Hi all, that's m first post. I did look around before posting, but couldn't really find an answer.

So, in short: an STB extraction from MHRB, following Noman's tek, but with sodium carbonate wash instead of the originally suggested ammonia was. A nice amount of snowy, crystally looking things in the collection jars after freeze precipitation. An attempt to filter them out was made, and this is where things turned sour. All of the crystals turned into an oily goo... some crystals melted into the filter paper, never to be seen again...

My question is what did I do wrong? Could it be that this particulat MHRB batch had too high fat content? Could I maybe defat the remaining naptha solution? And if yes, how should I go about it?

Thanks a lot in advance.

EDIT:

OK, so I read through the Lextek extraction method. Would the "Part 5: Defat Step 1: Acid Wash" work? The only difference is that Lextek assumes shellite is used, and I used naptha. Are they similar enough?

Second edit:

So, from what I gather Shellite is a brand of naptha... doh!

I guess this is what I will be doing then. Still, any comments and advice would be much appreciated.

When you do freeze precipitation, make filtering process in the fridge, its a bit tricky thing. If you make it outside, the crystals will melt and get sucked by the filter paper. I try to do it as quick as i can and scrape the most of the stuff from the emptied jar. Then whenever a drop of naphta appears in the jar im scrapping i put it on filter paper again and continue scrapping... needs some experience actually. Took me sum time understanding how to do such an operation in a half-full freezer, without spilling naphta on frozen fishes and stuff .. Now i can do it when the freezer nearly full up eheheh kinda juggling exercise for me

It's a good idea to cover any crystallization container or the naphtha smell could permeate into the food in the freezer. Also, by leaving the crystals to freeze much longer, they often stay stuck to the crystallization vessel much easier. SWIM slowly pours the solvent off the top of the crystals, making sure that no crystals are poured off with the solvent. He leaves a small amount of solvent on the crystals, to evaporate, rather than trying to catch the crystals with a filter, because as you described, they will melt back into the solvent and filter when the temperature rises.

I tried a partial evaporation of a small amount of naptha, but it really just turned into oily goo again. Impossible to scrape too... I fished out a crystal and put it into a pipe before it melted, and yes it is what it should be... but dammit, I want to get crystals...

Anyway, will try the defat from Lextek, and see how that goes... Can't think of anything else.

Was heat added when evaporating? If so, this could have melted the DMT a bit, causing it to be more oily when crystallizing (and also takes longer to crystallize). Also, one can wait a long time and the oil will sometimes crystallize, or they can scrape up the oily residue, and it will begin to harden quicker. The best way to clean this up (oily goo) is recrystallization, and when SWIM has the time, he'll post the recrystallization tek. SWIM rarely sees any difference when defatting MHRB solutions during the acid/water phase of the extraction, and it seems to work much better on plants that contain chlorophyll.

Also, trying to filter out the crystals is usually a waste, because the crystals are tiny and even a slight bit of warmth while trying to pour off the naphtha will cause them to start redissolving, and thus get stuck in the filter. Best to leave the naphtha in the freezer for a day or two, then slowly pour the majority of solvent off the crystals, and then let the rest evaporate off the crystals by use of a fan blowing over the top of the crystallization container. No heat should be used while evaporating the naphtha, as this causes the DMT melt, and the crystals take an extra long time to form. OTOH, if evaporating in front of an air conditioner, one will see the crystals fall out of the solvent as it evaporates, and one will get larger crystal structures.