Though the separation procedure outlined in the initial post seems to work perfectly well, a more accurate separation should be achieved with proper measurement of pH and using ammonia instead of sodium bicarbonate/carbonate. I wanted to include this as an option and q21q21 has written up a guide in a similar tek. So I've tried the separation procedure outlined here:
Wiki - Super-Easy No-Filter Harmalas Tek
The starting product had been based with NaOH, washed until the water was neutral, collected and dried, mansked, based again and washed until neutral again, collected and dried. I noticed during the second rinses that the water was becoming more and more strongly colored with each wash (like highlighter fluid, typical dissolved harmala bright yellow/green). This was with plain tap water.
I began with 17.2g of pale tan harmala freebase, 170ml of vinegar and 960ml of de-ionized water. 10% ammonia was added until a pH depression was seen at about 7.3-7.4. It gradually went down to 6.7. I raised it back to 7.3 plus the extra 0.5 to bring me to 7.8 to crash out the harmine. It kept dropping by a couple of points until I got a stable 7.8. I collected the result, raised the pH to the next depression at 8.3, where a slight drop of 0.1 occurred until I stabilized it at 8.3. I collected this mixed fraction. The next depression didn't occur until 8.9 and there was a lot of buffering as I tried to get it to go up. It seemed I was adding twice as much ammonia than before to see a change by 0.1 point. There was very little precipitation and I still had a lot of resistance to pH change all the way up to 9.4 when I stopped adding any more ammonia. Only a small amount of harmaline precipitated after a few hours so I added enough to bring the pH to 10 after collecting what had crashed out but no more precipitation occurred. The final dried yields:
Harmine: 14.1g
Mixed fraction:1.0g
Harmaline: 0.4g
I think harmaline must affect the color of the dry freebase quite a lot, as the initial product was very pale despite only containing a small amount of harmaline. I think the losses could be due the water rinses removing a lot of harmaline. Curiously this seemed to happen more after purifying with a manske and basing a second time than it did during the first rinses after the initial basing.
Perhaps ammonia could be used to basify the rinses to prevent loss of harmaline? Less rinses will be needed if ammonia was used to crash the harmalas in the first place too, as there won't be excess base in the dried product.
