GOD dreamed that he had completed the above extraction and was left with a red, tar-like substance (as opposed to the crystals he was looking for)
He now understands that the reason he didnt get crystals is because he didnt defat enough!
evidently, one needs to defat until the np one is defatting with shows up clear when mixed with the (acidic) aqueous solution.
so GOD tries his hand again, round number two, this time GOD goes out of his way to defat the hell out of the acidic solution in hopes of obtaining a clean product. He starts off with aproximatly 800 grams of dried, ground peruvanis cactus. 3 X MeOH soak/reflux. Evap/recover meoh. Add near boiling acidic dh2o (pH ~2, maybee a little under). Filter several times to remove sediment/undissolved tar. DEFAT.
ok, here is where the new problem lies. working with about 2.5-3 liters of aqueous solution in a four liter separatory funnel, GOD goes through about 1/2 to 3/4 of a gallon of dcm. The non polar layer gets clearer and clearer with each new addition of dcm. Hardly any emulsions are (seemingly) formed because for the first few washes, GOD very carefully adds the non-polar and is also careful not to agitate, he just gently swirls. Once the washes appear to start getting lighter and lighter (indicating that the aqueous layer is not as saturated with dcm soluble fats, tannins and whatnot) GOD starts to agitate the mixture progressivly harder as he notices that the emulsions that do form are rather thin and whispy and settle out within 10-15 minutes if GOD buggers with the sep funnel (he likes to use an electric massager to vibrate the sep funnel which helps speed the breaking up of the emulsion layer). The last wash GOD did with dcm, he noticed that he was just about run out of dcm. So he decides to shake the living shit out of his funnel in hopes of getting one last really good, clean wash. He figures that his aq layer is almost all clean now, so no big emulsions should form. WRONG.
He is left with a huge, spongey emulsion and very little non polar settling out. shit, theres hardly any dcm left and GOD isnt going to the chem supply store again -no way, no sir, no how. He's gotta go find someone to do it for him, but until he does (or until he gets off his ass and distils some from some stripper) he's gonna do some 'speramentin', well its experimenting for him anyway. He realizes that although dcm is what he's going to end up using for his final extraction (of freebase mescaline) he can still use any other non polar solvent to continue pulling fat from his aqueous solution. Maybee he thinks to himself, that by adding more non-polar, hell help make the nonpolar more nonpolar (the same way brine or salt can bee added to emulsions to make the polar layer more polar- his chemistry knowledge isnt that technically sound, but he says fuck it and gives it a try anyways).
He adds some xylene (straight outta the can from his local hardware shop). Fuck! GOD forgot that some solvents will float, and some will sink. He knows that dcm sinks (thats what hes been using up to this point) but now hes looking at a clear puddle sitting on TOP of the aqueous layer and his emulsion is on the bottom. Anyways, with just a little movement of the funnel, GOD watches the xylene drop through and pulverise the emulsion on the bottom! It didnt completly destroy it, but he noticed that it made the once geletanous emulsion now become thinner, and lighter. So GOD shakes (swirls) the shit out of the funnel and notices the emulsion continues to break even more. A few more of these xylene washes, and the emulsions almost completly gone! But now theres another problem- after the xylene has been removed, so now just the aqueous layer remains, GOD notices that the aqueous solution has gained considerable volume! He hadnt noticed this before (while he was using dcm) but it possibly could have been a gradual buildup while he was uding the dcm (his guess) OR it could have gained volume when he used the xylene, he isnt sure when it happened.
what the fuck?
there is no visable emulsion layer...
GOD is confused.
a few other tid-bits-
When GOD looks into his aq. layer, he see's tiny little specs and tiny little flakes floating around. He assumes the flakes may be fats that have settled out of solution..? They are really "light" and never really seem to settle ( theyre real small and move around like snow does in those glass christmas thingys you shake to make it look like its snowing)
also, the aqueous layer smells strongly of dcm (or so he thinks, it could bee xylene smell, theyre kinda close, and GOD really hasnt taken the time to become a conniseur of carsinogenic solvent vapors so he has a hard time differentiating the two).
and when the aq. is left to sit for a long time, the thinnest layer of those little spec's will settle to the bottom and take on the appearance of a thin (aprox 1 millimeter) emulsion layer.
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not knowing what to do, GOD empties his separatory funnel and puts his aq. solution into a bunch of canning jars (he is considering gently heating some of his solution in a distillation setup to see if dcm comes over, he'll record temperatures as shit comes over) in this way, he hopes to determine if the added volume is just unseparated dcm (which he hopes, but doubts because there doesnt seem to bee ANY form of an emulsion left)
he doesnt really know what else the problem could bee.
He aquired the dcm from a friend, maybee his friend accidentally added some h2o to the dcm? dunno, GOD has to wait for his friend to come back from vacation.
Do any bees think any kind of azeotrope may have formed?
any thoughts or ideas for GOD?
GOD is also considering just saying fuck it and continuing on with a little more defatting when he gets more solvent and then basifying and going on with the extraction- but he knows that it'd probably bee wise to wait and get opinions.
any help is appreciated
BEND OVER AND PROSTRATE YOURSELVES BEFORE ME!