Author Topic: Best extraction method. well tested  (Read 19494 times)

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geezmeister

  • Guest
naptha note
« Reply #20 on: September 15, 2004, 07:42:00 PM »
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.


evilscripter69

  • Guest
Beware of carryover
« Reply #21 on: September 16, 2004, 07:25:00 PM »
SWIM's had gakk come over  with higher temperatures and /or faster air flow, beware of this.,

evilscripter69

  • Guest
Modification
« Reply #22 on: September 20, 2004, 02:54:00 PM »
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

  • Guest
use more water
« Reply #23 on: September 20, 2004, 07:35:00 PM »
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.


abominator

  • Guest
Good post from Jacked on FB
« Reply #24 on: September 21, 2004, 05:24:00 AM »

Post 229882 (missing)

(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?


evilscripter69

  • Guest
copper should work fine
« Reply #25 on: September 21, 2004, 02:00:00 PM »
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

  • Guest
freebase
« Reply #26 on: September 21, 2004, 04:42:00 PM »
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! 8)

evilscripter69

  • Guest
Fine line in temperature
« Reply #27 on: September 28, 2004, 09:09:00 AM »

geezmeister

  • Guest
temperature is critical to purity
« Reply #28 on: September 28, 2004, 06:46:00 PM »
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.


evilscripter69

  • Guest
water will not work in collection flask
« Reply #29 on: October 01, 2004, 02:57:00 PM »
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

  • Guest
80% returns freebase extractions
« Reply #30 on: October 09, 2004, 07:46:00 PM »
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

  • Guest
peice of glass for SPD
« Reply #31 on: October 14, 2004, 03:35:00 AM »
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

  • Guest
dont try this
« Reply #32 on: October 14, 2004, 11:26:00 AM »
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 :o  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

  • Guest
Phosphine
« Reply #33 on: October 14, 2004, 11:54:00 AM »
"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 (missing)

(Scottydog: "Reply and question?", Stimulants)



Rhodium

  • Guest
The crystals are PH4I (PH3·HI) and not PI3...
« Reply #34 on: October 14, 2004, 03:37:00 PM »
The crystals are PH4I (PH3·HI) - see

Post 494033

(Rhodium: "The condenser crystals are PH4I, not PI3!", Stimulants)



geezmeister

  • Guest
overheating as well
« Reply #35 on: October 14, 2004, 04:10:00 PM »
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.


Radiumhero

  • Guest
herb extraction ?
« Reply #36 on: October 14, 2004, 04:47:00 PM »

evilscripter69

  • Guest
scottydog...
« Reply #37 on: October 14, 2004, 05:12:00 PM »
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.
;D 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. :o

geezmeister

  • Guest
increasing the heat
« Reply #38 on: October 14, 2004, 06:26:00 PM »
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...  :)


evilscripter69

  • Guest
Radiumhero .. ..
« Reply #39 on: October 18, 2004, 01:57:00 PM »
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.