Freeze precip yields sediment but no crystals

[CharlesBronson]

Alright, so here's a little info on the extract. Followed Norman's tek with revisions. I did also let the solvent soak for at least an hour per pull and agitated it much more than recommended, but no emulsion was formed as I was quite gentle.

100 grams of M**B powder
150 grams lye
1500 ml water (seemed like way too much, but I blindly followed)
pull 1 = 100ml solvent
pull 2 and on = 60ml solvent

I combined pulls 1 and 2 in a wide mouth 1/2 pint jar with a glass turkey baster, capped it and froze it before bed. I also added another 60ml of solvent to my basic soup to saturate overnight. When I woke up today (approximately 10 hours later), I check it out in hopes of a glimpse of some kind of goodies in there. No crystals but there's a thicker layer at the bottom starting to settle, there's not much color to it.

I'm assuming that I have just a little bit too much solvent in there. My first pull used a bit more because I was worried about separating such a small layer of solvent out of this giant pickle jar. So I have the dmt-rich solvent doing a partial evap before getting it back in the freezer for one last shot at crystallizing it before giving up and evaping the whole jar.

 

[Binary Drool]

1 hour is really quite a long time per pull. I've had great results with 5 minute pulls. As for freezer preperation you're on the right track. Let 50% of the solvent evaporate and stick it in the freezer again over night. Give it 12+ hours. If you're not getting good results decrease your pull time. It seems unlikely but the spice may be merging with aqueous layer the longer it sits. If you're going to stick with this Tek I suggest you invest in a seperatory funnel.

Good Luck!

 

[Ambivalent]

1 hour is really quite a long time per pull. I've had great results with 5 minute pulls. As for freezer preperation you're on the right track. Let 50% of the solvent evaporate and stick it in the freezer again over night. Give it 12+ hours. If you're not getting good results decrease your pull time. It seems unlikely but the spice may be merging with aqueous layer the longer it sits. If you're going to stick with this Tek I suggest you invest in a seperatory funnel.

Good Luck!

it doesnt matter how much time you leave the mhrb soup and the solvent together. dmt will always preffer to stay in the np solvent as it is more soluble in it. if anything more dmt should migrate over time in the solvent, not the other way around.

 

[Binary Drool]

Yea, seems unlikely.

 

[shardymarty]

Too much NaOH. Too much H20. How long did you wait after adding the NaOH? Remember to extract with room temp or hot naphtha, heated using a external heat bath of course. don't wait an hour for a pull it only takes 5-15 min to separate, especially when using a heat bath for your extraction jar!