Gakinator?

[geezmeister]

Use less naptha, use it hot, and freeze it for a couple of hours. Titrate for what remains dissolved in the cold naptha. Some of your pseudo will remain dissolved.

[Prepuce]

SWIM kept thiniing about his earlier results in attempting to extract with naptha, and nothing made sense so he tried it again. The results were the same as the last, but this time he's a little closer to understanding why. Somehow the presence of ammonia in solution with naptha makes the freebase soluble in naptha! To be sure, SWIM dropped a few NaOH crystals into the solution, and almost immediately some of the freebase started to fall out of solution. (NaOH alwasy causes ammonia compounds to give up some or all of the ammonia.)

Another update: In case he didn't make the point clearly enough before, DON'T USE NaOH!!! Don't add even a drop of it because you aren't sure you've based the solution enough. Better to add more ammonia. If you add NaOH you'll be sorry!

And now,, one last thing SWIP has been wanting me to say. I told him everyone knows this already, but he's damned insistent so I figure it's best to just go along with him on this---->  Be very careful you don't accidently mix ammonia with I2 or KI. You might make nitrogen triiodide, possibly the most sensitive known explosive. It's supposedly less so when wet with it's own solution, but SWIP has seen that debated. Suffice to say, it's not something you want to make by accident.

PP

[Prepuce]

Kris,

That sounds like it would work fine if the hcl salt is what you want. Less handling = better yeilds. Interesting idea.

PP

"As for vaporizing the FB, if you forced air into the vaporizing flask, and had an outlet tube bubbling into an NP, could this be an alternate way? E.g have two flexible tubes connected to your vaporizing flask. One connected to an air pump and the other bubbling in a non-polar. The FB pseudo would be forced through the outlet, into the xylene, where it may be gassed?"

[12cheman12]

swim has read in this post the MP of pseudo FB is 118, but if swim left his FB at 118C will it vaporize and move over at this temp? if not what temp is needed?

Also, swim thinks that the whole ammonia think is a waste of time and that its just the short path distilling that does all the cleaning.
So wouldnt it be best if the pseudo could be taken from pills and turned into freebase in the easiest/shortest amounts of steps?

Why doesnt one just
- Pull pseudo with alky and evap
- Dissolve whats left in water
- Add a pre made basic water solution to this until FB appear
- Collect FB with Xylene and evap Xylene for FB
- Distill FB

Swim has been wanting to try this for about a week now, ive even got a thread showing swim distilling setup

Post 518820

(12cheman12: "Cleaning Freebase", Stimulants)

[geezmeister]

I have tried this three times now with two successes. My one failure was caused by overheating the pseudo. One distillation yielded yellowish, oily pseudo. I redistilled this pseudo, oil and all, at a slightly lower temperature, and obtained clean pseudo crystals without any trace of the oil. The other attempt was successful on the first attempt.

The next time I distill freebase pseudo I will heat it in an oil bath, vaporize the pseudo in a distillation flask, and pipe air into the flask to bubble the vapor through solvent. This should be one way to scale up the method for larger batches of pseudo. Another thought was to use a flourescent tube the way Shorty uses one when he sublimes iodine.

My impression so far is that distilling is more effective at cleaning freebase pseudo than expected. I think any freebase pseudo is a candidate for this method, irrespective of the use of household ammonia. I will learn by doing, no doubt. I just hope it isn't a learning by failing type of lesson...

[12cheman12]

Geez, what temps did you use and what steps did you take for obtaining the FB, thanks.

[geezmeister]

I used ammonium hydroxide and Na2CO3 to base and extracted into xylene, gassed, freebase with Naoh solution, diluted with cold water, and filtered out the freebase crystals. I want to try the method with some freebase crystals obtained by the Straight to Bee method, and some from a tetra trap.

I set up a beaker to do this in, and used a round bottom flask and a few wraps of teflon tape for a seal. I used a little black silicone gasket adhesive to seal the pour spout area. I did not measure the temp, just took the temperature up slowly until I observed the pseudo melting, then observed the pseudo vaporizing. I left the room during the process and the heat control did not work properly and the element stayed on, overheating and scorching the pseudo and making a mess of the polymers and the pseudo. The temp at which the pseudo scorched was much hotter than I needed to do the distillation. The range between distilling temps and scorching temps is wide enough that you shouldn't have problems--- I had been warned about the control once before, but had never seen it malfunction.

Another example of the universal and automatic application of Murphy's law to any conceivable situation.

[psilly1]

Has anyone thought of setting up a condensor to cool/collect the fb xtals?

[Prepuce]

SWIP really likes the idea of piping the vapor into solvent as it will make recovery easier. Have to agree that the ammonia isn't working reliably. It does seem to have a unique effect on polysorb, however, if someone could just get a handle on the mechanixm.

The biggest trouble--and it's a big problem--that SWIP has had is the fact that it works one time and not the next.

The SPD seems to work regardless, unless you can't get the FB to dry. That may be the reason that NaOH will foul the works so badly. The residue absorbs moisture and holds it, so when you try to vaporize the powder just melts into an oily mass that won't vaporize.

What's been happening to SWIP is that he'll have a few good pulls and a few bad. Most are fairly small, however, so he has been combining them until he has enough to base and SPD. But it only takes one pull to come through with just slightly wet yellow gak still in it. When combined with the rest guess what happens? That's right. One bad apple does spoil the whole bunch.

SWIP believes that SPD will work on anything out there if you can get dry, not necessarily clean, freebase to work with. If anyone has a surefire way to do that please post it!

PP

[Prepuce]

Don't forget, another reason to watch the temperature is that if you take it too high you're going to be vaporizing gak. Just atart out slow and conservative the fist time. SWIP never measured the temperature either, just take it up to where the FB begins to melt and leave it there. It might take a half hour to find just the right spot the fist time.

If you do go too hot and your crystals are off color, just dump them back into the flask and run it again a little cooler. This is a quick procedure overall, and you won't save time by trying to run a little hotter.

One other thing to watch is that you don't seal things up so tightly that excess pressure can't escape without blowing up your rig. The setup SWIP described will pop open just enough to vent a little pressure, then seal itself back with no detectable losses when that happens. It does happen, too. Almost every time, and that's where the ice helps keep things in line.

PP

[Shane_Warne]

PrePuce, what happens when you vaporize right off the bat, with no cleaning?

I assume that that's been tested, and that there were impurities obvious.

I just wonder if certain pre-washes would make this possible in high yields and high purity.

[Prepuce]

Results vary, depending on what you started with. You still have to do something to turn the pfed into freebase, though. Early on SWIP tried processing a couple of 120s in a test tube. He's not sure he remembers exactly how he went about it, but he thinks he just ground it up and added a little acetone and NaOH--no water. The result was a blob of bubble gum that actually did produce some yeild in the SPD, but not enough.

In SWIPs opinion this is worth following up. Finding a way to produce the freebase without adding a hydrophilic residue to the mix will bee the key.

PP

[Shane_Warne]

I totally forgot that pills weren't freebase, or that the salts weren't easy to sublime... one or the other.

I've found the best procedures to bee the simplest procedures, while accounting for todays special gaks.

Ill come back with two small test results comparing the yield and purity of the AmOH/Na2CO3 A/B, and the yield and purity of a modded TT A/B.
Both extracted with xylene.

They'll probably both bring up yellow, so it might just be a uestion of yield, but Ill see.

[evilscripter69]

swim used ammonium hydroxide/sodium carbonate to base,extracted into xylene, three water washes of xylene(hot water) titrated fot the HCL (was short of hand of materials)then dissolved into naptha/ISO alchohol(50/50)enough to get it fully dissolved. final step waz Geezmeistars microwave pseudo precipitation method.outcome was pristine crystals and a green colored xylene. burn test was very clean, in fact it even smoked in a glass pipe, RX test coming later.

[Shane_Warne]

My impression so far is that distilling is more effective at cleaning freebase pseudo than expected. I think any freebase pseudo is a candidate for this method, irrespective of the use of household ammonia. I will learn by doing, no doubt. I just hope it isn't a learning by failing type of lesson...

that's how I'm seeing it to.
It's the method that will yield the best yielding distillable amount of freebase. hah, well I hope your right too, but I'm pretty sure your on the money.

What does everyone else think, is the route to base the key to high yielding, pure end product in this write-up?

12cheman12:

Why doesnt one just
- Pull pseudo with alky and evap
- Dissolve whats left in water
- Add a pre made basic water solution to this until FB appear
- Collect FB with Xylene and evap Xylene for FB
- Distill FB


You can do that, that's a good proven method for freebase. But you've got to do it correctly and not get too picky with the OH extracts (no filtering), and do many of them.

Ill show ya--Make that three tests.

It'll bring up yellow, but the yields should bee high.

[Shane_Warne]

Amonia water/Na2CO3

1.fGUP were added to a small beaker along with AmOH. But no creamy consistency was ever attained, the ammonia water just sat on top of the GUP.
2.Soaked overnight with stirring every now and then. What looks like a film forms after a period of time on it's surface. The film was thought to be pfed.fb, but it was wishful thinking to assume it all was.
3.The NH3/pfed was extracted 3 times with lukewarm xylene. At this point it becomes apparent that the film was made up substantially of cellulose ethers/hydrogels or similar
4.The yield was low, at .3g, but the result was clean, with no visible signs of orange, yellow or PEG, although the fb crystals were slightly elongated, they had a definite opalescent glisten to them, which is a sign of purity.

Problems: cellulose binders made a good yield difficult. But that could have been because the “creamy” consistency wasn't attainable.

TT (modified)

1.fGUPs were shaken up in a shaker with 2 tblspns of Na2CO3, then added to a coffee jug.
2.Xylene was added to the GUP/Na2CO3. Stirring and spraying with H2O was constant, and was continued with careful observing of the GUP texture. This was continued for about 30mins.
3.Stirring continued long after the spraying was complete, maybe 2-3hrs, at which point the temperature was brought up to about 30-35C.
4.1st Pull
5.Xylene replaced, stirring continues for another 30min, temperature was brought up to 30-35C - 2nd pull.
6.Repeated step 5 - 3rd pull.
7.A few cups of h2O were added to bring about a regular A/B situation. This was left along for 6hrs following fresh xylene addition.
8.4th pull.
9.Combined pulls are poured through two(just in case one has a break) filter papers to remove any rogue cellulose fragments or other.
10.Upon evaporation, a yield of .7g of pretty clean pfed.fb is formed.

Problems: no defense against yellow. Becomes increasingly difficult with scaling up.


Rough OH extracts, waterbased A/B

IPA was prepared using 70% rubbing alcohol, salted out with NaCl, and dryed with CaO. (MgSO4 can't be used)


1.fGUPm was added along with 3 volumes of 95% IPA, with stirring. Plastic wrap and a rubber band was used to cover the stuff.
2.After about 1-2hrs the first OH extract was carefully made, it was clear to slightly cloudy.
3.Repeated step 2, 4 more times.
4.The beaker containing the GUPs which was being extracted from has Na2carbonate and water added. A lot of cellulose shows it's face with the water and the base present.
5.The OH pulls are evaporated in a very small dish at room temp. to reveal pfed.salt, and a small amount of PEG. Water is added to the dish, syringed up, and transferred back to a clean beaker.
6.The H2O/pfed.fb is based with solid Na2CO3, tiny amounts of cellulose appear.
7.3 pulls were done with lukewarm xylene and added to the pull done in step 4.
8.evaporation of the xylene arrives at a yield of .6g of clean pf.fb.


Problems: no defense against yellow. Time consuming and a bit fiddly. Partly susceptible to cellulose binders. Difficult maintaining anhydrous alcohol over the course of the procedure.


The pills most likely didn't contain yellow of course~!. They were a popular brand of 12hr 120s, 1 pack per experiment.


Prepuce! What do you think went wrong? Has swim had any cellulose problems in his experiments?

[dasedbee]

Honorable Geezmeister,
Since swim has been living under a rock, happily getting good yeilds from the local generic 120's (untill swims last 2 dreams)swim tried lots of things to get the damn thing to dry. Swim used VE's "Straight to E" to begin, then followed the normal RP/I (1E,0.5R,1.3I), LWR then Kerplunked, and A/B'd (final PH 6-7). After trying to Flash the yellow product dry with acetone, Swim resorted to Worlock's 2 solvent recrystalazation. While the yields were lower than usual, freezing the 2 solvent solution did crash out the high quality end product. Swim doesn't know if this info helps in your quest to solve the 120's problem, but hopes it may.