Help with Pseudo Extraction from Syrup

[kris_1108]

Hi
Recently Swik attempted an a/b extraction of pseudo from two bottles of decongestant syrup. Each bottle contained 100mLs of liquid, and 600mg of pseudo, max yield would be 1.2gms. However, he yielded only ~450mg   . Swik thought it would be intelligent to attempt two bottles to see if it were possible, before doing ten or fifteen bottles.

Heres how it happened -
*Added the 200mLs of syrup to a 600mL plastic coke bottle along with 100mLs of dh20 (to dilute the soln)
*Added 50mLs Xylene and proceeded basifying
*Added NaOH, and more, and more, and more. No white cloudiness could be seen in the solution. Added more NaOH, and the solution went a piss/orangey color. Check the pH, 'twas about 12.6. AFAIK it needs to be atleast 12.8 so Swik added more NaOH. The pH was now a tad over 12.8, so he added a splash more NaOH and left an hour or so for lunch. The whole time he had been swilring/inverting the bottle; the liquid also heated (from the NaOH.)
*Returned an hour later and the base solution was BLACK. The Xylene was cloudy. Anyway, Swik speperated the 50mL xylene into a 300mL coke bottle, ready for washing.
*Added ~60mLs dH2O and shook. The solution instantly went like a crazy bubble bath, foam everywhere. Half a teaspoon of rock salt was added which dissolved after a bit of shaking. The bubbles settled, layers seperated, and the wash water was removed. (pH was ~10..
*Added another 60mLs dH2O, shook, and removed most of it from the NP. The ghetto sep did not allow removal of all of it.
*Addded 15mLs dH2O in prep for titrating
*Started adding hcl by drop, and swirling, waiting for the water layer to take on a light yellow tinge. No yellow was seen, so Swik had added about FIFTEEN drops of hcl before he thought "aah I think that might be enough". Swirled around a bit etc, smoke was seen coming off of the solution (!). It still had no yellow tinge to it.
*Pulled out the bottom layer. The very last bit of the water could not be easily removed, so another 15mLs of water was added and most of that was removed too.
*Evaporated and flashed to yield ~450mg. Acetone was yellow (acid.) Waiting for the p-fed to dry out but there was a sticky residue on the dish that seemed to stay, and not evaporate. (Later learnt that meant salt contamination.) Swik does not enjoy eating up his p-fed but anyway it had a musty taste to it, unlike normal clean p-fed.


Observations:
+The dark red soln WONT go white and cloudy when basifying. Next time Swik will just add untill no color change is observed.
+The Xylene wont go cloudy (from NaOH) if it is quickly pulled off (15mins, not a few hrs)
+Two washes isnt enough to rid the NP of Na ions. 3 or four different washes would be better. However, next time, if the NP isnt left on the BS for ages, it WONT become so laden with NaOH.
+When titrating, the water layer may not go yellow. Use a weak water/acid solution and pull from the NP a few times (not just once.)

So next time, he will -
-Basify quickly and do TWO pulls over 30mins
-Wash the NP with salt/water, NaOH/water, warm water, then cool water
-Pull the p-fed A FEW TIMES from the NP with (say) 5drops of acid in 40mLs of water

And here are a few questions that some other bees may bee able to help me with

a) Dilute the syrup or leave it? Swik thinks that an undilute solution may be too viscous, and slow down the p-fed molecules that are moving into the NP layer. On the other hand, a too dilute solution may be too dilute to recover all the p-fed from it, is that possible?. (remember its only 600mg/100mL. 1.5:1 dilution would mean 600mg/150mL (or 6gms/1.5ltrs)).

b) Volumes - with 1ltr of syrup (6gms p-fed), what volumes to use? E.G Xylene (2x 75mL pulls?).. NP washes (wash with 1/4 volume of NP).. Titrating (several pulls of 5 drops of HCl in 40mLs water?). These are the volumes that Swik will use unless advised otherwise.

c) Washing, will a salt/water, NaOH/water, warm water, then cool water wash be fine? What are the differences/benefits between a salt wash and a NaOH wash?

d) Yellow tinge - why didn't my dh2o take on a yellow tinge? Is it because the layer was only 450mgs p-fed in 15mLs dh2o?

e) Smokin', whats that smoke coming from the NP/dh20/HCl mixture? It seems to stop and then start again after shaking/swirling?

f) Musty, why did the p-fed taste unusual? Is this from salt contamination?

Ok thats it! Swik is keen to do this again, but he wants to get advice from other bees first.
Any input would bee greatly appreciated!
Thanks
Kris

[livid]

swim would try waiting for everything to migrate from the base solution, to the non-polar,add a huge amount of salt to the base  solution, until it has to release the pseudo, in order to be able to  grab on to the salt. swim doesn't know if this would work or not, but that is what he would try if he were you. Also,do this on the second pull, instead of the first pull, so if any crap comes over with it, it won't contaminate your first pull.

[carrie]

[kris_1108]

>>"DO NOT DILUTE SYRUP WITH DH20 "

Why? Why not?

[CharlieBigpotato]

what were the inactives in your wrestling match?
the sticky residue you mentioned doesn't sound like salt contamination to me. sounds like polymer contamination.
a redissolve in dry alcohol will reveal the salt contamination.
though , you should have been able to taste it.

the smoke?
acid-base rxn?

one time swim beat an insidious emulsion by stretching it out in a very huge amount of water beefore forcing it into a normal amount of np. not sure if there's a down side to using craploads of fluid in an a/b.
base is cheap; water is cheap; it can bee poured into a flat pan with a thin cover of np and still bee coaxed into giving up the free base.

[geezmeister]

Dilute the syrup or leave it? Right now, its anybody's guess. I suggest you use a 25% NaOH solution and let it dilute the syrup. You can dilute too much, but you won't do it with what you have in mind.

Volumes With a thick fluid I would suggest using more solvent to aid in getting solvent in contact with all of the syrup. You could use twice as much as you are considering without any problem. You could benefit from stirring the lower layer. You do not need to whip it up, or blend it with the nonpolar solvent; just keep it moving enough that all of the syrup has a chance to contact the solvent at the interface between the two. Low heating will do the same thing by creating convection currents in the syrup, but be careful as I seem to recall the syrup scorches pretty easily. If you titrate, I suggest you use hot water, and use about 75 ml at a time. On the first pull add eight to ten drops of acid, on subsequent ones add about five drops. Do a fourth pull and evaporate it by itself to see whether you produce anything. If so, do another unless you have your expected yield at this point.
This is more acid than you will need (unless the syrup is gakked and the label doesn't say so) but without pH strips and without experience doing this, it is one way to get the pseudo to salt out. I really think you might do better if you would gas using VideoEditor's

Post 265010

(VideoEditor: "New Clean Gassing Method!", Newbee Forum) or Shorty's modifications:

Post 492242

(SHORTY: "My ghetto gassing apparatus.....", Stimulants)

Washing Do a brine OR NaOH solution wash. If you are going to add dry NaOH to the syrup, use a NaOH wash. Then hot water, the cool water. The NaOH was will clean sodium ions out of the solvent, and the brine wash will help dry the solvent. Using xylene, you won't have a lot of drying problems, but you should dry the xylene with baked epsom salts before you gas.

Yellow tinge why do you want it to look yellow? This only means you have too much acid already. Or you may have some old acid that had gone dark yellow. The yellow doesn't give you any information about your pseudo.

Smokin' is probably the same thing you see when you open a bottle of HCl. It is the acid fuming.

Musty The p-fed tasted "unusual" because of the acid in it or salt you also created. Rinse it with acetone and let it dry. This should take the acid out of it. To remove any salt, dissolve the pseudo in MeOH and filter, evaporate the MeOH for the pseudo.

Good luck on the syrup. I decided some time back the cost was not favorable and the extraction not that effective. I you do come up with an effective method of extracting from syrup, it would certainly be welcomed here.

[kris_1108]

Hi
Thanks guys and especially Geez for your input.
I just had a quick read of VE's gassing setup, it seems super simple. Just need too find some calcium chloride (hardware store???.)

SHORTY sais something here

Post 479278

(SHORTY: "OK, i figured it was obvious...", Stimulants) about the water layer taking on a yellow tinge when the pfed moves into it.

As for washing, I wont be adding the NaOH dry so a brine wash followed by hot then cool water wash should be ok.

ok thanks

[biotechdude]

Calcium Chloride is sold as 'Damp-Rid' in Oz.  U can get it in big milk cartons for about $10.  Hardware stores are the best bet for the big cartons.

Also works a charm for its legal domestic use

[foxy2]

Before you basify it, wash the syrup with Xylene(2x)

That will probably help alot.

[kris_1108]

Cool so swik can make a gassing setup easy as!
What does VE mean by covering 2/3rds of the CaCL2? Does that mean fill the bottle with hcl (after adding the CaCL2) untill the waterline is 2/3rds of the way up into the CaCL2?
I like the idea of the aquarium pump.
OK HERES A FEW QU's
1. Do y'all think gassing (for my first time) would produce better yields than titrating?
2. What do I do? Obviously just stick the tube in an move it around the NP while its bubbling. How do I know when its stopped precipitating pseudo?
3. What do I do after that? Just filter out the pseudo and wash it with dry acetone?
4. How does the pseudo form? clumps? fine sand? shards? floats? sinks? suspends? if it sinks, and it is very fine, it think the filtering process would bee super slow...

thanks guys

[mickyfinn]

What does VE mean by covering 2/3rds of the CaCL2? Does that mean fill the bottle with hcl (after adding the CaCL2) untill the waterline is 2/3rds of the way up into the CaCL2?

Yes, and remember it's better to undershoot the mark...the bottle can get pumping and so very hot...(oh Aztec!)

1. Do y'all think gassing (for my first time) would produce better yields than titrating?
2. What do I do? Obviously just stick the tube in an move it around the NP while its bubbling. How do I know when its stopped precipitating pseudo?
3. What do I do after that? Just filter out the pseudo and wash it with dry acetone?
4. How does the pseudo form? clumps? fine sand? shards? floats? sinks? suspends? if it sinks, and it is very fine, it think the filtering process would bee super slow...

Having gassed unto near toxicity SWIMFINN would recommend you keep all electronic matter as far away as possible and do not underestimate the presence of this gaeous foe.

SWIMFINN hasn't gassed pre RXN but this is his mandate for post RXN gassing:

Float the tube just over the surface of the DRY DRY DRY NP in order to convince fred to appear. If you bubble you most certainly run the risk of suckback (not good).

Filter and rinse with MEK if possible...

Post RXN fred will be a cloud, in suspension and you will know it immediately...(not sure what the freebase form looks like yet.)

[SHORTY]

Post 492242

(SHORTY: "My ghetto gassing apparatus.....", Stimulants)