my freeze precipitated crystals turn to goo... sigh...

[Z E D]

so SWIM did a freeze precip using heptane as solvent, ok, at the first batch he took the solvent from the jar then let it dry, then scraped the crystals...

but at the second batch, when he takes the solvent and dry the jar, the solid thing starts to look like a goo, it simply doesn't get stable while in room temp, so he has to evaporate it at room temp until it crystallize again, but why?

Why is not solid at room temp? it should and SWIM is getting depressed...

Is there enough reminiscent solvent to dissolve the spice? Are the oils dissolving the spice? Why it didn't happened with the first batch?

 

[soulfood]

Hmm...

What's the exact process SWIY is using? The only form of evaporating in freeze precipitation I know of is to let the excess solvent dry off the crystals after the solvent is poured off at which stage SWIY should be looking at well formed crystals anyways.

I'd scrape up SWIY's goo, place it in a little solvent (just enough to disolve) and put it in the freezer for 24hrs. If crystals appear pour off the solvent then leave the crystals to dry. They should dry of fairly quickly. SWIY certainly shouldn't be looking at goo.

 

[Z E D]

The only form of evaporating in freeze precipitation I know of is to let the excess solvent dry off the crystals after the solvent is poured off at which stage you should be looking at well formed crystals anyways.

yes he should! =/
they look white stable at the start, they are really dmt crystals, then they start to melt and turn to a yellow goo LOL...

he'll try to make a recrystallization (one more) to try to take some oils that he thinks that are maybe, "bothering" the crystallization, the goo - he repeats - is yellow so...

and he doesn't think is dmt n-oxide, the bark used was just a couple of days new

 

[Z E D]

Problem resolved.

The goo had too much oils. SWIM froze the goo, scraped it, put on some heptane and on a hot water bath just to melt the spice. Then he evaporated the heptane until it was cloudy and let the jar get cold a little bit just to let the yellow oily stuff sit, then he could separate it, and the solvent pured freeze precipitade nice white - and solid - dmt crystals.

What SWIM noticed is that if he warm the recrystallization solution too much, the oil thing will get dissolved.