Gakinator?

[Scottydog]

Okay Swim got to the 2nd pull of the GUPS/ammonia/carbonate.

After gassing the Xylene and filtering out the pseudo HCL, he dumped the Xylene back into the GUPS mix to proceed with the 2nd pull and a plume of white gas began billowing from the jar.

Would this bee Ammonium chloride?  

Positive side is that the yield appears to bee good and clean just from this 1st step alone. He dreamed of an extraction using generic 120's. 5 boxes of 120's, 9 tablespoons of ammonia, and 50 gs sodium carbonate per 1 qt jar.

Appears to bee as clean as the tetra trap used to bee, without the tetra and heating of solvents.

After basing and decanting all of the liquid through a cotton ball. The liquid formed 2 layers.

He isolated the top xylene layer from the bottom ammonia water layer prior to gassing. The ammonia layer appeared to bee very small.

Maybee too much ammonia was used? Like the with the tetra trap, should all of the ammonia/water bee absorbed by the GUPS?

[geezmeister]

can't resist mentioning that he was astounded! by the yeild.

The most likely explanation for the improved yield is that the pseudo you reacted was much cleaner than you have been reacting before. Yield improves with the cleanliness of the feedstock under virtually any set of PIE reaction conditions.

[Shane_Warne]

Positive side is that the yield appears to bee good and clean just from this 1st step alone.

Scottydog, nice investigative work! That's exactly what I wanted to hear, myself.

This clean you've got here, has plenty of potential for customization Prepuce.
It has two novel purification techniques for the price of one.

swim will give it a shot next time he has pills, and tell you how it goes (yields and quality) and how he carries it out.

[Prepuce]

Scotty: Sounds like your gas generator is pleny powerful. SWIP thinks the vapor is from residual HCl in the xylene neutralizing some of the ammonia.

SWIP has not worked out the ratios yet because he has not yet determined what is optimum. If you get two layers, though, you are either using too much ammonia or not enough washing soda. It's a fine touch to get the balance just right, but use just enough ammonia to be sure everything gets moistened with it.

Geez: Yes, your explanation is what SWIP believes to be the case. He didn't want to crow too loudly, however, because he wasn't sure the increased yeilds weren't due somehow to residual gak. All indications are that it is not.

SW: Yeilds from two A/Bs are still better than SWIP was getting from any other procedure--by far! And clean, too.

Directly vaporizing after the ammonia/washing soda/GUPs dry out won't work because you will cook out the water absorbed by the soda.

SWIP agrees the product from just the first step is quite clean, but if you skip vaporization you still end up with yellow gak in the mix, and at the very least it will hurt your yeild. SWIP's not sure what it is, but the vaporization is so easy why not do it?

PP

[Prepuce]

BB, please let SWIP know what SWIBB discovers about the descaler. The bottle that SWIP procured lists H3PO3 but that's all, and it's obvious that it contains something else. Got to get past depending on RP, though, that's for sure!

SWIP thinks the ammonia works by breaking down the detergent. If he had to guess he would say it was being hydrolyzed, but that would be mostly speculation. He doubts if anything like that goes on in the body with regard to pfed in the pills. Then again, if it passes through the stomach unchanged, possibly bile in the intestine has a similar effect? Beats SWIP.

PP

[Prepuce]

First the good news:
Other bees contrinbuting to this thread have inspired SWIP, who went scurrying back to his lab to try an idea spawned by one of the suggestions. He took just a little of the GUPS from the 120s-maybe 3 pills worth--and added a bit of ammonia, mixed it into the usualy creamy paste, took a quantity of washing soda roughly equal in quantity to the GUPS and mashed it well into the mixture. Then he dtirred in some acetone, let it settle for just a moment, filtered through a peice of cotton and evapped. It was dry in a very few minutes, and SWIP was amazed to see a small pile of beautiful crystals glimmering on the plate. Very, very clean looking. Surely clean enough to vaporize immediately.

Now the bad news:
That was yesterday. SWIP has tried a dozen times to repeat this feat without success! Mostly he has been getting an oily residue that won't dry. He has tried adding more ammonia at the outset, less ammonia, more and less soda, acetone, etc. Changed everything he can think of.

The only hope? SWIMs has notoriously sloppy lab skills. Maybe someone with a bit more control can do better.

Sheesh! SWIP was imagining announcing the quickest and easiest universal cure since they started using povidone--five minutes work, minimal consumable materials, no boiling, high yeild. . .

It can be done, and SWIP thinks the trick is in getting the amount of ammonia and soda just right. It's also important to filter the acetone through a loose cotton ball. If it's compacted you will squeeze water out of the soda when you use a vacuum or pressure from the other side.

Come on, Scotty! Swip knows you can do it. You're the bee!

And you too, Geez. And Wareami, where has he been lately? Shane, Ning, BB? And, and, . . .

PP

[wareami]

PP: I've been following this with extreme interest and just been waiting for the right moment to jump in.
Testing has focused solely around this latest monstrosity to hit pills that will cripple any extraction technique short of applying real brassballz chemistry.
This yellow oil threatens to shut down shop if it's not dealt with and that is the focus of Ibee's attention at the moment.
Much is being gleened from the patent and still more from the manufacturers specs.
This is the largest amount of time Ibee ever spent on decyphering the literature, prior to experimentation and that extra time is being invested to eliminate the guesswork this time.
Realizing there will be know universal cure, this requires approaching from different angles.
With this yellow oil, You can buy a box at one store and the method will work great, go to another store a week later and you'll bee scratching yer head in disbelief at the results.
The one common denominator is this yellow oil and it's amphibious behavior....like a snakechameleon!
This happened with a method designed to rid the yellow oil and was working well until it forced Ibee back to the drawing board.
If them fuks started sticking one Blammo Pill in each blisterpack of a different formulation or a combo of each, bees might be hanging up their labcoats for a while

[Shane_Warne]

Prepuce!

So how fresh in your mind is what happened on the golden hour?

Ill assume that all these tests were done on pills from the same pack.

Do you suppose, that when you did the first test using acetone, that you used such a small amount of tone, relative to the water and NH4OH, that the acetone had no effect. i.e the pills might have came out pristine had no acetone been used at all.

Then, the following tests turned out worse, because you added enough acetone to actually have an effect?

Or definetly not?

[Prepuce]

Ware: SWIP has been keeping pretty busy with this thread, so he definitely could have missed something. However, thus far there has never been an instance when the techniques being discussed here were not effective against the yellow oil, as long as xylene was used to do the pulls, ammonium hydroxide used exclusively for basing, and vaporization was included as a final step.

PP

[Prepuce]

SW: You are correct in assuming that all of the work was done on the same batch--which was actually an indiscriminant mixture of generic and brand name 120s. Because you need something to pull the freebase out of the mass after basing it, and because nobody liked the double A/B, SWIP tried removing it directly with acetone. All that can be said about the quantity is that it was more or less "typical" for the amount of substance SWIP was working with, which must have been about a rounded teaspoon full of GUPS.

Acetone was chosen because it evaporates so quickly. The effect on the pillmass this first time was as intended. To relieve it of the pfed freebase.

Because the GUPS were a mixture it's possible, although not likely, that the powder was not homogeneous. It could be that the first attempt was on only the least gakked of the assortment which had gone into the mix.

One thing for sure, and that's that SWIP is going to be pulling with xylene, doing the double a/b, and vaporizing from now on. Even if the technique could be worked out for pulling with acetone it would still be necessary to vaporize or SWIM thinks you'd still have substantial yellow gak to deal with.

Someone asked earlier what the yeild had been the one time SWIM was trying to watch it. Before the vaporization it was 60%, and there was another small pull underway. That was fairly early on, and SWIP thinks he's doing better now.

PP

[thunderfvck]

I have nothing to say in terms of the extraction of the FB, but I thank you for opening my eyes to the sublimation deal.

A 500 ml flask is good for about 3 grams of FB, but one would do best to drop off the crystals that form every now and then (especially on the test tube). And BE CAREFUL when bring the test tube to the dropping zone, the slightest breeze will knock those bastards down.

I have the most perfect tool for placing the test tube in, but I suppose I just got lucky...Sometimes people use a rubber thing to ensure a better seal between a filtering flask and the buchner funnel. THis rubber bastard is ideal, but only if you have the perfect sized test tube which I did   . Just gotta tape it down.

Man, what beautiful crystals. So powdery and sexcellent. I thought the crystals after the tetra were nice, boy was I wrong!

It's amazing how much gak is left over. Really nasty orangey shit.

Edit:

Just wanted to mention that it takes a bit of heat to actually bring the crystals to melting. Once they've begun to melt you can turn down the heat a bit for that perfect temperature.

[Prepuce]

They do look nice, eh TF? SWIP uses a 500ml erlenmeyer, but he hasn't paid much attention to how much he dumps in at a time. SWIP generally comes back to find the entire inside of the beaker spiderwebbed with delicate, shimmering crystals. A bee does have to be careful in removing the test tube, but as long as everything is well cooled it won't hurt if they drop back into the beaker. (You just don't want them to fly away.) The bulk of SWIPs harvest comes from there, not the tube. It's mainly there to hold some ice to make sure there are nice places to start condensing.

SWIM was also quite surprised when he fist started using vaporization after doing what he thought was a very succesful tetra trap procedure. Lots of nasty gak left in the beaker.

What cleaning process do you use prior to vaporization?

PP

[thunderfvck]

Oh, for that particular batch I had used my orange tinted uglies. These resulted from the second pull of the tetra trap. The yield was horrible though. From about 3 grams of FB, I got back about [edit]2.6 g (had to keep emptying it/heating it again)[/edit]...It's pretty hard to scrape off ALL the crystals as some of it becomes a powder and just sitcks to the sides. There must be a better way of doing this.

But the crystals are breath taking.

I did get a few crystals that were rather flexible though...Hmm, how can I say this. Instead of nice shards, it looks as though I got little squares that were rather difficult to break up and powderize. They were kind of flexible! I was able to break them down into little shards though once I started stabbing them...Anyways, didn't see too many of those. Perhaps some gak got through? Or maybe just one shard formed on to another shard, etc...But I recall geez saying that real nice FB should powderize rather easily. Hmmm.

Oh, and one more thing! The smell of vaporized FB is really starting to make me feel sick!  

Edit:

Just wanted to mention that it's imperative to redo the whole heating thing after collecting a batch! I have about 3 g in there and I'm still collecting crystals after taking it off of the heat three times!

Edit 2:

Ice isn't really necessary I find. I get just as many crystals forming on the test tube without ice. I still keep water in there though because we all know that water can absorb a great deal of heat, condensing the FB..

[Scottydog]

"If you have freebase after gassing, you are carrying the Eudragit polymers with you and they are preventing the conversion to the salt form. Scottydog noted this in an earlier thread about 120's."

Have yet to try this out but maybee a shortcut to all of this is possible?

Swim is used to using only Na carbonate, water and heat. The ammonia has plenty of water.

From all of Swim's theoretical dreams, he has noticed that when it comes to evaporation, the yellow oil doesn't evaporate, it just becomes concentrated and absorbs the pseudo like a sponge.

I wonder, after the first gassing step, if the crude pseudo could bee filtered from the xylene and then scraped from the coffee filters and then sent straight through the short path distillation step?

Swim has yet to do a ph test of this crude pseudo after the first gassing. Has anyone using 120's, checked the ph of the filtered pseudo after this first gassing?

If the ammonia doesnt kill the eudragit on the first basing, the crude pseudo will probably give a basic reading. Therefore a majority of it is still in the freebase form, ready for the distillation/sublimation step?

What would bee wrong with mixing the GUPS 50/50 with the carbonate and then adding the ammonia? Swim's problems have been with the adding of too much ammonia...

*The main question is, does the ammonia deal with the eudragit or is it the actual, short path distillation step?  So in theory, what does the 2nd A/B do that the end step won't already handle?*

Swim may revisit the tetra trap and take the crude pseudo after gassing, knowing that it is predominantly freebase anyway and use the test tube distillation/sublimation as a finishing step. I feel that this method could benefit from some pre-cleaning of the GUPS because after the ammonia is introduced, the pills turn to a marshmellow polymer blob.

Is some of the pseudo now trapped in this blob or is it squeezed out of the matrix. I'm willing to bet that ALOT of it becomes encapsulated. I feel getting most of the polymers out first, so that all there is left to deal with is the yellow oil may result in better yields?

[ballzofsteel]

Prepuce,

Just curious to know if you have tried "dry basing" your pills
(like Ive heard of in other methods,e.g grind with some salt,base,acetone,minimal h2o,evap to dryness)and then distilling your freebase?
This may leave all the inactives inactive?
Sorry for my ignorance on gakk`s,but how many adulterants will distill/sublime at the low temp fb does?

On the other hand,if ammonia plays a major part,hows about basing/de-gakkifying using an ammonia saturated alcohol,
or even liquid Nh3  as apposed to ammonium hydroxide  to base/freeze your feedstock,evaporate either(not to serious about the liquid Nh3)then distill away.
Just a thought...For the lazy....

Nice work btw.

[Prepuce]

TV: SWIP began looking for another alternative to the tetra trap after he worked up a batch that potentially could have yeilded over 20g, and ended up with less than 2. And that after all the choking solvent boils, messing with nasty stuff like japan dryer, etc. It was then that he fist began with vaporization.

SWIP is convinced that it's worthwhile to add the ice. For one thing it will usually keep the test tube from popping out under pressure. It also helps cool the interior of the beaker. Maybe not a lot, but some.

SWIP thinks you probably are getting the beaker too hot if you're pulling contaminants. It's very important to find that sweet spot in the temprerature and always use it.

As for residuals, leave them there for now. Don't try to scrape out every particle. Get the sides, especially near the bottom where the crystals are heaviest, but be careful you don't scrape into the gak. Then the next time you use it, just scrape the same areas and you'll have full yeild.

When it gets to the point that the beaker needs a good cleaning, SWIP first rinses the interior with acetone, which is then filtered, evapped for the pfed and vaporized in the clean beaker.

PP

[Prepuce]

Scotty, for some experimental results that suggest something about the activity of the yellow gak, see SWIP's post

Post 515408

(Prepuce: "Another data point", Stimulants). It appears that ammonia causes the yellow oil to sink to the bottom when mixed with xylene, releasing the pfed which was completely converted to freebase by the ammonia with maybe a little help from the NaCO3. Better to get the job done, he now believes, with ammonia only, but he's the NaCO3 will still be needed to absorb H2O and the gak. He agrees that there is no need to add additional water.

In his experience the creamy mix isn't a problem, and you can really see this with the white 60s. You can see the mass decrease when the xylene is added, as the pfed freebase goes into solution.

SWIP would dearly love to find a convenient way to pull the pfed from the xylene directly, but remember, it's freebase and soluable at that point. He's not interested in evaporating xylene and isn't aware of any other options at the moment. The only purpose served by the second A/B is to get freebase, since vaporization doesn't work well with the hcl salt.

He believes that it's possible, and of course highly UN-desirable, to squeeze water/gak/yellow oil from the pill mass if it's squeezed or subjected to other forces that could suck it loose. But as long as only ammonia is used for the basing and in sufficient quantity--NO NaOH!!!--that the yellow gak completely releases the pfed. SWIP wouldn't be getting 60% plus yeilds if that weren't the case.

SWIP tried what you are suggesting with the tetra trap a long time ago, and it failed because the pfed just wasn't coming out. Your method may be slightly different, though, so by all means give it a try.

SWIP also tried just grinding pills, basing and evapping the whole mess. You actually get some yeild, but it doesn't work well because of the H2O, which comes out when you start heating it. It also stands to reason that the procedure is going to work better on reletively clean pfed than it will for a sample that still contains all the gak.

PP

[geezmeister]

Have you considered extracting with preheated naptha and chilling the naptha for freebase crystals? Use warm naptha, stir well, and pour off, repeat. Freeze.

[kris_1108]

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? Or is that just a tweakers idea   . It was just something that went through my mind, though I would share it.

[Prepuce]

Geez: As a matter of fact, that was the first method SWIP attempted, and he should probably try again. Oddly, on the first try the FB crystals would not precipitate, even after an hour of refrigeration. Only when the naptha was gassed would the crystals come out of solution. Makes no sense but that's what happened.

PP