Help with sulfate!

[Ondatom]

an A-B extraction was done on swim's Pseudo sulfate- used was Dh20 and xylene and the NaOH solution was also used and after repeated attempts shaking etc swim has been left with 3 layers.. 1st layer -fine white crystals... 2nd- H20 solution.... 3rd- Non polar layer. Why is swim's pseudo not being dissolved and scooped up in to my np ? Is more shaking needed to get it over into the np ? please any help greatly appreciated.

[unionpacific]

I'm sure it's in there, seperate the non polar layer ,Can you see any oil floating around in it? if you can wash it with dh20 a couple of times and take it out of NP with the proper dose of hcl

You should also check the pH of the solution before you do any of the above to make sure all the goods are in the NP.

[Ondatom]

the bottom layer of crystals that has not dissolved into the non-polar (which looks pretty much like what swim started with ) is not pseudo ?? and when extracting sulfate is it visibly seen left behind or does it just dissolve and get thrown out with the wash solution or something...i was thinking along the lines that swim should may be seperate the np layer and put it to the side and dilute the aqueous/crystal layers with a lot more DH2o , make sure it all disolves first then try with the xylene again . is that anywhere near right?? please any help would be greatly appreciated as swim hasnt done too many a/b extractions before and quite a large amount is being used now and its not working!!!

[unionpacific]

When you have pill mass and h20 with a NP layer on the top and add a base (naoh) the pseudoephedrine turns into freebase and gets dissolved in the NP, put this NP layer up to a light (preferably flouro) you should see a oil suspended in it, this oil has no sulfate attached to it. You then wash this layer with dh20 a couple of times, then add a layer of warm dh20 and extract with aqueous HCL, there is now pseudoephedrine hydrochloride in the dh20.

Keep in mind any gaaks that survive a a/b can be left in the aqueous layer to evaporate in the end.  Most people boil the pill mass in NP solvents a few times before they start anything to dissolve any gaaks soluble in NP, the goods won't go anywhere until a base is added.

[Ondatom]

swim is using already pure pseudo sulfate, and i do understand what your saying cause thats exactly what i thought would have happened usually, but for some reason its not completly dissolving. Can i take it that i should give it another go shaking the F@#kers out of itand anything that does not dissolve is definatley Pseudo of anykind..? is that a reasonable assumption?

[callen]

Yes ...most of us do some solvent boils of various kinds on the powdered pill mass before we ever add any basifying solution to it.The Hydrochloride salt is highly soluable in dH2O but soluble only a little or not at all in organic solvents...try dissolveing table salt in Toluol...don't work....There are a couple of possible reasons for the layer of xtals...I'll cover that shortly, but first...here is my universal panacea for removeing any organic solvent soluable additives(GAKK'S) from the pill mass....1)Boil the powdered pill mass in TURPENTINE for at least 15-minutes...this gets rid of the long chain polymers like Povidone,etc.evaporate off the TURPENTINE...then, filter off the contaminated liquid, keeping the powdered filter cake...let dry out... 2) boil the dry pill mass for at least 15-minutes in METHYLENE CHLORIDE, a.k.a. DI-CHLORO-METHANE...TRI-CHLOROMETHANE will work also...so will DI- and TRI-CHLOROETHANES...a.k.a. ex., di-chloro-methanol or di-chloro-ethanol, or di-chloro methylene or di-chloro-ethylene., etc.,...certain automobile brake cleaner solutions and certain electronic circuit board contact cleaners are sources, avoid the -FLORO-, or FLOURO- varieties...they are incompatible with strong alkalies and will liberate free flourine which will fuck you up badly...filter off the resulting contaminated solvent and dry out the resulting pill mass(filter cake)...now we change up... the HCL. salt is highly soluble in ALCOHOLS...but we put our alcohol in the freezer for 30-minutes to cool it down some... cold alcohol...either methyl or ethyl or dry isopropyl will dissolve a lot of the Hydrochloride salt that we are interested in...but not very much of the GAKK's that we don't want...so shake up the pill mass-alcohol mixture and filter out the insoluable GAKK'S...the SUDO is is in the alcohol filtrate...upon evaporation ( preferrably useing some sort of condensor arrangement to recover the solvents used in this entire procedure)...you will recover some very beautiful pinwheels.
   Most of the adulterants added to today's pills are poly-morpheus, not xtalline in nature...most likely you have a super-saturated solution involveing SODIUM HYDROXIDE,PSEUDO SULFATE,or SODIUM SULFATE...there is nothing else in the mix if you used clean sudo to start with...evaporate off the aqueous part and start again with clean precursor material...!    

[elfspice]

I thought they were crystals of pfed too, cos they appear after basification...

there's a number of other things in pills that do that, i think microcrystalline cellulose does that, it's not very soluble in water or nonpolars (especially when wet) it comes across with alcohol extraction. I'm not certain whether it's a wax or the cellulose or some polymer to be truthful.

I've seen the same thing in slow release pills before when extracting. the stuff is a bitch, some of it you can filter out, but a little dissolves in both phases via colloidal means and it's so fine you can't filter it really (osmosis might block it). It usually ends up contaminating the alkaloids, along with all the other shit like polymers etc.

[unionpacific]

I'm against shaking while basing or acidifying, I prefer to swirl it clockwise and/or counter-clockwise to make a whirl pool in the seperation apparatus, (I don't know if your decanting or using some type of seperation apparatus)

Heating the flask a few degrees while basing will make things easier to dissolve because hot solvents dissolve better than cold, but make sure your not super-saturating the NP with more freebase than it can hold. You should do around 3 pulls with the proper dose of NP then combine them together.

I also suggest buying a 500ml or larger seperatory funnel it makes seperation of layers clean, easy and fast and is well worth the cheap price

[Ondatom]

I am fairly confident that i am not dealing with any gaks of any sort but i supose you never know so ill give them ago, but also how will i now if my non-polar is super saturated? what are the correct ratio's when doing A/B extractions with sulfate, i usually wouldnt ask a question like that which would get a definate Rated as UTFSE.. but i have not been able to access TFSE recently. Is anyone else having this problem? thanks again for all your help O great Wisebee's ...

[unionpacific]

"how will i now if my non-polar is super saturated"
You should estimate, according with how much grams of pseudo your working with, it's fairly easy to estimate how much solvents you should use. (Make your aqueous base solution now)
1. If you have dry PM at 200ML make a aqueous layer of 350ML with no base,
2. heat it up a few degrees,swirl, it's a option to wash the polar layer with NP or not,
3. add enough NP to reach to 450ML,
4. add base, swirl around a minute or so (or longer)
5. seperate,and repeat #3, 2 or more times, then finish the rest of the procedure.

Most common solvents will hold a substantial bit of alkaloid at room temp (anybee feel free to post statistics) but you don't want to waste solvents while you can use them properly (and limit ammount of waste)and conserve, but you also don't want to use not enough so there is goods still in the polar layer before you throw it out (thats what happens when you try to conserve your solvents a little too much.)

If you really want to get the last of all the pseudo do more than 3 of the seperations menchined above. (solvent costs!)

also: pH measurents will not work with NP solvents only with polar.

[elfspice]

microcrystalline cellulose is just a tabletting aid i think.

[kris_1108]

See here for Microcrystalline Cellulose info

http://www.fao.org/docrep/W6355E/w6355e0l.htm

or

http://www.grokfood.com/jecfa/additive_0721.htm

[Ondatom]

what micro cellulose is . just say that it was present in swims sudo sulfate would re crystalizing prior to the A/B help ? if not what would happen ? cause i checked the sites above out and as im pretty sure it not what i have there are a lot of resemblences with the solubility's of both.

[Rhodium]

Insoluble in water, ethanol, ether and dilute mineral acids. Slightly soluble in sodium hydroxide solution with swelling. Upon shaking MCC with water, the result is a hydrogel, or a

colloidal suspension

(http://dictionary.reference.com/search?q=colloidal+suspension)

[elfspice]

Yeah, that's the crap that swells up and floats at the top of the base solution. At the time I saw it, i thought it was pfed crystals too, but I know better now.

You don't even see it if you extract in the first instance with alcohol, as you can see it's insoluble in it.