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Fluorescent sediment after zinc reduction Options
 
Jagube
#1 Posted : 2/28/2020 1:16:07 AM

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I did a zinc reduction on a mix of harmine and harmaline. The procedure was like the standard way, but with additional HCl added to the solution. I brought the pH to somewhere between 1 and 2.

The reduction seems to have completed and it ate almost all the zinc.

I filtered out whatever zinc was left and let the supernatant settle. After settling the solution has no UV fluorescence, but there is a green fluorescent sediment at the bottom. Any idea what it is? It's rather acidic (pH around 3), so it can't be freebase.
Could it be undissolved harmala hydrochlorides? But why would they have passed through the filter? Could there be more of this trapped in the zinc?

Also, I thought harmine was fluorescent; it turns out it's not, or not always.
Jagube attached the following image(s):
fluorescence.jpg (243kb) downloaded 42 time(s).
 

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Jagube
#2 Posted : 2/28/2020 3:14:47 AM

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After sitting in a cooler room more fluorescent crystals appeared. It must be harmala HCl's.

My plan:
1. Wash the zinc in the filter with hot water to flush out the hydrochlorides
2. Add those to the main jar. Heat it to dissolve the crystals and see if the solution is still glowless.
3. If it glows, repeat the reduction.
 
 
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