Brown Sludge and Inseparable Naphtha

[acrosstheveil]

I did a 1 lb. extraction STB style in a one gallon jug. First pull came out dark yellow and subsequent pulls all were a dark brown sludge. We've tried to get it to separate with salt and adding more lye but nothing happened.

We tried a recrystallization and the brown was still everywhere (both with naphtha and heptane). We tried adding 500mL of basified water to the solution and now the water and the naphtha layers are a dark muddy color. What is wrong? Is there anyway to get these layers to separate?

This is a picture of the naphtha recrystallization attempt with about 430 ML of basified water.

 

[endlessness]

Check the FAQ before overcomplicating yourself. Pull the naphtha layer leaving the basicwater layer behind, salt it out, discard naphtha, base again, pull again.

 

[acrosstheveil]

yea, i read the faq but I am still confused. Is it possible to add washing soda directly to the solution containing the lye water and naphtha? Would the sodium carbonate settle on the bottom wwith the water? Then I could just syphon the naphtha off the top?

 

[Thre365ive]

That's not how a sodium carbonate wash is done. You'd have to pull the solvent off, then wash it with an aqueous solution of sodium carbonate.

I've had the same problem lately, and I haven't really found a good solution. I just decided to go with shredded bark next time.

 

[endlessness]

What are you confused about? In this case you should do a Mini-A/B, as explained in the "brown naphtha problem" FAQ question