Author Topic: NP wash gone wrong  (Read 2499 times)

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12cheman12

  • Guest
NP wash gone wrong
« on: June 12, 2004, 02:11:00 AM »
swim was working up some pills.
60mg pseudo hcl and 2.5 trip.
Had his NP filled with pseudo FB in a jar, chucked in some water shook up nicely, let seperate, removed water.
Decided to do a second wash, put more water in, the second he shook it up everything turned milky white.
He thought who cares it will seperate into two layes, after about 30 mins he comes back and its all one glorous whole, NP and water looking like MILK. Swim is scared and does not know what to do.
Why did it happen on the second wash and not the first?
Swim thinks the water might of brought the PH down and fucked things up so maybe some NaoH might help.

Edit: Update:
Swim made a strong NaoH water mix and added that to the water washes. Behold... some fb crystals floated to the top.
Now he added some of this NaoH/Water to his NP/water Milky substance and it started to seperate. Bit more went in with some more NP and now theres a visible interface.
The NP has some cloudy looking substance in it, Swim is thinking he should Decant the NP, filter it to get the cloudy shit out then evap the NP. Orh is this couldy looking substance something he wants to keep?

kris_1108

  • Guest
Just water
« Reply #1 on: June 12, 2004, 06:05:00 AM »
Hi man hows it goin

Hey I think the 'cloudy' look of the NP is just that the NP has been 'wet' by the water washes. From shaking so hard, there is tiny water molecules suspended in the non polar, giving it a cloudy appearance. I think. And, I think by drying out the NP with dried epsoms, it will clear up alot more.

As for the antihistamine present in the GUPS, an acetone boil should remove it. The antihistamine may follow the pseudo through an a/b extraction. If you haven't allready done an acetone boil, you can wait untill the pseudo is extracted and then perform the acetone boil afterwards.

About the washes themselves, AFAIK, the standard procedure is to do a NaOH wash, followed by a warm dH2O wash and then a cool dH2O wash. The NaOH wash is to remove any excess Na ions that may have made their way into the non polar. (but you knew that allready, didn't ya  :)

Hope it all goes well,
Seeya

12cheman12

  • Guest
swim made a mistake when he said the NP was...
« Reply #2 on: June 12, 2004, 06:23:00 AM »
swim made a mistake when he said the NP was cloudy, what he meant to say was their was this gel like substance suspended in the NP.
Anyways he cleaned it up nicly (he hopes)
and he is evaping the NP, but there is gak coming through.
Swim wants to know of methods of cleaning the NP.
- Is water washing the only usefull thing for FB or can acetone be used to clean aswell?
- What other methods can be used or is swim best off gassing to get HCL?

barkingburro

  • Guest
no dont use acetone
« Reply #3 on: June 12, 2004, 08:39:00 AM »
try instead using one of the two following methods.

a> wash with very NaCl (use ground up rock salt marketed for use in making iCe cream) laden d/h2o. d/h2o will hold 36grams of NaCl per 100 ml as an fyi. don't saturate the shit, but get a pretty good amount in, say 50-75% saturated. 

b> if you have a sep (and if you don't, make one *hint* perrier or similarly shaped glass bottle with a dremeled hole on its bottom and a twist or pop sports top from a pint bottle of water works well), setup your seperatory funnel and pour in about 2-3 inches of unground rock salt. oh have the sep closed at this point. then pour in just enough d/h20 to where you can see about a cm or two of water above the top of the salt line. measure this water (obviously b4 hand and keep track of how much is poured in)now add your NP. once everything has settled open up your sports top and let the water start flowing, drain it off into a measured container and when it begins to reach the the amount you poured in, slow it to a very slow drizzle. keep an eye on it and when the npreaches the nozzle there will be a slight pause as the last residual water acts as a temporary barrier. at this point close the nozzle and replace your drain container. now reopen nozzle, to a slow to moderate flow rate and once drained you will prolly have a very small amount of water at the bottom of the NP, remove this with a pipette or eye dropper and then filter the NP to remove any chance solids that came along. swibb has used this filtering method on MANY occasions to remove all sorts of shit. this is usually how swibb filters his honey prior to the hcl step. hope this helps, cheers.

DrLucifer

  • Guest
Povidone
« Reply #4 on: June 12, 2004, 08:08:00 PM »
Which method did you use to extract the pseudoephedrine?
I hope you realise that those pills contain povidone, which definately needs to be attacked prior to kicking off!
If you didnt give the gups a long turps soak, then i suspect you will run into trouble very shortly!  :o
Before you finish evapping your solvent, i suggest you hit the search engine and find out if its possible to partially/completely remove the povidone present in your solution. I have no clues here, i used to remove it before i started, certainly is alot easier!
Just out of curiosity, how much water did you actually use to wash your NP? Another possibility is that you didnt add enough base to begin with...we will see anyway  :)


Shane_Warne

  • Guest
swim made a mistake when he said the NP was...
« Reply #5 on: June 12, 2004, 09:01:00 PM »
swim made a mistake when he said the NP was cloudy, what he meant to say was their was this gel like substance suspended in the NP.

If you see physical structures, then filter.

If a solution is thick, then dilute.


It's odd that water and the NP formed a single layer. If you use acetone or alcohol it will form one layer, if you use a small amount.

Boiling acetone will cost you yield.

12cheman12

  • Guest
yeah what happend was i used too much water on
« Reply #6 on: June 12, 2004, 09:12:00 PM »
yeah what happend was i used too much water on both water washes, i used about equal amounts of water :S
The extra base fixed up the problem, i think the excess water used in the washes brought the PH too low.
I did give it a turps soak to start off with so that shouldnt be a problem.
But why is a turps needed to remove Povidone, xylene does not dissolve pov right? so that means it wont come over in the a/b and if pov does dissolve in xylene then all you have to do is boil the PM in xylene before the a/b, isnt this correct?
So if you are doing an A/B all you would have to do is boil the PM in your NP your using in the A/B and all pre soaks and boils are pointless. All they cause is extra loss right guys?

Shane_Warne

  • Guest
But why is a turps needed to remove Povidone,...
« Reply #7 on: June 12, 2004, 10:45:00 PM »
But why is a turps needed to remove Povidone, xylene does not dissolve pov right? so that means it wont come over in the a/b and if pov does dissolve in xylene then all you have to do is boil the PM in xylene before the a/b, isnt this correct?
So if you are doing an A/B all you would have to do is boil the PM in your NP your using in the A/B and all pre soaks and boils are pointless. All they cause is extra loss right guys?


It's insoluble in xylene.

DCM and tetra are good pre-cleaners, they'll remove povidone. Other polymers aswell even at room temp. PEG, swims never had a PEG problem when using either of those, but pills with certain types of dyes seem to take up a lot of tetra or DCM.
I don't know if the dyes or the polymers, and which polymers get preference to dissolve first.

The only time he'd ever use anything else as a pre-clean to an A/B would be like Gee's mentioned several days ago, when he said he'd soak in xylene, before extracting with xylene further on in the A/B process.

Leave tone strictly to crystal rinses, where you can keep tabs on how much it's dissolving.

That's SWIM's opinion anyway, and he can bee dumb.

12cheman12

  • Guest
so are you saying you pre clean with tetra and
« Reply #8 on: June 12, 2004, 10:52:00 PM »
so are you saying you pre clean with tetra and dcm before the a/b and sometimes you let it soak in the np your using for the a/b correct?
But why would ANY clean be needed before an a/b apart from just a clean with the NP that is going to be used to pull the pseudo?
Because if you clean once in say Xylene and then A/B with xylene the ONLY thing in the xylene will be pseudo FB right? so why would one waste time pre cleaning with tetra, dcm and turps?

Shane_Warne

  • Guest
so are you saying you pre clean with tetra and
« Reply #9 on: June 13, 2004, 12:09:00 AM »
so are you saying you pre clean with tetra and dcm before the a/b and sometimes you let it soak in the np your using for the a/b correct?

It depends.

Since Geez told me the other day that boiling naptha pulled PEG nicely, along with pfed. Something which was blaring swim in the face, but he was letting tone rinses and recrystallizations deal with it.

The right thing to do (if boiling naptha was the extraction solvent) would have been to rinse in rt DCM or tetra beforehand. To both remove PEG, and to avoid a boiling solvent. Although as you said a few days back, orange will only be activated with heat AND a base.


The reason for pre-rinsing, if you decide to do them, before an A/B on pills, even though the actual A/B itself will remove them in THEORY, is to hopefully weaken the particular pills defenses.

See, an A/B should be near quantitative (100%), a pure aqueous solution of pfed.salt, should give a near quantitative migration up to the NP of pfed.fb.

But it doesn't happen that way, because of gaks, mechanical losses, human error. But mainly gaks.

So you either try to remove them, or work around them, so that they can't do what they want to do.


So then you might think, 'oh! Ill just hit it with every solvent I've got before I do the A/B', but if you do that, then you could well have lost as much, or more yield in mech. loss and human error than you would have lost if you left the gaks in.

So you need a balance. DCM or tetra are worth it.
Acetone boils remove a lot of gak, but they'll also cost you yield because it DOES dissolve pfed fb or hcl and sulfate a bit when boiling.

Best chance of a first crystallization that needs no more cleaning:

DCM or tetra rinses at rt
soak in NP you intend to extract with

A/B

Then again, there's that eudragit shit, so just play computer games for a while.  ;D
I know it's a lazy thing to say, but nevermind.

12cheman12

  • Guest
if PEG is that gooey substance that comes when
« Reply #10 on: June 13, 2004, 01:10:00 AM »
if PEG is that gooey substance that comes when the NP holding the freebase is evaped and scraped up and when the pseudo HCL is scraped up its gooey and has a yellowish tint to it, then swim hates PEG as it wats gaked him... but he did do a mineral turps soak before anything... so whats up?

Shane_Warne

  • Guest
It was probably PEG. Boiling xylene, boiling...
« Reply #11 on: June 13, 2004, 10:27:00 AM »
It was probably PEG.

Boiling xylene, boiling naptha, DCM and tetra remove it.

acetone does too, when you've got just PEG, pfed, and other small amounts of gak on an evap dish. :)

what kind of pills were they?

geezmeister

  • Guest
aromatic solvent soaks
« Reply #12 on: June 13, 2004, 10:52:00 AM »
Povidone can be removed by a long soak in an aromatic solvent such as xylene or tolulene. I know what the Merck says. I also know from experience that a xylene soak will do it. The mineral turps products in the US have a xylene base in common. We know its not the turpenes that get the povidone out, so what is it? Give the pills an overnight soak in xylene and you've accomplished the same thing as you would with an overnight soak in mineral spirits of turpentine.

You will also find that hot naptha is a far better solvent of PEG 400 than xylene or tolulene.


12cheman12

  • Guest
they were the oz white 60s with 2.5 trip...
« Reply #13 on: June 13, 2004, 08:24:00 PM »
they were the oz white 60s with 2.5 trip... 30 to a pack, youse all know what they are ;) lol
anyways ive got my pseudo HCL and its no longer gooey its just a bit yellow and its very acidic, but it scraped up into a powder easily. Too much HCL on the titrate.
So would just an acetone clean up the yellow and extra hcl?

Shane_Warne

  • Guest
they were the oz white 60s with 2.5 trip...
« Reply #14 on: June 13, 2004, 10:45:00 PM »
they were the oz white 60s with 2.5 trip... 30 to a pack, youse all know what they are ;) lol

haha keman, your such a dag.

So would just an acetone clean up the yellow and extra hcl?

Yes mate. glad swim got something, myself.

12cheman12

  • Guest
haha :p yeah shane, swim is so happy to ...
« Reply #15 on: June 13, 2004, 11:36:00 PM »
haha :p
yeah swim seemed pretty happy bout it too.