A Simplified A/B?

[Trickster]

SWIM did Noman's STB on 50 g of MHRB. For some reason the yield came out very dirty. She combined 2 first pulls and tried re-xtalisation. SWIM used 15 ml of heptane for it but after an hour in the fridge she got about 20 ml of dark yellow rather homogeneous jelly. After half a day in the freezer SWIM noticed certain amount of crystals lodged in the mass of brwnish goo.

SWIM read in a lab manual that re-x does not work well on very dirty mixtures. She decided to try an A/B on goo with crystals. Browsing the forum she did not find a description of an A/B, modified for processing dirty STB yields. She suspects that there is no need for 3 acid pulls.

Any suggestions?

 

[q21q21]

Although it sort of sounds like you may have pulled some bark-water or part of an emulsion, these teks should work


1.you could try the simple version with a sodium carbonate wash. Redissolve the stuff in naptha/heptane then add equal parts water with a pinch of sodium carbonate.
Shake it really well. Evaporate to 1/2 then freezer precipitate.

SWIM hasn't had much success with this but many have...


2.If you really think that the stuff is too dirty and you aren't worried about a little loss, you could try to change your STB to a B/A/B

Take your dirty crystals, Dissolve it into some naptha/heptane.

Then add equal or greater parts HOT vinegar. Cold = loss of product.

This will take all the alkaliods back into a salt form. Shake it up good, emultions are really fast-resolving

Take the bottom layer of vinegar and put the naptha/heptane asside if you need another vinegar pull later.

Basify the vinegar with sodium carbonate or lye.

Then Pull with some naptha/heptane. You can really shake it good this time too.

Evaporate to at least 1/2 then precipitate in freezer


SWIM finds that if you take a really small pull of naptha first it will dissolve most of the yellow alkaloids out, then the second pull will be much less yellow.

SWIM has done this quite a few times and always gets nice white crystals. Although he has not established the efficiency in keeping the yield.

 

[Trickster]

Thanks q21q21,

Although it sort of sounds like you may have pulled some bark-water or part of an emulsion,

Don't think so. Originally SWIM had a lot of emulsion, but after she added about 30% of basified water to the solution two layers separated very well and there was no emulsion at all.

She said she doesn't mind some loss, so she will try the second tek.

2.If you really think that the stuff is too dirty and you aren't worried about a little loss, you could try to change your STB to a B/A/B

Take your dirty crystals, Dissolve it into some naptha/heptane.

Can you give SWIM an idea how much heptane is needed?

Then add equal or greater parts HOT vinegar.

Equal to the amount of heptane? How hot?

Cold = loss of product.

This will take all the alkaliods back into a salt form. Shake it up good, emultions are really fast-resolving

SWIM can borrow a magnetic stirrer/heater .

Take the bottom layer of vinegar and put the naptha/heptane asside if you need another vinegar pull later.

Why bother with the second pull? Is this because of possible vinegar saturation? Otherwise night-long stirring should do the trick.

Basify the vinegar with sodium carbonate or lye.

What pH should she aim at?

Then Pull with some naptha/heptane. You can really shake it good this time too.

A day of stirring should be enough? Room temp or higher?

SWIM finds that if you take a really small pull of naptha first it will dissolve most of the yellow alkaloids out, then the second pull will be much less yellow.

What do you do with naphta from the first pull? Discard? Is this what they call "defatting"?