Author Topic: Success on generic 120's  (Read 3707 times)

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evilscripter69

  • Guest
Success on generic 120's
« on: July 30, 2004, 10:11:00 PM »
Had this dream last night.. yeild was 7 grams, rx was excellent.
6 boxes 20count 120's with PS80 and definitely the orange gakk, yellow oil was also present(saw it sink to bottom of sep funnel)
extracted with 3 pints 99% IPA Pills were dumped in flask unshelled and unground., 4 boils were done to them. pillmass gummed up a little, but shaking it put it back into circulation.
Extraction fluid was evaporated to 50%  starting volume.
then 20 grams KCL nuggets were added(dont know if this helped, SWIM's using a mix of KOH and NaOH figured it wouldnt hurt)then added mixture of KOH/NaOH to mixture slowly(weight measurements were not taken, last time SWIM used a premeasured amount the pfed yellowed and burned)when a solid white color was attained,boiling was incrasing w/out more heat, these signs SWIM was looking for. Heat was increased until a steady boiling was going on, condensor attached and left for a time.
The flask was refluxed for 1 hour, during this time a cloud of cottage cheese precipitate started coming out. Mix was filtered while hot through 2 coffee filters. remaining residue in filters washed with small portion IPA. Extraction fluid was evaporated down with low heat and fan until thick and creamy. this was mixed into 1 litre of xylene and placed into a 2000 cc seporatory funnel. THIS NEXT STEP SEEMS TO BE VERY IMPORTANT 3 water washes of 500 cc DH20 were done. entire volume was shaken with the water wash and allowed to separate( this took some time) but behold the YELLOW OIL fell to the bottom. above it was the green layer (PS80?)Xylene also turned a green color. By third wash water was clear, titrated to get the Hcl salt(gassing might have been faster here)but SWIM did'nt have it set up. one light acetone boil was done on the pfed to finish(geesmiesters microwave precip would have been done if it wasnt for SWIM's impatience at spending 2 nights having gakk failures)Microwave precipitation

Post 432344 (missing)

(geezmeister: "pseudo precipitation technique", Stimulants)
of pfed is a stroke of genius geez.
 SWIM will post a unique ghetto microwave/vacuum driven fume hood setup. all flammable and noxius fumes pumped right into sewer mainline.Fire and explosion risks are greatly reduced !  Only smells are when working on it outside of the microwave. SMIM doesnt know how he ever got by without a vacuum pump, highly recommend every bee acquire one :)

Prepuce

  • Guest
Sounds like nice work.
« Reply #1 on: July 30, 2004, 10:34:00 PM »
This sounds pretty good, ES, but SWIP has a couple of questions. First, why do you use KOH? Would NaOH alone be as effective? SWIP knows that some cleaning products contain KOH, but is not aware that the pure chemical is available OTC. Is it?

Polysorbate 80 is a yellow to slightly brownish liquid, but after an hour in that brew who knows.

SWIM will be very interested to see the design of the microwave exhaust system. He freaked thinking about all of the exposed switches inside the case of most microwaves and quit using it to heat volatiles. At one time he tried installing a vent hose made of the strong, braided stuff they sell at the hardware store, but it melted right down when zapped so the project was scrapped.

PP

evilscripter69

  • Guest
taking pictures of it now
« Reply #2 on: July 30, 2004, 10:52:00 PM »
Tried NaOH several times without success, looks like oversaturating mix with KCL first might have corrected that problem, as to KOH, theres a certain drain opener with a 50/50 mix of KOH and NaOH, SWIM underwent many chemical irritations evapping that shit in Microwave, took several hours at full temp, then working it before it solidifies was tricky. In addition it has a tendancy to suck water out of the air and become watery again,
More tests on NaOH will be done as its more easily found
back in a bit with some pics( will have to edit some parts of course, like backgrounds )
SWIM's going to be up all night as bioassy of rx was very good.

evilscripter69

  • Guest
camras charger missing
« Reply #3 on: July 31, 2004, 12:24:00 AM »
here's design

Post 522890

(evilscripter69: "GHETTO  microwave/fume hood", Chemicals & Equipment)

pics up later. it works damn well!!