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Problem scaling up Cyb's hybrid salt tek Options
 
Demeter42
#1 Posted : 6/27/2017 10:59:10 PM

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Hi folks!
I didn't want to start a new thread to ask for help, but i tried looking for the answers in old posts and only could find things i already tried and didn't work.

I've had many successfull extractions using both Cyb's Hybrid Salt Tek, and the Max Ion Tek. At this point i felt confident enough to try and scale up the Hybrid Salt Tek, and it became a little complicated when it comes to phase separation.

Here's what i did:

I followed the Tek as it is, but used 100gr of MHRB instead of 50gr. All the rest was the same, except i used 100ml of hexane per pull. Problem is it is taking forever to separate, when in previous attempts following the teks to the letter, it only takes a few minutes.

I figured out the basified mix was way too sludgy for not doubling the ammount of water/base when doubling the amount of bark, so i added more water, always making sure the pH didn't go below 13.
Now the ammounts of bark to water/base are correct acording to the tek, since i added another 350ml of water to the bottle.
The problem is, it's still taking forever to separate, and even after many hours in heath bath, and also leaving it to separate overnight, the hexane never goes completely to the top, only a thin layer does (less than half of whats actually in the bottle).

Any clues on what can i do to fix this? I'm thinking on adding some more NaOH, but pH is already above 13 now, so i don't know if that could help.

Thanks in advance for your help!
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blue.magic
#2 Posted : 6/28/2017 1:03:10 AM

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Have you used the same MHRB? And how finely was it pulverized? Have you ran the freeze-thaw cycles first?

Something similar happened to me when I overcooked the MHRB - it became sludgy and then hard to get rid of the sludge.

I have avoided this issue next time by filtering MHRB, then reducing, then filtering again (finer particles concentrate by reducing). Also letting the particles settle before filtering helped a lot.

As for the basing, I would not run the pH over 13 - just somewhere around 12.5 (I think that's the sweet spot).
Note that pH 12-13 is already enough to saponify plant fats forming a soap (i.e. bubbles and soap particles attaching to everything). I am not sure if that is an issue with MHRB though...

I would also avoid NaOH next time. Maybe calcium hydroxide or sodium carbonate as they are said to work as well, especially for DMT.

I'm looking forward for what experienced extractors here will come up with.
 
Demeter42
#3 Posted : 6/28/2017 2:00:45 AM

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Hi blue magic! Thanks a lot for your reply! It has helped me to clarify things.

First, it's a new batch of MHRB, i'm thinking that maybe this one has more fat in it than previous MHRB i used?
It was very finely pulverized. I didn't ran the freeze-thaw cycles because last time i did the Max Ion Tek, i didn't get a higher yield than with the hybrid salt tek using the same bark. But now i see that the cell lysing provided by the freeze/thaw may be what allows for a very quick separation of layers in that tek.

Now i remember another mistake i made, and maybe thats why the pH got to 13.4. When i basified, i put 200ml water and 50gr NaOH, but forgot to add the extra 140ml of water to the bottle. I noticed my mistake like half an hour later, after i already added the NPS and had the bottle in the heath bath. I added the water then, and hoped the little mistake would make no difference.
I added water several times later hoping it would make it easier to separate, but it's still the same.
I think there's a lot of NPS trapped in the basified mix and i don't know how to get it out.

When you say you filtered and reduced the bark, you mean when? In the acid step?
 
blue.magic
#4 Posted : 6/28/2017 2:32:12 AM

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Demeter42 wrote:
When you say you filtered and reduced the bark, you mean when? In the acid step?


Yes, in the acid step. The first filtering done with cheesecloth, then reduced, second filtering done with a large Buchner funnel, flat paper filter and a big 2 L vacuum filtering flask. More layers of cheesecloth would probably also do.

Maybe adding excess NaOH, leting the mix sit for few hours, stirring occassionally and THEN filter may be better as this will chemically break down the plant material (in an STB fashion). But I don't know if this is really necessary since we work with powder.

Not sure about removing the trapped NPS (I usually cook the excess out so it won't end up in the drain - NOT a safe practice though).

I did just a handful of extractions, but I always make sure the tea is smooth and watery (not gunky, thick, sediment-containing etc.) before basifying. Since DMT salt is dissolved in water, filtering won't remove much of it anyway.
 
Demeter42
#5 Posted : 6/28/2017 3:29:30 AM

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Well actually i've only done a handfull of extractions myself...i tought 5 were 'many'...obviously i still got a lot to learn. And actually, mistakes like this one teach you a lot more than when you have straight success following a tek to the letter.

Besides the time it's taking to separate the layers, and the fact that not all the NPS is coming to the top, i managed to take a first pull out, freeze precip, and after drying it yielded just over 0.5% wich is not bad at all for a first pull not getting all the NPS out.

Does anyone know what can i do to help the NPS trapped in the basified mix go to the top?

Another question: will the alkaloids be affected for staying so much time in a pH above 13?
I started the extraction process two days ago, and don't think i'll finish in another two days by the time it is taking to separate the layers.

thanks for your input
 
blue.magic
#6 Posted : 6/29/2017 9:59:12 PM

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Demeter42 wrote:
Another question: will the alkaloids be affected for staying so much time in a pH above 13?
I started the extraction process two days ago, and don't think i'll finish in another two days by the time it is taking to separate the layers.


Look at this topic - it seems letting the base soup sit for even weeks does not affect the freebase DMT.
 
Demeter42
#7 Posted : 6/30/2017 7:06:32 AM

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Thanks for the link blue magic!
It came very useful at this point.

After 3 pulls (completed in five days!) yield is 0.8 % , wich is the same obtained from this kind of bark in the past. A fourth pull is in the freezer.
It bothers me because i used to get close to 2% from previous bark. That one had been harvested by a friend of mine in Brazil, it came shredded and i had to pulverize it.
The bark i used this time came from another source, and it was a very fine powder, no fibers at all. The REMOVED said i could get 8 grams out of a kg. That's 0.8%, exactly the yield i'm getting.
I wonder if it is not only bark but whole root? I didn't expect alkaloid content to vary so much between sources.
 
DoorSeeker
#8 Posted : 7/3/2017 5:52:41 AM

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I had the same issue. Bumping up the heat a bit solved the problem for me. Letting it sit forever works too but why bother if a little heat can do the job in 15 minutes?
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cyb
#9 Posted : 7/3/2017 3:39:48 PM

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For 'slow to rise' or 'trapped' solvents ... Add a bit more lye and/or slowly heat the solution (in a hot water pan...no flames)
Also make sure your mixture isn't too 'thick'... if it is, add more water.
Thumbs up

Also 'Scaling up' extraction does not mean doubling up all the ingredients. Only the water/acid/base amounts will change slightly ... Solvent pulls should remain more or less the same amount.
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DoorSeeker
#10 Posted : 7/4/2017 2:46:55 AM

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cyb wrote:

Solvent pulls should remain more or less the same amount.


This is very interesting. Why exactly is this? Wouldn't you have to do more pulls?
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Demeter42
#11 Posted : 7/7/2017 9:08:35 PM

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Thanks for the replys guys!

I did add some more water always checking for pH. And i also did heath baths wich helped a little, but it still took too long to separate completely.

Next time i'll stick to the Max Ion Tek.

I completed 5 pulls after 10 days, with a yeld of 1.1%. Last pull was 0.1% so i'll stop there. I'm quite happy with the results after all.
 
blue.magic
#12 Posted : 7/7/2017 11:21:04 PM

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I think the point is to never get a sludge in the first place. Add enough salt water if needed.

I am now also performing MAX ION extraction on 100 g MHRB powder in a 1 L bottle. So let's see if any emulsion will form.

If you seen "The DMT Workshop" video with David Barrow, you may saw he resolves emulsion by putting the bottle on a hotplate stirrer and let it stir the mix slowly (with a magentic flea inside the bottle) until the emulsion resolves.

I think he used triangular stir bar which I think causes more turbulence and removes sediments from bottom. There was however only a mild vortex in the bottle.
 
 
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