Gakinator?

[Prepuce]

Swip heard about a bee who had tried another approach to the degakification of feedstock, that in his opinion looked promising. At first he was considering sharing only with a few who have been especially helful, but then he read a bit of Geez's "making me sick" thread and reallized that others are probably having similar problems. SWIP was. So he decided to share what is thus far an unperfected technique, in hopes that others may improve on it.

However  his decision to share didn't come before he had already contacted the fist bee on his list, and this was another reason he decided to tell me to post the information now. He heard nothing for several days after sending the PM. Finally it dawned on him how he might react if the situation had been reversed--especially considering the kind of questions he was asking. (Sorry, Shorty. SWIP was feeling enthusiastic and didn't think it through.)

As a final preface, SWIP wants to again emphasize that this procedure has not been perfected, it just seems better than the presently available alternatives, and has been working moderately well for SWIM for several weeks.

Here's what SWIM's acquaintance said to do:

Grind up some 120's as fine as possible and put them in a beaker or a glass that will hold them without being more than about 1/3 full. Run out to the grocery store and buy a bottle of ammonium hydroxide, or as it's usually labeled, household ammonia. (Don't get sudsy ammonia!) Also pick up a box of washing soda if you don't have any. Poor some [edit]ammonium hydroxide [/edit] into the glass with the GUPS--not too much, just enough to turn them into what looks like smooth marshmallow cream.

Pause a moment to laugh maniacally as the GUPS turn to slime--a pitiful attempt to thwart your intentions.

Next take your jar of washing soda and add a volume approximately equal to the marshmallow creme. The amount isn't critical but it's better to have too much than too little. Stir well, pressing the washing soda into the creme as thoroughly as possible. Now add xylene. Again, be generous, but not so much that you will have trouble getting the pfed back out of it. Stir this mixture and right away you may notice the volume decrease as the freebase disolves. Let it sit for at least fifteen minutes. Leave it overnight if you wish, or continue on immediately. Decant off the xylene into a funnel with a moderately compacted cotton ball in the barrel and a coffee filter. Gass the pfed to extract. Be patient during the gassing. SWIP says he was used to having the pfed fall right out, but that it took much longer than usual. (Maybe his HCl generator wasn't working well?)

After capturing the product in the coffee filter, rinse off the xylene with some acetone, and allow it to dry.

Now go back and do it again for better yeild, beginning by pouring the xylene back in with the GUPS. The second time through you might want to add a little dH2O*. No more than 5ml for two 20 count boxes of feedstock. Swim hasn't yet determined the optimum amount, just be conservative. When you finish, pull again and again until you're happy with your yeild. SWIP doesn't think heat helps at all, and in fact may cause you to pull some gak. If the last pull you made is sparse but you're nowhere near the theoretical yeild, add a bit more dH2O.

When this is all finished, combine the fruits of your labors in a beaker and add enough concentrated NaOH solution to thoroughly wet the product. Stir well until it's all been converted to free base. Add a little more NaOH if you aren't sure. Then add dH2O in about the same quantity as the liquid already in the beaker. Swirl and filter through two coffee filters. Rinse again 2-3 times with cold dH2O, and don't discard the rinse water. [When you have saved enough of the rinse water to make it worthwhile, add a layer of xylene to pull, separate then gas to recover more pfed.) Spread out on a plate to dry, but don't use heat. Remember, pfed freebase turns to vapor at a reletively low temperature, and even warming it will cost you yeild.

While you're waiting, take an ehrlenmeyer flask and match it up with a test tube with a diameter nearly the same as the mouth of the flask. If what you have is too small, cut rubber strips from an inner tube about 3/4 inch wide. Wrap this around the top of the test tube, stretching it snug as you go. Keep at this until it makes a nice snug fit with the mouth of the flask. Now cover all of the rubber with several layers of teflon tape pulled snug.

Crush some ice and fill the test tube, dump your dry freebase into the flask and insert the test tube. It should fit snuggly enough that you have to push with moderate pressure to seat it in the flask. Not so much you rusk breaking it, but enough that you don't have to worry that it might fall inside. If it's too loose add more rubber and teflon. If it's too tight, take some off.

Now place the (borosilicate) flask on a hotplate or a burner covered with a flat metal plate. Don't try to substitute anything else. Cups and jars can't take it and may break explosively. (Also, don't ever put your glassware directly on heating coils!)

It's a little tedious the first time through this because you've got to find just the right setting for your hotplate. Turn it on but keep the heat very low. Wait five minutes and if the freebase isn't melting, turn up the heat just a little. Keep at this until you find the setting that will just cause the freebase to melt and subsequently vaporize. If you mark the spot on the hotplate you won't have to go through this again. Having found the right temperature you might want to watch it for a few minutes to make sure it isn't going to get lots hotter as soon as you turn your back, and once you're satisfied set up a fan to blow on the outside of the beaker and go do something else for 1/2 hour. If you think of it, come back after fifteen minutes and suck out the now melted ice from the test tube with an eyedropper, and replace it with fresh. Try not to distrube the beaker though, because the crystals will fall back to the bottom and melt again. Not a big deal, just another few minutes wait.

After 1/2 hour take a look, and you should see the sides of the beaker are now coated with freebase crystals, and there will likely be some gak at the bottom that hasn't done much of anything. Remove the flask from heat and set aside to cool, being as gentle as you can so as not to disturb the fragile crystals. When completely coooled turn off the fan, and carefully pull out the test tube. Holding it over a container, scrape the crystlas from it's sides. Invert the beaker over teh container and shake out the loose crystals. Finally, reach a scraper into the beaker and scrape the remaining crystals off of the sides and into the container. The clean crystals will be found on the side down to just above the bottom of the flask, and it will be easy to see where you want to stop scraping. Be careful not to scrape loose any of the gak at the bottom.

*On dH2O, listen to what everyone has been saying lately. If you don't believe it makes a difference, the next time you need to mix up some NaOH, mix two batches. In one use dH2O and in the other use tap water. It may not be immediately obvious, but after  a few days the batch made with tap water will have particles floating around in it--a really visible contamination. SWIP used to think it was because his drain cleaner NaOH was poor quality but he was wrong!

Looking forward to hearing of improvements and other comments.

PP

[ning]

Since you're sublimating the freebase (or could this bee called a short-path distillation?), why not use something flat with a wide top, to collect the crystals better?

For example, a round, shallow pyrex baking pan or bowl with a glass plate or bowl sitting on top of it with cold or ice water in it might do quite nicely, and would surely make cleaning easier.

A very interesting approach....

[Prepuce]

Strictly speaking it's not sublimation, since the freebase melts before becoming a gas, so SPD is a good term.

In SWIPs experience a beaker is easier to deal with. A pyrex pie plate with ice in the top has been suggested by others, but if it doesn't seal well around the sides it will leak during the process. The ice or water must be removed when the process is finished or you risk dumping it into the collection container, all the while workign with crystals that are so light and fragile that the slightest breeze makes them fall away.

The psuedo-cold finger that SWIP suggests is the easiest and most efficient method he's come across. Other than the test tube, which could probably be eliminated in a pinch, your end product is nicely contained until you're ready to deal with it.

PP

[Shane_Warne]

Base with carbonate, extract with NP, Gas out as pe.HCl, collect, base (again) with NaOH, vaporise?


I can't see where the ammonia water is used.

[Prepuce]

but not quite. First the GUPS are mixed with ammonium hydroxide, a base. Then the washing soda added, followed by the non polar to extract. After extraction the non-polar is gassed, then the freebase is vaporized and condensed back into a solid.

SWIP is not a chemist and doesn't understand exactly what happens, but here's his speculation. The ammonia kills the detergent's hold on the pfed HCl. The xylene is now able to pull the pfed freebase without the polysorbate fighting to keep it in solution and countering everything you try to do with it. The gassing precipitates the pfed from the xylene, and the alternative would be to let it evaporate. Unfortunately we need it in freebase form to do the vaporization step, so it's based again.

SWIP isn't happy with the last step but hasn't found a way around it. He tried hot VM&P but oddly, the freebase wouldn't come back out of it just by letting it cooled. It had to be gassed or titrated. The only conclusion he can draw from that is that either pfed freebase is soluble in naptha unless it's mated with PEG or relative, or there's another gak that follows in xylene that causes the pfed freebase to become soluble. Regardless, the best solution seems to be a double A/B in spite of the associated losses.

The good news is that the product is very clean, there's no boiling of solvents, and it's a comparatively quick procedure to perform.

PP

[Shane_Warne]

I like it Prepuce, well done mate!

Basing two times does seem tedious though. What was the yield like from the ammonia/carbonate step?

White 60s?

hehe, the ammonia water is what I really like the most, because it cuts out a lot of sodium that they've probably been working around for years.
I wonder how the hydrogels and cellulose binders react to the presence of the ammonium hydroxide instead of sodium compounds, because I know that sodium chloride makes some of them contract.

Do you think you would get a complete basification with ammonia water if you just added more?

[Prepuce]

SW, it actually takes a lot longer to explain it than it does to do it. SWIM says he can get through the first part of the procedure in about five minutes, then it's a matter of waiting for some acetone to dry. Even if you stand there and wait it doesn't take long for that. The second basing is even quicker than the first, and why bother with the vaporization until you're completely finished with all else. In other words, that part only needs to be done once.

I believe SWIM said he's done this on generic and brand name 120s, generic and brend name white 60s, and recently on something he found for the first time--white 30s with no antihistamines. He usually does three pulls on the GUPs. Yeilds have varied because he was working through the mechanics of the procedure, but he checked after working some white 60s and the yeild was about 60 percent. That might not sound very good, but before he came up with this his average must have been somewhere around 10 percent and it was still full of nasty gak.

Vaporization is a good way to see how clean you're getting your pfed, if nothing else. You might be reallly surprised what you find left over. SWIM has convinced himself that the detergent gaks don't actually inhibit the reaction very much, as many have speculated. The pfed is never finding it's way into the reaction. Even though it looks sparkling clean, SWIM has over and over found it to be loaded with crap--especially piss yellow oil--after vaporization.

As SWIM keeps telling me, the procedure needs fine tuning. Aommonia is a fairly strong base and should be capable of basing the pfed on it's own. He has thought about doing so, but so far hasn't thought of an advantage to doing so. (One disadvantage would be dealing with all the water.) He thinks the contribution of ammonia is primarily in breaking down the detergent gaks. In fact, he's been meaning to try adding a little NaOH to the first basing to see how yeilds are effected.

PP

[geezmeister]

Gassing for the freebase form of pseudo? I don't think so.
You gas for the salt form. You convert freebase pseudo to pseudo HCl by gassing with HCl gas. You could evaporate the solvent for the freebase, or you could freeze the freebase out of naptha. If you are having problems with the freebase not precipitating from naptha... you are using too much naptha. Pseudo freebase is soluble in naptha, it just isn't anywhere near as soluble in room temp naptha as it is in hot naptha. In VE's striaght to bee, there was always some pseudo left in the naptha, which could be had by titrating. But titrating carried gakk with it.

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.

I like the approach with ammonia, though. You may be correct in your assumptions that it breaks a lot of inerts down that we aren't breaking down by solvents. I also applaud your purification step, and look forward to your honing it down even more. Thanks for the writeup. If I can gather enough pills to mess with, I'll try this out.

[Prepuce]

Geezmeister-sama,

SWIM has been going over his posts to see what might have given you the idea that he thought he could gas for freebase. The only thing he could find, and for which he is unable to post an edit, it the statement,

"He tried hot VM&P but oddly, the freebase wouldn't come back out of it just by letting it cooled. It had to be gassed or titrated."

He should have completed that sentence by stating that gassing or titrating caused the hcl salt to precipitate. What he had intended was chilling it out of the hot solvent, ala Straight to B. When SWIP used that process there was always freebase crystals that would fall out as soon as the solution even began to cool. Not so in the incident he describes in this thread. The only way he could get the pfed out of the solution at all, short of evaporation, was to gas for the hcl which did precipitate.

SWIM is famous for leaving too much between the lines, however, so if there's something else please point it out specifically so he can correct it. The technnique is all about getting past the gassing/titrating gremlins, which coincidentally are also the reaction thwarting demons.

As for trying the procedure, SWIM did most of his testing on 3-5 pills at a time in a test tube. Two or three is enough for 120s, and should be sufficient to decide if the technique is workable or not.

The purification step--vaporization, is working well for SWIM the way it is. (Although he would heartily welcome any suggestions for improvements!) When he first started with it he found it messy and prone to waste, but with a little practice he has come to regard it as quite workable. The keys are to not disturb the beaker, keep cooking until there is no liquid remaining at the bottom, then gently remove from heat and let it cool before further disturbing it.

PP

[ning]

my uneducated guess is that if there's gaks designed to hold onto freebase amines, the ammonia overwhelms them and takes the place of the pseudo.

I like the idea of ghetto short-path distillation much better than chromatography (yes, no fun, I know)

[geezmeister]

After extraction the non-polar is gassed, then the freebase is vaporized and condensed back into a solid.

That comment will mislead six thousand newbees into disaster. How about filling in the missing between-the-lines comments so you don't confuse the new ones, or the old geezers like me, who have nothing to do with their hands these days but bitch at the keyboard...  Damn pill laws! I have to drive a couple of hours just to get enough pills to make it worth my time to try any new method. (Get ready folks, its headed your way before you know it.)

[Prepuce]

Thanks, Geez. Guess SWIPs ADHD is kicking up worse than he thought. (Good thing he has a supply of the temporary cure.)

For some reason the option to edit that post is not offerred by the board, but the sentence should read:

=============================
"After extraction the non-polar is gassed, the hcl salt is collected and based with NaOH to turn it back into the freebase. The mixture of NaOH, dH2O and freebase is filtered, then dried. Finally the freebase is vaporized and condensed back into a solid."
====================================

Gee, it sounded so much easier before. It really is harder to write about it than to do it, though.

You have to drive 2 hours to get enough pfed to react? SWIM didn't realize it had gotten that bad. He assumes it's because of ID checks in SWIGs locale, but not in the other. That's exactly the kind of thing SWIP had in mind when his intention was to not make this method public. Whatever people may think of the WOD, however, neither I nor SWIM can imagine that anyone could see making people sick as the right thing to do.

Since I'm on my soapbox anyway, consider this: The war on drugs makes no sense to any reasoning individual if you look at the results. Who benefits? Follow the money.

Even honest politicians alert enough to think it through wouldn't dare to suggest decriminalization because it's political suicide. (What became of the mayor of Baltimore, anyway?) Those in favor of continuation are driven by emotion, and could be made to see reason if reason were presented. So who is making the money as a result of the WOD anyway? Who benefits? There's a lot of money being spent. Someone likes it very much.

So much for the soapbox.

PP

[Prepuce]

is certainly easier than chromatography! Faster too!

"I like the idea of ghetto short-path distillation much better than chromatography (yes, no fun, I know)"

PP

[Shane_Warne]

What are the gaks the like to hold on to amines? I could name orange, and that's it.
I've ignored polysorbate too, either rightly or wrongly.

Prepuce, what detergents are you refering to, mate?

Prepuce, so have you had any issues with condensation of water with the freebase, due to the ice-filled coldfinger?

swisw would expect that and would add CaCl2 to the fb before heating.

I didn't know fb vaporised so rapidly by the way. Warming will cost yield? Didn't know that.

[ning]

do you think the pfed-salt could be sublimed as well?

After all, people smoke meth HCl...

[Prepuce]

SW, ning:

The two that SWIM is most familiar with are PEG and poloysorbate 80. Both are non-ionic surfactants. Detergents. Polysorbate in particular has been difficult to deal with, but PEG has also been a big problem in the past. For more information on the subject than you probably want, see the thread  "Know the enemy: More data on polysorbate 80." Never have figured out how to post hyperlinks here, so you'll have to UTFSE to find it. Sorry.

SWIM has had some issues with water when vaporizing fb and it makes it really messy. Tends to drip off the end of the test tube and recycle itself. Fortunately it's not difficult to let it dry out well first. You don't need to do anything special since it doesn't tend to absorb moisture. SWIP puts it in a box with an exhaust fan, and that's all. No heat, no fan blowing on it for obvious reasons.

The test tube with ice in it usually has only water by the time it's removed from the beaker, so condensation is not a problem. Removing it early complicates things anyway, since you'll shake loose some crystals that will fall back onto a hot spot, melt, the vapor will escape since the test tube is out, etc. The test tube isn't such a big deal anyway, since most of the crystals cling to the sides of the beaker. Just cook it until there's no liquid in the bottom that wants to vaporize, and don't be tempted to turn up the heat if all of it doesn't turn to a gas. That's a sure way to start vaporizing gak. It might break your heart to leave it there, but if it doesn't vaporize it's not what you want.

When you find the temperature where vaporization occurs, most all of your freebase will vaporize just by letting it cook. After you harvest the results, scrape everything remaining into a pile on the bottom of the flask and heat it again. SWIM doesn't clean out the beaker until it gets pretty nasty, because there's always a little more fb mixed with the gak, and the gak doesn't hurt anything as long as it doesn't get too hot.

Adding CaCl2 will probably get you wet freebase and dry CaCl2. There's no reason to do that anyway. Just let the fb dry before you start. If it's wet and you chop it into small peices it won't take that long.

It does vaporize easily. Really easily. The melting point is only 118°C, and the vaporization temperature is not much higher. The HCl salt, on the other hand, melts at around 180°C, and it seems to prefer burning to vaporizing. If you're careful enough to get it to vaporize, at 180+ you're going to probably be vaporizing a lot of gak as well. So you see, this really only works on the freebase.

PP

[ning]

First, to post a link to a post, put it's number in brackets. Your post number is 513459, put that in square brackets to obtain

Post 513459

(Prepuce: "Gaks that hold amines", Stimulants).

Now, those annoying detergents are of the polyoxoethylene type, eh? It would be ideal to perform an acid hydrolysis to crack those ether groups, but I don't know the conditions required or whether it would harm the pfed.

So let's imagine that they boil really high, and leave them as-is. Say we follow the following imaginary procedure:

pills are ground up with ammonia water and sodium carbonate until it is a pasty, chalky sludge. Then, the mixture is gently evaporated to yield a hard greasy cake which is crushed up and distilled as prepuce describes. Hopefully good yield of pfed.

Something worth trying, I guess.

Best luck  

[Prepuce]

ning: SWIM has been continually amazed at what he has neglected to mention with respect to this thread. What was presented is a procedure that evolved over the course of several weeks, so there have been many less than successful tests. What makes it difficult is that SWIP has been less than conscientious about recording all of his findings.

Having said that, he may be mistaken, but believes that the xylene plays an active but, at least for SWIM, unknown role in the process. In his tests he never allowed the GUPS/ammonia mixture to dry, however, so it's surely worth a try. In a similar vein, SWIM has tried other non polar solvents, but everything tried pulled gak along with the desired product.

When ammonia is mixed with GUPS, depending on what kind they are they usually melt into a smooth gooey paste. The transition when xylene is added can be somewhat striking to watch, as the gak withers and dies before your delighted eyes, a fate similar to that of the wicked witch when doused with water. If only it could scream!

Ahem. Sorry.

SWIP has a feeling that the next major improvement of the process will come with the addition of another as yet unidentified substance to the mix.

SWIP dreamt that he recentlly completed the first reaction using only the product of the gakinator process. He want's to double check the results before saying too much, but can't resist mentioning that he was astounded! by the yeild. Especially since he doesn't think he has ever achieved better than about 45% by weight of pfed, with some portion of that gak. . . This looks to be by far the best yeild he's ever produced by means of an rp/i reaction.

(Speaking of which and the associated difficulties, has anyone succeeded in extracting useable H3PO3 from pool antiscale additive? It boils down to a waxy solid when cooled, but has a pink tint, and SWIP has no idea what the contaminant may be.)

Thanks for explaining the link markup, btw.

PP

[Shane_Warne]

SWIP dreamt that he recentlly completed the first reaction using only the product of the gakinator process. He want's to double check the results before saying too much, but can't resist mentioning that he was astounded! by the yeild. Especially since he doesn't think he has ever achieved better than about 45% by weight of pfed, with some portion of that gak. . . This looks to be by far the best yeild he's ever produced by means of an rp/i reaction.

You'd want a good yield from the RPI, to make up for all the losses from 2 A/B's and a vaporization.  

ning's shortened version is more to my taste, except you'd have to wait a long time to evap, and heating wouldn't be possible, because it would steam distill off.

How about just vaporizing after extracting with a NP? Worth a try?

Have you ever weighed the yield after the gassing?

[barkingburro]

swibb is at this very moment working on this. first step was to dry using dessicant rather than boiling it down. heat causes h3po3 to degrade when it is aqueous. the secondary chemical in swibbs descaleant is polymaeic acid.

thoughts on why the ammonia may work... ok the gaaks are designed to be activated and released in the body. is ammonia not pretty similar to chemicals in the body produced as waste? i suppose that would be more urea than anything.... hmm, just a thought

[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

[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.