beautiful

[livid]

swim does his own thing. it is a combination of things on rhodiums site. I have never posted it because it's nothing special. some bees prefer one solvent to another. ect. ect. The biggest improvement swim has noticed lately, is the brake cleaner thing. You bees that do that know what i'm talking about

[spectralshift]

Trap works fab! Even w/out following instrcts!

Now you see the evidence of truth.  
Fuk with it a bit too dude, well done for trying this out. Dry basing will aways get some phase transfer.

If you look up to my (halfkast's) first comments in this thread you'll see that swihk stated that he had done this without tetra a long time ago.

A pre-wash or boil with tetra and then dry-basing will do better than the tetra trap itself haha. Isn't it obvious?  

The damage is already done. More like the progression is finally upon us...

[Prepuce]

Shorty,

Thanks for your work on this. (And thanks to Geez for refering SWIP to the post.) SWIP had used the tetra trap to produce what he originally thought was very clean fb crystals, and only discovered his error after a really shitty yeild on a RPI rxn.

After another workup using tetra trap SWIP followed up with H2O wash of the crystals, and found the water thick with some sort of polymer-like substance that appeared suspended but never settled out. That peice of advice, plus using sodium carbonate instead of drain clearner made a huge difference.

PP

[geezmeister]

I second Prepuce's observations, based on experiences with Perrigo 120's in particular.

[Prepuce]

Geez: "I second Prepuce's observations, based on experiences with Perrigo 120's in particular."

Damn! It didn't last long. Listen to this. SWIP processed a batch of 120's and 60's in the approx. ratio of 2/3 - 1/3. He then did the boililng water, scoop out the melted crystal thing, and the result looked quite nice. He then did a burn test and the results weren't so good. Back to the drawing board, he noticed that when he boiled the fb crystals that some particularly foamy material tended to float to the top, but it looked different than the melted crystals. He decided to filter rather than skim.

It was a little more difficult to do because he needed to get all the crystals to disolve before filtering, and then he had to work quickly. As it happened, he added more water to facilitate and ultimately added too much. "Insoluble" is a reletive term, he discovered after loosing a bit more than half of his 20+ grams. He still recoevered almost 9g and eventually hopes to get most of the rest via slow evaporation. The 9g he had in hand looked good. In a burn test they went up far more quickly than he had previously observed, and only the faintest indication remained on the foil. May have been a slight discoloration from the heat. Next he checked the MP, becuase he didn't want to risk another failed rxn. Using a previously saved reference, he watched for the temp to reach ~123 C, and was almost caught off guard when the sample melted at what he judged was about 118 C. Wondering what might cause the MP to go down, he went back to his archives, and found that according to another source the MP should be almost precisel 118 C. SWIP was startign to feel pretty good about this.

He decided to take another stab at a FB reaction, since his feedstock was so clean. He had gone to similar pains with the MBRP and I2. His mix was roughly 8g fb, 12g I2, 4g mbrp and 8 ml H2O. The rxn went just like VE described, and when he set the temp up for phase II he was comfortable that at last he'd end up with a decent yeild.

Right to the end, everything went just as it should. The post rxn mixture was by far the cleanest he ever saw. Finally it was time to base so he could extract with VM&P, but he wasn't going to make the mistake of using NaOH again, or taking the PH too high, so he used TSP. One teaspoon, and almost no effect. In went the second teaspoonful along with a bit of heat to start moving the oil up into the non-polar. Maybe a little stirring. . . But what's this. The glob of gell that now filled the beaker was quite difficult to stir. And the PH wasn't even 10. What the hell could it be?

Before going any further he decided to pull what he had. He filtered the glop but still ended up with enough of it to clog the funnel. A little forced air cleared that, and he poured the remaining naptha into a beaker to gas. Disaster. Not even a gram of yellowish product. Three cold acetone washes and thorough drying later it looked better, but when sampled, according to SWIP, it reeked of naptha.

What went wrong? Damn if SWIP knows. He can't discard the possiblity of the bonehead effect, but he had been unusually careful and doesn't think he mixed up something he hadn't intended. However he's thinking--hoping, actually--that that's the only likely explanation. Comments?

PP

[gluecifer69]

And the PH wasn't even 10. What the hell could it be?

Should not the pH be at least 13.5, for meth to move to the non-polar?   Pseudo moves across at 12, I believe.

Relax, and try pH'ing up to 13.5 and see what happens, this could very well be the reason for no yeild while gassing.

However, there is believed to be a new gakk on the block, if not then coming soon.

[weaz1dls]

It's been swiw experience that unless the fb is rid of all the that xtra base (Naoh,etc) more HI is required to counter it. It may not seem to be much, but weigh it in relation to the amount of base needed at the post workup to reach 7.0.  If HCL was the solvent of past reactions under 100 deg.  and we know it is present in the hcl salt form of the rxn, then don't give up till ya smack that bitch up er down so to speak. Muratic fumes, as does HI in high conc.

Also you may have tripped onto something here!
don't some pills use a phosphate in the mix. Then it is in a reaction the produces more of it.  But along the way it is safe to say it was removed.  Then upon addition at the end..boom GEL, or an environment where water can be held like a sponge, similar to caffine.  Caffine mixed with water will disolve at first.  Let it sit or draw into a syringe and it will go oatmeal on ya.  But guess what, slightly acidic environments increase it's soulubility or decrease its ability to hold water.  It also slowly destroys the caffine. Anyway try going the hcl salt on the front side. After the addition of hot water at the end of reaction, plug the mouth of the flask with a coffee filter so as to restrict but not block flow.  Put in the micro and zap, swirl zap swirl.  Not to much though.  You will know when it's enough by the change in color, increase bumping, and evolution of white whispies in spight of the aditional water present.  Go to far and kill those yeilds!
Then filter, carefull that phos continues to radiate heat and is much higher in temp than the fluid. If possible tap with tce just a squirt and some jap...this is not always needed.  Test a small amount as is by mixing with base. Does it milk or flock? Flock= TCE Jap, then np rinse.  Also in this neck of the reaction Kosher salt and micrwaves are you friends.

[geezmeister]

Prepuce: if you had the pseudo that clean, go ahead and base the fluid enough to freebase the meth. You stopped too soon.  TSP is messy as hell, IMO, and to get the solution to a high enough pH to freebase the meth HI you have to saturate the solution with TSP. It will do the job if you stay after it, but you will have undissolved TSP in the reaction fluid when you get to the desired 12.8 pH. TSP is messy, and the glob you describe could be the TSP and water in the fluid.

IMHO you didn't get any meth because you never got the meth freebased so it could be extracted with a nonpolar solvent.  Even with a load of orange gakk, you would have gotten some yield if you based with NaOH. You do not need to over do it, but you have to at least do it to get meth. Add enough NaOH to reach pH 12.8 or 13 and quit basing. But get the solution at least that high.

[geezmeister]

he following information details my "tweaks" of the tetra trap method as used to extract pseudo from the generic 120 mg time release pills. These pills are heavily orange II gakked, and have a lot of polyethylene glycol. They are not that easy to extract cleanly, and have long been one of the more problematic pills. They are also, for that very reason, more available OTC than white 60's of any type in my area. My habitual use of these pills derives from their availability rather than any other factor.

II ran the tetra trap on seven twenty count boxes of 120's recently. I used xylene as the np, rather than my standard VM&P naptha.  I ground the pills very finely, and placed them in a liter beaker. I mixed dried acetone and Japan Drier at ten parts acetone to one part JD, and boiled the 120's pill mass in this for five minutes, then allowed the pill mass to sit and soak in the solvent until it settled and cooled. The liquid was decanted and the pill mass boiled twice in VM&P naptha. The pill mass was then boiled one time in xylene, also used to extract the pseudo.  A final acetone rinse followed the xylene boil and the pill mass dried, mixed with sodium carbonate, and the two were thoroughly ground together.

The pillmass was then saturated with TCE, and the pseudo extracted three times with xylene by the tetra trap method.  I combined the three volumes of xylene, and washed the combined xylene pulls three times with a 10% NaOH solution. I followed with three washes with distilled water. On each of the first two water washes, and emulsion appeared at the polar/nonpolar interface. This emulsion was gray in color and the bubbles making it up were very small.  The third water wash produced no emulsion. The xylene was dried with epsom salts and gassed for the pseudo. Yield was about 55% of the available pseudo, which is par for yield from the 120's IMHO. The pseudo so obtained was dissolved in MeOH,  MeOH was used to rinse the pseudo remaining in filters, and the pseudo laden MeOH was  filtered into a 50-50 mix of naptha and xylene approximately five times its  own volume, which was then heated to evaporate the alcohol and precipitate the pseudo HCl. The Pseudo HCl was filtered out when the naptha/xylene reached 105C, and rinsed with MEK.

The pseudo so obtained was reacted in a hypo synth. The meth obtained after a standard workup was acetone flashed and rinsed. It burned with some residue; a a single recrystallization yielded clean-burning meth with no taste.  The very tail end of the acetone rinse/motherliquor from this recrystallization was reduced over low heat, and when very nearly completely evaporated had the slight orangish tint seen when OII is present, but had a different smell. Crystals of meth formed  even in the final bit of rinse acetone/motherliquor. These were not souble in MEK or dry acetone, and I was able to wash them fairly clean and leave the remaining small bit of residue behind. All of the meth recrystallized readily.

I think this process sucessfully removed the OII gakk. Had the solution been laced with OII, the meth crystals that formed in the final remnants of the acetone rinses and mother liquor of recrystallization would have dissolved with the OII into the acetone, if they had formed at all.  These did not. The smell was different, not as noxious, I saw no problems with crystallization and lost little yield in recrystallizing.

I did not have a good yield from the reaction. Whether this was the result of misjudging the completion of a hypo cook (which is likely) or the presence of some gakk (which I think is the less likely  answer) I will not be able to say without repeating the process.  My impression is that the process worked to remove the OII from pseudo obtained from dry matrix formulation pills heavily gakked with OII  and  PEG. . The effect of the Japan drier is not easy to assess. I used very little of it mixed in acetone and got a green coloration in the pill mass that washed out with subsequent solvent boils and rinses. My final product seemed OII free, or free enough of it that OII did not appear to be a problem.  I will run the process again without the JD to assess the efficacy of the other steps against the orange gakks in themselves. I note the emulsion that fell out of the nonpolar during the basic rinses remains an emulsion nearly forty eight hours after being separated out.

[auntyjack]

swij noted a while back in this post someone asked if it is necessary to boil the dcm out of you tetra brake cleaner before you use it and months later my brain has vomited up a response..now for washes of the pill mass, leaving the dcm in the tetra is probably a good thing considering dcm is another gnarly solvent but it occured to swij a minute ago that if you run the tetra trap with your tetra being only 30% and the dcm 70%, the bottom layer will reduce in volume quite dramatically as the dcm boils off(don't they form an azeotrope?)...anyway, this would seem to be detrimental to the whole bottom layer holding the pill mass principle...but swij is not sure exactly so.... have fun...swij is drunk!!

[Prepuce]

Geez, it seems as though SWIP is forever thanking you for your advice, and it's his pleasure to do so once again. Thanks also to Glu and Weez.

SWIP is guilty of leaving a bit too much between the lines as he rushed to complete this last post. SWIP knew that he hadn't made the solution basic enough, but figured that some product would probably come through regardless. In fact it did, just not as much as he had hoped.

Also he did try additional basing. (He didn't mention it previously because he was so disgusted about the reaction going bad in spite of his efforts.) He took a small sample of the post rxn mix, of which the gell had mostly settled to the bottom of the beaker following the addition of enough H2O to triple the volume. He placed the sample in a test tube and added NaOH to see if it would get worse. (How much worse could it get, he reasoned.) The NaOH didn't cause any problem so he based the rest of the batch to PH13, and with a lot of messing around he coaxed out another couple of grams of product, this time with toluene to be sure he didn't leave anything behind. He also aaved the acetone wash of the first pull, and expects that this will yeild more polluted product with the application of sufficient effort and time.

Following the last gassing operation, this being the fist time SWIP had gassed anything out of toluene, SWIP was surprised that the product didn't fall to the bottom as quickly as it does when gassing from naptha, so he left the cloudy suspension to sit overnight.The next day the problem with the rxn came into sharper focus when he again checked to see if the product had settled out. It had, but now the toluene looked more like a beaker of weak orange Kool Aid.

SWIP racked his brain to figure what had gone wrong, after he had taken such pains to ensure the cleanliness of his starting materials. He can't be sure, of course, but he thinks he has a likely suspect. The I2 he used in this rxn had been harvested from the acqueous layer of previous rxns. Although it was as clean as any I2 he had ever extracted from tincture, and that means it appeared completely clean, SWIP would have gone through the messy process of sublimation if it had occurred to him that he might be spiking this batch with OII or equivalent.

If that doesn't make sense, then the only other explanation he can think of is that he must have inadvertently combined some feedstock that hadn't completed the process he outlined earlier. (SWIP has a bad habit of experimenting as he goes when things aren't working out, and often a single beaker divides into four, eight or more, and this occaission was no different. He's not always as conscientious as he should be about keeping everything labeled.

Geez, SWIP wants to encourage you to try the H2O boil and filter process he described for cleaning FB post tetra trap. Reading the procedure you desribe makes him think that this just has to be easier, even though you've got to be careful not to add too much H2O. (If you do you can always wait a week or more while it evaps.)

At one point during the preparation of this last batch, SWIP made about 3g of hcl because he wanted to try something SWIG had suggested--he doesn't recall how long ago. It was disolving the pfed in alcohol, mixing with Xylene and nuking until that alcohol was gone. He dreamt he did this after performing the tetra trap but without the follow-on H2O boil. Well, he nearly did this, but chickened out on the microwaving. As he was waiting for the solution to begin boiling, and all he could think about was what it might be like if the alcohol vapors were ignited by a spark in the oven, blowing it and SWIP into little bite-size morsels, perhaps. So he took it out, connected a condensor and boiled it off with good ol' heat, then filtered, let cool, and filtered again.

The FB product he tested after the H2O boils burned almost perfectly pure, with only the smallest hint of residue, and melted at as close to the correct temperature as it was possible for SWIP to determine. The hcl that had been treated as described melted at least twenty degrees too soon, (although SWIP blamed his technique for that at the time.) The burn test left the inside of a test tube coated with a dark brown residue that could not be fully removed when it was cleaned. He guesses it was burned PEG, which would have no doubt been removed had he been following the rest of the procedure SWIG outlined.

At any rate SWIP would like to hear of others experiences with boiling the FB because he believes that this yeilds the cleanest product he's ever seen. Obviously there is some question on whether OII is fully removed, and it would be interesting to hear what others say of that as well.  (SWIP should point out that the only thing original in this, if it can be called original at all, is the fact that he filters the FB after boiling.)

PP

[ahgreich]

now that some time has passed, and significant experimentation done by others - do you find overall that this method is valid and/or superior to other methods, or are there sufficient limitations to downgrade its universality?

[SHORTY]

As one of the first beez to try this method when you posted it over a year ago (without the fancy writeup).  I must say that i still use it, to this day, with a little tweaking to fit my situation such as gassing and precipitating in xylene etc.  However, the basic procedure remains pretty much the same ie; sodium carbonate is used to base, pillmass is saturated with tetra, and water is added in small amounts.

I can say that i now have a consistent procedure for extracting from the pills which are available and affordable to me.  I have managed to set up a nice agreement with a local pharmacy in which i purchase a bottle of 1000 white 60's once a week.  This is divided into 3 equal portions which i extract seperately throughout the week.  1 portion can be extracted in about 3 hours from start to finish and yeilds between 13 to 18g of clean pseudo.

My only concern is that the formulation will change on these pills and i will have to start all over again.  Until then i am quite happy and glad that that i gave this method a try back when many beez did not take this method seriously. 

Thanks again Algreich!!!!!!!!!!!

[geezmeister]

I've used it a number of times lately. My yields have been equivalent to yields from the straight to Bee, and a little better than yields with a "waterless a/b." I've done it enough times to get a decent feel for it. The method moves quickly, gives a little margin of error, and seems to hold some gakk problems at arm's length. 

I do not consider it effective by itself. The method does not eliminate OII without more, and depending on how the pseudo is harvested, you can find yourself PEGged as well. A few precautions before the a/b and/or a few polishes after it will give clean pseudo or pseudo HCl. I described a number of those a few posts earlier in this thread.
The choice of which to use depends on the inerts in the pills you wish to extract from, just as it does with the  STB and "waterless" a/b's.

I've been using it to extract pseudo from OTC pills. That  suggests my opinion of the method's usefulness.

[Prepuce]

For all his whining, SWIP is quick to ackowledge that the tetra trap is far and away the quickest and most efficient gak cleaning method he has used. If not for SWIA and a handful of others, the rest of us would be having mostly bad dreams these days, so many thanks for all the time and effort. SWIP wishes he had come across the TT method a year ago like Shorty did!

SWIP is about to give it another try, this time being very careful not to introduce contamination from outside sources. The pills he has been using are easily the most gak laden he has ever seen, but like Geez mentioned, it's even sometimes difficult to find these. With ever increasing frequency SWIP has been finding the store shelves layed nearly barren. He finds that surprising, because it appears that it's harder than ever for a bee to pull off a successful reaction. Especially for a newbee. So many ways to go wrong.

But unless alergies have begun running rampant the empty store shelved could only be due to the pollen gathering of bees. SWIP wonders how much longer it can last.

PP

[SHORTY]

Almost a year ago 02-26-03

Post 411902 (missing)

(ahgreich: "Please critique: simple flexible STB", Stimulants)

[phillyphil79]

This is one of the best write-ups a newbee could have ever seen....hopefully through my searching I will find more like this.......thanks

[Prepuce]

Geez,

SWIP was so busy prattling on about what he thought might make the tetra trap more effective (boiling in H2O, filtering), that he at first didn't stop to consider what you had offered here. After satisfying himself that the boil/filter combo wasn't going to take care of the problem he came back to read again, and this time read better. He followed the steps you laid out with painstaking attention to detail, and the result was just as you suggested. Very clean pfed-hcl.

The only trouble now was that he really wanted to do a FB reaction since he has yet to be able to avail himself of rp alternatives. On that note he foolishly decided to turn his hcl back into FB, and the yeild was even worse than he expected. This started him thinking about several packages of highly gakked generic red hots he just happened to be hoarding in reserve. Ignoring your caution that the procedure you have was for 120's, he started back at it, and before long he had some nice FB crystals. (Of course this time he deviated from the procedure and performed the tetra trap with VM&P instead of xylene.)

Testing the FB with the burn test he was at first pleased. The sample melted quickly and uniformly into clear liquid, and upon further application of heat from the match, it all vaporized and left nothing at all on the foil. SWIP noticed, though, that the sample seemed to give off a burst of vapor very quickly, but then it took a little more heat to get the rest. Hard to say for sure when melting powder on foil with a match. But also, the first vapor was clearly FB but the smell of the last was different. He tried it again, watching more closely, and sure enough, right after the powder melted a puff of pfed smoke was produced, but the clear liquid remaining required additional heat before it vaporized, and did not smell as it should.

Thinking this over a bit later, SWIP thought that the delayed melting point of the unknown gak might be an advantage. He set up a coffee pot with an inverted cup that he used to sublime I2, and placed about a gram of FB. He then filled the inverted cup with ice and applied heat to the pot. As he watched the FB melted, vaporized, then crystalized on the sides of the pot and into the cup. Eventually there was a quantity of liquid that would not vaporize at this temperature, which was about the same as used for the tetra trap. SWIP didn't measure but he thinks it's right about ~100 C. He was careful because he didn't want to burn anything, or to contaminate the end product by getting the gak hot enough to vaporize. In the end he was left with some very fluffy crystals that actually resembled those you get from sublimation of I2, in form, that is. Remaining in the pot the liquid had now taken on a familiar brown color. SWIM isn't sure what it is, so for lack of an alternative he will refer to it using the scientific term, "brown shit."

Following this procedure it was clearly evident that the FB was completely clean. A small sample went up in smoke almost immediately when heat was applied, and left no trace behind. Overall SWIP has been quite pleased with this method, one drawback being the fact that the method is rather messy. (If anyone has a better method for sublimation, SWIM would love to hear about it!) The other difficulty is with yeilds, which aren't actually bad from the vaporization, but SWIP doesn't approach fifty percent yeild once he has treated with JD, xylene, VM&P and on top of that run through the tetra trap. He is careful about overheating in each step, careful about using too much H2O in the TT, but evidently has yet to develop the proper technique. (He would love to bee a fly on Shorty's shoulder during one of his extracts.)

One other detail that SWIP doesn't want to leave out is the newly revised gak list of the red hots he used. He actually tore off the list of inactives to be able to list them here, but somehow lost them before he made it to the computer. It was the worst list he's seen from the evil Gak-Mongers yet. Several items he has not previously seen listed, and which he had never heard of previously. At step beyond cross povidone, PEG, O, OII--whatever that is.

 At any rate, SWIP has yet to try it, but suspects he can get similar results just by running the TT then vaporization cleaning. One other possibility is that, with careful heating, it should be possible to melt only the FB, or if not to pan it off to the side of the container, since the FB tends to seperate from the brown shit once it's melted. SWIP was going to try it with a couple of raw pills ground up with some sodium carbonate and MeOH. While he doesn't really expect that to work, you never know!

PP

[Scottydog]

After messing with the stainless steel carafe as a replacement for a glass carafe in the tetra trap extraction, it got Swim to thinking.

Does anyone here think that it might bee possible to run a tetra trap in Dwarfer's patented PP/SS (Stainless steel pressurized pipe)?

Heat at 100C for 5-10 minutes, remove from water bath with tongs, allow to completely cool, place in vice, open one end cap and then filter through a cotton ball?

[clandestine]

Heres how swim does his napthenic (vm&p) version of the tetra trap.. swim likes ending the FB pull with an acetone evap for maximum yields.

With this version you just chill the freebase out of the naptha(24 hour chill) and filter it washing the glassware you used to chill out with acetone and scraping up the evap.

HEre goes the tried and true ez-ass super extraction... ez as pie.

You need
************************************************

sodium carbonate (washing soda or ph up at wallys) check the label is sais sodium carbonate

Vp&p Naptha (a must for the chill)..

pseudoephedrine pills... any compilation make or model.

(dh20 or methanol) your choice just need a little anywayz.

Tetra - TCE.. you know.. if you dont oh well.

**********************************************
SO just grind your pills to powder and mix in an = amount of sodium carbonate.. too much carbonate is better than too little so dont be shy with it.... mix the fuck out of it... you cant mix enough so dont be skimpz either... grind that shit.

put the shit in the flask and spray it down with Tetra... spray it good... make it a big damp cake but not too runny... you want it super saturated with no free running tetra ok.... thats all.

then next add a nice amount of pre-warmed naptha... a good inch or so above the pill mass... and then add 15cc per 100pills of DH20 or METHANOL... your choice both work fine.

now let this all heat up to boiling and stir it up real good... once the naptha is burning hot take off heat and filter out the clean naptha while its still very hot with a cotton plugged filter and coffee filters on top... also be sure you pour the flask totally upside down when enptying the oils this ensures a little more yield if using bigger glassware getting the oils out as hot and as fast as possible.


Next just chill the naptha for 24 hours in the freezer and come back and filter again... then wash the glass out with cold acetone and then evap the washings on a pyrex and scrape off the nice crystals 5 hours+ later depending on the amount.

This trap yields the purest FB swim has seen in a long time for such a short stright to the point extraction.

swim will post a pic or something if he can find the right time of some really pretty fb crystals.



HERE is Some TIPS for the NEWBEEZ to this tech



1. Save that naptha.. just freeze it for 24 hours and filter and its good to go again many times.. (you use a lot over time so save it all).

2. Keep your pill masses and never throw them away until all yields are pulled.. you will be suprised how much FB is still in the masses.. (swim saves all his in a special bucket and does a big pull on the pile when its overloading usually netting 10G FB extra any given time.) so its worth saving.


3. Chill it 24 hours atleast (for maximum yields).

4. be sparing with the tetra its the most used vital took..... use it like holy water if you have less than 5 cans.


5. always wash your glass with TONE and save the tone evaps for lost yields.. it works good.

6. it may look cloudy like a gack in the naptha when its first chilling but be rest assured that cloudy mass is crystals when its dried on a pyrex or tone washed and evaped.