12cheman12 (Stranger)
05-05-04 15:24
No 505023
      xylene pulls     

swim boiled his pill mass in acetone and xylene 3 times each, one the 3rd pull his NP was coming off clean. When he dry based and added xylene to pull the first pull came out pretty clean and is in one jar the 2nd and 3rd pull come out a bit foggy and are mixed in a second jar, swim wants to gas these pulls so should he filter them to there clean or just go ahead and gas?
 
 
 
 
    morpheus
(Hive Addict)
05-05-04 16:02
No 505030
      clean pseudo     

Swim does not want to have a failure after so much work.
He always recrystalizes pm twice.
So swim would combine,filter and do a two solvent recrystalization at least once,which includes filtering again if alky is foggy when hot.
 
 
 
 
    geezmeister
(Of Counsel)
05-05-04 21:16
No 505092
      wash them and dry them     

Wash the nonpolar before gassing. I suggest doing a wash with NaOH solution, particularly if you based the pill mass with it. Follow the NaOH wash with a water wash or two. The freebase pseudo should not precipitate out of the xylene as it does with naptha. (All the same, hang onto the wash water until you finsih the pseudo extraction.)

After washing, dry the xylene over baked epsom salt before gassing. Your cloudiness may be trash floating the xylene, and if so, the washes should get it out. It may be moisture. Xylene will not absorb water, and if some is in the xylene in the form of fine droplets that have not settled out, the xylene will appear cloudy. Drying should clear it if moisture is the problem.

mostly harmless
 
 
 
 
    12cheman12
(Stranger)
05-06-04 14:42
No 505287
      when swim gassed his xylene, it went from...     

when swim gassed his xylene, it went from clear to cloudy and then there was some kind of substance forming on the bottom, didnt look like crystals looked like some kind of gak. Anyone know what this might of been? Swims gassing setup was pretty dodgy so he forget about gassing for now and is just going to evap the whole NP and see what he gets then go from there.
 
 
 
 
    geezmeister
(Of Counsel)
05-06-04 15:51
No 505299
      gakked pill source     

It would be nice if pill extraction was so easy that a few solvent boils would take out enough of the foilants and extraction inhibitors to allow a simple a/b to give clean pseudo. There are some pills left in the US OTC market that allow this, but I suspect these will be things of the past before you know it.  You do not identify your pill source. Chances are you have extracted polymers designed to foil an a/b extraction along with the pseudo, or the extraction inhibitors in the pills foiled the extraction attempt. The former is the more likely. Flaws in your gassing technique also can cause the type of problems you describe.

You may want to titrate to salvage what you can from this effort. I suggest you recrystallize any pseudo you get from the solvent multiple times. After a second or third crystallization the polymers will begin to break down and you will be able to separate the pseudo from most of the debris. This is a tedious way to salvage your pseudo, but it carries no risk of damaging what you have left.

mostly harmless
 
 
 
 
    12cheman12
(Newbee)
05-06-04 16:00
No 505300
      if yield is none, swim wont be disapointed, he     

if yield is none, swim wont be disapointed, he is still in experimenting phase. Down here in Oz where JD is non existent its F&#^$N hard to extract pills, and water can't be used in the slighest or will activate swelling gaks but swim says his still working on it. The hardest part is gettin the dry a/b to reach the right PH level to let the pseudo move over but keeping the PH low enough to not activate the orange GAK, i guess only experimenting can work this one out.
 
 
 
 
    deadman
(Stranger)
05-06-04 18:40
No 505329
      japan drier in oz     

this is by "Bees knees":

      

Hello childeren,
                  If you are an oz bee, and are having difficulty locating japan drier, it is probably because it dosen't exist here in our neck of the woods. Well actually it does, it's just called something different!
We here, down under, like to call it 'terebine'. Available from all leading paint stores as a drying accelerant for oil based paints.
A little research has turned up the following:
Terebine:
72% liquid hydrocarbons(mineral tupentine)
14% cobalt octoate
14% manganese octoate
From what Swibn can gather, this has very similar properties to the jap stuff.
Swibn is about to run out and grab some as well as some MEK and give it a go on some der...der....you know what-azin.
Shall post results soon.

birth is the real killer
 
 
 
 
    wareami
(Hive Addict)
05-07-04 01:17
No 505424
      Swelling agents=exotic beauty :     

Treatment of the pillmass(PM) with tetra prior to moving onto the next steps should ease the situation to ware adding h2o in small amounts to the waterless a/b should assist in raising pH allowing pfed migration

a little less conversation, a little more reaction
 
 
 
 
    geezmeister
(Of Counsel)
05-07-04 03:22
No 505479
      using sodium carbonate     

Ware's comments are demonstrated by a tetra trap very clearly. If you employ the method be sure to saturate the pill mass with the solvent before adding water.

You can use NaOH in a waterless a/b if you avoid the use of water. A little too much water here will make things too hot too quickly.

If you use sodium carbonate to base and mobilize the base with a mix of alcohol and acetone you will not need to worry about pH harming the pseudo.

mostly harmless
 
 
 
 
    auntyjack
(Hive Bee)
05-07-04 22:57
No 505650
      naoh/h2o     

Geez, does pseudo only get burnt in the exothermic stage, after having added the base to water or is the burning inherent in naoh/h2o solution in general?....in other words, could one use water/naoh if the solution is allowed to complete its reaction and cool down?

the horror
 
 
 
 
    DrLucifer
(Hive Bee)
05-08-04 08:03
No 505739
      Dry Basing with NaOH     

Swim has never once had a problem with runaway exothermic reactions whilst dry basing pill mass with NaOH & NaCl.
Swim uses MeOH to mobilize the base when working with HCl salt, and dry acetone when working with sulfate.
Swim usually achieves good yields, 60-80%, however could this lack of exothermic heating be a result of the base not being fully activated?
Swim adds 1g of NaOH/NaCl for every available gram of pseudoephedrine, as stated in the waterless a/b procedure.
Seeing as you are the author of this process geez, i assume you can shed some light on this. Thanks in advance!

I'm a diamond that is tired, of all the faces i've aquired.
 
 
 
 
    geezmeister
(Of Counsel)
05-10-04 18:42
No 506245
      burning pseudo with NaOH     

I noticed with waterless a/b extractions that if the basing reaction proceeded too fast, or started getting out of hand, yield in pseudo went down. I learned by experience that it was far better to do a slow basing with dry alcohol than it was to use a little water, since water seemed to make the process heat too much and yields were always off when this happened. Even with no water or very little water being used, heat is generated; holding the beaker in your hand as you stir the pill mass in a waterless a/b will show that the freebasing reaction itself is exothermic, although not so exothermic as the disassociation of NaOH in water.

I do not think the "burning" of pseudo is the result of the freebasing of the pseudo itself, divorced from the disassociation of NaOH in water. I don't even know that what happens can be called "burning." Pseudo is pretty tough molecule. In dry environment the rapid heating of NaOH caused by a little moisture may be too much. I doubt this is due to the freebasing of the pseudo molecule itself. I was seeking in the waterless a/b method to avoid releasing water activated foilants in the pill mass which made using a NaOH solution impractical.

The use of a cooled aqueous solution of NaOH should not harm the pseudo. It may activate any water-activated foilants present, however, and make a mess of the pill mass.

mostly harmless