hamhurricane wrote:ok acolon my friend has finished the procedure, the two main difficulties were deciding how much solvent to use, you said so much that it would not fog upon freezing, which would be more than in the initial pulls meaning for a gram i would be working with approx. 500ml seems like way too much?
my other problem was when melting down the unwashed dmt a fatty oil immediatly would settle to the bottom should swim just keep pouring off from the oil or dump it in as well, how much dmt does this oily crud contain? i poured in as much as wouldent stick to the sides of the beaker (its really sticky) and it fell to the botom of the sep funnel, then stuck btw the water and the naptha layer, the naptha did not become clear after washing nor did the sodium bicarb soln turn cloudy...
its in the freezer now, will update
EDIT: the amount of solvent used was perhaps too little as the soln fogged after about an hour of freezing, acolon do you think this might have reduced the yields, i still have the water, is sodium bicarb insoluable in naptha?
NO!!!! WAIT!!!!
I don't think I was clear enough. During recrystalization the naphtha is heated up quite a bit to dissolve the spice. What I was saying is that when the naphtha/bestine cools down to ROOM TEMPERATURE it should not precipitate out any spice. 150mL of bestine per gram of spice has worked well for me. 500mL is way, way too much. The reason for this is that we don't want the spice the to precipitate out into the wash layer. At no point in this wash should anything go in the freezer.
With the oil layer, you can dissolve most of it if you want, but some of it will end up in your final product. I would leave about 1/2 of the oil puddle.
You are going to need to reduce the amount of solvent you have or not much will precipitate out.
After my wash I usually let my spice recrystalize at room temperature. It allows much larger crystal growth and thus gives a cleaner product. I then melt it down.
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