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	Stimulants

	All 43 posts		Subject: Best extraction method. well tested		Please login to post		Down

		evilscripter69 (Hive Bee) 09-02-04 15:16 No 529156				Best extraction method. well tested
						Tested on 30's, 60's and also 120's,(known gakk filled,PS80 and eudragit)  rx product is top notch.SWIM's yeilds have been averaging 60% on the E Extraction, and 70% on the Rx, Tetra Trap followed by SPD. Scaled up version SWIM uses 2 flasks one filled with xylene, 3/4 inch glass tube connecting the two. light flow from aquarium iar pump to drive the FB across, SWIM's last attempt yeilded a nearly solid mass of E upon gassing the xylene, this also seems to have killed the smurf (trip) Do at lest 2 pulls on the tetra trap, Use naptha, yeilds will depend on your amounts of water added and ther temperature its boiled at, SWIM finds a vigorous boil , right as the color of pill mass starts to change pull it fropm heat and filter it hot, crash in freezer, THIS WORKS VERY WELL, any Bees need guidance with this pm me, will be glad to help, so far this seems to be a universal cure to the new gakks.
		ChemoSabe (Hive Addict) 09-02-04 16:11 No 529163				Combining Pill types?
						Has combining some different pill stocks on a run yet been tried? Like for example do you think pre euradigit WW 120's mixed with current issue (fully gakk loaded) name brand 240s would be compatible to run simultaneous with this? And more importantly can you diagram your short path distillation setup for us? Even a crude drawing would be helpful. I read this Post 520830 (evilscripter69: "Scaled up SPD ?", Stimulants) but a diagram for something like this is worth more than a thousand words. About how much time does the distillation take? Would a setup like this do the trick? Or for an even shorter path the 200mm lickbag condenser could be eliminated with only the straight vac adapter between the still head and the collection flask. Without the existence of idiots geniuses would simply vaporize into thin air
		evilscripter69 (Hive Bee) 09-03-04 03:44 No 529264				here is the setup
		evilscripter69 (Hive Bee) 09-03-04 03:58 No 529267				takes about 90 minutes for 30 grams
						but knowing now the melting point 325*F +/-  it will be faster nest run.
		Shane_Warne (Hive Bee) 09-03-04 05:01 No 529275				is this right?
						es69, in that first flask is the TT powder mix or gups and base, and it distills as it's formed? (either by steam or SPD)
		12cheman12 (Hive Bee) 09-03-04 05:18 No 529280				evilscripter69 can you crop your pictures down
						evilscripter69 can you crop your pictures down before you post em up? Your an individual just like everyone else
		evilscripter69 (Hive Bee) 09-03-04 06:51 No 529287				first flask has the FB
						Freebase Pseudoephedrine via TT - cleaned up with SPD - dissolved in xylene - gassed for finished product = happy reactions and killer shit.
		abominator (Hive Bee) 09-04-04 03:21 No 529501				Gluecifer's experience on running differnt pills
						When all types of pills are cleaned properly swim has never had trouble combining different pill types in a rxn.  gluecifer almost always uses a motely of pillz.  He cant tell any differece from those runs than ones with the same pillstock. G69 out of I 4 ever
		Prepuce (Hive Bee) 09-08-04 16:51 No 530322				Why gas the FB?
						ES, I really like what you've done with this. Your method does away with the double A/B, which is the major liability of mine. Nice work. Now if I can just find some of those glass tubes you used! [edit - the rest of this post has been deleted, as the authors thinking was obviously short circuited at the time of writing.] PP
		evilscripter69 (Hive Bee) 09-10-04 20:41 No 530696				Try Naptha
						try using Naptha in the collection flask, it shouldnt be suceptible to melting from the solvent like the xylene, SWIM's currently testing this out. One word of caution, the crystals in the melting flask may contain Gakk in them, recycle them until nothing remains in the flask but the Orange/Yellow gakk layer. Orange plastic doenst smoke well(WHICH YOU WILL HAVE)if you rx the flask xtals.
		evilscripter69 (Hive Bee) 09-10-04 20:46 No 530697				Why gas the FB?
						the Hcl salt is easier for most bees to work with. SWIM will try it in FB rx, see how it runs.
		Prepuce (Hive Bee) 09-11-04 00:47 No 530731				FB reactions not difficult
						ES, you write, "the Hcl salt is easier for most bees to work with. " You're right, but only because that's what they're used to. If  they try VideoEditor's Wet Start Reaction Post 362507 (VideoEditor: "Free Base - The Wet Start Rxn", Stimulants) they might decide otherwise. Your method might be interesting if the second beaker contained VM&P naptha to catch the FB. Of course you'd have to freeze to get it all, just like you do with TT. Most of the other commonly used solvents would hold the FB and would have to be evaporated--not a desirable way to go. PP
		Prepuce (Hive Bee) 09-11-04 01:39 No 530742				pfed FB melting point
						ES, SWIP just noticed this. "but knowing now the melting point 325*F +/-  it will be faster nest run." The melting point of pfed FB is 118 C = 244 F. For pfed hcl the MP is roughly 180 C = 356 F. PP
		Jacked (Ancient Alchemist Delux) 09-11-04 03:02 No 530770				Reply
						Freebase makes better dope. I was the first one around here to get a grip on freebase reactions in a push pull, It is the answer to OTC reagents and good starting reactions with strong finnishing results.  Freebase is much easer to control in a LWR than it is with a push pull but both is doable and easy.. It makes better dope bottom line and thats the main reason it is done. Tighten Up!  (UH)
		Prepuce (Hive Bee) 09-11-04 05:55 No 530794				You're not going to get any better than that
						You're not going to get a better endorsement for freebase reactions than the one from Jacked. He doesn't post very often but most bees who have been around the Hive for any length of time have learned to listen when he does. Yeah, kind of like the old Payne Webber commercials. PP
		74L (Stranger) 09-12-04 23:43 No 531074				E S thanks 4 the reply
						Swim thought u forgot about him.  He figured naptha used with plastic 1/2 in. tube mite bee the getto solution .      he put the TT FB in a 250ml rb flask /tube going 2 jar-o-np.    Didn't work out 2 hot.      Heated at 250*f,  bubled at other end just like he beleaves its supposed to yet, after 1.5 hrs he got 1g nice angelic FB cristals from tube & top of flask ,tryed crash'n the np in freezer 2 find nothing. This from 5.5g fb.  there's still alot in the bottom of spd flask. looks kinda yellow but might still bee holding.   The free base should bee pretty klean from TT, only got about 45% back from that. Used  30-120s,48- 60s,then 3x96-30s sepretly then combined 4 spd.  he's thinking 2 cut the bottom off a test tube & use at bubler end with exyleen 2 c how that works.     Any other Bee's on the same page?    My thanks 2 ES 4 all his help. I'm GETTO as HELL and an't gon'a stop, but I like u guys.
		ChemoSabe (Hive Addict) 09-13-04 00:43 No 531086				EF Hutton?
						If you can do an LWR with pseudo hydrochloride you can do one with FB no sweat. Just be sure to get your ratios straight. It's on the short hot ones where you need the extra precautions. Prepuce wrote yeah, kind of like the old Payne Webber commercials. wasn't that EF Hutton ? Unob may actually have a point that I've got a sharp mind for useless trivia
		Prepuce (Hive Bee) 09-13-04 02:57 No 531097				EF Hutton?
						Damn Chemo, I think you're right. Thank you, Payne Webber. PP
		Prepuce (Hive Bee) 09-13-04 03:22 No 531100				So you wrote the mystery message
						74L, that ES was responding to. SWIP's advice is to scrap the plastic pipe and use a short peice of copper pipe if you can't get glass. Although the temperatures should not be high enough to melt plastic, especially if you use CPVC, the solvents will be pretty hard on it and you might end up with residue in your product. Heating to 250 F is pretty conservative, especially if you're measuring the temperature on the outside of the heating flask. That equates to ~121 C, which is only three degrees higher than the melting point. If you can get the FB to vaporize at that temperature great, it's good to keep the temperature as low as possible. It's not unusual to need to repeat the process several times to get through a batch, or at least that's been SWIPs experience. Between each scrape the bottom of the flask and break up the FB that has melted together. It often begins to seperate into areas that are tinged with yellow and others that are not. As long as you're going to cook it again you can ignore that and just grind it all up to powder. SWIM recently tried ES's procedure, although because he wanted FB as the final product, instead of condensing the SPD vapors into another solvent he put the receiver in an ice bath. He then installed another tube into the receiver and connected it to a second receiver which was also in an ice bath, then applied heat to the FB and activated a pump. The second receiver was insurance in case all the FB didn't condense into the first receiver, but it did not work well. The second receiver had an exit tube for safety--didn't want to build up pressure that couldn't somehow be released--but the smell of the air exiting this tube told SWIP that it wasn't only air escaping. Therefore he went back to his original method using a coldfinger test tube in a flask, which has always worked fine with the quantities he processes. For the record, he has no doubt that condensing the vapors into a sovent with a high affinity for them, like xylene, for example, would work much better. Naptha might be another matter, especially if it isn't heated. It would be interesting to know. PP
		evilscripter69 (Hive Bee) 09-15-04 17:27 No 531486				you need more heat
						Heated at 250*f  bubled at other end just like he beleaves its supposed to yet, after 1.5 hrs he got 1g nice angelic FB cristals from tube & top of flask ,tryed crash'n the np in freezer 2 find nothing. This from 5.5g fb.  there's still alot in the bottom of spd flask. looks kinda yellow but might still bee holding.heat it to minimum of 325 degrees F. SWIM has a new setup that works better , excuse the hasty sketch.
		geezmeister (Of Counsel) 09-15-04 17:42 No 531488				naptha note
						freebase pseudo is soluble in room temperature naptha. It is simply MORE soluble in hot naptha. Even very cold, the naptha will hold some dissolved pseudol fb... as a titration of the naptha after collection of the fb crystals in the STB method often showed. Use too much naptha for the amount of pseudo, and you won't get a thing by freezing it. The fb pseduo will simply remain in solution.  You can evaporate the naptha down (slowly-- don't boil it off, that is far too dangerous in any event) and at about half the original volume freeze it again. You may get crystals to crash out at that volume. I used to reduce the volume of the naptha after harvesting fb crystals with a STB method, then freeze again, and always got more crystals. Don't discard the naptha, though, until you titrate it for the remaining pseudo. I saved this up in a "corners" jar, where I tossed odd lot ends of pseudo from various extractions. Over time you get a healthy amount of pseudo that needs a good a/b cleaning at least... but its like having free pseudo... otherwise you tend to toss the dirty end lots of pseudo because they don't amount to enough to clean further... this way, you wind up with a pile you would have tossed if you hadn't started saving the little piles. Comes in handy when cash is low or you can't get pills. mostly harmless
		evilscripter69 (Hive Bee) 09-16-04 17:25 No 531640				Beware of carryover
						SWIM's had gakk come over  with higher temperatures and /or faster air flow, beware of this.,
		evilscripter69 (Hive Bee) 09-20-04 21:54 No 532378				Modification
						Jacked is definitely right about FB reactions, UTFSE for info on starting it off,For the hot and fast method SWIM mixes red with FB pseudo, places in flask, which is in turn placed in freezer, Iodine weighed out and placed in freezer,ICE water bath is prepared. flask and iodine removed from freezer, flask placed in the ice bath. Iodine added -flask quickly sealed, A 3 cc syringe with DH2O is insereted in tubing, Remove flask from ice and slowly warm contents with palm of hand. Once the glass is not so cold to the touch inject a small amount of water, adding it a few drops at a time DONT OVER DO IT HERE.WHAN WATER CONTACTS INGREDIENTS A NEARLY SPONTANEOUS REACTION OCCURS, KEEP IN ICE BATH UNTIL RX CALMS DOWN SOME.  THEN EXTERNAL HEATING WILL CONTINUE THE RX. the second illustration shows a better appoach. most of the Pseudo FB falls out in tube, vacuum is used to pull instead of push , the fb melts quicker, and airflow is increased, moving fb over much quicker, a solvent trap is required still, evap solvent to get Fb pseudo, this cuts off several steps, one more thing....  SWIM's had 85% yeilds lately, USING TOLUENE FOR THE np IN THE FINAL WORKUP, IT DOESNT TEND TO FORM EMULSIONS AND LYE WILL NOT STAY IN IT. To Those unable to find glass, you can replace the horizontal 2 inch pipe with another material and use a shoter/ smaller diameter  glass tube from the end of horizontal tube into the solvent flask
		geezmeister (Of Counsel) 09-21-04 02:35 No 532417				use more water
						If you just use more water you won't have to jump through all those hoops to do a fb reaction, it won't run away from you, and you still get the great yields. Water does wonders to slow the exothermia of the fb to pseudo HI reaction. It also keeps the rP/I2 from firing off too fast. Water is a great addition to the reaction. It helps limit by products, helps control the reaction... its your friend. I've done it the way you describe. I've also ridden to town on a mule, but I'd rather drive a truck with an air conditioner running. Its easier. And it works as well. mostly harmless
		abominator (Hive Bee) 09-21-04 12:24 No 532487				Good post from Jacked on FB
						Post 229882 (Jacked: "Re: reacting freebase pfed", Stimulants)  Here is a great post by Jacked concerning the FB h/pull rxn.  ES69 gave a great description too.  Swim supposes that copper could bee used for the SPD as well?  Is this correct? 69
		evilscripter69 (Hive Bee) 09-21-04 21:00 No 532565				copper should work fine
						thanks for bringing that up Gluey, Glass tubing of large sizes are not easy to find in some places, disadvantages are not being able to see the crystal flow in pipe, if u tune the vacuum to where the floating crystals are falling out in pipe, you wont have much to reclaim from the solvent trap, allowing much smaller amounts of solvent to be used in the collection flask, last run SWIM did 85% of FB came out of the pipe, dry and ready to go. BE SURE TO SLOWLY RAISE TEMPERATURE JUST TO THE POINT THE FB MELTS, ADJUST AIRFLOW AT VACUUM SOURCE AND LET IT RUN
		refukendiculous (Stranger) 09-21-04 23:42 No 532590				freebase
						using the TT/SPD with 7 boxes of 20 120s(5 generic and 2brand name) collecting in room temp naptha got 11gms of freebase back, using VEs wet start to get it going, ran it just like any normal LWR right at 28 hrs( the post reaction fluid before boiling was real milky so wasnt sure i didnt get gakked)but after around 10 minutes of light boiling it cleared up and looked better than i have seen in a while...anyway the end results were about 7gms. for what its worth i like the TT/SPD to FB via VE and LWR 24 or more. thanks again GEEZ!
		evilscripter69 09-28-04 07:09				Fine line in temperature (Rated as: ALL CAPS)
		geezmeister (Of Counsel) 09-28-04 16:46 No 533584				temperature is critical to purity
						Do not forget that this is a form of distillation. Temperature is critical to purity. You only want what comes over when pseudo vaporizes. Going very much above that temperature will bring you to the temperature at which gakks in the mix may vaporize. You do not have a big flask of fluid here, you do not have a large volume to buffer the rise in temperature, you do not have a volume that will absorb all the heat energy coming in vaporizing one substance at a time. Slow down, get the temp when the pseudo starts vaporizing, leave it there and give it time. mostly harmless
		evilscripter69 (Hive Bee) 10-01-04 12:57 No 534025				water will not work in collection flask
						SWIM tried using water in the collection flask, did not work well.  was a test of someones idea.  pictures of the setup have been taken, will post later after editing out certain background details.
		evilscripter69 (Hive Bee) 10-09-04 17:46 No 535057				80% returns freebase extractions
						try this out, works very well. tetra trap procedure utilizing NH3 in place of water,it also works  works without the TCE using only the sodium carbonate.However a few squirts of tce helps to keep the pillmass fluid.here is a brief description on method, pills are ground up to fine powder with the sodium carbonate(works on 120's,red 30's and the 60's with chlorphen and or tripolidine,cover pill mass with at least an inch of NP xylene/toluene are the best. slowly mix in NH3 , a spray bottle works well, do this slowly while stirring until the pill mass is flowable don't overdo it or you will suffer a big yeild loss heat slowly until it starts a gentle boil, pour and filter and then repeat the NP boil with a smaller amount of the NP, this seems to get the rest of the  FB out, dry in front of a box fan or whatever method you prefer.so far the yeilds have been at least 80% then do a SPD to degakk the FB
		refukendiculous (Stranger) 10-14-04 01:35 No 535731				peice of glass for SPD
						it just dawned on me after re-reading your post, if your having hard time finding a glass tube, go to your local music store in the guitar department and look at the slides...they should have various sizes
		evilscripter69 (Hive Bee) 10-14-04 09:26 No 535794				dont try this
						SWIM did away with the pushpull tanks, now is using condensor and balloon, after a reaction there were some of those square crystals ( sorry forgot the name of them ) typical from a reaction that got a little dry, some gas remained in balloon, took a razorblade to it to release the gas, it wanst very much about 5" in diamter, damned it a big flame shot over SWIMS head with big puff of smoke ! Obviously this stuff spontaneously combusts upon exposure to air. Just another reminder to always wear safety glasses in the lab
		Scottydog (Hive Addict) 10-14-04 09:54 No 535800				Phosphine
						"Obviously this stuff spontaneously combusts upon exposure to air." Was there a firecracker pop just before you saw the flame? Any difficulty getting the flame extinguished? The squarish crystals are PI3 (phosphorous triiodide) and the gas producing the flame was PH3 (phosphine) SWIM had a run-in with the deadly gas as well... Post 454750 (Scottydog: "Reply and question?", Stimulants) Refuse/Resist
		Rhodium (Chief Bee) 10-14-04 13:37 No 535811				The crystals are PH4I (PH3·HI) and not PI3...
						The crystals are PH4I (PH3·HI) - see Post 494033 (Rhodium: "The condenser crystals are PH4I, not PI3!", Stimulants) The Hive - Clandestine Chemists Without Borders
		geezmeister (Of Counsel) 10-14-04 14:10 No 535813				overheating as well
						You will have this happen more often at higher temperatures than lower ones, and in drier reactions than in wetter ones. The experience was not uncommon working with concentrated hypophosphorous acid if the temperature was increased above 120C. I have not seen it in reactions using dilute hypophosphorous acid. mostly harmless
		Radiumhero 10-14-04 14:47				herb extraction ? (Rated as: UTFSE!)
		evilscripter69 (Hive Bee) 10-14-04 15:12 No 535823				scottydog...
						no fire, it was just a firecracker pop and a flame shot out along with a nice amount of smoke which rolled around the lab ceiling. Altogther the experiment was a success, the cook was intentionally hot and dry. SWIM had another gakked batch(still finetuning the SPD apparatus) and instead of flushing the contaminated dope,and since SWIM had a nice amount of lab grade red, porceeded to re react it. Hoping that vigorous cook might burn out the gakk. Ratios were 7 g tainted meth, 10 g iodine from tincture, and 7 grams second run red phosphorous. results were quite astounding !! the reaction fluid was the clearest seen in many months, totally clear like river water, the basing went real  well without any emulsions or layers, or colors, only white and clear fluids, pulled with toluene, gassed, then recrystallized per warlocks dual solvent method, have not weighed it yet but looks to be at least 5 grams, bioassay currently under way, smoke test went well, IV test next, SWIM would recommend any bee with a gakked batch to try this if precursors arent an issue. SWIM thinks the hard cook helped burn off the gakk. The excess red was to accomodate the gakks tendancy to kill the red during the RX. note..  SWIM will slowly release the gas if this occurrs again.
		geezmeister (Of Counsel) 10-14-04 16:26 No 535830				increasing the heat
						I think you might find that increasing the temperature over the length of a wet reflux has much the same effect... without the bang at the end... mostly harmless
		evilscripter69 (Hive Bee) 10-18-04 11:57 No 536341				Radiumhero .. ..
						ephedra has become ashard to find as ungakked pseudo pills are in SWIM's area. Yes it definitely would be worth the efort if u had some.
		evilscripter69 (Hive Bee) 10-18-04 12:23 No 536342				the latest modification..
						use cold naptha in the collection flask. it can be filtered offright after the SPD is finished, the FB  does not dissolve in the naptha providing its cooled down enough on its trip down the tube. encase the horizontal pipe with dry ice, use an aluminum flex duct or a pvc pipe sectioned into halves and fill with dry ice, this worked very well. eliminating the evaporation of the NP from the collection flask, and greatly shortened the time of the process, SWIM's last run took about 1 1/2 hours to process 29 grams. at a temperature of 300 deg F  in a 1 1/2 inch oil bath.
		evilscripter69 (Hive Bee) 11-04-04 20:44 No 539700				modification to SPD
						if using dry ice do not place the ice into the tube until everything is running up to temperature, or you will have condensation problems the cooling of the glass tube allows the  FB to condense before it hits collection flask, use of cool naptha keeps the FB in a solid phase, and makes it real easy tofilter and dry as a final step,elimination of a last solvent evap cuts down time greatly, also you can speed up the process a lot by increasing the vacuum. SWIM has had the cycle complete in under 30 minutes. but be careful not to overdo the airflow too much as it PULLED GAKK Last run SWIM did.
		geezmeister (Of Counsel) 11-04-04 20:53 No 539701				patience pays
						One mantra to keep in mind here --- patience pays. mostly harmless

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