Final yield of 1.96 grams. The crystals aren't delicate crystals like I've seen in the pictures, but they are pure white and powdery, and much prettier than the HCl crystals I've made.
If anyone cares, I think I would make the following changes to the procedure outlined in dg's simple ditration/dual solvent crystallization procedure:
- Ideally, use a separatory funnel. It's much easier than using a baster to decant the bottom layer.
- If a sep funnel isn't available, increase the amount of distilled water added to the organic extracts from 1/2 cup (~120ml) to 200ml, because it's easier to baste up a large volume of water than a smaller volume of water. Reduce the aqueous layer to the same amount (~50ml) in either case.
- Once the acidified aqueous layer has been reduced to about 50ml, don't add the acetone quickly. Instead, while the solution is still hot, slowly add acetone until the resultant solution begins to cloud up. This will most likely result in a crystal that is more pure. I base this advice on the dual solvent procedure found here:
https://ocw.mit.edu/cour...301IAP12_Two_Solvent.pdf- Gravity filtration with coffee filters isn't that great. It took forever to drain, and even then some of the crystals flow through the coffee filter, as evident by a milky white filtrate. An attempt was made to process the filtrate a second time but, again, it flowed through the coffee filter. Scraping the crystals off the coffee filters was also a pain in the ass, as the filters don't hold their shape very well. A cheap hand-operated vacuum filtration setup can be had for $30-50. A finely-fritted Buchner filter would probably work, although a porous Buchner filter might be better as the filter papers can be fine or coarse, as needed.
Overall, I'm happy. A 0.8% yield of dry material on San Pedro isn't too bad! Next time around, however, I think I will try pete666's STB procedure, Elrik's acidifcation advice, and my own suggestions. I might even try a hot-water recrystallization after the dual solvent crystallization, to get those beautiful mescaline sulfate needles I've seen pictured