does naptha seperate from water?

[ashleytea999]

my glass container broke during the non-polar wash step. I was doing the lime tek and the bottom of my container broke off and all of the bark and naptha that were inside slid right into the water and now im not sure what to do. if i try to evap the water what would happen to the naptha? or will the bark mixture still be useable if i evap. all water and naptha? is there any way to seperate the naptha and dmt from the water/bark mix?

there was 100g mhrb, 100ml naptha, 75g lime inside the container and like 1.35L of water in the bowl that had the hot water to warm the bark/naptha mix.

 

[padawan]

oh man, that sucks I've had mason/bell jars do the same several times - highly basic solutions plus heat just destroys cheap glass.

The naphtha will separate from the rest of the solution. Sift out the broken glass, pour it all into some kind of tall glass jug (with all the water the PH will have gone down - less chance it will weaken the glass again) and let it separate (maybe overnight if needed - if you have emulsions then do some searching on here because there are various ways to break it down). Siphon off the naphtha (keep this - it has some of your goodies inside). With the remaining solution you can either add a LOT more lime to get it back up to PH 12-13 and do more naphtha pulls (not recommended), or evap it down with a fan (may take a fairly long time) until it's a more manageable volume then increase the PH back up again and resume your naphtha pulls.

Goodluck and invest in good quality borosilicate glassware!

 

[ashleytea999]

thanks!!!

 

[downwardsfromzero]

The perils of thermal shock!

It's always a relief when the water bath has saved your working materials. As padawan says, it's straightforward enough to separate the naphtha off and proceed from there. A quick way (i.e. without evaporating) would be to add sodium carbonate, preferably anhydrous, which will react with any remaining lime to produce sodium hydroxide. This pushes the pH up nicely so you can then pull with more naphtha.

And, if you made your sodium carbonate using food grade bicarbonate, this is a simple way of producing food grade NaOH solution.

 

[ashleytea999]

this might be a dumb question but i add the sodium carbonate to the water/bark after i siphon the naptha right? i left it overnight to seperate which worked fine, the only thing is that i dont see a layer of clear naptha on the top.. its kind of milky looking. does that mean i had emulsions?

 

[downwardsfromzero]

Milky after cooling could - and most likely does - mean your DMT already has started precipitating from the saturated solution, so syphon it off and stick it in the freezer.

BUT - because you used lime, it might (also) mean that some lime particles are in the naphtha. To check for this, gently(!) warm your naphtha in a heatproof(!) dish, of course for safety's sake using a warm water bath. The milkiness should clear completely.

If it doesn't go away after heating up to the initial extraction temperature, you'll need to leave the lime to settle out and syphon off the clear naphtha, or filter the naphtha. An alternative to separating out the lime would be to proceed with the freeze precipitation and then clean up the DMT afterwards with a mini A/B.

With the remaining bark soup, optionally add the sodium carbonate - because it sounds like maybe your pH has stayed up pretty well - and do a couple more naphtha pulls.

 

[ashleytea999]

thank you so much!