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Why GRAY, then BLACK? Options
 
der-seemann
#1 Posted : 11/8/2018 7:41:33 PM

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Does anyone know what exactly is happening when basifying an acid MHRB extract?

The dark bordeau / red / brown acetic acid extract from the MHRB (containing the salt nn-DMT-Acetat) will turn gray when lye is added. The gray particles may then accumulate and build bigger clusters.
What is this gray matter? nn-DMT freebase?

When more lye is added, the whole solution will turn black. The gray matter will disappear. OR accumulate at the bottom.
Why? where is the gray stuff going?


I guess the gray matter is already alkaloids that get seperated from the acetat and are now unsoluble in the aqueous solution.

But why will it disappear again? and where is it then? Why not extract with NPS while it is gray?
 
 
der-seemann
#2 Posted : 11/11/2018 9:13:36 AM

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Just been reading about proteins in the psilocybin extraction...
Can the white / gray stuff be proteins? So they could get removed by filtration?
Once the ph is high enough they might get anyway totally destroyed, that's why the solution might turn all black...?
 
pete666
#3 Posted : 11/11/2018 10:25:55 AM

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I am not sure, what you mean by "acid MHRB extract", but...

Imagine extracting dmt from the material by non-polar, then salting by HCl. Then When I basify result of the salting containing high concentration of dmt HCl by NaOH, it turns white/grey cloudy. I am not measuring NaOH and add enough to be sure pH is high enough. Yes, I may add twice or even more NaOH than is needed. No problem at all. The cloud is obviously almost only alkaloid freebase, as we are already after initial A/B and doing subsequent mini-A/B. I can add as much base as I want and nothing happens to the dmt cloud. Basic environment doesn't hurt it

So I don't know what your grey cloud is, I just can tell you what (imo) likely it is not - dmt
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blue.magic
#4 Posted : 11/12/2018 2:30:20 AM

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Something similar can be observed when basifying the acidic rue tea.

When you add base, there are local spots of highly basic water, causing visible milky precipitates.

Upon mixing however, the base will spread out, weaken and the acid will take over again, making the milky clouds disappear.

At one point, however, the base will take over and the whole solution make a "phase transition" - alkaloids will crash out.

However, unlike with harmalas, DMT is still somewhat soluble in water, hence you get dark solution instead cloudy.

There are more factors at play, since the MHRB tea is a complex mixture. There are surely many complex chemicals affected by the strong base, giving it darker colour.

I once basified water containing just DMT salt and indeed the water become couldy and then uniformly opaque.
 
pete666
#5 Posted : 11/12/2018 7:48:43 AM

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blue.magic wrote:
However, unlike with harmalas, DMT is still somewhat soluble in water, hence you get dark solution instead cloudy.

I would correct this, blue.magic. I don't think dmt freebase is soluble in water in some considerable way. I would say it is almost insoluble.
It is very different from mescaline freebase, which is partially soluble in water.

blue.magic wrote:
I once basified water containing just DMT salt and indeed the water become couldy and then uniformly opaque.


I would bet this was due to lack of base, not dissolution of the freebase.
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Orion
#6 Posted : 11/12/2018 2:21:34 PM

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pete666 wrote:
blue.magic wrote:
However, unlike with harmalas, DMT is still somewhat soluble in water, hence you get dark solution instead cloudy.

I would correct this, blue.magic. I don't think dmt freebase is soluble in water in some considerable way. I would say it is almost insoluble.


I think some information came to light a while ago that showed DMT freebase was more water soluble than we thought. It was well discussed in chat. I'm unsure but there may be some info on the forum about this.

As for clouding, DMT is as visible as based harmalas if the solution is clean enough. I always assumed the grey and black colour in extractions was just something once dissolved becoming insoluble due to high PH levels, but nothing useful. DMT crashing from clean water looks like a gunky white cloudy mass which tends to float to the top.
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blue.magic
#7 Posted : 11/12/2018 4:08:12 PM

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Hmmm... how come that basified MHRB tea does not form precipitate that settles down?

This is very similar to my recent experiment with L-tryptophan. Tryptophan, like DMT, is almost insoluble in cold water, but once dissolved in hot water, I've let the water cool down and even leave it in the fridge for days (!!) with no precipitation occurring - and there was not even clouding, just clear yellow solution. Even scraping the glass did not help, though crystals started forming very very slowly over days around the scrapings.

Tryptophan, just like DMT, seems not to mind staying dissolved even in supersaturated solution.

I once observed DMT crystallizing directly from basic MHRB tea (it was very concentrated) - the crystallization was only partial and took days.
 
Jees
#8 Posted : 11/12/2018 4:31:57 PM

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blue.magic wrote:
Hmmm... how come that basified MHRB tea does not form precipitate that settles down?...

Guessing: too low a concentration in a bark tea for that to happen.

A backwashed acid liquid containing dmt (note that the concentration is very much higher than just a bark tea), add ammonia and the dmt will settle on the bottom and form crystals in the ammonia liquid.
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pete666
#9 Posted : 11/12/2018 6:50:01 PM

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Orion wrote:
I think some information came to light a while ago that showed DMT freebase was more water soluble than we thought. It was well discussed in chat. I'm unsure but there may be some info on the forum about this.


I am not aware of that. And I am not able to find anything. Any reference or numbers? Thanks!
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Jees
#10 Posted : 11/12/2018 8:00:19 PM

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^^^^ I'm very interested too.
Might have repercussions for water pipes? Base your water (sodcarb)? Contact time is limited though.
 
pete666
#11 Posted : 11/15/2018 1:47:44 PM

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pete666 wrote:
Orion wrote:
I think some information came to light a while ago that showed DMT freebase was more water soluble than we thought. It was well discussed in chat. I'm unsure but there may be some info on the forum about this.


I am not aware of that. And I am not able to find anything. Any reference or numbers? Thanks!


Well, no response. That's a pity. Anyway, I would doubt the solubility is of any significance, doing titration for every pull and seeing the values for third pull, which are negligible. I would say the curve would look different, if there was more dmt fb in the aqueous solution. Just assumption though
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blue.magic
#12 Posted : 11/15/2018 2:13:25 PM

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Okay I would dismiss the hypothesis that color change is due to DMT freebase solubility. This effect does not occur with when freebasing DMT salt in water, though making the water black first with some dye and freebasing then will be more convincing.

It is probably something else in the tea. The tea itself gets darker when heated and this have more to do with solubility of tannins. Could tannins be broken down with a strong base? That would explain the darkening.

I have not observed darkening when freebasing very hot solution (not recommended!), but when at room temperature, it is more of a brown color that turns black.
 
 
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