point that I can blow on it and it turns cloudy white.


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Edited by IgnorantOne (03/03/19 05:28 AM)


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Re: Freeze Precip Question [Re: IgnorantOne]
    #25849247 - 03/03/19 09:38 AM (1 year, 11 months ago)

Any pH over 11 is basic enough. I agree the mag stirrer is probably not enough. Gotta wear an oven mit and shake it up good while hot so the layers mix as much as possible. Sounds like this next pull should be good if it's clouding.


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Re: Freeze Precip Question [Re: Icon]
    #25849920 - 03/03/19 04:53 PM (1 year, 11 months ago)

Yeah, that is definitely a good sign if your pulls are cloudy white on the surface when you blow on it. Sounds like it just wasn't getting mixed well enough like you said. I've never used a mag stirrer for D extraction, I've always gently flip and roll the container over during the soup stage.


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OfflineIgnorantOne
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Re: Freeze Precip Question [Re: hummingbird]
    #25849984 - 03/03/19 05:40 PM (1 year, 11 months ago)

Quote:

Icon said:
Any pH over 11 is basic enough. I agree the mag stirrer is probably not enough. Gotta wear an oven mit and shake it up good while hot so the layers mix as much as possible. Sounds like this next pull should be good if it's clouding.



Quote:

hummingbird said:
Yeah, that is definitely a good sign if your pulls are cloudy white on the surface when you blow on it. Sounds like it just wasn't getting mixed well enough like you said. I've never used a mag stirrer for D extraction, I've always gently flip and roll the container over during the soup stage.




Alrighty, I am just going to pull and test each pull till I get one that remains clear when I put it in the freezer for a temp drop. The soup is in one of those 3000ml beakers, maybe I will just pour it over into my gallon wine jug so I can do some manual mixing.


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Re: Freeze Precip Question [Re: IgnorantOne]
    #25856519 - 03/06/19 06:10 PM (1 year, 11 months ago)

Back with another question.. HAve you ever dealt with naps that will cloud in the freezer but does not precip anything out? Would the ideal way to deal with this be either A) evaping half of the naps off. Or B) just let it sit in the freezer longer.

Possibly the naps is not saturated enough?

I am curious, would dry ice work to freeze precip quickly?


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Re: Freeze Precip Question [Re: IgnorantOne]
    #25857860 - 03/07/19 10:15 AM (1 year, 11 months ago)

The clouding means there is insolbule molceles in suspension. Theres nothing you can do except to wait for them to settle or evaporate the whole solvent.

Less solvent will increase precipitation. A small volume saturated at 100% when hot will precipitate compltely within 12-24 hrs. of freezing.


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Re: Freeze Precip Question [Re: Icon]
    #25857923 - 03/07/19 10:43 AM (1 year, 11 months ago)

If the freezer is cold enough, it can finish in as little as 2 hours.  You need to saturate the solvent for this to work optimally, that usually means doing a reduction.  If you want to see a demonstration of this, search YouTube for 'GordoTEK'


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Re: Freeze Precip Question [Re: GordoTEK]
    #25858828 - 03/07/19 06:15 PM (1 year, 11 months ago)

So, essentially ya'll are saying I need to reduce the naps. Alrighty. Thank you for your guidance.


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Re: Freeze Precip Question [Re: GordoTEK]
    #25858854 - 03/07/19 06:31 PM (1 year, 11 months ago)

is there a known rate at which naps will reduce at room temp? I figure a fan would quicken the process but also would introduce dust particles floating in the air to the solution and pollute it.


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