contaminated harmalas extraction

[NormPeterson]

I am hoping for some help with a situation I have gotten my self into.

I am in the middle of extracting harmalas from rue seeds and on a Manske step. I had around 10 grams of harmalas dissolved in 75ml vinegar, added 200ml hot water and had a nice deep red clear liquid. I put this on a magnetic stir plate and added 30g salt. While this was dissolving I noticed some salt was stuck inside the neck of the flask. I tried to flush it down with a little water from a wash bottle, but the red liquid turned to a mustard colored froth. For some reason, thinking I was precipitating freebase, I tested the pH and found it near neutral, so I added another ~75ml vinegar. That did nothing but lower the pH to around 5.

Stopping to try and figure out what is going on, I notice my water bottle is on an upper shelf and I likely used a 99% IPA wash bottle instead.

What I likely have is a mix of 10g harmalas, 200ml water, 150ml 5% vinegar, 30g NaCl, and ~10ml IPA all whipped up into a thick froth.

Does anyone have suggestions for what I should do?

 

[TransistorBass]

Could you gently heat until you can't smell any alcohol, it will be the first part to evaporate, then you could continue your extraction. "The boiling point of ethanol is 78.23 °C (172.81 °F)"
IPA does dissolve Harmalas, assuming you dry your extracted Harmalas to powder you won't get any residual IPA in them.

Unless anyone knows of any chemical reactions that would cause issues???

 

[Sakkadelic]

It's possible your harmalas just crashed out as they cooled down as intended in the manske step, adding room temp water probably cooled it down too fast. The harmala concentration is also quite high so the whole liquid turning into slushy like consistency is normal, don't know if that's what you meant with froth.

I would heat it up until everything dissolves, it'll be near boiling before that happens. If it's taking too long on a hot plate use a double boiler. Any potential IPA should evaporate during heating. Then let it cool down slowly undisturbed.

 

[doubledog]

I would evaporate IPA by boiling it for a bit, then dilute with some water. Add salt to adjust increased volume and go on with manske.

 

[NormPeterson]

Thanks all for the responses. I heated it and at about 60C it turned back to a clear red that I expected. I continued to heat until the temperature reached 90C. I was unable to smell IPA because of the vinegar. Still uncertain what I did, I set aside 3 test tubes with some samples to play around with later. The rest went into an insulated container to cool and I expect is forming needles as I write this.

I was a bit curious about what I did. I’ve extracted harmalas before and never had anything like this yellow froth either in color or consistency. To the three test tubes I added room temperature water, cold water, and to the third IPA. The two that I added water to remained clear, but the one with IPA formed needles almost immediately and looks like what I’d get at the end of the Manske crystallization. There is no yellow froth. Adding IPA to one of the other samples again caused needle-like crystals to form.

I’m guessing what happened is that I did accidentally add IPA and that it immediately caused crystals to form, but since that was happening while the mag stirrer was running, they presented themselves as yellow and remained suspended. (When I returned to my mess after it had rested overnight, only a tiny bit of clear liquid had appeared above the yellow froth.)

Maybe IPA can be used to speed up the Manske step...