Salting out xylene pull

[MachineElf88]

Hey guys, I'm using xylene for the first time to pull right at the end after all my naptha pulls.

I'm trying to salt it out so I've added some acidified water to the pulled xylene, mixed it up and let it settle. When I remove the water using a turkey baster and put into dish to evaporate it stinks of xylene. I've tried a few times and it's always the same.

Am I doing something wrong?

 

[endlessness]

You could put the vinegar with limonene traces in a container in the freezer. The xylene should stay on top and not freeze. Once the vinegar is totally frozen you can do a quick IPA or acetone wash which should pick up the xylene on top.

Im not sure if dmt acetate is at all soluble in ipa or acetone so I wouldnt recommend you to wash the room temp gooey acetate directly with those solvents.

Thats an advantage with working with fumarates /FASA, because you can wash fumarates with ipa or acetone, and there wont be traces of the non-polar.

Are you planning on consuming this orally or turning back to freebase for smoking?

 

[MachineElf88]

Thanks, I plan on turning back to freebase. I used water with phosphoric acid so it's DMT phosphate.

So I freeze the acidified water and any xylene will sit on top. I have some IPA but what exactly does an IPA wash entail?

 

[endlessness]

The IPA will pick up the xylene and take it away from the frozen acidified water which should have your alkaloids. Not sure about phosphate solubility.

In any case if you mix with sodium carb and then pull with IPA later on to freebase it, any remaining xylene will probably have enough chance to evaporate off.

But yeah doing the wash while acidic and frozen may help that even further. Youll just need a little bit for a quick wash, then you let the whole thing thaw and dry it to mix with sodium carb and pull.

 

[MachineElf88]

So to wash I just add IPA to the dish with the frozen water and xylene on top, mix and then pour off the xylene and ipa mix?

Why can't I just basify the acidified water that now contains the alkaloids like in a mini A/B and then pull with naptha rather than doing the whole evap and sodium carb thing?

 

[endlessness]

You can, yes.

The naphtha will pick up any xylene traces there are left. If you freeze precipitate and it was a lot of xylene, some of the alkaloids might not precipitate. You could try anyways, it might be so little xylene that it will make no difference.

I'd keep the naphtha after freezing even if freeze precip works, and I'd evap that naphtha and/or reuse for more pulling, just to make sure you're not losing anything

 

[pitubo]

Why can't I just basify the acidified water that now contains the alkaloids like in a mini A/B and then pull with naptha rather than doing the whole evap and sodium carb thing?

Because these are the alkaloids that wouldn't dissolve into naphta very much to begin with (as you wrote in the first post)?

 

[frobot]

The same happens for me. The thing I don't like about xylene/toluene is how strongly they smell. Seems like just a fraction of a drop is enough for a strong odor.

 

[Jees]

Freezing will split the two phases better indeed.
One way is to freeze in a beaker kind of recipient, closed with plastic and rubber band.
Then poor of the top layer (to be re-used) and use a paper towel to dry the frozen acid surface as much as possible, as soon as the watery layer is frozen. The paper towel gets little wet by sucking up remaining hydrocarbons. I've never done the IPA or acetone wash to work like the paper towel trick, I did not know of it until now (thanks!), but both tricks can be combined.

Option from there: boil the acid solution hard (adding some water now and then to remain level) to strip off hydrocarbons that found a way in there, until most (all) smell is gone. The steam bubbles coming from the bottom attract the hydrocarbons (due the ultra low partial pressure of hydrocarbons inside the steam bubbles, hence boil hard) and then take them up and out with the steam. Fume hood = On of course.
I've no idea how effective it is in absolute removal, but one can boil the smell out to large extend.
After that, evaporating, sod-carb...etc.. as said.

Toluene's solvability in water (0.5 g/l) > that of xylene (0.2 g/l).

IIRC, it has been posted that phosphoric acid is not the best for salting out due having multiple pKa's. I've never checked out how that plays a practical role, but the word was out and vinegar is such an easy alternative.

I've never found toluene smell as much like xylene does.