05-08-04 05:58
No 505783
24 h ago swim starts his first lwr dream , after 4 month of reading....
it starts with 1:1,2:0,5:0,8 (e:LGI:LGRP:dH20). First mixed e+rp+dh20, then fixed a 40cm west-condenser on his 250 rbf. then let fall 4 portions of iodine through the condenser. magnetic stirbar mixed it well a litte white smoke was visible. after a few moments the flask was clear again and the ballon become little inflated.
then turned heat on till 98° C inside the flask was reached. little bubbles are visible and a nice slow reflux
(2 drops/min.) is going on. everything o.k. so far.
after 12 hours of refluxing first HI cryst. appears in the condenser. after 20 hours the ammount of HI cryst. is very high, so swin decided the wash this crystals down with 1ml of dh20. after this, a thin fog appears. this fog "circulates" in the flask, falls out of the condenser,
goes up and down..., ballon is unchanged.
Here comes the point where swin needed some advice:
now (after 24h)there is a very low rate of bubbling avtivity and refluxing (1 drop/minute).
swim plans to go for 48 hours, but what should he do now???
add a additional gram of iodine and some water? or better do nothing ?
there is no change of volume visible and the size of the bubbles is unchanged.
what is a shure sign, that the reaction is done?
thx
wer einmal leckt, der weiß wie`s schmeckt
(Stoni's sexual toy)
05-08-04 08:29
No 505798
You told us the ratio of the reaction, that you use a 250ml flask and that you added 1ml of water at some point. What you didn't tell us is how much pfed you used. So how can you expect a useful answer?
> what is a shure sign, that the reaction is done?
There is none. Just crank up the heat a little more if you want.
BUSH/CHENEY 2004! After all, it ain't my country!
www.american-buddha.com/addict.war.1.htm
(Hive Bee)
05-08-04 08:40
No 505800
add a additional gram of iodine and some water? or better do nothing ?
Is it really necessary to add I22, water etc. late in the reaction? Don't you get a hugh sky of HI fume out in the head when you open your condenser?
(Hive Addict)
05-08-04 09:13
No 505807
> what is a shure sign, that the reaction is done?
The 48hr mark is your sign!
Too simple isn't it?
Don't figgit with it.
The HI xtals forming and being washed back down is fine....just avoid adding too much dh2o once the rxn is progressing!
Os: there is no useful answer needed based on ratio.
E=1
I2=1.2
LGRP=.05
DH2O=.08
a little less conversation, a little more reaction
(Stranger)
05-08-04 09:58
No 505817
hi folks !
thx for answers! now 30 hours are left and swim wasn`t able too wait longer. never was so horny before :)
yes, maybe too early, yes maybe swim killed the reaction with too much water, but read on:
after filtering, np washing, basing.... THIS GOLDEN OIL appears, like fat om a soup, more and more, till a complete layer ist there. never before swim has seen something more beauty.
o.k. time to cool down, doing my further work. write later more
thx thx, hive rulz
wer einmal leckt, der weiß wie`s schmeckt
(Hive Addict)
05-08-04 10:26
No 505824
Next time....You'll need one of these in order to help in the patience dept.
Hope it AWE comes out okiedopie!
a little less conversation, a little more reaction
(Stranger)
05-08-04 14:01
No 505856
i try this till the pyrex dish stands on the warming tray
wer einmal leckt, der weiß wie`s schmeckt
(Hive Addict)
05-08-04 14:08
No 505857
Sounds like you're setup for success. If you're not sure, do what Os says and turn up the heat a little. SWIF usually does that anyway towards the end.
If you're able, I suggest steam distillation for increased yields and better purity.
(Stranger)
05-08-04 22:08
No 505926
what a day. sittin here since 6 hours and look inside this pyrex dish. the volume of water sinks and the certainty that swim received nothing increase in the same rate....
then god hat compassion and show swim that lynard skyn...
at the edge of this - i can´t trust my eyes - crystals appear, clear like water or glass.
it must be a dream
wer einmal leckt, der weiß wie`s schmeckt
(Stranger)
05-09-04 13:39
No 506048
back on this
the stuff is complete dry now. weight is 6,1 g. swim starts with 8,3 g sparkling needles of pfed.
this meens a yield of 75%. think, this is too good to be true. can someone tell me the avarage yield of an lwr?
made three titrations, first at 8,5 second at 7,5 and third at 6,5.
o.k. anyway. next day swim re-x the whole shebang and we will see more. but the stuff is real meth, snorted a nano line and it kicked my damned newbeeash like nothing before.
forgot to give a thx to geez, placebo, worlock, videoeditor
wer einmal leckt, der weiß wie`s schmeckt
(Hive Addict)
05-09-04 14:04
No 506055
Had the whole 48hr or at the very very least 36hr been employed....That 75% could have easily been bumped up a few notches. Even with less than topskilled work-up techniques!
You think I shytin ya!
Yeah well...GO's with the territory so I'm use to it!
a little less conversation, a little more reaction
(Of Counsel)
05-10-04 09:04
No 506233
Congratulations Dextro, and welcome to the club. The reaction itself is amazingly simple, isn't it? I will chime in with Ware that a little more improvement in yield can be had by the full forty eight hour reflux, but the increase comes at a decreasing rate over time. The improvement in subjective quality of the product is hard to discern, as the product at thirty to thirty six hours is hard to tell from the product of a forty-eight hour cook, at least by bioassay. Both should be excellent. There are times the longer cook time produces a product that is sufficiently different that even without knowing which bag contains the product of the longer reaction, friends will consistently pick the same batch as "better." Most of the time, this is the bag that is from the longer refluxed batch. The inverse of this phenomenon can be seen when the product is tested by tweakers who "...like a little trash in their dope." Most of these folks prefer the product of a shorter cook time.
mostly harmless
(Stranger)
05-10-04 14:58
No 506297
today swip made an analysis with an polarimeter:
measured optical turning is + 0,2° (with 1g in 100ml dissolved)
the meaning of this is: 0,2
_____ = +20°
0,01 (1g/100ml=0,01/ml)
this + 20° is the specific turning angle.
exact this angle stands in the merck index for meth, likewise. ergo > this should not be racemic.
another bee told me RP/I yields always racemic meth cause
the reaction conditions are too DRASTIC. don`t know what drastic means in this case, but my result is another.
edit: write this whole stronzo di merde with my fucking school dictonary, so please be so kind and imagine you are
talking with an horse. (would translate wareamis latest post, but failed)
wer einmal leckt, der weiß wie`s schmeckt
(Hive Addict)
05-10-04 15:15
No 506303
RP/I method for production of meth via pseudoephedrine or ephedrine does not yield racemic meth.
05-10-04 15:36
(Rated as: insignificant)
(Hive Addict)
05-10-04 17:21
No 506329
Don't hertz yerself there Dex
No need to translate what ware said as Geez so eloquently chimed in to reiterate my point exactly.
Like fierceness points out, The HI/RP reduction of eph/pseu-eph yields d-meth not 50%-d 50%-l meth(racemic).
a little less conversation, a little more reaction
(Stranger)
06-15-04 03:23
No 513526
back again :)
swip did another lwr, the 48 hour mark is gone, but there is still activity with small bubbles and the balloon is still inflated, temp inside flask is 98° C.
is the rxn complete despite this signs?
should he wait longer (till what happens?) or is this not necessary ?
thx again
wer einmal leckt, der weiß wie`s schmeckt
(Hive Bee)
06-15-04 03:42
No 513529
congradulations Dex and thanks for caring about civil liberties.
I suggest you read Post 428410 (geezmeister: "The post-reaction workup: a cook's summary", Stimulants)
and Post 505807 (wareami: "48hr mark....", Stimulants).
Wareami answered this for you last time through and the
Geez is phenominal from what I've read here.
Geez know's the facts and has taken the time to express
them in a way that is understandable, efficient
and thorough.
Your results, if this post is followed accurately, should
be optimized and of high quality.
Congradulations again and I am sure you will post results.
og
(Stranger)
06-15-04 05:01
No 513537
yes, swim read geez writeup again and again (are you finished)..... but:
there IS small bubbling activity/reflux and when he add dh20 (to see how fast the red falls down) he will kill the rxn :(
is this fucking ballon no indicator? swim means the ballon must be empty at the end of rxn, cause there is no further HI production??
small bubbles=HI production o.k., the quetion is: when all the pfed is reduced to meth, is there further HI production or not? he will not cook this stuff much longer then 48 h, cause he didn`t know, when this small bubbles disappear.
P.S. swim can`t stick his nose is the flask to surch "the smell" cause there are lots of HI fumes
(Hive Bee)
06-15-04 05:40
No 513542
Dextro, my friend, it's finished! Work it UP! The bubbles, the baloon, blaa blaa, it doesn't matter! If you have cooked clean pseudo for 48hrs with clean RP and useable I2, (with enough water of course..) then that's it!
(Of Counsel)
06-15-04 06:57
No 513558
I'd call it done. If its not done by now, something is seriously wrong, and its something that more time isn't going to fix.
Then again, I don't know your feedstock source or whether you have any of the new polymers in it. It is possible that you are having some problems associated with polymers, and if that is the case, your product may benefit from increasing the heat another notch or two for another four or five hours.
You are well past the point where byproduct formation should be a problem, and you have reduced anything you are going to reduce at that temperature. If you have some of the new reaction inhibitors stalling completion one thing you can do to degrade them is to apply more heat. I know this is contrary to what I have preached in the past, but in the smaller reactions I have been forced to run of late the gakks have succumbed to the application of more heat in the last part of the reaction.
I still adhere to starting with a gradual increase to temperatures and a wet start. I still think the reflux needs to be done under 120C; I just have the sneaky feeling that the new inhibitors may degrade slowly under these conditions and increasing the temps significantly after the bulk of the reduction should have been accomplished may be a final assault on the inhibitors that overcomes them. Increasing the temperature after the reaction has progressed for a good period of time may break the remaining gakks down and let the reduction complete.
I can't say that I've done this enough to verify results, but the last few small batches I've done I have raised the temp significantly several hours into the reaction, and the product has been far closer to the standards I seek than it has been without the temperature increase. After forty-eight hours, I don't think you are going to hurt the meth by cranking the heat up some, and you shouldn't be making tweaker dope dope since you should be past the stage where you make those by-products. Its speculation, but it seems to work in the few trials I have done. Placebo may be more correct than ever on this point since the introduction of the new gakks.
My best guess is that your reaction is done at the 48 hour mark. If you have serious questions about whether it is, why not take the temp up another twenty to twenty five degrees C for another four hours? I'd pull a sample now and work it up, then compare that with what you get four hours later. Your results might tell all of us something about the effect of heat at this stage of the reaction.
mostly harmless
(Stranger)
06-15-04 07:43
No 513565
thx for help !
last question about these HI crsystals in the condenser:
till rxn is running, swim washed them down with a few drops of dh20. a few hours they appear again, again washed down.... now, at the end of rxn, they are again in the condenser.
should swim wash them down again direkt before workup or better let them stay in the condenser ?
what is this stuff in detail?
thx, for help
(Hive Bee)
06-16-04 04:05
No 513771
Look at Post 494033 (Rhodium: "The condenser crystals are PH4I, not PI3!", Stimulants)
Let the reaction cool and settle. Rinse them down with dH2O. Work up; you're on the home straight!