1st pull. Only 1/2 of NP has been recovered. Where is the rest?

[Trickster]

Noman's tek (150 mg of finely powdered mhrb + 150 g of lab grade NaOH + 150 ml of n-heptane).

SWIM waited for 3 days shaking the jar vigorously very often. There was no emulsion. He used a glass pipette and sep. funnel to collect the NP solvent. He only got 85 ml of heptane that after being reduced to 40 ml started to produce nice crystals at around 0C. SWIM still wonders where is the rest of the solvent and how to get it out.

 

[Noman]

With finely powdered bark and a STB, the NP can frequently get stuck in the aqueous layer.
Try adding half again as much water and another 100ml or so of heptane and see what happens.
If that doesn't do it, 100g of table salt and a warm water bath might kick it out.
Mind you, I'm guessing a bit here as my Antarctican friend has only pulled A/B's with heptane before.

 

[Trickster]

Thanks.

SWIM used 2250 ml of water for 150 g of mhrb. Unfortunately his mixing jar is almost full so atm he managed to add another 300 ml of water only.

He added 150 ml of heptane before reading your post. If heptane does not separate he will have to divide the mix into 2 jars to add more water. Is it just water he should add or some lye as well?

How much heptane (percentage-wise) should he expect to get back?

 

[Trickster]

Can SWIM do another pull after adding salt?

Do you think a magnetic stirrer may help to get the trapped heptane out?

Another question. SWIM accidentally spilled heptane from the 2nd extraction in water. He run both liquids through a sep funnel and collected most of heptane. But after evapping he only got yellow oils. Not even a trace of spice. Could it dissolve in the water?

 

[XENONSION]

You used 15ml of water per gram of bark (just like the tek calls for)

but with finely powdered bark, you need more water/lye solution added. You probably should have started with about 3000-3300ml of water (20-22ml per gram of bark)

Just adding the extra h2o should do the trick. Pull out whatever solvent you can, add the water, and mix again. Then try pulling from it.

If your container doesn't have enough room, perhaps you can split the mixture into two smaller containers, and work from both.

 

[Trickster]

Just adding the extra h2o should do the trick. Pull out whatever solvent you can, add the water, and mix again. Then try pulling from it.

If your container doesn't have enough room, perhaps you can split the mixture into two smaller containers, and work from both.

I forgot to mention that SWIM already did that. Now his water/bark ratio is 21.5 ml per gram. He also added some salt (NaCl). Still he did not recover all the solvent. Should SWIM add more water? Does he have to add lye too? How much?