First time brewing - Test E

[bigforyouben]

Im a synthetic organic/inorganic chemist by education and trade. Since im new on meso, i will offer my expertise if wanted. I really like recrystallization. The companies ive worked for (the last one is a trillion dollar company- thats with a T) have made millions on the stuff i purified with a simple recrystallization. Fun stuff.

No doubt. But I am (or was) just a dude with 100g of raw and a hot plate stirrer.

 

[james13]

No doubt. But I am (or was) just a dude with 100g of raw and a hot plate stirrer.

I was edumakated at some backwater university and partied a lot during grad school.
If I can do this, you surely can. Just follow the instructions from that @TheScholarOfBrew guy

From what i see, your test E is supposed to be a waxy goo at room temp. Im not too sure if thats supposed to be that yellow though.
1. Dissolve test E in hot (50C or so) 100% ethanol : Add minimal anhydrous EtOH to the goo in a beaker or flask.Heat in a water bath (60–70 C) with stirring until everything dissolves to a clear solution, leaving only insoluble trash (if present).
2. Without burning yourself, quickly filter through a funnel/filter to remove particulates while solution is still hot/clear.
3. This is the part that requires patience:
While stirring with a magnetic stir bar, use gentle heating of around 70C to 78C in a water bath to get your test E and ethanol solution to evaporate off the excess ethanol until you see the test E become as concentrated as possible. I havent done this before, but what I would look for is the color of the solution to darken somewhat. It should be darker than when you first mixed it with ethanol. In other words, the total volume of both your test E and ethanol should be LESS than when you started. For example, if you needed 100mL of ethanol to get your mixture of ethanol and test E to suddenly become clear, and the total volume went up to 200mL, then you should aim to reduce your volume with gentle heating to around 160 mL.
You do NOT want any solid to crash out at this point. If it does, add a little bit of ethanol to get everything to dissolve. The point of this is to make the solution as dense and as concentrated as posssible.
4. Cool your dissolved solution to 4C. Once its cooled, if youre lucky, you may see some crystallization. If you dont, thats fine.
5. This is another tricky part: pour COLD water very slowly on the side of your solution vessel. It should not completely mix. This is called layering. Maybe theres a youtube of it somewhere. "Organic layering and recrystallization." If the interface of the ethanol and water produces tiny particles, thats okay. They will serve as nucleation sites for your precious crystals. You should see a layer of water, about equal roughly volume of your "mother" solution. If you can fit more water without disturbing the layer/separation, thats also good. This is literally called the mother liquor haha.
5. Carefully put this back in the fridge. The water will eventually diffuse into the ethanol, and the crystals will form. This will take some time at 4C for the crystals to form. If the water and mother liquor had mixed and you still dont see much crystals form, put it in the freezer.
6. Vacuum filter the crystalline solid, wash quickly with a small amount of cold aqueous ethanol (high water content) to remove colored impurities. Put the wet crystals in a dry glass jar or beaker that you weighed previously. Once its dry, you can weigh both the beaker or glass container and your crystals (or white to cream wax) to get your yield.

You basically need a buchner funnel, a filter funnel, a cheap vacuum pump, and whatman filter papers that fit flush on your buchner funnel. I like whatman #5.

If all else fails, panic. Jk. Dont throw anything away. Boil it all off, water and ethanol and you will get your wax back.