Oh God no, the brown goo-spook again! As for now, we don't know the exact reason why it sometimes appears and at other times it doens't. What we did find out was that when you stick to the experimental details in chapter 2 of VDS's paper, it stays away. So adding the ammonia slowly under stirring might be a good idea indeed. Yieldwise as well, it will surely help. Also, you could try keeping the concentrations of the reagents as similar as possible to the ones in the paper. You're so close, Ijahdan, good luck !

This batch you had it precipitated before with ammonia without a problem, the only difference now is that there was a reduction step in between.

First white that disappears is normal and should be like that exactly, that is a good sign that your ZnSalts go to soluble Zincate
Then the white that stays is the alkaloids precipitating, also very good.

If I look at that pictures it looks like brown yes, but not sticky? It looks non sticky brown, is it?
I've had some brown too before (not that much like yours) that was not sticky, I could easily remove it from the pH probe. I would consider this not a disaster.
But the real stricky-spook you just cant remove it easily because it is actually like glue, it formed a hard layer almost, now that was something else.
I'd like to know what kind of brown yours was please.

You said before that there was a lot of sodbicarb/sodcarb contamination that you removed with an acid/base (vinegar/ammonia) treatment, do you believe that all the sodbicarb/sodcarb was out? If there were still remains these might have added to the brown syndrome.

If I were you I'd just redissolve the brown in vinegar and re base with ammonia. Hopefully you get white THH because there are (quite) no zincate in the equation this time.

VDS added water in the cases that could lead to (sticky) brown syndrome, so perhaps making the solution less concentrated might help, worth trying I guess.

Keep us updated pls

BTW I did some couple of A/B transitions on TUV and lo and behold the pH depression got lowered to around startpoint 7. By this one could easily start thinking harmine now, but the crystals (vessel and in-situ) still differ from harmine. Yet taste is the same as harmine, meaning nearly no taste for a harmala. This in huuge contrast to DHH which is a true pest of taste and it simply doesn't go away LOL.

I could try to reduce it (TUV) with Zn though, while the totally absence of DHH taste gives me low expectations for such to succeed.

I've essayed harmine once at 200mg and it was very clear in body and head. Stomach had no issues at all, this was so great. I could feel it's workings as a harmala alkaloid nonetheless while it was not combined with another alkaloid to check out maoi potency.

I can't wait for the analysis results.

Jees; The pictures show the brown precipitate after soaking overnight and then the liquid decanted. This has now dried and is more like a tan coloured powder, but when it first formed it was quite sticky. I had to scrape it off the spoon and the sides of the jar. So maybe it was a mixture of crystals and goo? Maybe, as you said, some residual carbonate/bicarbonate affecting things.

Ill do another vinegar/ammonia stage and see what happens.

Taste-wise, I had the same experience as you, the harmine being almost tasteless and harmaline leaving a bitter aftertaste for ages. Thats reassuring. Looking forward to tasting the pure thh when I get round to reducing the harmaline.

Bad news guys, the 10 samples that I've sent for analysis still did not arrive. I do have most of the samples still in the freezer, so I could send them again. Let's wait one more week and keep our fingers crossed...

Just a stray thought here about this TUV substance. As a (stretched) analogy, benzoquinone and hydroquinone co-precipitate from solution as a 1:1 complex (known as quinhydrone). So the idea that TUV may be a mixture of harmine and DHH is certainly not far-fetched.

Keep up the good work, peeps!

Thanks for a stretch. Without lab equipment and dito knowledge its black box symptoms, I wish Benzyme was my neighbor but then again he might have barricaded his door by now

All we can do from a kitchen perspective is having an approach that dodges the booby traps, and VDS had very likely his own fair of those before he got to that paper.
An1cca was smart to align soon with the paper, I am more the stuborn type skirting on the edges and facing the how-not-to effects here and there
But I consider it all learn-some and even better than game of thrones or any other brain deadening pulp-ish time killers.

I admit, I've always been the conformist type


And then there is that small detail where we have these timeless experiences of ineffable beauty and understanding ....

Seems that our alks have been taken away from us before they could reveal their true nature . I add a picture in their honor...Next week I'll send some more of my baby-crystals

No post = a bummer, feeling sorry for that, but in the end it is delay only, the truth will prevail eventually.


* * *

NEXINE
My post #198 was about it. The pic shows brown and white nexine shards in that little plastic box, obtained from different runs on rue, the one better cleaned than the other.


I never did in situ crystallization on it so it is about time to happen. These are pictures of the brown version:

Characterizing: two long axial feathers that are attached to some kind of a cross.


These are pics of the whiter cleaner version:

^^^ The cross gets pimped at the expense of feather, more bulky overall.


I repost here now pics of DHH (Harmaline) to compare it with:

I never really took much notice on a cross in DHH before, it's finer feathering camouflages the subtle cross a bit. But definitely it is the very same core structure between nexine and harmaline. They taste same too btw. They are same blood family, as in "the same" but with a twitch. Mainly falling out at complete different pH's, and nexine didn't ZN reduce as DHH did.


A veil dropped... but mystery remains...

Intermezzo Interludium

This sequence is harmala crystals that dry out on the glass.
This is not relative to the OP actually but just for meeting crystals
It's shape shifters
Again indications that the setting plays a huge role in crystal form.

Some extract of Banisteriopsis Muricata got in situ crystallized. It looks like all harmine according to our pictures a la system VDS. If we consider Caapi as a reference for harmine, then this looks re-assuring for our works here, these vine crystals appear as an out of the book harmine.

No THH bolders? The batch wasn't boiled, I believe it was a muriatic acid cold water extraction. If boiling vine adds to formation of THH (this is an existing hypothesis) then it might make sense to fail on them here in CWE.

Jummie! Love this research, Jees! It's so beautiful down among the microcrystals.....

It's difficult to believe that Nexine and DHH are not the same. But as you say, if it can't be reduced bij Zn...??

Taking pictures of in situ recrystallized caapi-extracts might be a (very crude but low-effort) qualitative and semi-quantitative method of analysis. Good thinking of you to introduce it here! And what would a brew look like..?

I'm planning on resending the samples later on this week (quite busy at the moment). Keep up the good work!

I would love to debunk nexine as DHH, and TUV as harmine, so that would simplify things much more, and all would boil down to my very own unpolished method spin offs and bothering you guys for nothing.

Agenda:
* I'm going to try Zn reduce nexine once more, there was only one attempt so far;
* my recent batch of ongoing rue extracts has only seen pH 10 as highest, expectations are to not encounter nexine anymore. It's now in the 3rd A/B cycle, then going to manske like hell.

If nexine and TUV has learned us something so far: crystal growth is a very sensitive balance, things can skew it rapidly. Without VDS and you (An1cca) I would have been lost, rigorous "diet" of influencing parameters is mandatory.

Thanks for the support

Looking back at post #5
I didn't want to search though the whole of this thread (sorry), and although I might foggily recall seeing a bit of TLC take place, did the 'nexine' and 'TUV' ever get tested via TLC?

Nope, no TLC-expertise here...

Would surely help a lot, though!

I wouldn't say TLC required excessive expertise. Looking at the meticulousness of execution here, any efforts made would likely be most informative. It will be a while before I get anywhere near that stage myself, so I wanted to offer you those words of encouragement!

Thanks for that, I'm going to dig into it.

* * *

A second attempt to Zn reduce nexine, these pics are right after the vinegar and Zn got in.
The first two are the archetypes, the third pic illustrates that there are a bunch of deviations of the archetypes like here the middle cross is comparatively under developed. Sometimes a cross-leg develops as another feather leg. Then there are a bunch of broken up archetypes etc. It is a challenge and a sport to find the archetype and then realize all the others are parts or modifications/deviations of that archetype.

Working with the crystals is dangerous because it is very addicting
Remember that I failed til the point of discouragement before I got to a proper in situ crystallization. I had to know where to end to get there, I could never done that on my own without the paved path I gratefully had here. This is not to discourage people here, many things in life are like that, like making an extraction etc. Just want to say that the feeling of reaching success is priceless. Before I fall into sleep, those crystal forms are imprinted somehow and start to tune the vibe of being, if you let it