Author Topic: New Straight to E -- a novel extraction tech.  (Read 58347 times)

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CainTwister

  • Guest
In Koledge...
« Reply #100 on: June 28, 2003, 05:45:00 PM »
..our professors always told us to keep a notebook handy to snuff fires in glass containers with. Never had to do it, personally.

platcat

  • Guest
reruns successfull!
« Reply #101 on: June 29, 2003, 01:57:00 PM »
Well for what its worth swip worked up his rerun ,recycled pfed and recovered 60%(M) so far and more to come tomorrow.nicest rxn he has seen in a few.no signs of unreacted I2,no piss yellow post rxn fluid,and definate CNS activity on bio assay.proper amount of RP was missing and swip is a happy camper.
 swip will do the STE over on stock that has had a good dusting and overnight soak in xylene with a TCE quick dip on the dried pfed after the STE.
 Swips previous failure seems to have been an incomplete rxn.only 2/3rds of the nessessary rp was missing so he assumes (1)it was tired, or (2)povidone stopped it, or (3)MissCats refusal to do the obligatory titty dance w/incantations, or (4) all of the above.Alls well that ends well,PC out.


geezmeister

  • Guest
"Straight to E" extraction: Yield report
« Reply #102 on: July 03, 2003, 01:04:00 AM »
I can't believe no one is posting reports about the yield of meth from pseudo extracted by this technique.

Remember the 9.6 gm of pseudo HCl SWIG got on his first attempt of the procedure, the one from Scottydog's favorite drug store white sixties? That 98% yield?

Added that and 5 grams of fairy fresh red phos, 11 gm of I2, 10 ml dH20, put in the oil bath with the condenser running  and a balloon on the top....brought it up to temp and got the reflux going well...and left it for 48 hours.

SWIG's first incursion into the lab in five weeks was fraught with discoveries, like how light a one gallon can of xylene is and how empty that full gallon can of acetone is, and how naptha can just disappear into thin air without anyone knowing what the fuck is going on...I don't mind if the alchemist's assistant uses the equipment, but I hate like hell to find out I don't have supplies on hand and wind up at Wallyworld at two in the morning.

Rant over.

Very good smell, and the honey was very very pale whitish, maybe just a suggestion of yellow.  Washed once with xylene then three times with TCE and once with hot naptha. The hot naptha was clean.  I used boiling naptha to extract the goods two times, as that was all the naptha left in that new gallon...(grrrrr....where's that shotgun?) Did the third pull with the last of the xylene.

I started adding 20% NaOH solution and my suspicions were confirmed. Bubbles fizzed outta that fluid like from an only-left-open-since-this-morning soda--which is a good sign in  this situation. The fluid based so quickly with so little NaOH solution it surprised me. I take that as a good sign.

(I forgot to mention that I had no emulsion, had a mirror-like interface, and had more bubbles fizz up when I added  salt to the fluid.)  For the fun of it (okay, odd sense of humor here) and to see whether there was any emulsion potential about, I shook the sep funnel with the fluid and xylene the same way I would shake the xylene and aquous HCl later-- I used the the same stomp dance and the regular chant. SWIG does not recommend this to anyone, mind you. This is asking for emulsion hell and tempting the meth gods. He put the funnel in the ring stand and that mirror interface was right there, ready to shave by. No emulsion at all. The reaction fluid fell right to the bottom.

Okay,Okay...SWIG will cut to the chase.

Net yield: 7 grams of meth HCL, very nice sparkly white, not recrystalized due to the late hour and work today. This re-rocks right now, has legs from here to Georgia, leaves almost no residue on glass unless incinerated. Nice! Has no taste.

The last puff SWIG had was two o'clock this morning, or sixteen hours ago. You might guess at the quality.  ;D

I figure that 7.8 or 7.9 grams of meth HCl from 9.6 grams of pseudo HCl would be a 100% reduction, so seven grams is a good number. I might expect that from a freebase reaction, maybe, but I didn't expect it from a HCl reaction. (To nettle the chemists, thats about a 72% yield by weight of the precursor or about eighty eight percent of the pseudo if its all meth-- and I haven't found anything else in it yet... ;D  (Okay, okay...about a 67% molar yield. Sorry.)

OF COURSE the next question will be whether the yield is the product of the longer reflux, or the extraction technique.

Hey Scottydog! Grab them while you can!

That seven grams of final product is from four boxes of white sixties...twenty five bucks worth of OTC pills.

You hear that Payin2Much?

Well, gotta go now. Think I may take up cross country for the fun of it...even if it is July  ;D


VideoEditor: I believe!


VideoEditor

  • Guest
just to add...
« Reply #103 on: July 03, 2003, 02:19:00 AM »
Thanks Geez and to all that have contributed to this thread.  I would like to add one more observation after getting feedback from many bees.  So far 99% of all STE failures have been due to water. If your having snot or gak appear your still wet.  Dont be afraid to up the quantity on the drying agents and/or let it sit longer if your having problems.  Also remember the psuedo will crash out around 85C but keep boiling to 105C, its an important cleaning step. Please Please Please use your head when boiling flammable liquids. Always bee prepared and if your scaling up do several batches. Ignition of 1000ml of flammable solvent will engulf a small room faster than you can reach for the extinguisher.

peace and bee safe -VE


dwarfer

  • Guest
A-firm
« Reply #104 on: July 03, 2003, 03:11:00 AM »
Marvin said if I didn't commend VE
on his clarity of communication,
above and beyond the technical procedural breakthrough
that the technique represents,
that he was going to

A: cut me off

B: get his own "screen name" and post his own rambles.

Both scenarios are unacceptable:
thus I raise my profile
to give kudos to Video Editor,
who well deserves them!

sincerely,
dwarfinger

==================================

PS: showing that even "wet dreams" can be screwed up,
 a friend of mine was so entranced
with the bubbles rising from the evaporating alcohol
in the hot naphtha,
lit from below by the red hot heater filament,
that he went to get his camera
and turned off the light to take a picture.

Deciding to get more "swirl" in the bubbles
from the stir bar, he cranked up the RPM,
and the nearly superheated alcohol in solution
suddenly came ALL out at once,
generating a vertical spout of pre-molasses-laden NP,
which cost nearly 50% on the yield side..  <duh>  ":<(

Moral: Don't mix chemistry with photography.
sub-moral:  when the alcohol is gone,
the temperature climb rate is amazingly fast,
so watch it!

sub-sub observation.  any WATER in the mix
goes away at 100C, so if it starts poppin',
you HAD some.  ":<)

PPS: Hope geeze isn't alone
when he crosses the dry, hot desert.
The horny toads might get 'em.. ;D



wareami

  • Guest
Thanx VE!
« Reply #105 on: July 03, 2003, 05:18:00 AM »

So far 99% of all STE failures have been due to water



Boy did you hit it on the head!
Ibee been tellin bees this for months!
Much appreciation from the bottom of Ibee's heart!
Keep it UP Bro!

Peace of the reaction

Have FUN-Bee SAFE



grokstar

  • Guest
Sulfate Crystallising Temperature
« Reply #106 on: July 04, 2003, 02:58:00 AM »
Evening Bees,

My how it pays to drop in every now and then.  LAst time here I marvelled at crystallising pfed HCl out into xylene.  Now faced with this seemingly universally approved method,  I have a couple of questions that folk may/ may not have experience/advice in answering.

Firstly -
The 85C crystallising out temperature for pfed HCl in xylene
-Trial and error will give me the answer but for sake of a heads up - can I expect the temp for pfed sulf to be lower or higher? ?

Secondly - SWIG was planning to do some tone boils after this procedure to kill chlorphen. 
Since not already mentioned,  is this necessary?  or does the MEK rinse have some magical properties to kill antihistamine?

Otherwise, VE`s STE brings the stealth SWIG needs. 
The Stress combined with a little meth psychosis makes the usual long soak/decant dry pre-prep unpleasurable.
(and one SWIG does not like to repeat all that often)

This takes at least a day of hot potato off the schedule.
WICKEDness.  And no crushing!!!  Hooray ! ! !


halfkast

  • Guest
Just a late thankyou
« Reply #107 on: July 04, 2003, 10:36:00 PM »
TY VideoEditor and geez for nicely written test results.

grokstar

  • Guest
On reflection - sulfates
« Reply #108 on: July 05, 2003, 06:36:00 AM »
OK - scuse my ignorance in the previous post. 
The temperature 85C is when the iso has mostly boiled off - 105 helps rid excess water.  And psuedo sulf is insoluble in np.


Glacial_Refluxer

  • Guest
A/B
« Reply #109 on: July 05, 2003, 08:41:00 AM »
Im not sure but swim believes those locking pill deturrent
patents only apply to pseudoepedrine hcl type pills/syrups.

Waterless a/b without all the solvent boils might bee all
you need for a full return, plus it gives you the freebase
or hcl


ici_rhi

  • Guest
FINALLY to Work
« Reply #110 on: July 06, 2003, 01:17:00 AM »
Well, SwiI_R is finally back at lab for too short a time, after a while away, but is very quickly embarking on an STE and subsequent NANO just for quick testing, hopefully the quality she is used to. Posted pillz bee4, using those with few inactives for this experiment,,,know how to deal with all, pov in 48 out of 96 only troublemaker. (4 mg antihist in both) Short rest then to work, doing each 48 ct. separately..TCE rinse on POV SUzE, so all nighter,only buddy is budlite..?? is?? washing soda need not be dried as far as she knows...used it to "lite" base not for drying agent bee4. Wants to please Swim several hours from now so wishes to know for sure bout said sodium carbonate....use as is, right?
Thanks in advance,


tpower9s2003

  • Guest
SWIT agrees STE seems to be the only reliable...
« Reply #111 on: July 06, 2003, 02:10:00 AM »
SWIT agrees STE seems to be the only reliable method. 1st try results were inspected visually then lost (SWIT being stupid dropped onto shag carpet accidently) though 2nd 47% yield and sufficient for his recent rxn3. Passes foil test.

SWIT thinks that 91%IPA (even with dry NAP) needs more drying agents NaCl and calc carb though SWIT is guessing VE def was using 99% or dry IPA. Not totally sure how much is sufficient but probly thinking 2-4x each as a little overkill insures DRY and a dualed coffee filter/funnel should pull any suspended solids. He didnt realize it wasnt dry until popper bubbles seen on boiling mostly in the first 2 pulls and sees this as primary reason to the 47% yield of cleaned PFED with 2nd run (both with 1 48x60 box). SWIT also adds TCE wash prior to 2nd with the orange gakked CPM whites and the fine sifted powder seemed preferable since whole pills didnt want to dissolve consistenly fine. The 1st result before losing did appear somehow gakked though the orange tint was out, but maybe it was just bc that H20 problem. SWIT isnt sure as to whether TCE would be better before, after, or both.


VideoEditor

  • Guest
yes dry it
« Reply #112 on: July 06, 2003, 04:19:00 AM »
If your using washing soda as a drying agent yes it should bee oven dried, using the same method as epsom salts. Yes if you can get 99% ISO use it.


chronic_cook

  • Guest
posting results here
« Reply #113 on: July 06, 2003, 05:07:00 AM »
same as before, great yield. Some pseudo goes thru the filter into the trashy under-filter-beaker, & he wants it but it's in there w/ that crap. Would cooling to room temp, release any gaks into my pseudo from the xylene?


ok SWIC did some research. His pseudo went thru because his filter was not fine enough. (SWIM used generic coffe filter 2x.) The xylene/naptha sol. must be hot for gakks/waxes to filter. quality filter paper disks help alot. (unless SWIY wants to wait an hour) filter flask/vacuum is recommended. But just his experience shows a fritted disk would immensely improve his yield. just for any bee on the STE trains info  8)

it's not how well you can sell a bad product, it's how easy a good product sells  ;)

ici_rhi

  • Guest
THANK YOU --VE!!!!
« Reply #114 on: July 06, 2003, 05:10:00 AM »
She thought so...thanks so!!!! Can one use the red bottle 99% ISO for the process?? It seems to boil so fast not real sure about that...Getting ready to go to dream land, so since the only thing prepared is dried epsoms and 91%, rhi will just add a tad more epsoms, if red ISO not acceptable for this purpose..She really wants to report on sweet dreams in a few hours.......
THANKS one and all...many successful dreams have been had but lately, lost so much pseudo cleaning the shit out of it am excited as, well excited, about STE..


autumn_lamb

  • Guest
yield report and the devil's playthings...
« Reply #115 on: July 06, 2003, 05:56:00 AM »
okay geezmeister, another yield report from the field after a setback (which presented itself in the form of water when she forgot to dry the acetone that she used to de-red her redhots).

she decided that she had had enough of the red-hot saga for awhile (even though they were not to blame) so she went with 2 boxes of 48ct. national brand white 60's and 2 boxes of 48ct. generic white 60's which included a bit more gaak than the name brand.

in her opinion, the beauty of VE's method is the pure simplicity of it, so she finds it perplexing (short of not having access to a required ingredient) that anyone would feel the need to deviate. thus, she has no deviation to report (but for that not pertaining to this subject matter) except for this:

she knew that the next month or so would find her short on time and with limited access to her work area. so she proceeded to make a large batch of the extraction solution (91% alc/ VP&M Naptha/ salt/ epsom phase) and stored it in an airtight container for later use. one of those "later"'s came and its storage proved handy indeed.

yield from the aforementioned 48ct 4 box extraction: 8.9gms of beautiful product. after several runs, she continues to be surprised (and delighted) by the quality and the yields because the simplicity of this method was so unexpected (despite the many sudden "i've always known this"'s).

so now she has all this time on her hands! what's this hogwash about "idle hands are the devil's playthings" anyway?

um, so VE, geez...can you come over and give my hands something to do? hee. 8)


ici_rhi

  • Guest
Hey autumn---
« Reply #116 on: July 06, 2003, 06:42:00 AM »
Question..since time and suddenly availability is a factor at this Ranch, did you combine the brands, with that success, with said STE?? Getting ready to go to work, and that would shorten time for sure..first STE and combining with other methods have gotten very dodgy to say the least...
?


autumn_lamb

  • Guest
did you combine the brands, with that success,
« Reply #117 on: July 06, 2003, 07:01:00 AM »
did you combine the brands, with that success, with said STE??...first STE and combining with other methods have gotten very dodgy to say the least...

oh sweetie, yes, she combined brands, but not methods. she says that if you'll try this method (VE's straight to e), 'dodgy' won't be one of the adjectives you'll use to describe it.  ;)


ici_rhi

  • Guest
THANKS - lamb
« Reply #118 on: July 06, 2003, 07:38:00 AM »
OH NO luv, will not at all combine methods..will use 2 brands white 60's together with our hero's STE and have results ASAP, saves bout 3 hours I imagine..was gonna do 2 separate STE's but with only a couple extra inactives in one brand, will save lots of time..
me, computer, and bud(lite) will be at work all nite, no lab rat partner currently so THANKS A BUNCH!!!
Later


autumn_lamb

  • Guest
ooops
« Reply #119 on: July 06, 2003, 07:38:00 PM »
okay, i understand what you meant now that i read your question in the light of day. i was very tired last night when i read your post. sorry.