Worlock (Tweaker God)
01-17-03 17:41
No 399065
      Super High Potentcy Push/Pull dope     

Refluxers Like to talk about Low heat, well, here is a cold shot!!

Make up your Push pull reaction. exactly the same as you always do,
Watch it bubble a little ,asnd make a white fog.
Tape on the  Stopper/Hose leading to the P/P tanks
or tape a large balloon/ condom to the mouth of the flask,
Place it in a warm area,
Come back in 4 days.
Add water, Filter, and  Finish ptocessong the Best GoGo you ever had.

Did someone write that no heating is needed
NO heat
The longer you wait the better it will bee.

Muuuuaaahahahahahahahahaha

No shit Bees that is all there bee to it
Please post your results or if you prefer anonymity then PM me or any Bee so it can bee posted  under the Nym of SWIM

My Hive Private Mail address is: Worlock

Worlockium
 
 
 
 
    alphacentauri
(Hive Bee)
01-17-03 18:15
No 399076
      Worlock, have a look at this: 250 ml rb distil     

Worlock, have a look at this:
250 ml rb distil flask charged with:
pfed + H3PO2 (1 cc every gram of pfed) + I2
quick shake, then I apply a baloon specially designed for collecting gases diameter 130mm capacity 1 lt (it's supposed not to break easily).
Then I leave this system aside for, say, a week?
Then usual a/b separation, washings, etc..usual procedure.
Will this work? If it does I've got all the necessary already at home. I lack only pfed. I need 4 more boxes to reach the classic 5 boxes batch, that is to say I have to visit 4 pharmacies, and tomorrow afternoon they are closed.
Next monday then. I'll post the result asa I've got it, that is to say, a couple of weeks. laugh
 
 
 
 
    zibarium
(The Abyss)
01-17-03 18:57
No 399091
      i don't understand how     

this could work...


but i like it.

any confirmations?


(hmmnn..its not april fool's day, either!)
 
 
 
 
    The_Animal
(Deranged)
01-17-03 19:11
No 399094
      zib, In answer to your question, here is my...     

zib,

In answer to your question, here is my theory

The reaction produces its own heat, when you do a normal p/p, you are just quickening the reactions speed. So in the absence of external heat the reaction will progress - but at a much slower rate.

.em evigrof doG yam neht emirc a si parc gnitsop fI
 
 
 
 
    zibarium
(The Abyss)
01-17-03 19:26
No 399098
      so, how long in a refrigorator?     

in dreams past, swiz seemed to need heat just to get the reactants homogenous.
but then, swiz didn't wait long to see if the reactants would have eventually become fluid.

good gosh.

why isn't this the way to go?


or is it?
 
 
 
 
    ZingoBingo
(Hive Bee)
01-17-03 19:34
No 399100
      Good to here from you, Wor . . .     

Place it in a warm area,
Come back in 4 days.


Where's a warm place to be found this time of year?  And if left in doors where air is heated via thermostat what about the temperature fluctuation between low/high heat that triggers the fau?  Is there a median temp +/- that seems to work best?  I take it the 96 hours is not Venution time . . . cool

ZB
 
 
 
 
    alphacentauri
(Hive Bee)
01-17-03 21:59
No 399135
      Re: Where's a warm place to be found this time     


Where's a warm place to be found this time of year? 



on the top of the kitchen furniture, where it's constantly warm, even when the stove is not lit. And then I've got an idea: some time ago I wanted to use a yogourt making thermostat as a constant low heat source for BOD5. Why not using it for the "cold" hypo reduction? In this way we should have constant 37C, and to reach the temperature it takes hours, so the increase of heat would be very slow, slower than anything else.

 
 
 
 
    TomGreen
(Hive Bee)
01-17-03 22:05
No 399137
      Re: in dreams past, swiz seemed to need heat...     


in dreams past, swiz seemed to need heat just to get the reactants homogenous



are you serious? i was under the impression that one wasnt supposed to add heat until the reactants had become a homogenous fluid.

 
 
 
 
    Scottydog
(Hive Addict)
01-17-03 22:52
No 399155
      From TFSE     

I remember this post from TFSE like it was yesterday. To think this was rated as misinforming?

Post 315874 (TWEEKAZOID: "Room temp reduction via HI", Stimulants)

Maybe it really wasn't?

Maybe his percentage of HI was off or unverifiable but the method?
___________
Refuse/Resist
 
 
 
 
    BenWiFFen
(Line Monitor)
01-17-03 23:06
No 399157
      After trying a 24 hour rxn..     

After trying a wet 24 hour rxn with a 40w light bulb for the heat source. The results were the same as a 12 hour reflux (simmer) The best results was placed in the freezer for 5 min then placed into a ice bath just damp. Then add a few mls of h20 and standard P/P rxn let it push and pull. Then add more h20   along with incresing heat and time for 12 to 14 hrs.

*#746o25625#
 
 
 
 
    Dexter
(Stranger)
01-17-03 23:37
No 399170
      is that you     

wow worlock is that you! can i have an autograph!
Swim made his first steps into tweaker world with your write up.
 
 
 
 
    zibarium
(The Abyss)
01-18-03 01:47
No 399226
      tom g.     

awhile back, all the rage was about not flooding the rxn...swiz leaned toward too dry...which seems to blend well w/ some heat.

also, marginal precursors could demand heat for action.

swiz was also in to pretending that mbrp was lgrp..such a rxn fantasy needs the heat.
1st attempt, otoh, was fb rxn...fired off w/ hand heat, even though all was iced down.
 
 
 
 
    epistemologicide
(Hive Bee)
01-18-03 01:55
No 399228
      wooow     

that means i can take my flask camping and do a dream in the woods!!!

ill sit on it to keep it warm like a goose

hailz and support worlok, there truly is no prize for second best, you are the mansmile

FEAR MY GEAR
i cook to save the planet!!
http://www.counterorder.com/nihilism.html
 
 
 
 
    Worlock
(Tweaker God)
01-18-03 03:48
No 399262
      Alphacenturi     

Alphacenturi a great handle
I'll have to check with some ex-purts on the reaction, to see if it might possibly run without heat.
A lot I am sure will depend upon the concentration of the hypophosphorous

Worlockium
 
 
 
 
    Worlock
(Tweaker God)
01-18-03 04:09
No 399267
      Zibarium     

It is all possible because instead of heat, there is concentration
6.5 - 7.0 molat is thick, with powerful chemicals,
Plus the reaction is  exothermic.

Now if it were outside in the snow, I doubt it will work till spring, but you never know ,

At 75 degrees it will go slowly
At 90 degrees, it won't take very long at all,

This is no April fools joke, this is only January
,
It can bee all watered down, and diluted to hell, then and boiled for seven days  or make it thick and wait 4 days,

Many doubted  it could be cooked in an hour, it was believed. it had to be refluxed for 2 days.

The best dope you ever made. If it does fail ( it won't ) what's to stop you from putting it over the flame, and finish with a rush.

Worlockium
 
 
 
 
    Daphuk_up
(Stranger)
01-18-03 04:10
No 399268
      more nooberish question     

Ok, so given this "have some patience you damn fiend!!" method, would it be possible to use a smaller amount of rp?  It seems that because of its catalytic nature in the reaction, that if one gave it more time and perhaps a touch of heat (warm lightbulb), the reaction should go to completion (at least all the I 2 will be converted to HI).  To be perfectly honest, SWID is god awful tired of cleaning mbrp, and is wondering if the reaction can be run with less.

Also, from what SWID has read, he has deduced the following steps:
1.  Mix pseudo, RP, and dH2O in vessel.
2.  Add I2.  (This where he is confused...wont adding the I2 slowly with the bottle open to atmosphere allow the HI gas to escape?  Surely the I2 is not dissolved in alc. or something.  Can the I2 be added all at once, and THEN patience be exercised, waiting 1-4 days for rxn completion?)
3.  Little or no heat is applied, the rxn vessel is set on a shelf and forgotten for a while.  (Does this have to be in classical reflux set-up?  For the more ghetto inclined, is a regular party balloon satisfactory?)
4.  Work-up as per usual.

SWID certainly appreciates every little bit of help he can get. laugh


Regal Sir Palladium and the Harlot Chlorine...they make such a cute couple. ^_^
 
 
 
 
    Worlock
(Tweaker God)
01-18-03 04:57
No 399276
      ZingoBingo     

Those are the same questions I have, beem wrestling with.
There are so many climate zones, radiators, central heating.
 A bathroom with a small electrix heater at 75 - 89 degrees is easy.
Withon a few feet of a radiator is vety warm
In some warmer climates , in a closet will wirk.
The unheated tool shed out back is not too giid.
Temperature fluctuation is no problem, how much fluctuation us there heating it by hand, turning the heating element up and down a lot,
Just think spo,e of thge best you ever made,

As more bees do this we will get a nuch better picture of time and temperature effects.  It well be a week before  some bees get this fone and written up as more reports come more will take the plunge. before long we will all wonder why were using heat, all this time. All I can say is that is how it was introduced to us,

I often wondered why it was called the Cold reaction, when the thing would get so hot. this answers that question.

The fast reaction blasted the ephedrine into D and L meth,
This slower method  gives the pseudo Ephedrine time to change configuration then rips off the oxygen, giving more of the d form of meth
It is still to be determined what time and temperature is ideal for potency and highest yield.

It is a BIG step in the right direction, but much more needs  to be figured out.
and the Bees true to their reputation are riding on the cutting edge of the technology. Even with the home made equipment, We kick ass.

Worlockium
 
 
 
 
    Worlock
(Tweaker God)
01-18-03 05:54
No 399284
      Daphuk_up     

I wish I could be more certain about the potential of MBRP/
 
One thing to note is this: it is not the weight od RP that is important, but the amount of available surface area/
The reaction occurs on the surface of the RP. for this reason finely powdered RP is more reactive than course grainy RP.
Used RP will have a waxy build up that reduces its potencty until it is cleaned off.
The iodine supplies the fuel to drive the reaction, the phos helps determine the rate of the reaction.
 with a low RP getting it to pop off in a fast reaction is difficult,

I am not going to say this will solve your problem . but it is easy to imagine if you have low phosphoroue it will be better if you can cook it longer and at a low enough heat, that the HI that is made is not blown into the push pull.
 With the HI staying in the reaction flask your chances of success go way, way up.
I always run my hose from the flask upward a few feet first, so some of the escaping HI will drip back down, I have had situations where that drip down made the difference in the reaction completing or not.
This may be your answer MBRP, low heat, wait it out 4 days.

1. I always mix powdered E with  powdered I2 first
( the I2 is broken up by putting it in a strong walled glass jar with some marbles , shaking it easy for quite a while)
2. A snall amount of water is added so they clump up into a dry mudball
3. The E and I2 are gently heated , until they melt and begin to flow, if iodine begins to vaporize remove from heat immediately it is too hot
4. when homogenous, the RP is dropped in, and the flask is rolled mixing it completely. Usually it will begin to bubble and develop a white fog, you can feel the heat on the bottom of the flask. At this point the stopper to the P/P is put on with a few pieces of tape.
5. The mixture gets more fluid lIke as the REaction proceeds, a SNALL AMouNT OF WATER IS PRODUCED AND SOME OF THE rp IS USED UP.

 put it in the warm place and wait it out.

Worlockium
 
 
 
 
    MnkyBoy78
(Hive Bee)
01-18-03 06:48
No 399291
      5 month old results     

SWIM was putzing around in the lab several months ago and noted 2 g of e and 3 g of I2 about.  So SWIM plopted these into a 250 ml fb flask and stoppered it.  Then 3 ml of ~ 75% Hypophosphoric acid was injected.  The rxn became exothermic and fogged up the flask quite nicely.  It was then placed on a shelf in a lockable cabnit. The room remained ~75 - 85 F.
When SWIM returned 6 days later, the contents of the flask were a orange/yellow color. Work up as usual.  Bioassay revealed e/go-go.  (Partial conversion)

The same procedure was followed as above, except 60% hypo was used.  Six days later the contents were checked.  Orange/yellow color.  Flask was set aside and forgot about as there were other things at hand to deal with. 

2 Weeks Later (20 days) the flask was re-discovered.  Now the contents were more yellowish/clear.  Contents were worked up as usual.  Bio-assay revealed go-go and that bitch PEG. 

Further research via this aproach where canceled due to funding shortages, but now there is perposed research SWIM might just have to go dust off that flask.
 
 
 
 
    Worlock
(Tweaker God)
01-18-03 06:55
No 399295
      Scotty Dog     

I am not amazed that the hive establishment is so close minded that they would censor Tweekazoid's Post
In the time I was a moderator I never sensored any ones post.
I did not agree with every one, but this is a public forum, differing opinions make us stronger, and less complacent.

Several times threads I was heavily into have dissappeared
just vanish.
Not a good sign, makes me wonder who is in control
The members of the forum or someone else


Worlockium
 
 
 
 
    FeatherWood
(Stranger)
01-18-03 07:12
No 399298
      da trueth     

similar situation was experience but not intentionally. goodies were dubed pook and choke people said the old days are back...uhhuh yes warlock thanks for the confirmation.


Take care all
FeatherWood
 
 
 
 
    Daphuk_up
(Stranger)
01-18-03 07:51
No 399307
      Alright, got it so far...     


Thanks Worlock for your help, very much appreciated. laugh

SWID has one more question for the more knowledgeable bees, however.  Is a push-pull set up really necessary for smaller batches, say 2gRP, 5gE, 8gI2?  Would a simple 18" long 1/4" dia. hose with a balloon on the end be sufficiant?  SWID guesses that it would, that push-pull set-ups are only for larger batches.  Help here for this noob would be, yet again, appreciated greatly. smile

PS  It somewhat shames SWID to admit that his reaction vessel is a brown-glass beer bottle.  Anyone see any particular problem with that, other than SWID can't see the rxn too well? frown


Regal Sir Palladium and the Harlot Chlorine...they make such a cute couple. ^_^
 
 
 
 
    Jacked
(Ancient Alchemist Delux)
01-18-03 08:48
No 399327
      A balloon will do     

No you don't haft to set up a P/P system, a balloon will do for those amounts just fine. Just run a couple feet of hose first and attach the balloon to the end of it.

The end result is directly connected to the effort applied
 
 
 
 
    AbSoLuTe
(Hive Bee)
01-18-03 10:36
No 399349
      So is the proof in the pudding?     

Hi Worlock Ive not been in here for a while.
Have you done a M.P.on the product and if so what is it?
Also colour pre acetone/ethanol wash.
I personally prefer the fast route, the closer to a flask fire the better. MMmmwwwhhhaaa. But then again reading one or two of your posts, it looks like your brain was way ahead of your fingers. LOL

'I see in my reflection,I'm looking slightly rough.
 
 
 
 
    Organikum
(Hive Addict)
01-18-03 10:40
No 399351
      if the higher concentration     

If the higher concentration of the HI is to do the trick (what I would like to be true very much as I was convinced of this for quite long a time) some pressure might be the way to go (if someone wants, as there are more ways to heaven...).
Three to five bar should be enough to hold quite high concentrations of HI solvated - also at elevated temperatures.
I claim that if the flask is set to rest for 48 hours after short heating up for starting the reaction and a overpressure is maintained during this time and temperature is about 25C to 35C, there will be first class product yielded. And the needed amounts of Iodine and RP or the correspondending acids may be reduced also. Applying a soft shake from time to time or a stirrer on low speed optimize the procedure - and prevent that the cook feels useless. wink


ORG

now or never
 
 
 
 
    Scottydog
(Hive Addict)
01-18-03 11:09
No 399355
      Simply stealth     

Theoretically speaking...

Warmer climate bees could literally slap on a balloon and dump it in the back of a broken down junk car. crazy

The possibilities are endless. The method is simply stealth.

The transient down the way could have a hole dug out in the desert covered up with plywood for all we know. smile

With clean precursors a rxn will kick coming off an icebath. So maybe cooler temps will reduce as well?

Temperature vs time?

This could open the floodgates to bees who had been previously limited due to an unrealistic living situation.

Can't believe the electricity Swis has wasted over the years.

Will be interesting to see some feedback.

Set it and forget it. laugh

Much respect...
___________
Refuse/Resist
 
 
 
 
    Worlock
(Tweaker God)
01-18-03 13:55
No 399369
      Swi D srr arr asrr     

In the city you can run up to about 1/2 oz  without the  P/P  when it gets up to an Oz it gets smoky so run it through kitty litter make sure the litter can't get sucked back into the flask

2 oz wull put out quite a bit of smoke

under 1/2 pz wait until dark then run the hose outside,

SWID SHOULD BE PROUD OF HIS LITTLE BROWN BOTTLE,
true cavemnan equipment
If it were too hot it might break

  I broke a 12 liter flask first time I used it because I did not heat it evenly, it was a very stupid mistake, talk about scrambling to find 2-6 liter flasks. Lost vey luttle of the contents, it cracked but did not shatter,
I had just walked out of the room then I heard that sickening sounding crack, it could only be one thing

Worlockium
 
 
 
 
    BenWiFFen
(Line Monitor)
01-18-03 14:17
No 399371
      Daphuk-up     

Does that say 8g of I2? I'd go with 3-5-5 or 3-5-6 but 8 is a tad high not that it wouldn't work. Worlock your comming in loud and clear but your voice sounds different.

When you get the bomb everything else was practice.
 
 
 
 
    Worlock
(Tweaker God)
01-18-03 15:52
No 399380
      Organikum     

Yes you appreciate the importance of forcing the relative diastemers of ephedrine to change configuration, and yet  have an environment mild enough to remove the oxygen only from the preffered form of ephedrine to make d-meth and exclude l-meth
Evidently the window of opportunuty is large.

 We have been blasting the ephedrine to both d and l meth m with a harsh and fast reaction

 we need to locate the best condition to make only d-meth,
The refluxers are doing it and the few that have done it under high concemtration agree the quality is much  higher, the dope is cleaner, but the yields are staggered and inconsistant. but I believe this is because of the newness and uncertainty about the endpoint

Worlockium
 
 
 
 
    aquagirl
(Vamp-Bee, Retired)
01-18-03 15:56
No 399381
      small stuff...     

I was the one that coined the phrase "nanoscale" ( a spin on a legit marine science accomplishment of mine).

there was never any one way to do it- all depended on what was onhand at the moment.  50 ml boiling flask sitting in hot water with a balloon on it for all day worked (I let the reagents start cold and slowly react.  Used a microwave granite thingy that held heat as a heat source.  Used IR heating lamps.  Used lightbulbs.  Used a rubber stoppered and taped coke bottle on a lightbulb.  worked great once.  another time it disintegrated into high velocity glass shards and droplets while I was still holding it.  not even a scratch, but luck was on my side.  my bedroom wall was henceforth painted a nice HI color (faded over time).

on a slightly larger synth, I used the hotplate from a coffee maker as the heat source, and a length of braided hose taped along the side of my frozen windows in the dead of winter.

there's no need for this p/p vs reflux pissing match- the long reflux is a historical fact passed down.  the p/p has some theoretical merit (high conc under pressure).  Of course a controlled p/p (not the incendiary fun) is acting as (a relatively  inefficient) condensor to a ccertain extent..

I  used to place flasks with fitted condensors pumping icewater through them in the presto kitchen kettle with a rheostat and an oil or sand "bath".  I'd run a braided hose off my condensor, up a wall, and sometimes in some h2o for backpressure.  worked great. put the street rp/i to shame- probably because of a little xtra time to react.

if I find time and privacy to post it. I'll detail my "final" method that was the last one I used for a couple cooks before I gave it up.  It's another kinda hybrid reflux-p/p.

method alone accts for a relatively s mall variable- you put rp/i together in proper proportions, and it's gonna spin the pfed 'round regardless of what you do.  I believe there are plenty of other variables, denaturants in pills, contaminants hiding in your glassware.  then there are the steps that are ONLY honed by practice.  you learn to trust your eyes, your nose, your tactile senses- the stuff that comes into play after the rxn and it's time to  separate shit and tweak pH, and dick with emulsions, then properly form a salt, wash it, and xtylize in ways that make your friends green with envy.  you cannot learn much of the truly important skills- lab techniques, without performing them many times, fucking up, refining, etc.  Yeah, I fucked up a lot of shit for a long time- but one day it was kinda like it all clicked.  my failures had forced me into good techniques that seem to be the cornerstone of a rxn. 

anyone else just kind of have it happen this way?  like finally learning to ride a bike? and after that, you had to try pretty fucking hard to screw it up.



(retired)
She Who Dances With Hampsters
 
 
 
 
    SHORTY
01-18-03 17:34
      What is the deal with d-meth & l-meth
(Rated as: UTFSE!)
    
 
 
 
    SHORTY
01-18-03 21:31
      What the hell is going on?
(Rated as: insignificant)
    
 
 
 
    sean1234
(Stranger)
01-18-03 22:03
No 399458
      SHORTY: The powers that be are simply trying...     

SHORTY: The powers that be are simply trying to eliminate redundance and make searching easier for newbees. You might try asking via PM.
 
 
 
 
    BenWiFFen
(Line Monitor)
01-18-03 23:33
No 399481
      The city or the sticks     

The city or the sticks? There's no differance unless you have some kind of under ground lab with an elaborate ventilation system I don't recomend testing what your neighbors nose knows.  I've ben in houses that you could tell cooking wasn't just done for dinner.

When you finally get the BOMB you'll see everything else was good practice.
 
 
 
 
    Worlock
(Rabble Rouser)
01-19-03 00:07
No 399495
      Aquagirl     

Thank you for coming out of retirement to set us all straight again.
I always enjoyed  your nano write-ups. I was given a brass mortar and pestle that was nano, it would crush one or two pills at a time,

In the beginning I also had many failures, then one day it began to make sense, Now it seems if I try to fuck it up it still turns into gold.
I shattered much glassware until I started cooking in sand , the sand gives a slow even heating, Nothing can ruin a yield like broken glassware on a hot plate. In sand if it does break, your chemicals are  caught in the pot holding the sand, seems like a safety net if everything does not burn up in the hot sand.
I have no gripe with reflux, it is a result of their success that has launched this revision of the technique.
Cooking it for 7 days is not as hard as it seems.
It is unacceptable to me since there is another that takes less time
I have done the 48 hour reflux and the results were the same as far as quality and yield. The hypo method produces a better quality product, but not as good as this cold method.
I have a couple of grams of E and have an urge to do a nano.

 
 

Worlockium
 
 
 
 
    Phlegm
(Stranger)
01-19-03 00:23
No 399500
      Low temp reflux?     

Just for the record, a low temp reflux of an HI/RP/pseudo mix is a bit of an oxymoron - at least at the Hive it is, being that there are two camps on this issue: those that favor long, long incubations at about 180F, and those that reflux for a much shorter period. The problem is that by definiton, reflux implies a boil. So to reflux in HI means that your rection temp is 260F - way too hot for the cool crowd.
 
 
 
 
    ZingoBingo
(Hive Bee)
01-19-03 00:28
No 399503
      Worlock & Aqua Girl . . .     

. . . whose next, Popeye?laugh

A thought has occured that an ambiant temp could be realized within, say an 96 qt. EE-glue cooler, by placing a shop light within. The hard plastic shield around the light would protect the inner plastic of the cooler. External temp flucuations would be hindered internally  by the insulating qualities of the cooler. A 24 hr trial run could then be monitored using a long stem meat thermometer or digital incubator thermometer with flexable probe inserted into drain plug.  Temp's could be varied by changing light bulb wattages until the 70/80 degree range was stabilized.  PP/balloon unit could be placed within and lid snapped shut.  Should flask break (highly doubtful) goodies would be retained within cooler and, what the heck, might even continue to react. A clandestine cooler off to one side would draw less attention than wine bottles duct tapped together on top the fridge or radiator.smile  Now, if a battery source could be introduced within the cooler with sufficient amps to power the light for 4 days at a constant wattage then we'd truly have an airtight, closed system.  Heck, you could load it up in the back of the 'ol station wagon and head on over to Yellowstone for a picnic at Old Faithful and no one would be the wiser . . .cool

ZB
 
 
 
 
    ZingoBingo
(Hive Bee)
01-19-03 00:59
No 399512
      Hmmm....     

If the higher concentration of the HI is to do the trick (what I would like to be true very much as I was convinced of this for quite long a time) some pressure might be the way to go (if someone wants, as there are more ways to heaven...).
Three to five bar should be enough to hold quite high concentrations of HI solvated - also at elevated temperatures.


Perhaps then, for an oh-zee, the goods could be placed in a large open bowl within a pressure cooker.  After the lid is secure the combined works/cooker could be placed within the EE-glue warmer previously illustrated.  Maybe we could call this system the 'hatchery'.

ZB
 
 
 
 
    Organikum
(Hive Addict)
01-19-03 02:22
No 399542
      shake it if no reflux     

Low speed stirring or better a swirl/shake from time to time is IMHO favorable if there is no reflux and there should be no reflux under elevated pressure as this would say temperatures far exceeding 127C. And thats whats to be avoided. Pressure like temperature enhances reaction speed (as a rule of thumb) so  this is thought as an exchange: Lower temperature in exchange for higher pressure. The bonus plus  coming with this setup is a much higher HI concentration and the reaction running in a more or less sealed vessel whereby stink can be avoided/reduced with ease. Push Pull pressurized. Why not? Handling the pressure of a automobil tire or tapwater is no rocket science.

Why slow and not hard stirring? I cant tell. I have some ideas but nothing I would throw in here by now as its only guessing in alpha stage. smile

ORG

now or never
 
 
 
 
    Daphuk_up
(Stranger)
01-19-03 04:37
No 399576
      Given the above...     

Given the above methodology, and the reagent ratio I am using (2gRP:5.5gE:7gI2), would 2mL be an appropriate amount of dH2O to add before adding the I2?  Note that psuedo and RP are very very dry, but the I2 was left slightly moist to make it more stable (less likely to sublime away).  Thoughts, ideas, suggestions? smile


Regal Sir Palladium and the Harlot Chlorine...they make such a cute couple. ^_^
 
 
 
 
    BenWiFFen
(Line Monitor)
01-19-03 10:49
No 399638
      Sublime what?     

The reason for placing your flask in the freezer and then a ice bath. Mix your dryer I2 with your P/fed chill for 5 min only. Add your r/p slowly and mix. You will have plenty of time before any white smoke never purple.

When you finally get the BOMB you'll see everything else was good practice.
 
 
 
 
    AbSoLuTe
(Hive Bee)
01-19-03 12:27
No 399658
      Melting Point/range     

Hey again Worlock, could you give us the Melting point of product and colour pre acetone/ethanol wash. Am interested as the proof isn't in the pudding, it's in the M.P
Yeah BenWiffen Worlock voice does sound different not like the old Worlock @ all. Maybe he has grown a bit, Dunno

'I see in my reflection,I'm looking slightly rough.
 
 
 
 
    SPISSHAK
(Hive Addict)
01-19-03 12:35
No 399660
      I have tried this too     

It does work and yeilds are good but you need a lot of time and the acid has to be super concentrated for this to work, and the red P has to be grind fine to give more surface area.
I'm too impatient for this.
 
 
 
 
    cthulhujr
(Hive Bee)
01-19-03 15:06
No 399684
      Re: The fast reaction blasted the ephedrine...     


The fast reaction blasted the ephedrine into D and L meth..We have been blasting the ephedrine to both d and l meth m with a harsh and fast reaction
.




Swim is not trying to be a pest, but how does that work?
Swim thought this was a strictly stereospecific reduction.  

Illustration of the commonality of these syntheses is seen in the following
facts. Stereochemistry implicit in the first route I also applies with
hydriodic acid/red phosphorus reduction. That is, only (-)ephedrine and
(+)pseudoephedrine yield (+)methamphetamine.


this is from the 'meth impurities' document


I-R'lyeh! Cthulhu fhtagn! I I!
 
 
 
 
    SPISSHAK
(Hive Addict)
01-19-03 16:19
No 399697
      This is how     

Your not a pest, the reaction produces methylaziridine, this is in the cis-trans form that's where the epimerization occurs, the aziridine then gets reduced as confirmed by NMR the ratio of isomers is 25% trans and 75% cis so 25% D, 75% L isomers is a typical result.
 
 
 
 
    alphacentauri
(Hive Bee)
01-19-03 22:48
No 399754
      Hypo concentration, reply to Worlock     

The hypophosphorous acid concentration I'm referring to is 50%, density (as stated on the label): 1,206. This makes the solution slightly less than 1M (one mole hypo per liter solution), or 10-3 moles per ml.
I read that water is a reaction killer, but, for Christ sake, a bit of water to bring the hypo, pfed and iodine together in touch.....or we want to react dry reagents!?!?!?shocked
 
 
 
 
    Worlock
(Rabble Rouser)
01-20-03 00:22
No 399777
      cthulhujr     



The fast reaction blasted the ephedrine into D and L meth..We have been blasting the ephedrine to both d and l meth m with a harsh and fast reaction




Swim is not trying to be a pest, but how does that work?
Swim thought this was a strictly stereospecific reduction.  

Illustration of the commonality of these syntheses is seen in the following
facts. Stereochemistry implicit in the first route I also applies with
hydriodic acid/red phosphorus reduction. That is, only (-)ephedrine and
(+)pseudoephedrine yield (+)methamphetamine.


this is from the 'meth impurities' document





Life seemed much simpler back then, too, but it created confusion and we need to be more accurate in describing configuration.
There are two chiral centers in ephedrine and psuedo
The (+) pseudo and (-)ephedrine have a similar configuration at the chiral carbon not attached to the oxygen

Ephedrine is a relative diastereo isomer (diastemer),it can exists in four non-mirror image configurations.
L- ephedrine is imported then racemized by the distributers , the racemic mix being a better nasal decongestant.

The process of racemizing the E creates a mix of isomers
Remember Ephedrine with 2(two) chiral carbons can have 4(four) isomers.
[R,R],[S,S],[R,S], and [S,R] configuration of ephedrine.

[R,R] and [S,S] are also known as pseudoephedrine.
[R,S] and [S,R] are commonly called ephedrine.

The terminology of (D,+ and L,-) refers to optical rotation, a hold over from older literature that does not describe configuration.

So we are beginning with 4 types of ephedrine that will form the two types of meth (D+ & L-) or [R] & [S] meth. Depending on which form the ephedrine is in, will determine what form the meth will be.
The longer timed  and colder reaction allows the E to racimize again changing form,
For some reason the preferred form of E reacts more readily than the others, this creates more of the (D+) or [R] Meth, when  under the milder conditions.
The fast reaction did not allow the E to change form it  just reduced it all retaining the fornm it was in.

To confound the issue, the reaction is a two step  SN2 reaction with the formation of an intermediate carbonium ion (Alcohol addition of a halogen)
This type of reaction is not stereo specific.
However.
It seems that the size of the iodine prevents the bonds from rotating at the moment of reduction of the ephedrine.


Worlockium
 
 
 
 
    Worlock
(Rabble Rouser)
01-20-03 00:44
No 399780
      alphacentauri     

Check your Private Mail

Worlockium
 
 
 
 
    morpheus
(Hive Bee)
01-20-03 20:09
No 399946
      Congratulations Worlock     

About 2 years ago Curbshot and Super Ass Man(where is he?) were trying to come up with a sure fire no fail synthesis
for the Newbee,that would guarantee some product.It looks like you did it,and without fire(heat).Of course they could always screw up the a/b or gassing.Oops forgot about cleaning the precursors too.Anyways the reason for asking for your old post was a friend is interested in rp/hi reduction.Swim can't begin to tell him in laymans terms
whereas you have a rare gift of communicating chemistry
so a grammar school kid can understand it.Thanks,will let
you know results of my dream.
 
 
 
 
    methylaminorex
(Stranger)
01-20-03 20:47
No 399955
      @WORLOCK     

good work  ;)
how about if the rxn does not fire off from self?
should one use some heat to start bubbling, before setting the flask aside for 4 days?
 
 
 
 
    methylaminorex
01-20-03 23:05
      up :)
(Rated as: insignificant)
    
 
 
 
    handsfull2
01-21-03 05:32
      incubator
(Rated as: incomprehensible)
    
 
 
 
    handsfull2
(Hive Addict)
01-21-03 07:26
No 400104
      huh?     

Ok moderator''I see your having fun with the buttons again huh.


I was merely trying to help with some sugestions on how to keep the rxn warm while waiting for the 4 day time limit that worlock suggested in this thread.

seems a egg incubator would solve the problem of maintaining a constant temp'' and the egg turner would slowly keep the rxn moving while beeing incubated""so what part dont you understand?
  smile

  "Surpassing what is common or usual or expected  "  

 
 
 
 
    Worlock
(Rabble Rouser)
01-21-03 15:04
No 400178
      How to screw up     

The simplest and most popular way to screw up this reaction method, is  easy to do  and easy to fix. Is the addition of too much water.
I know we think of a reaction as being wet, but this reaction must be started out dry, it gsts wetter as time goes on.,

How dry is dry
When the E and I2 and RP are put together it should be so dry and thick of a mud that when you roll the flask slowly the reactants barely move at room temperature. within a minute the reactants will begin to fire off.  At this point you can roll the flask slowly and the mud begins to flow and mix together, you will feel the heat being generated through the flask. Keep rolling the flask you will notice that rollong it slows the reaction dowm.
 
If none of this has happened and the reactants are still stuck to the flask and look dry add a small amount of water, if doing under 1/2 ounce you might add four drops of water. If doing over 2 ounces  add 2 ml of water.
If the reactants flow while you roll the flask, but there is no white fog or heat or bubblingm then give it a blast of heat, until it bubbles.

Once it is mixed and the smoke is starting to escape from the flask. then put on your stopper and hose.



Cold reaction
In the cold reaction. you are done for now, just keep it warm and mic it when you get a chance over the next few days.

fast reaction
In the fast reaction, when the bubblimg dies down, add heat, until it gets all turbulent and blows gas(185 F) After the gas expands it sucks it back in violently . you are done with the reaction. let it cool.  add water bring it to a boil then fllter out the RP.

Too much water
If you added too much water, and did not see any of the reaction signs then gently heat it, without the stopper, until it boils. Maintain the boil with out the stopper for 1 to 4 hours until most of the excess water is  gone. It will be a thick soup, that does not stick to the sides if the flask. When swirled it runs down the sides within a minute. At this point the reaction will be completed, add water bring to a boil and filter off the RP.  



Worlockium
 
 
 
 
    placebo
(not quite as irritable lately)
01-21-03 16:07
No 400183
      I'll see you in 4 days!     

I'll see you in 4 days!
One question, you spoke of quality, what's the yield like? I assume no worse then before.
Good to see you back master!

Intelligence is not the recall of knowledge, but the ability to use it. (Rainman was a retard)
 
 
 
 
    Jacked
(Ancient Alchemist Delux)
01-21-03 21:49
No 400247
      Water ratio     

Use 5 Ml H2O per 28g starter. add 1 ml for walls of the container holding the calculated amount of H2O sometimes 2 if it is say a 125ml beaker but the ratio is ample enough water..

During the regular P/P event one will wonder if they added too much H2O at these ratios but just don't rush it. It always reaches 2en phase. I don't see why the same ratio wouldn't work here...

Swim knows some will have a problem controlling the starting of this reaction, normally Swim doesn't mind the first phase reacting so vigorously after it has mixed and molted to chowder with no heat being applied but this time he felt it would be to hot.  A S/S bowl with crushed ice and acetone had to be used to slow down this event. The idea of adding acetone is to help the thermal transfer of temp through the glass happen at a faster rate because by time the eye sees the need for cooling it's late, cooling needs to go down quickly due to the eye lag thing. It takes a little bit for the contents to see a temp change and settle down for you..

The end result is directly connected to the effort applied
 
 
 
 
    Worlock
(Rabble Rouser)
01-22-03 08:26
No 400376
      "...the result was very potent..."     

Here is a Bee describing the results of cooking meth a second time.
It indicates  that there is probably unreacted E in the product.
Not only that but the E is undetectable by tasting the product,
A longer cooking time should convert more of the E to Meth.


In reply to:[Worlock}

Its interesting that you mentioned cooking a second time.  A few months ago, i was doing alot of reactions, at least 2 a day and was not getting very good results.  Then one day i ran out of pseudo and thought what the hell and just tossed all the meth which wasn't very potent in a flask and rereacted it.  The rxn didnt take long and after steam distillation and titrated which was alot easier to do compared to first cook. the result was very potent. i assumed that i had not been getting the pseudo clean enough the first time.  Never thought about it being the isomer.  anyways from then on I always keep all the not very good meth and rereact it.  So far have never been disappointed. 
Thanks again for your reply.




Worlockium
 
 
 
 
    Worlock
(Rabble Rouser)
01-22-03 09:13
No 400386
      Absolute     

Sorry I don't have a melting point apparatus.
I do agree that the proof is in the M.P. and in the abi;ity too obtain a good sharp melt, Nothing is worse then 1/2 of it melting too soon and the other 1/2 melting too late.

A polarimeter would be great also, a home made version would be easy to make , except locating  small square sample containers


Worlockium
 
 
 
 
    AbSoLuTe
(Hive Bee)
01-22-03 10:29
No 400392
      No MP apparatus?     

Do you have 'Organic chem lab survival manual' by Zubrick?
It has a very simple 'apparatus' for doing an M.P.
I suggest you buy it or go to a library or download a copy of it. You should have all the equipment and expertise, worlock.
Waiting your results.

'I see in my reflection,I'm looking slightly rough.
 
 
 
 
    AbSoLuTe
(Hive Bee)
01-22-03 10:40
No 400394
      As far as half melting to soon and half ...     

As far as  half melting to soon and half melting to late goes , YOU HAVE SHIT OR NO METH.If it is your product then it should melt at exactly its MP and within its range, which if I remember correctly is 172deg C(correct me if I am wrong) I have been given and bought stuff that was guaranteed to be pure, straight out of the gasser to the dryer, or stuff made with the Hypo method and uncut and it is not MethAmphetamine, It may well be something similiar to it or it might contain small trace compound of it , but it IS NOT meth.
The only (simple)true test for purity is to do a MP, unless you have access to a Analytical Lab
As they say, garbage in garbage out.

'I see in my reflection,I'm looking slightly rough.
 
 
 
 
    lugh
(Moderator)
01-22-03 15:00
No 400419
      Apparatus     

Speculations about the identity of the product should bee kept to oneself until proper analytical work is done, the melting point apparatus mentioned in Post 254885 (lugh: "Re: testing the purity", Chemicals & Equipment) is adapted from pages 80-3 of Vogel's 3d Edition, which can bee found at:

../rhodium/djvu /vogel/vogel.3rd.djvu

As far as polarascopy:

The effect can be demonstrated by examining with Polaroid sunglasses light reflected at various angles from ordinary window glass. The reflections from ordinary glass will be adsorbed most strongly when the rays make an angle of about 33 degrees with respect to the surface of the glass. The angle of reflection at which the adsorbtion is strongest is related to the refractive index of the transparent reflector.
It's possible to make a rough estimate of the unknown refractive index of a substance with a pair of sunglasses and a protractor. Measure the angle at which reflected rays are absobed most strongly. Subtact the angle from 90 degrees. The trignometric tangent of the resulting angle is equal to the index of refraction.


smilelaughsmile
 
 
 
 
    Jetson
(Title Addict/Eraser)
01-22-03 16:00
No 400426
      ...     

melting point should be around 172 in Ferenheit swij believes.  he'll check.  either way he's pretty sure it's only around a 10-15 degree difference from psuedo so one must be pretty accurate in determining the exact mp.  swij'll check(don't have notes here) and if need be and you can't find it here on tfse he'll post it.

the devil is so lonelymad
 
 
 
 
    Organikum
(Hive Addict)
01-22-03 16:29
No 400437
      Testing by melting point wont work     

Methamphetamine hydrochloride, melting point: 170C-175C
d-pseudoephedrine hydrochloride, melting point: 180C-181C

You wont detect this without serious equipment and a lot of training. In difference to ephedrine.HCl is pseudoephedrine.HCl soluble in chloroform so there is no way to separate them this way. I started a thread on this not long ago, but interrest was low.

ORG

Post 399486 (not existing)
 
 
 
 
    Jetson
(Title Addict/Eraser)
01-22-03 16:58
No 400445
      ...     

yup that's it.  Celsius.  and very little room for error.  shite man,  little interest.  in seperating meth from pseudo?  or is that e.hcl from p.hcl?

the devil is so lonelymad
 
 
 
 
    anOrangeDrip
(Hive Bee)
01-22-03 19:16
No 400470
      i don't have a merck     

I remember reading that the melting points of ephedrine sulfate and ephedrine HCl differ by about 30C. So maybe the melting points of meth SO4 and pseudo SO4 will be a big enough difference to use this test? Or maybe other acids which won't be listed in the merck

When you meet a swordsman, draw your sword: Do not recite poetry to one who is not a poet.
 
 
 
 
    superman
(Stranger)
01-22-03 23:33
No 400532
      a little input on rp/i/e ratios?     

i've read way to many ratios that vary from each other way too much.  i'm looking to end up with about a 1/2 oz finished product via coldsyth method using a rubber instead of a p/p.  can someone reccomend a good RP:I:E ratio?

very much appreciated!
 
 
 
 
    Jacked
(Ancient Alchemist Delux)
01-23-03 00:28
No 400541
      cold method??     

This cold method is what worlock is posting about. The P/P method is not cold by any means. The amount of I2 will be gram for gram, The ratio of your RP is determined by its quality, Is it from match book? or how many times has it been reacted? was it cleaned afterwords properly? and so on and so on. The amount of H20 is what you should be asking because that varies greatly depending on what your wanting to do and the time you are willing to invest into what your doing..

Questian:

Mp's of meth. If one was to cut meth with something that had a MP one deg less than the meth itself, would it register or effect the overall MP?

The end result is directly connected to the effort applied
 
 
 
 
    Jacked
(Ancient Alchemist Delux)
01-23-03 00:35
No 400546
      hand held     

For a polarimeter, the cover of an led screen off one of those little hand held game's for kids would work, and there is enough to use a hole punch for two disk, with two screw together lens you can get for your camera holds them flat and secure. this clipped to a gravity protractor with v block would work as well as anything I would think.

The end result is directly connected to the effort applied
 
 
 
 
    Worlock
(Rabble Rouser)
01-23-03 02:36
No 400583
      MP thermometer     

The melting point needs a good thermometer
a delicate piece of glassware.
Mine is nowhere that I can locate @#$%^&*dang tweakers around here break everything with their foolhardy experimental bullshowers.
If it ain't broke , hand it to a tweaker,

As  stated one needs a bit of experience in reading the M.P.
 because a partial melt indicates how much contamination and will give almost as  much insight  as the actual temperature.
The correct approach is as stated  by another bee, change the compoud being tested,
That way  the two forms of meth could also be analysed , By using a optically pure compound to attach to the meth,
There once was discussion of Tartric acid being used to separate the isomers of meth

I like the polarimeter because the mathematics will wash out the weak minded

Worlockium
 
 
 
 
    superman
01-23-03 03:23
      ratios:
(Rated as: redundant)
    
 
 
 
    Worlock
(Rabble Rouser)
01-23-03 12:13
No 400780
      Morpheus     


The information you requestee in Layman terms  os at this address

http://www.geocities.com/zabba_alba/lib/Alkyl.zip
It nust be downloaded 1 mb
the password to open the file is: hive
the inner file is unzipped to a folder and started with "Start.html"



Worlockium
 
 
 
 
    WHiPPiT
01-23-03 12:42
      I would like to hear from anyone who has ...
(Rated as: insignificant)
    
 
 
 
    placebo
(not quite as irritable lately)
01-23-03 16:36
No 400836
      Who the hell can wait that long?     

Who the hell can wait that long?
2.7 in 1.7 out after 2 days at 90c in small jar with a condom and wet like lava.

Intelligence is not the recall of knowledge, but the ability to use it. (Rainman was a retard)
 
 
 
 
    WHiPPiT
(Stranger)
01-24-03 12:02
No 401087
      So you're saying that after 48 hours you got...     

So you're saying that after 48 hours you got 1.7g of product from 2.7g of precursor. What was the quality like?
 
 
 
 
    Jacked
(Ancient Alchemist Delux)
01-24-03 23:43
No 401204
      freebase or HCl     

I was wondering if pseudo base would be more adapt for this reaction the HCl?

The end result is directly connected to the effort applied
 
 
 
 
    placebo
(not quite as irritable lately)
01-25-03 00:17
No 401217
      It was crap, it was prolly 1/4gm meth.     

It was crap, it was prolly 1/4gm meth. This would be the smallest rxn SWIM has done by a factor of 10. And a big waste of time. SWIM didn't have the patience to wait 4 days, so he went with a water bath and 2 days and was heavy with the RP/I2. SWIM aint saying it won't/can't work. But you got buckleys chances with small amounts. It just doesn't have enough inertia to take it anywhere. Just pissed SWIM off coz he waited 2 days to get shit that he could have had primo in 2 hours.

...Sad part was, that is the first 2.7gm of pfed he has seen in prolly a year.

Intelligence is not the recall of knowledge, but the ability to use it. (Rainman was a retard)
 
 
 
 
    Worlock
(Rabble Rouser)
01-25-03 02:37
No 401238
      Practical Application of Theoretical Chemistry     

A friend, of a friend, related this dream, as told to her mother, by a stray dog.
 The pooch stated that she/he(the dog had been neutered, and was not sure which sex it was, although it had a shlong, it squatted to pee) Anyway it saw one of it's many former masters, mix  together:
 
SETUP
-----

 20 gm pseudo/ephedrine,
 24 gm Iodine,
 12 gm Red Phos
  3 gm water
 In a 1000 ml flask, fitted with 
 10 feet of  braided 5/8 inch  OD hose,
 placed in a sand bath at 100 F - 105 F.
 The hose was run from the flask upward for four feet then horizontally three feet, ending up curving  upon itself in a loop, the way that type of tubing tends to curve. The end of the tube was near a vented fan.


PROGRESS
---------

Initially- The mixture was heated until a light white smoke appeared, mixed well and placed in the sand bath, It was remixed intermittently

12 hours - mixture was less viscous(more watery), the surface of the solution was lumpy. When mixed ,1 mm particles of Iodine,pseudo/ephedrine,R would adhere to the glass.

18 hours - mixture less thick, the surface was smoother. When mixed .26 mm particles adhered to the sides of the flask.

24 hours - mixture was notably less viscous, surface was smooth. When mixed, small Red Phos particles adhered to the glass.

30 hours - less thick, smooth surface , color was the same red as always. White crystals had formed in the flask neck and the  first few inches of tubing, these were shaken down into the solution. The tubing was stained red along all but the last foot . About 4 ml of a clear fluid  formed in the loop and was drained back into the flask. When mixed, the contents drained down the sides of the flask , leaving a thin reddish film, containing almost microscopic particles.
Estimated to be 80%- 90% complete by fast reaction standards.
 The temptation to retrieve a sample was, ignored, in favor of waiting until a      color change was observed.  
 
36 hours - viscosity like a runny syrup. Flows easily off the glass surface.
 Color changed to a darker , dull red-purple.
 An aliquot was removed, processed,
 ABSOLUTE WAS RIGHT, A MELTING POINT IS NEEDED, What would I give for a 16 inch, 250 C thermometer right now.
The bio-assay - just put a little bit in a pipe and    WwoOowW , it has got some zing, zip, definitely a level above my usual bug juice. Not devastating, yet quite powerful. Almost Scary.  I will not go back to the 1 hour blaster method, This is "mo' betta, fer shure".

This is not the end



Worlockium
 
 
 
 
    morpheus
(Hive Bee)
01-25-03 02:45
No 401240
      pseudo base     

Was wondering the same thing as Jacked about using pseudo
base.Only thing is if lab grade rp & lab grade sublimated
iodine crystals are used.
The rxn is supposed to be started bone dry and there is no hydrogen present.
H2O would have to be added or I2 from tincture(not sublimated) used since pseudo hcl is not being used.Correct?

 
 
 
 
    Worlock
(Rabble Rouser)
01-25-03 04:44
No 401265
      Freebase E - bee careful     

The reaction  uses up 5 molecules of water and returns 8 , so a little water must be present, to get it started , then it produces its own water as time goes on evidenced by the consistency of the mixture. Water, being a product of the reaction , if in excess will  tend to inhibit the reaction, due to  equilibrium considerations . Evidenced by the length of time it takes the reflux method (which uses a lot of water),  to complete.

The freebase is highly reactive, before adding RP, it is best to chill the E and I for five minutes.
Adding RP at room temperature, may cause an eruption of the chemicals. Not explosive, but violent enough to expel the contents of the flask all over the ceiling, and produce an awesome red cloud of smoke.
Chilling the chems  for five minutes, in the freezer, before adding the RP  prevents this.
Once past that initial introduction, the E will forms into an iodide salt, and is safe again


Worlockium
 
 
 
 
    Jacked
(Ancient Alchemist Delux)
01-25-03 04:47
No 401266
      H20     

H20 is needed to make HI. When you are using I2 from tincher there will be a small amount of moisture present. No H20 No HI. When they call this a dry reaction it must be by comparison only and not to be taken literately.

The end result is directly connected to the effort applied
 
 
 
 
    wareami
(Hive Addict)
01-25-03 18:31
No 401401
      1000th degree     

In a perfect world, this post(1000th) would have included a link to the official Egull Right-UP! But we don't live in a perfect world! Ibeeware has been beset with many set-backs since april and operates at a disadvantage that many have yet to experience! Given time, these will be disclosed and mucho understanding will fall on the heads of many!
Mainly detailing the mystery's surrounding Wareamiese speak as opposed to chemspeak!
Since Ibee stumbled on the 5day cook last year, much research has been done and many factors have been disclosed. Ibee regrets not being in the position to partake in these discussions as of late, beecause they are right UP his alley! Ibee is using a borrowed laptop at the moment and the next few daze will be dedicated to setting up a new MoBo so enlightenment can continue.
Worlock: It is truely a pleasure to have you back in the sandbox, kicking the rabble to the curb, as it were, ARR-rousal Style! And it's always a pleasure to hear Jacked's thoughts in these fields of study! Bee looking for Ibee's two sense! The Kidz will be back and when they do, look for them to cum UP swinging! Hopefully, they'll be able to address some of the findings brought UP by many so far!
Excellent Work as usual Worlock!!! Kudos!!!
Peace of the reaction

Have FUN-Bee SAFE
Ibeeware and The NervousBrakeDown Kidz

PharmulationPhreek!
http://www.chemhead.org
 
 
 
 
    lugh
(Moderator)
01-25-03 23:25
No 401465
      Index of Refraction     

Post 401464 (lugh: "DIY OTC polarimeter", Chemicals & Equipment) smile
 
 
 
 
    Worlock
(Tweaker God)
01-26-03 04:29
No 401519
      Wareami if only it were true It is my ...     

Wareami if only it were true
 
It is my intention to support the thinking of many Bees who express honest concerns of Quality, Heat was thought to be a big cu;prit in the production of toxins, well ... we did away with heat 40 C  is way down there.

The truth of impurities is in the reagents that are used ,
Hardware industrial grade solvents can be cleaned up with resin exchange tubes and activated charcoal, aand some easy to apply methods.
Lye is Lye, Red devil is not NaOH , It can be fixed.
Muratic acid is shit, and It is fixable.

The second cause of impurities is in rushing through the clean up , it does no good to wash the product and then not wait until the layers separate fully, that just leaves the shit in there.

It is my hope that there will be some desire to solve these problems, and to turn away from the rhetoric.

Almost universally Bees desire better results, and want improved products, Bees are naturally light years ahead of a common street cook. This is the elite, the cream of the crop, we have here  and not the rabble, they are dedicated, and willing to strive for perfection.


Worlockium
 
 
 
 
    AbSoLuTe
(Hive Bee)
01-26-03 05:20
No 401525
      A Bit more on M.P's     

Simply put if your final clean washed dried product melt above say 175 deg C, you could assume there is still sudo in it, the closer to the magic temp the purer, and I can say this from experience. If it melt lower than that, i.e much lower, then the only thing I can think of is that it isn't dry, as there is not much in this reaction that would reduce the M.P below 170 ish.
Once you have personally assayed 173 degC shit all others pale in comparison.
I am talking about a match head sample that will just about make you cum in ya jocks. And the colour of these has always been slighty yellow , even after ethanol/acetone wash.  My personal favourite was once observed as the result of almost a flash fire Melted @ 172.5 on three seperate samples, and was the wildest shit ever, bar none.
[b]Worlock[b/] , you dont need a 16" 250deg C therm, just get a 100-200 deg (range) 12 incher, the ladies will still luv ya.

'I see in my reflection,I'm looking slightly rough.
 
 
 
 
    Jacked
(Ancient Alchemist Delux)
01-26-03 05:56
No 401530
      flooding the phase     

I think the trick is going to be flooding out the second phase and refluxing this for 12 hours or so.. Swim did it in the past and received good results, his post on this was at another board. I do think he posted his findings on this here as well..

The end result is directly connected to the effort applied
 
 
 
 
    wareami
(Hive Addict)
01-26-03 06:20
No 401534
      Ahhhhh...Soooo....Where's Uncle Ho???     

Lugh: Thanx for that little peace of en-Light-enment! The Kidz will head right down to the Ghetto Variety Store and set upon fashioning one of them Do-Hickeys!wink
Worlock: Ibee agrees with the intented purpose, as we all want the same. Efficiency...Quality...Quantity! Many trade off's have existed in the playing field and settling for less of one or the other has become the norm. Or so it would seem! Ibee's been drug over the coals in the past for admonishing bees for settling for less. Not that he's better than any bee here or rides atop a HIGH horse! But based on what he reads here and based upon his own experimentation! Many of the avenues he's explored were the result of following the earlier teachings from yourselfium and Jacked! He's expounded on some of what your discussions proposed early on!
First he set about curing the extraction problem and had sufficient success. Enough to move on to the rxn phase! Upon remembering the teachings about a slow, controled reaction, he set out with those words of wisdom first and foremost! He accidently stumbled on a fiveday cook marathon that fully tested Jacked's "Patience" theory. The best gear ever sampled was the result and Ibee thought it was the result of the magic chant....initially! He was wrong! Last week Ibee revisited that once in a lifetime arena! Only this time trying to reduce the time under reflux. 30 hours! And he found the same as was discussed here earlier about "Too Much dh2o" spoiling the end result and throwing off the cooking time!
Ibee feels he has it down and will repeat one more time before disclosing the magic formula...just for a consistancy confirmation!
Although Ibee and the kidz are resilient little fuks, they don't want to engage in any more pissing contests such as they have been noted for!
Facts will speak for themselves and the challenge from then on will be to simply confirm the facts and let the rhetoric remain "Text in the Box" as the Kidz Plough Ahead.
Much Respect!
Ibeeware


PharmulationPhreek!
http://www.chemhead.org
 
 
 
 
    Worlock
(Tweaker God)
01-26-03 06:25
No 401538
      Lugh     

It is the sample tube that was the Kavetch.
Instead of a crystal. It will be a solution of known concentration
the formula corrects for length of the tube  and concentration. Finding a tube that is squared was the problem. I figure I'll just square up a test tube with heat.
It is easy to calibrate , put pure water  in the tube and adjust lens to zero, then put sample in tube , read refractivity, make corrections foe concentration and kength of tibeto (



Angle           Measured  angle
of          =  --------------------
rotation        Concentration x Length

concen = gms/ml
length = decimeters



Worlockium
 
 
 
 
    Worlock
(Tweaker God)
01-26-03 06:49
No 401541
      AbSoLuTe     

Thanks for the infornation on the melt. It will definitely come in handy , since I would have anticipated a two phase melt.
Also the lower than 172 C melting  would have confused me.
Are tou sure the 12 incher will be as good as a 16 inch, I guess if they are not side by side the girls would not notice.


I continued the cook to the 52 hour mark,
The product lost the gut wrenching physical effects , and retained the mental hyper-activity. Which is fine with me.

The color darkened.???? 
The product is smoother than the 36 hour sample, have not yet acetoned or recrystalized it. In fact have not evaporated more than a small sample, no idea of yield yet.
Test monkeys will report in as soon as they run out of stuff.


Worlockium
 
 
 
 
    Worlock
(Tweaker God)
01-26-03 07:23
No 401544
      Jacked     

My good friend, guess what,
a reflux condensor could be fitted to the
reaction flask and the P/P tanks done away with.

The temperature and conditions are mild enough.
In fact it is pretty much a steady state, with slow even turn over , there is no violent phase 2
It just cooks at low temperature No surprises .

If you flood it then the temperature would have to be more than doubled.
From what was proposed, by the bees,  it is the excessive heat that caused production of toxins.

We now have the ability to control
time,  temp, and concentration, and still be sucessfull.

more or less water , or more or less heat,  affect the time required,

more water at 40 C  = 14 - 21 days?????
more water at 100 C = 7 days
less water at 40 C  = 2 days
less water at 100 C = 12 hours???
should be able to plot concentration vs temperature and arrive at the time needed

or concen vs time
or temp vs time
and arrive at the third variable

Some where in there will be the ideal conditions

Exactly how much water is used to flood the reaction, that is unclear, I have not seen the numbers .


Worlockium
 
 
 
 
    Worlock
(Tweaker God)
01-26-03 07:28
No 401545
      methaminorex     

The reaction starts when you combine the chemicals
I don't think it requires any push to get it started,

Worlockium
 
 
 
 
    Worlock
(Tweaker God)
01-26-03 07:44
No 401548
      Wareami     

I thought you recently discovered the benefits of the seven day reflux ?

Has someone else known about this before ?

Sodium Thiosulfate


Worlockium
 
 
 
 
    lugh
(Moderator)
01-26-03 14:22
No 401585
      Hard Way v Easy Way     


The melting point needs a good thermometer
a delicate piece of glassware.
Mine is nowhere that I can locate @#$%^&*dang tweakers around here break everything with their foolhardy experimental bullshowers.
If it ain't broke , hand it to a tweaker,





If you want to do it the hard way as in Post 401538 (Worlock: "Lugh", Stimulants), go for it (just keep it away from the other tweakers:), somehow I think most will like the easy way better laugh Polarimetry was first used in sugar analysis, and a long treatise on the subject is available, but with the 10k limit on posts, it's not practical to make available here frown Digital pyrometers are far sturdier than thermometers, but more costly as well smile

 
 
 
 
    Jacked
(Ancient Alchemist Delux)
01-26-03 16:35
No 401608
      How much?     

Well at the time of flooding Swim was at the 5ml per 28g mark on a 100g start and it was just getting ready for phase change, Sides of flask glass over as all reagents settle into the mix sliding effortless into the obis, the glaze in the flask turns slyly darker then  approximately 40ml of scalding hot H20 was added then a reflux condenser was added and flask was adjusted to a light reflux, 12 hours later it was shut down and processed by ker-plunking and evaping instead of gassing.. Swim would see 70% by weight sometimes a few % more but only a few, The result was good gear by any standards, Swim was hoping at the time to increase yield better than 65% average (by weight). Cant recall anything else about it, I have a backup of the zonze that was taken a few months before its shut down, I'll dig it up and see if I can find my notes.. Not that they would say any more than that.. Shit All Swims dope was the best around, even if it wasn't... Just ask Swim.  

The end result is directly connected to the effort applied
 
 
 
 
    WHiPPiT
(Stranger)
01-26-03 18:31
No 401623
      SWIWHiPPiT mixed 20g eph 30g semi-wet I2 and...     

SWIWHiPPiT mixed 20g eph 30g semi-wet I2 and 15g rp in a wine bottle with a 3 balloons over the end secured with duct tape. It is winter here, and all the ingredients had been hidden outside for some time before they were wieghed and mixed cold. The bottle with the chemicals in it was then taken to a large apartment building and hidden in the warm boiler room on the roof. Hopfully no one will find it. SWIWHiPPiT will report back the results in 4 days, if it is still there by then.
 
 
 
 
    Worlock
(Tweaker God)
01-26-03 19:34
No 401632
      Practical Applicaion of Theoretical Dhenistry     

P.A. T.C. continued

52 hours - The reaction was halted, more crystals had formed.

Results
---------
The reaction mixture had not shown any changes from the 36 hour appearance. But the product was quite different from the sample taken at 36 hours
The effect of the drug was mellower as far as none of the that geared up body rush feeling, While maintaining a potency that won't let go. Not even considered sleeping for  last 30 hours.

The reaction was purposely overcooked to determine what and how long , and anything else that might be learned about how not to do something.
However, it would have been wiser to stop the reaction sooner, probably near the 40 hour mark. Due to the overcooking, the white crystals were slightly yellowed at 52 hours and the return is at the 50% mark.
Without any acetone washes or recrystallization the product is palatable,except the very last puff has a touch of residue, not a evil residue taste, but an undefined small dark splotch.
I think a result of reused but poorly cleaned RP.

It takes a very small amount of this gogo to keep you well fired up.
That is the main thing , Since I am accoustomed to a certain level of buzz, I naturally stop at that point, it takes about 1/2 to 1/3 as much dope, and it is a better buzz. Prices will go higher, for this
rare hi-test commodity

End Point
----------
Once the white crystals form in the flask and the
color has made a change to a duller darker red, the
particles in the solution are small and easily flow down the sides , and the viscosity has decreased to a soup from a syrup,
pull it , Don't continue the reaction, more than a couple of hours ,
It will be at its prime
The main sign to watch for is the color change of the solution.
At no time during the process , was there a noticeable boiling of the contents, with the exception of my artificial initial quick heating, which  is not necessary to initiate the reaction,
At no time was there a violent rush of gasses, although gas production did increase near the end of the reaction evidenced by the red staining on the hose.

Concentration
----------------
If you run the reaction wetter , the temperature can be increased
The reaction was as dry as they get , and it appeared that it would still have reacted at 90 F with no problem.
It seems that if run very dry,  the length of the reaction will be under 40 hours  as long as it is between 80F and 160F.
This was started with  3 ml of water for 20 gm E.
Easily 6 mls of water could have been added and it still would have been dry.
9 mls of water and the fast reaction would have been hard to obtain.
15 mls of water and the fast reaction would not occur at all, this would probably be close the ideal concentration and the estimated time need at 110 F would be about 3 days .

Temperature
------------
The critical temperature seems to be about 80 F, below this the reaction is very slow, above this point it proceeds at a noticeable rate. The upper critical point is between 160F and 180F above 180F and it will go ballistic in no time. At 160 F the reaction may or may not gather enough energy to get violent  it depends upon the conditions.
If you have seen numerous reactions in the past , you will quickly get a feel for the time, temperature , concentration relationship, and will be able to get it to finish whenever you please.

Advantages
------------
It is a great feeling to really have control and no longer be forcing it to pop off soon, with sometimes unpredictable results,
A reflux condenser can be easily set on top, and do away with the p/p tanks and hoses if that is your desire.
Gone is the expansile rise of reactants , no more bubbling, no more. pac man signs, no more whoosh, no more doubts if it hit the mark,. you simply take it to completion, by changing the temperature 5F-10F.
Best of all none of that stinky gas, vaporous HI,  trying to kill you little by little.
Less of the smell that can alert someone who is not cool about  your hobby.
It can be done easily in 2 days or 4 days or however long,
It can even be done in 12 hours, but I suspect 12 hours is pushing the lower limits of time.
Not much else to relate except,  "try it, you will like it"

My thanks to all the bees who are now deeply embroiled in this project, you will not be disappointed in the results, in fact you will be  pleased with yourselves,  for quite a while,
because it works like a "dream".


Worlockium
 
 
 
 
    geezmeister
(Bee of the Month)
01-26-03 20:09
No 401648
      great conceptualization     

I have been following this thread closely, while playing with a different synth for the moment. The observations Worlock makes the point about how user friendly his sample was, with the absence of body aches and side effects. The correlation between temperature and toxins is something I have noted in past experience, although only from an observational basis. I realize that two things occuring in sequence is not proof they are related to each other, let alone proof of cause and effect. The consistency of the negative side effects at higher temperatures and the consistency with which they dissappear as cooking temperatures decrease persuaded me there was a correlation between temperature and toxins. I find some confirmation in Worlock's comments on his slow cook, low temp batch's samples.

Perhaps this slow, cool synth can achieve what most of us are really trying to achieve-- pure meth.

This thread, and the Bees active in it, is a tribute to the Hive and how it works. Instead of seeing posts defending entrenched positions, defending turf, or proclaiming some ultimate truth, the very people I admired the most when I first logged on here are still at it, pushing the edges of the envelope, trying to find the better way to what we want. The cooperative spirit of this site continues to amaze me.  What amazes me even more is the ability of Bees to test their own opinions about the synths, and their willingness to consider and verify new thoughts and ideas.
You might expect a more rigid stance from the elder bees-- and you would be wrong.

This may not be anything but an observational note, as there is no correlation between cause and effect at this time, but I suspect that attitude is what makes this place work in the first place.

A salute to the elderbees for everything you have done for the rest of us! Long live the Hive!

 


Mostly harmless
 
 
 
 
    Worlock
(Tweaker God)
01-27-03 00:49
No 401723
      waY TO GO wHIPPETwHIppIT     

WHippiT i LikE YOUR STYLE
JUMP IN wITH BOTH bare FEET

The wine bottle reaction flask, and balloons,
the perfect mix of good taste and good times, ahead.

The boiler room on the roof- How Clandestine can one BEE
This is already a classic setup, It is a poetry of meth madness
Bee back in four days- some artist work with canvas and oils, some chisel on blocks of marble.
Your medium is well defined wine bottles, and ballooons.
Bravo, Bravisimo,
well done


Worlockium
 
 
 
 
    zibarium
(The Abyss)
01-27-03 02:03
No 401739
      ya'll bee trippin     

science-guy who lives in zib-biz is hearing an alarm now.

mostly concerning subjective analysis.

frankly, some b.s. is beeing spewed here now.

even though i'm empathetic w/the new news; and have been for a couple years; even after wrestling w/turps-man and lightening-man.

sounds like you're all about to go mystical on each other; complete with mega-back-patting; over some b.s. about a shitty drug.


its all good, fellas...

just don't let it get to your head.

so far, this has not been a chemistry related conversation.

what about pressure?
3 balloons?

what about rxn volume?


what's up w/ subjective states beeing weaved into data?


there is some wrong science here.

even though the vibes are swell
 
 
 
 
    Worlock
(Tweaker God)
01-27-03 02:15
No 401743
      geezmeister     

Thanks for the uplifting words,
I am very glad that you stopped in to make the post.

Ws can now manipulate temperature and concentration, to achieve a superior product., These bees are going to experiment and modify the conditions,  hitting on the ideal blend that unlocks the E and produces D-meth. It may be a certain energy level or the sequencing of reaction  conditions , like Jacked is already fired up aboutd. It won't take them very long to figure it out. This will be a good year.

Worlockium
 
 
 
 
    cthulhujr
(Hive Bee)
01-27-03 03:18
No 401757
      Swim agrees it's nice to see an idea ...     

  Swim agrees it's nice to see an idea introduced, and considered for trial, without alot of fuss and arguement.
 
After all, there is only one way to know anything with certainty, in the end.

  Thus far swim sees no reason why this reaction could not work, but everyone knows the value of an opinion. Exactly what the optimum of the conditions are, is the biggest question.

  Swim is, however, wondering about the possibilty of the reaction going to long.  Swim believed that once reduction to meth was achieved, that was about it, for the newly transformed molecule. Is that not the case?
 


  

I-R'lyeh! Cthulhu fhtagn! I I!
 
 
 
 
    wareami
(Hive Addict)
01-27-03 03:20
No 401758
      Vibes Are Groovy!!!     

These are some try-umph-ant dazes at the Hive and jubilant ones to boot! To have the MethGodz all rapped up in one thread, methodically analyzing a route that has proven superior to the conventional wayz handed down, is a sight to beehold! It demonstrates the versatility and open-mindedness that is essential in this areana! Ibee often regretted not being around during the early daze to partake in discussions such as this! The when the chance exposes itself, HDD's start frying themselves right and left! That's okay...if the kidz need to hotwire a modem to a typewriter...Wild horses couldn't drag him away!
Geez has a much better way with wordz that Ibee does and he alwayz means what he sayz! That's Cool! What's better still is his openmindedness in exploring new ideas proposed!
Worlock: The Kidz ain't the best at Art-tickle ate'ing what they see, but they try! For instance....Ibee dug UP some old posts that kinda sum UP some findings from the Kidz points of view regarding the long reflux! These posts were attempts to get bees to head off in this direction as it had produced a rare breed of Gear for them.
Post 260505 (wareami: "Re: Let's try this again, but in the right forum:", Stimulants)
Post 276696 (wareami: "Re: SWIM isn't shitting!  This really happened.", Newbee Forum)
Post 383732 (wareami: "Old Dawgs...New Tricks!!!", Stimulants)
Now, in regards to the sevenday cook, Zib and Ballz have also inquired and have been patiently waiting...so here goes!
But first...Worlock mentioned sodium thiosulfate. Ibees experiece is that when he utilizes it to clear the yellow(or orange depending on concentration), in the post rxn filtrate, he winds up with clear crystals as the end result, with no rextalation or acetone wash following the work-up. When he doesn't use Na2S2O35H2O, he'll wind up with White Xstals(yellowish tint if over acidified). Tone wash will rid the yellow, but the White color stays! Ibee doesn't like Overacidifying because he doesn't like re-collecting the gear from the tone later. With short cook times...there is no way Ibee would trust the quality or cleanliness without tone washing! He has no problem using gear as is after a long-reflux. His mindset is at a consistant 48hour at 140-160F. He use to use h2o and heat to bring on phase II! Now he uses h2o throughout the process and just waits it out! Ibee always sees signs of the conversion left on the flask, even if he isn't around to witness it taking place!
Those seven day cooks weren't benefits, per se. Unless one looks on the bright side and uses Ibees experience as a guidepost to "Don't GO there". Because after that time, Ibee thought all would be good to GO and proceeded with the work-up to find ~70% p-fed in the mix. The smell wasn't there either. Not like it had been at day five! From day five to day seven...let's just say that Ibee was being greedy in trying to achieve higher octane! If two daze is great and 5 daze was the greatest...would 7 be the greatestest???? Well no!!!
Ibee can't say for sure if a reconversion took place or not. But what appeared to be a finished product at day five turned out to be a dud at day seven...it left this bee wondering! Maybe it was the addition of impurities as Clean rerun red P was used! Who Knows!
Ibee repeated this again like a fool! But he had to know! Same amount 3g E 3g RP and 4.5 I2.
Same result! Day seven a sample was pulled and the same exact result was worked-up. Okay now what? Recover....right? Wrong!!! Day sixteen was all the torture Ibee could take! He added a shitload of aluminum, some more rerun red, some I2 and cranked UP the Heat.
Very substandard gear with p-fed present and a reminder to never go there again!
Ibee doesn't have the heart (or the hair) to repeat this scenario! Maybe there was a variable that was overlooked and Ibee can't analyze scientifically what exactly happened and where the GO went, but his only explanation is that a re-conversion took place sometime after day five on both samples!
Sorry for the lengthyness...
Hope this sheds some light!
Peace of the REaction
Have FUN-Bee SAFE



PharmulationPhreek!
http://www.chemhead.org
 
 
 
 
    Worlock
(Tweaker God)
01-27-03 03:21
No 401759
      You da' one da't be trippin'     

The Theory was proposed regardibg the availability of  The racemic forms of Ephedrine,

The conditions  had already been proposed that a slow cooler reaction might take advantage oe this E, instead of leaving it unreacted or allowing it to  form L- Meth.

A method was devised that would neet the conditions.
Results of previous reactions have been suppoetive of the plan
The first few pilot runs have been favorable,

And you say we are mystical and not scientific.

You are full of it, That is your opinion and it has no basis in fact.
Run the reaction  yourself ,then you can say what you want, Until then you are just  making up stories, and slinging crap,
 
Didn't your daddy beat you for telling lies????.

It won't be long before it is  well established

You said the one hour reaction was impossible too.
Go back where you are appreciated , and  tell your stories  to someone who gives a shit.

Worlockium
 
 
 
 
    mr_pyrex
(Head Coach)
01-27-03 04:15
No 401767
      Well I know this thread isn't the ideal place...     

Well I know this thread isn't the ideal place to post this but I am short on time and since I don't frequent the hive as much as I used to I am not fully aware of all the details, but Worlock I must say it is nice to hear from you once again.  I mean the few people I spoke with kept speaking of you in the past tense and would not explain why...it bothered me not to know why they did this...but at least now it looks as if they were mistaken...which I am glad to hear.  Well I'll bee round now and then...again nice to hear from you.  Pyrex out

Yeah and if ya don't PAID me well, I won't INFORMANT you of the answers you are seeking ;-)
 
 
 
 
    Ed_Bullwinkle
(Newbee)
01-27-03 04:17
No 401768
      This is cool ( ha ha ha PUN )     

Really though,

with clean PC's and patients, the NANO can be done with a 'coffee maker', jar, hose & baloon !!

Nice !

Bee nice,,  unless they earned it: 
then let the Flaming begin !!!
 
 
 
 
    zibarium
(The Abyss)
01-27-03 04:59
No 401773
      zib ain't the usual party-pooper     

and have already taken flak defending what it is you are promoting...and i don't mean speed...i mean the longer; wetter; less hot rxn.  the boring one; that zib spoke of over a year ago...that one that showed none of the classical signs...the pushing; pulling; b.s. misinterpretations of obvious vol/pressure...
and that same dipshit bee went to the wall to ask you all to not fall prey to the meth-god crap...and to not allow it to skewer your data.


beyond that, insults are a bit shamefull

i kill god

that's my job

any of you that don't want to bee killed?

don't play god





how many times do we have to bee wrong beefore we gain a trace of humility?
 
 
 
 
    Worlock
(Tweaker God)
01-27-03 16:36
No 401887
      Hey Hammer     


I am not sure what it is he is saying, Maybe after some sleep the mysticism will wear off,
Amazing what a few good hours of sack time will do for ones outlook,


I used to be a "Hammer" also, in a previous Cyber life,
It was a good nym
My Hammer persona mutated into "The Claw"

I coulda been a
Ballpeen, a jack , or a sledge but no had to be a Claw.

Worlockium
 
 
 
 
    Worlock
(Tweaker God)
01-27-03 17:12
No 401889
      cthulhujr     


Once the ephedrine becomes meth by loosing the oxygen, tt part of the reaction is not reversable, with the "O" gone  and no "I" or double bond, in its place that spot on the molecule is fairly Unreactive 

THe next hot spot would be one of the "N-C" bonds, and after that whatever was on the end of the chain or part of the ring depending on what the conditions were.

THe timing of the reaction has become a stickler because the aigns are not coinciding exactly with the end point of the reaction, there seems to be a eight hour period where the color says it is done but it still may need additional cooking.

 If it is cooked overly long then it appears that the molecule can either join with another at the nitrogens or begin to fall apart with a damaged aromatic ring  or the damaged rings hook together,

What is looking like the answer to be investigated is once the reaction takes on the signs of being complete to run it another 4 four hours  just to be sure
or flood it and reflux for 12 hours

The one thing I can say for certain is to not cook it for 12 hours in its dry or concentrated state , even at a lower temperature, because the yield suffers , you can be sure it is done.

The end point , escapes me how to pin it down
One way might be to add a drop of peroxide to see how much I- ion is still present, but that  may just always be present
it is not convieient  to process and bioassay a sample each time , the bioassay is so subjective , that it takes nultiple trials to be accurate
 The only thing that is a for certain is the M. P. or polarimeter
UNless you can rub an infrared spect or NMR on it.



Does anyone know if the Screen on an LCD Monitor is polarized or it it just LED  display screens that are polarized

Worlockium
 
 
 
 
    wareami
(Hive Addict)
01-27-03 17:19
No 401892
      Go'ing with what ya know!     

Okay Back on Topic!
The Kidz are pretty much set in there ways. And new proposals rarely come with a set of sure-fire guarantees! The variables are too numerous to avoid interjecting one's own technique or methodology. We all tend to "go with what we know". In that "one dimensional" thinking, we also tend to dismiss, sometimes unintentionally, following suggestions to the letter and exactly as outlined! We become set in our ways! Some things leave no room for deviation! For christ's sake, in most cases, we are trying to describe procedures and principals that could fill a book! And trying to convey these things in 1000 words or less leaves many voids and avenues open to the interpretation of the reader! I know for a fact that I won't interpret a write-up the same as any of you! Pre-conceived notions often become a fault resulting in a slight, but critical miscalculation, in the application of such proposals! Jacked provided us with an excellent example when describing the steps and processes employed in attempting the Long Reflux. He also took it a step further and openmindedly admitted that his miscalculation resided in the fact that the proposed guidelines didn't jive with his practice and experience and also was man enough to set aside his past experiences and re-stab at it with an open mind! That takes HUGE balls considering how long he's been at it! Worlock had done the same when bees proposed a refinement could reduce p-fed in an HI/RP synth that would yield a greater percentage of d-meth thus producing a more potent end result! All this shit made sense to Ibee from the word GO, but Ibee didn't know how to explain or convey it to others! Ibee is no more a chemist than pHarmacist is a test strip schooled in the art of apothecary working at the RX Storeblush
Massive amounts of time, energy and work go into the preparation H<__shockedI/RP synth and noone wants to be left holding a bagfull of shit for their troubles!
Many would rather completely dismiss some proposals as being Hogwash without even attempting the proposed. They make no bones about showing how ingrained their level of denial is either!
The long reflux has had Ibee's stamp of approval for a solid year and it is failsafe, for the newest of newbees as long as they use clean precursors and clean starter feed!
Worlock and Jacked are constantly refining as is Geez, Ibee, and the other notable Do-Bees that offer their advice, suggestions and findings!
Ibee guarantees that all bees willing to set aside their preducices and pre-conceived notions who try the long reflux proposed here, will not walk away the worse for wear or disappointed!
The worst case scenario is cushioned and can still be recovered from with the addition of heat!
It's idiot proof and Ibee is the best idiot here! He Does Not Fail, unless he's trying to 1up his own idiocy to head ya'll off at the pass!
Giving back to the collective is what proves your worth and defines true gratitude.
The credibility of fact will stand on it's own!
Peace of the REaction
Have FUN-Bee SAFE



PharmulationPhreek!
http://www.chemhead.org
 
 
 
 
    ballzofsteel
(Miss High & Mighty)
01-27-03 17:31
No 401894
      Long reflux?     

Wareami,aint it a cold push/pull?smile
 
 
 
 
    zibarium
(The Abyss)
01-27-03 17:45
No 401896
      my panties are in a bunch     

not from lack of sleep, however.

zib's trouble w/ this is all about the subjectivity of the bio-assay...which is very, very far from double blind.

just worried that an entire new science was trying to emerge from the subjectivity.

zib's experience has shown him; several times, that the very same gear; excellent gear; will vary in effects exactly as is described in these tales of two meths.

its not me going mystical here.
i was responding to the mystics.

ignore me
 
 
 
 
    ballzofsteel
(Miss High & Mighty)
01-27-03 17:54
No 401897
      Bios     

-zib's experience has shown him; several times, that the very same gear; excellent gear; will vary in effects

Especially when doses are taken in succession through the duration of the cook.
 
 
 
 
    simonsays7
(Hive Bee)
01-27-03 18:13
No 401901
      Exactly Balls     

I agree with Zib in part.  We are our own means to test the purity of the cook.  We are the best and can be the worst judges for that. 

Great to have you back Worlock.  Have you read any of the arguments that were posed by 12345x regarding whats going on in the reaction? 
 
 
 
 
    wareami
(Hive Addict)
01-27-03 18:33
No 401903
      Excuse the terminology     

Yes Ballz....my bad....you are correct...Ibee would also be wrong in calling it a "COOK", I suppose. This demonstrates my inability to effectively get my point across in addition to my hardheadedness/preconceived notionness! Any process that utilizes the necessary time to more completely reduce p-fed which yields a greater percentage of d-meth thereby reducing the amount of impurities and l-meth or unreacted p-fed, for lack of a better term, Ibee refers to as a "Long Reflux"
....mistakenly!
Sorry!
It's not really a cold method either as the rxn is exothermic and creates it's own heat!blush
Ibee will now attach himself to the whipping post and figure out from there how to administer his punishment!tongue
Peace of the REaction
Have FUN-Bee SAFE

 

PharmulationPhreek!
http://www.chemhead.org
 
 
 
 
    MnkyBoy78
(Hive Bee)
01-27-03 19:48
No 401913
      Hold On, bite down on this     

Ware...Allow SWIM to assist you in the art of "Self punishment and Reform your thinking through pain".

This procedure was once again tried by SWIM, implimenting H2PO2 ~ 80% concentration inplace of rp.  No heat at all was added as the rxn began with the rb still in ice water.  RB vessel was stoppered and placed near a base board heater and covered with a blanket.  Temp was monitored with a Fluke 50D digital thermometer.  Temp varied from 78 F (min) to 86 F (max). At t + 12 hrs, the contents were a (pale) yellowish color.  At t + 52 hrs, the contents were clear w/ only a slight hint of yellow.

Will report back for SWIM after the full 96 hrs is completed.

Why 78...I just dont know? But the voices said it sounded good
 
 
 
 
    Organikum
(Hive Addict)
01-27-03 21:32
No 401952
      Worlock     

H3PO4 - phosphoric acid is what you are looking for. Add phosphoric to the starting mixture, how much depends on the quality of your gear but its not critical like water. This is the inert to the reaction, high boiling, heat mediating and HI dispersing fluid you are after.


this is not a guess
ORG

something special
 
 
 
 
    Worlock
(Tweaker God)
01-28-03 03:42
No 402028
      Zibarium     

I agree the Bioassay is very subjective and the same persom will obtain different results at different times.
 For that reason it is good to keep am open mind and read different authors,
It takes at least three separate trials on any product to begin to accurately describe it.

This synthesis was  a learning process for me , I  tell what I discover, If it were bad idea, I would have dropped it and moved on
however
This procedure works, it works better than expected. it appears to be  better than the old method. It is not for everyone, It is not mandatory that everyone switch
 Bees are going to give it a try, in their own good time and they will decide for themselves no matter what someone else clains .
In doing so they will toss me a bone, more data and information.

Now if you posted your methodology and results, your opinion would be highly valued. 
however you have not expended any energy or put any effort into this,
So your opinions were noted, nothing more needed to be said.
 
I do apologise for the insults, I shot in your direction, they were uncalled for and I am proud of my attitude.

Worlockium
 
 
 
 
    Worlock
(Tweaker God)
01-28-03 04:14
No 402031
      Organikum     

SWIM will give it a try next run, SWIM has some on hand.
What concentration of  phosphoric acid is best so SWIM will  know if he need to hunt for a stronger brand.???

Can you give a general idea of how much is commonly used with an oz ephedrine? SWIM I realizes will be referring to the  a standard reflux

By HI dispersion ,do you mean to dilute the solution so there is improved continuous mixing of chemicals.
or
do you meam the formation of 2I-  from I2 is improved
or
both

Worlockium
 
 
 
 
    zibarium
(The Abyss)
01-28-03 04:31
No 402036
      my pissiness; not to worry     

an odd thing that zib should sound oppossed to this approach...as he is certainly not.

i love nuance; but felt that conclusions were beeing jumped to based on raw enthusiasm.

i would love to add something of value; hopefully will; until then, my apologies.
(i was pricky all over yesterday; big time back pain)
 
 
 
 
    Worlock
(Tweaker God)
01-28-03 04:38
No 402037
      Mnkyboy78     

Ah-ha very interesting, 
Alphacenturi's friend, "SWI-Alphacenturi" was wondering if that would work, it is good news.

SWIM's dog has a few H2PO3 reactions  planned I'll let them know, they are dreaming some E  will  show up, the limiting factor recently.

Worlockium
 
 
 
 
    Worlock
(Tweaker God)
01-28-03 06:28
No 402056
      sinomsays     

I have read most of 12345x's  posts 
I have not read anything in the last 2 weeks
Is there a particular article or thread that you have in mind?
If so I'd like to check it out,


 

Worlockium
 
 
 
 
    Worlock
(Tweaker God)
01-28-03 06:44
No 402057
      zibarium     

That's too funny, arguing the same point
just misunderstanding each other

My fault,  I catch so much backwash from this kinda thing
that I assumed you were flaming. If I would read what you wrote, carefully this could be avoided, One blast leads to a rebuttle flame, 
Time for my  reality check..    lucky we did not have guns.

har har har



Worlockium
 
 
 
 
    MnkyBoy78
(Hive Bee)
01-28-03 13:43
No 402096
      Worlock     

SWIM just reported that a crystal garden has formed on the flask walls.  They are of shapes not seen before.  The base (part attached to the flask walls) are rectanglular.  The portion extending inside the flask are triangle like.  (Shaped like rooftops).  What would be your opinion as far as how much longer.  The temp has been ~91.3 F for 24 hours, no additional h2o has been added.

Why 78...I just dont know? But the voices said it sounded good
 
 
 
 
    ballzofsteel
(Miss High & Mighty)
01-28-03 15:30
No 402115
      The only correlation between this and 12345x...     

The only correlation between this and 12345x theories are the time periods involved.
He mentions longer cooking times,e.g 7days ect.
I dont think much else is relevant,except perhaps the order in which he introduces his reagents,and maybe his ratios.
Forget the rest.
 
 
 
 
    Worlock
(Tweaker God)
01-29-03 06:21
No 402270
      Organic Chem books & fake Equations     

His theory that to compensate for the shit they put in pills these days ,
you need to a ratio  1(E) : 1.75(I2) because the E is not E,
Is pretty wild, but I believe him.


Then he pulls these two equations out of Organic Chemistry books and neither one of them makes sense, they look good , but when you attempt to take them apart, it can't be



123455z  makes the HI from RP and I2 and water  then   adds the
E to that which makes sense.
But when 12345x tried to support this fact , he hit a brick wall.
there are major inconsistencies in the Organic chem literature regarding the reaction. 12345x found these two references, the man is diabolically funny with his hidden humor. These equations are like stage props , they look good from a certain angle but they are fake.

1. P seens to be oxidized? (loss of electrond
while I2 is reduced  and Ephed is reduced. that can't be right
6E-OH + 2P + 3I2 --> 6E-I + 2P(OH)3

2.in this one I is oxidized and E is reduced, let's just ignore P
and forget about water too
2(E-OH) + 2(HI) --> 2(M-H) + I2

but 2 should be
2(E-OH) + 2(HI) --> 2(M-H) + I2 + 2(OH)


I messed around with these equations for a couple of hours, and could not get them to break down into a system of equatioms that make sense.
The numbers add up almost but the individual steps are a joke . maybe its just me ,


 12345x handled it this nutty way...


if HI reduced phudo it would go like this :
     2(R-OH) + 2(HI) --> 2(R-H) + I2
now you find this reaction in a book ...
 and the book states is a valid reaction 
with not just primary
 but also secondary or tetrary alcohols
"phudo has a secondary type alcohol group "

anyway find this reaction

and ill ........

ill.........

ill say

well hot damm
your the phudoephedrine man! 





ha ha he he  "well hot damn"


Worlockium
 
 
 
 
    Organikum
(Hive Addict)
01-29-03 06:23
No 402271
      Worlock: 85% H3PO4 with RP/I2     

no additional water. Count the phosphoric as inert addon and the 15% water (if 85% H3PO4 is used) counts to the water you would add anyways. Also 92% H3PO4 works.

And here I fucked something up with the equatations. I will join Worlock chained to the heating balancing equatations.

till later
ORG


nothing special
 
 
 
 
    Worlock
(Tweaker God)
01-29-03 06:35
No 402276
      drop back 20 and punt     

Mnkyboy 78

From what I read and have been told,
once SWIY are at this point
crystals and a color change.
add a little water ,
turn the heat up  + 5F
run it 6 more hours and SWIY will be there,
To be extra sure toss in a little bit more I2
It is not quite cooked fuilly yet
 SWIY must have had some good reagents

Worlockium
 
 
 
 
    Organikum
(Hive Addict)
01-29-03 07:07
No 402282
      Why I2 ? He might add H3PO3....     

To get the reaction to completion a raise in th amount of reducing agent present should be the way to go. And this is what Mnkyboy gets by adding H3PO3. I2 should be be enough there from all the pseudo(ephedrine) already reduced. It should be still in the flask if not emigrated to flee the WOD.
H3PO3 is used up. Time for a stop and refilling the tank. You might check the tire pressure now too. smile

ORG



nothing special
 
 
 
 
    Worlock
(Tweaker God)
01-29-03 07:14
No 402284
      H3PO4     

Now that is something that many
newebees think of using H3PO4.
And for them it never works, because the environment
they put it in needs the high energy  oxidation number that is supplied by R4, This Phos is an amazing substance. A living Cell uses P-P bonds as the energy source that powers a cell, .
When it comes down to it every human has one function to make ATR the cells form of currency( cash.) Stop making ATP and you are  dead.

And the gov't wants to control it, then there will be a black market in phos
In response to TV propaganda, the Cartels came into existence the day the gov't put restrictions on a substance, cause effect, the gov;t maskes criminals,

You think they would learn after prohibition created the mafia
Well gov't did learn and they learned how to line there own pockets with drug money, that what this is all about, some greesy fingered elected, appointed, officual on the take,

God bless America
Land that I love
Stand beside her,
but don't bend over 

Unless your into ButterFingers

Worlockium
 
 
 
 
    Organikum
(Hive Addict)
01-29-03 11:38
No 402307
      H3PO4 is used as solvent not as reactant     

yes thats it, and it mediates the temperature peaks and holds HI solvated for not to vanish as white smoke.

Worlock what are you referring to in your last post?

I am confused by your advise to Mnkyboy on adding I2 to his reaction for bringing it to completeness. I would think on adding H3PO3?
What is the point I overlook?

The equatations are almost complete.
Soon.

ORG

nothing special
 
 
 
 
    ballzofsteel
(Miss High & Mighty)
01-29-03 13:16
No 402322
      Wouldnt the heat generated by the reaction...     

Wouldnt the heat generated by the reaction between the relatively dry reactants dissapate more readily through a solvent and therefore perhaps not allow enough energy to kick the reduction off?
Im talking in relation to the fact that very little exteranal heat/energy is applied to this cold
push/pull and that it relies on the heat generated within.

Like,the reagents wouldnt react so readily if their molecules are buffered from each other in an inert solvent.If they were in solvent and heat was applied, well thats more along reflux lines.
A variation on an old theme.
We cant forget the ephedrine and what it needs to perform.
Lights?

This is not the same as a long HI reflux.


PErhaps
 
 
 
 
    wareami
(Hive Addict)
01-29-03 14:53
No 402332
      Y Eye Too?     

The Kidz have yet to explore the acidic side(H3PO3), But they have used UP their share of RedP. In every stalled or incomplete rxn, they never had any success with bringing it to completion with the addition of extra RP. They alwayz wound UP with excess RP to be filtered off in the end. They don't know the mechanics behind it, but never stopped to question the success they had when bumping the rxn back on track with added I 2. Usually in .5g increments.
The calculations involved in starting a reaction, ratio wise, should be sufficient to supply the P4 molecule and the only loss it seems is the generation of HI. If a good amount of H3PO3 was used at the proper concentration, the addition of I2 should provide the needed boost for a recycling to take place and thereby create a re-generation of HI!
IMHO....
Peace of the REaction
Have FUN-Bee SAFE




PharmulationPhreek!
http://www.chemhead.org
 
 
 
 
    Worlock
(Tweaker God)
01-29-03 23:33
No 402439
      Organtikum     

You enjoy this too much

If one is using P,P tanks and doing a fast reaction, it becomes apparent that most of the iodine escapes from the reactin flask and passes doen the hose to be trapped in the water.

This water after 4 oz or so is red and thick with iodine & HI
If one were to recover the Iodine after a reaction  most of it cones from the tanks ans a snaller amout is recovered from the wastes generated in the reaction  flask,
The hhose is always stained red on the inside  whether you do a fast or slow reaction. 
Even in a reflux reaction with a long condensor  Iodine is escaping, the proper technique is to bring a hose off the top of the condenser, attach it io a funnel and invert the funnel letting the wide end rest in a tray with a few inches of water, this  captures the gasses enitted from the reflux.

The way most reactions are rin from the stoicochemistry
Red P is added in abundance and a big mud pie of it sits in the flask.
It is common  knowledge that the I is producing the driving force of the reaction ,
It is the fuel  the Red P is like the spark plug ,
Now I doubt that Mnky boy has any H3PO4  available if he did he would have used it.
He wants to be certain ther the Ephed is reduced to the iodate and changed to meth m there is a theory out that hther pills are never cleaned well enough any more , the 10 grams of E is more like 6 grams of E and the rest is either a sulferouds compound ar a spiral macromolwcule like povidone that traps E and I. Silfer is a inhibitor of iodine in this reaction, it will shut a reactionm down

So because of the dirty E
THe certain losses of I
and  from prior experience ,

 adding a little I2 will refresh the reaction fuel and allow it to complete, immediately upon adding the Iw it begins to react it is visibly apparent.
Now I hsve no problem with H3PO4, but I have to stick with what I know so until I actually use the H3PO4 , I am not qualified to reccommend it, suppose something happened that Mnkboy did not understand, If I can't ecplain what he needs to do I look like a fool, and my credibility is ahot, and mnkyboy could lose the reaction or get hurt You see  I only advise bees on actual knowledge about, I don't speak from Knowledge of aquaintence.
that rule seems best  from emnarressment.
So although I will try new things on my own , I don't send a bee into the trenches first.
The additional I2 was needed in his reaction did you note the temperature he was running at 91 F 
not C but 91 F that is  around 33 C
The phospjourous is famose for changing its activity in quantum leaps
 and not in a linear fashion , but in sudden stages the next major excitation for the phos is around 110 F, then at 150 F, 189 F .

His chances of increasing the heat to any of those levels is slim
the theory is that heaty is ther culprit in creating toxins.
Six more hours on a dryside reaction is going to make it very dry m so a little water is efficatious, and a litrtlw \e iodine will definately drive the reaction to the right.

Now C'mon you know this stuff, don't you? Making me explain it when I need to get on with the Cosmic Power thing. It is difficult to type that much, for me it is anyway, two years ago I had a reaction , to some bad antibiotics , and it left me almost totally blind Stevens Johmsons Syndrome  you can look it uo on the web
















Molecule: meth ("c1(ccccc1)CCC[NH2+]C ")



Worlockium
 
 
 
 
    Worlock
(Tweaker God)
01-30-03 00:03
No 402446
      Ballz     

Nards of steel,
Nonads 
 the phosphorous is not very active at these cold temperatures, and the amount of exothermic reactionm heat is not noticable, some external heat source is needed, infra red at the frequencies that show up on the spectroscope would be a wild way to control a reaction, just at the freqwuency needed and the side reactions would be minor in some  systems















Molecule: meth ("c1(ccccc1)CCC[NH2+]C ")




Worlockium
 
 
 
 
    alphacentauri
(Hive Bee)
01-30-03 00:53
No 402470
      There is something I don't understand in the...     

There is something I don't understand in the theoric aspects of the reduction: wether you start from elemental P4 or H3PO2 (hypo) or H3PO3 (phosphorous) you start from a substance in a reduced oxidation state, and what remains of that at the end of the reaction should be a form of P at a higher oxidation state, if not the highest. At the end you should have H3PO4 (phosphoric). In the meantime elemental I2 is reduced to its negative anion in acidic environment. So you have the species HI not all dissociated, maybe, due to the high concentration in very little solvent (water). So the first of this reduction chain is the redox reaction between reduced P and elemental Iodine. Then appears pfed, E-OH, let's call it. We have as intermediate product iodo-ephedrine ( synonimous of iodo-methamphetamine). What does this mean? That the first reaction in which E-OH is involved is the substitution of the alcoholic group with an iodine. But OH is a very bad leaving group by itself, and the species I- (anionic) is not enough nucleophilic to replace OH, so chemical theory teaches us that the neutral H2O molecule is a good leaving group and iodide can kick it off, so we have first the protonation of the alcohol with the formation of the species E-OH2+, from which H2O goes away leaving E+, the carbocation of ephedrine, a secondary carbocation, and this reaction is favoured in acidic medium (the H+) of HI and H3PO2 or 3. It is a SN1 reaction, a monomolecular nucleophilic substitution. I think this should be settled. What I don't understand is how the species E-I reaches the full hydrogen state (E-H, that is to say the honey, the cake, the fabulous meth). Can someone give me some light and drive away the darkness of ignorance ruling in my drug-fucked brain, please?
Then Organikum says that he can use H3PO4, that is to say phosphorous at the maximum oxidation state (+5). At that state P can't give away any more electrons, since it has the same electronic configuration of Neon. So how is chemically possible that the P(+5) species reduces I(0) to I(-1)? I can't understand that, or there's something I miss. It would be too nice if we could use phosphoric, since it's freely available even in industrial quantities!
Worlock, I'm still on the Ac..t..ed extraction phase. I'm pretty long because this is a period in which I work a lot, when I'm ready with the cold reaction I'll post or PM. Bee patient, I work over 48 hrs a week!crazy
 
 
 
 
    alphacentauri
(Hive Bee)
01-30-03 01:46
No 402486
      kinetics involved     

Another consideration before going in bed: an SN1 reaction has by its own nature a kinetic law of the first order. I don't know how the reaction proceeds, but I know that since I deal with a SN1 I'll have only one species determining velocity. We have an intermediate state costituted by a secondary carbocation, a pretty unstable particle. So, since the carbocation reacts rapidly as soon as it is formed, the reaction will proceed with considerable speed (the carbocation is craving for something negative, a base, a nucleophileto saturate its positive charge). So if the carbocation reacts rapidly as soon as it is formed, that will not be the decisive stage for the reaction speed. But the formation of the carbocation is indeed; in other words everything speeds up the formation of the carbocation speeds up the whole reaction. And what promotes the formation of the carbocation? It's definitely not the species I(-1), otherwise we had an SN2 and not an SN1 reaction - as a matter of fact I(-1) is involved after, when the protonated alcohol has already expelled the neutral H2O from the molecule (this process is favoured by a polar solvent, water) -. The carbocation promoting species can't be other than H+. Where does this H+ come from? Or from HI or from H-H2PO2 (monoprotic acid), or H3PO3. If we use redP, obviously the only source of H+ will be HI. If we accept this becomes understandable why we can use H3PO4 as Organikum states: if, instead of using I2 we pour in the flask directly HI solution, then phosphoric acid enhances the formation of the carbocation, because it works as a simple generator of acidity, not as a reducing agent to generate the anions out of iodine. Am I wrong? Then if my considerations are verified, we can increase the conversion of pfed to meth only adding more hypo or phosphorous or redP, and not iodine; the concentration of iodine above a certain quantity would be ininfluent, isn't it? Folks, while there is early evening, here is late night. I'm going to rest my tired whitish bones between the sheets. Good night, or better, good evening for you.
 
 
 
 
    Organikum
(Hive Addict)
01-30-03 08:07
No 402606
      No this I didnt say alphacentauri!     

Please read my posts on this, I did say that H3PO4, phosphoric acid can be added to function as an inert aka in no way participating in the reaction, solvent. It has the function to work as "heat spreader" eliminating "hot spots" and mediating the "dry" reaction for being less violent. Water forces the the reaction and is not   useful to add. (of course you can add so much water or H3PO4 to drown the reaction complete but thats another story).
H3PO4 is no reactand.
It can in no way substitute red phosphorus, H3PO2 or H3PO3.

I thought halogenations are direct radical substitutions? I maybe wrong.

Worlock! I know Mnkyboy so I was sure he would have some H3PO4 handy and his pseudo will be clean. So I thought I overlooked something as my practical experiences with RP/I2 are limited. It was never my favored reaction - to violent to messy - but the new developments regarding HI in special made me change my mind and walk the HI path as a HI only reaction is for sure after my taste. (thanks to Ballz as he never gave up on this)

Worlock? I didnt tweak your name as you will have mentioned....
And I didnt post the questions for teasing you as I regard thus as very bad style.

FREEDOM
ORG

special
 
 
 
 
    MnkyBoy78
(Hive Bee)
01-30-03 14:37
No 402655
      Typo     

In my post above (Post 401913 (MnkyBoy78: "Hold On, bite down on this", Stimulants)) the term H2PO3 is wrong.  It needs to be H3PO2 or hypophosphorous acid.

I edited your post for you /Rhodium

Why 78...I just dont know? But the voices said it sounded good
 
 
 
 
    Daphuk_up
(Hive Bee)
01-30-03 20:01
No 402721
      Ok, damnit, I give up...     


Could some bee please tell me where in the hell you guys are getting this stuff.  I have hit the blue roof, orange roof, the marts, and a couple of local nurseries, none of which have anything resembling a phosphorus based acid anywhere in the entire nursery department.  Sure, they got triple super-phosphate, but I dont think that is going to help any. crazy

Someone, just please PM me with a brand name, description of container, or something which will clue me in.  I would be forever and ever grateful for this help. smile


Regal Sir Palladium and the Harlot Chlorine...they make such a cute couple. ^_^
 
 
 
 
    alphacentauri
(Hive Bee)
01-31-03 01:42
No 402812
      halogenations for Organikum (and anybody else)     


I thought halogenations are direct radical substitutions?



Halogenations can be radical or ionic, and can be substitution or addition reactions. I would like to explain in details, it would be very enjoying for me, but I don't know if a post is the right place for a beautiful chemistry discussion like this. Anyway if you irradiate chlorine with UV you obtain free radicals. Those are single atoms with an unpaired electron each, 17 electrons, practically the neutral chlorine atom. But why neutral, and so unstable? Because the valence shell has two sublevels, one full, and one should have 6 electrons to be full, but chlorine has only 5 electrons. So, in order to get the 6th electrons the chlorine radical snatches an electron from anything, anybody. If sir chlorine finds mr methane, well, mr methane remains without an hydrogen. Yes, because the only way sir chlorine can take one of mr methane's electrons, is "convincing" one of mr methane's hydrogen to divorce from him and marry sir chlorine. In doing so mr methane becomes a radical and when he finds a happy couple of chlorine gemini, he says:"hey, chlorine, now gimme one of your atoms, and tell the other gemini to fuck off", so mr methane radical becomes mr methyl chloride. And the other gemini? He is a radical now (once runs the hound, and once the hare) and he repeats the cycle. But in chemistry there are two ways of breaking a bond: the omolisis (the bond breaks right in the middle like sir chlorine and UV rays before) or the eherolysis (one of the gemini is greedy and keeps all the two electrons). In this last case we have an ionic couple, or better, a positive part and a negative one. Imagine sir chlorine gemini approaching mr ethylene. Mr ethylene has a negative crowd between the two carbons, and the electrons of the chlorine single bond are not very friendly with this negative crowd, and run by the opposite side of the two chlorine gemini, leaving one of the gemini uncovered, and the other supercovered, so one part of the chlorine molecule becomes partially positive, and the opposite side partially negative. The positive part is oriented towards the ethylene double bond, till one of the double bond, the easier to move (pai bond is called), leaves the carbon-carbon axis and joins the positive part of the chlorine molecule. Doing so the other carbon becomes positive, because it has one bond less: he is a carbocation now, he has two electrons less than what he should have, and so he wants to fill this gap, searching for something negative. And what does he find? The negative chlorine anion, the gemini left apart by the positively polarized chlorine of before. When he left his brother, he remained near, so now he can join the carbocation and says to his former gemini:"fuck off, my old mate, I'm better with this carbon now than before with you", so we have 1,2di-chloro-ethane out of ethylene and chlorine. This is an addition reaction, of ionic type. And there are susbtitution reactions as well, in which the particle is something thirsty of nucleus: they want protons, big massibe bulky protons. Usually nucleophiles (nucleus lovers) are conceptually associated with bases, at least with coniugate bases after acidic ionization, but not necessarily a strong base is a good nucleophile. Too many parameters in between: temperature, solvent, the leaving group. Yes, a nucleophile to behave as a nucleophile needs necessarily something he can kick off from a neutral molecule: in the case of ephedrine and iodidric acid the leaving group is water, it can't be the alcoholic oxydril, since it has a negative charge, and it is more basic than the iodide anion, but the oxydrilic oxygen of the aminoalcohol ephedrine has two couples of electrons not shared with anybody, and an hydrogen ion is attracted by one of those couples, doing so the OH turns out to be water, and the positive charge of the original hydrogenion is distributed to all the "acid coniugate" ephedrine. Now the alcoholic group is a good leaving group, as water, and can be kicked off even by weakly basic and pretty lazy iodide anion. In this case the iodide anion is a nucleophile and water the leaving group.
Organikum, we could go on all the night, I'm enjoing too much, I love chemistry, I reach climax if I keep going like this........I leave all now. If you need other explanations I can manage to give you, you're welcome, I'm at your complete disposal.laughlaughlaugh

 
 
 
 
    MnkyBoy78
(Hive Bee)
01-31-03 05:13
No 402866
      Thanx alphacentauri, a understand was obtained     

Thanx alphacentauri, a understand was obtained through your explanation with the "drama" in your post.

Rhodium: Thanx cheif

Daphuk_up:  doubt the "anything -ous" would be found at Wally-World, (any) Depot, or what not.  Well, unless your local chemshop has a yellow or orange roof.

Why 78...I just dont know? But the voices said it sounded good
 
 
 
 
    BenWiFFen
(Line Monitor)
01-31-03 13:44
No 402919
      Urea looks promising     

Urea looks promising. Found at good garder or farm supply. How about using starch with a little bit of your post rxn liquid. Won't it detect any traces of I2? Freebase will heat up right now. Hcl will take longer to heat up on it's own.

When you finally get the BOMB you'll see everything else was good practice.
 
 
 
 
    Worlock
(Tweaker God)
01-31-03 20:57
No 403040
      Organikum     

Gottcha on the phospohoric acid,
I was making it more difficult than it is.
Just woke up in the middle of a dream, about this prospector
in the Alaskan North slope, was cooking some chili in the cold, damp
reaction flask method thing. The old timer was real wxcited about adding phosphoric acid to the solution,  Wondered if it would be beneficial to add it in the begining or just at the final cook off?
It was a dream that was on going, so I had no answer for an imaginary old woman (who says prospectors can't be female),



Worlock? I didnt tweak your name as you will have mentioned....


Don't know what you mean.



And I didnt post the questions for teasing you as I regard thus as very bad style.



I know that, it is how you ASK IT HHEHEHE, just kidding. You said nothing out of line, sometimes I just need some sleep, and I make odd posts, there is nothing amiss

Hey ,tease me go ahead! I have had worse,
Don't worry about me, if I could not take the heat, I would not stand in the fire, all the time.
The story about blindness is true, except that several months ago, thanks to God, and a good doctor. and my own effort, the vision has improved, I am a bit of road hazard but I can drive during the day.
A little sad because when I could not see, I was really into playing music (guitar), noW i CAN SEE PRETTY WELL, HE MUSIC LOST ITS IMPORTANCE.


Worlockium
 
 
 
 
    zibarium
(The Abyss)
02-01-03 00:45
No 403103
      perhaps you could close your eyes?     

and stay with the music?

wink

glad you're with us!
 
 
 
 
    Organikum
(Hive Addict)
02-01-03 06:42
No 403191
      Worlock: H3PO4 is added at start     

This is the way I can testify it was done in countries far away by the local wizards.

ORG

nothing special
 
 
 
 
    Worlock
(Tweaker God)
02-01-03 07:54
No 403203
      Zib     

Good one,
That's pretty much the way I had it figured, too.
But I open my eyes and 'ur still here


Maybe I can get a gig every night,
playing in that Old Man's piss bar, The one you hang at
Wit the rest of the pud slappers 


Oh take my Cadiiillllllllac, and take my heaaaaarrrrrt
Soooooooeein U'll leave me\,  must we paaarrrrt 
before I drink your beeeeer and you smell my fart.

Yeah its The Space Soldier of Texas,
fomerly known as The Cyber Corn
all the way from across the road
music to slap a pud by
Hey Space why did you change your name from Cyber Corn

{"Bug off")

It was cause they kept calling you "Cyber Corn holer"
Hey I heared they called him the "Cyber Bunge holer," cause his music stinks.

("Man, lemme outta here")

That's what your chili tastes like, "Bunge hole"

("Flap")

Yeah how come it always tastes like dog bunge hole?

("Suzy, Come up here, show these stub legged, short horned cowboys, your modified sudiferous glands, while I get the pony warmed up, this is gettin' ugly")

yeah thats what we wanna know

("It tastes like dog bunge hole cause it IS doggy bunge and you been byn' it for a month, 'bout time you fingered it out")

Get him boys

("Lets blow , you drive babe")
(" Ha Ha  Smokers of dog Bunge, is what you are")

Zooooommm
MMuuuaaaahahahahahahasha

Worlockium
 
 
 
 
    Worlock
(Tweaker God)
02-01-03 08:18
No 403207
      Hey Alph     

Easy for you with your Sn1 reaction,
Sn1 - dehydration
                      H+
E-OH  +  HI  ------> E-OH2+   +   I-
E-OH2+    -----> H2O  +  E+(carbocation)
E+   +    I-  ------>   E-I



But what about the Sn2 reaction,
                   P4I3
E-OH  +  I2 ----->  E-I  +  OH-  +  I-



Both Sn1 and Sn2 have the intermdiate carbonium(+)ion
or Carbocation(+)
How do we get the I off the E ?
Does it fall off when it hits   H I ?
Does it stay on until the solution is made basic?
What about forming double bonds, or reforming the alcohol?

Seriously I would like to know what you think about the final step.



I am positive(+) it is a CAT  ion
NA its an ANion(-)


Worlockium
 
 
 
 
    ZingoBingo
02-01-03 18:30
      Dang , Wor . . .
(Rated as: insignificant)
    
 
 
 
    Worlock
(Tweaker God)
02-01-03 20:12
No 403364
      Zingo Bingo Knows good tunes     

I see you are a Maestro and appreciate the subtleties of a love ballad, THe way a good man rakes and takes, so she may give.
but he keeps takimg from a bad woman,

You are also  Able to see between the lines, his years of sacrifice and his displeasure at her disloyalty .
Who is realy the Sadist,  who is at fault. It matters little any more, drunk, bad digestion,

 works for me.

The Tabs I'll get 'em right out, same story , same song, that's been repeated over and over with a variation  so slight.
It is classic 12 bars of country blues, Chuck Berry style , As written byt Claptin but played by the Ventures with  the drive of Axels  full flanger &  gain maxed for optimal feedbach.


http://www.geocities.com/zabba_alba/tab2.htm

Where the hell is my Do-bro
The Sultan of Korn
Or maybe you would prefer  Cool edit pro 4.0

Worlockium
 
 
 
 
    alphacentauri
(Hive Bee)
02-02-03 17:18
No 403630
      I think this, Worlock.     

I think this, Worlock. E is a secndary substrate, since the leaving group is a secondary alcohol and leaves a secondary carbocation. Apart from any consideration, a secondary substrate could react with both the mechanism, SN1 or SN2. You know, SN1 is favoured with tertiary substrates (a tertiary carbocation is much more stable than a primary one), and SN2 is favoured with primary substrates. Now let's consider two parametres: the steric hindrance and the effect of the solvent. The OH bearing carbon atom is between a massive lipophilic aromatic 6term ring at one side, and a carbon bearing a methylaminic group at the other side. All these groups are pretty voluminous and they don't allow easily the formation of a penta-cohordinated transition state, as would be in a SN2 in one single stage. So, if we consider the steric effect, we could say that a SN2 would be not favoured in the formation of iodomethamphetamine. Now the solvent: SN1 proceeds via the formation of a carbocation, so it requires a medium that can solvate charged particles, a polar solvent, in a word. SN2 not, is favoured in apolar solvents, particularly if a solvent can solvate anions less than cations, so the leaving group (less nucleophile than the attacking nucleophile, so less basic) can be solvated a bit better than the nucleophile. Such solvents are only slightly polar, and usually don't contain hydrogens that can be removed as acidic hydrogens, the so-called aprotic solvents (DMF, DMSO, crown ethers). Now what we've got in our rection flask? Water, HI, hypo or phosphorous acids, polar medium anyway, even if we use RP. For these reasons I think SN1 way is more probable. But it's only my opinion. Which reactions could compete with a SN reaction? Elimination ones, thus forming an alkene unsaturated on C1-C2, but....who knows? Anyway when eliminations compete with substitutions, eliminations are favoured by a high temperature (other parameter to consider), and the low polarity of the medium (an alkene needs apolar medium to get solvated). Obviously in acidic water and low temperature elimination is not favoured and substitution should be the main reaction. Ah, I was forgetting this: the more ramified is the forming alkene, the higher probability you have of elimination instead of substitution (Saytzev's rule, if I remember). Now a secondary substrate is liable to give elimination more a primary and less than a tertiary. In the end the reaction will be a compromise between all these factors, for this reason I think that your way, the cold reaction, can give better results than a long initial reflux. I think the best is some days with the cold reaction, and then finishing it with some reflux. I liked your way from the beginning and frankly I can tell you that I believe in it.
About the second stage (the full H state) I'm still thinking about it.
cool
 
 
 
 
    alphacentauri
(Hive Bee)
02-02-03 17:28
No 403637
      Shit, I forgot the stereochemical aspect.     

Shit, I forgot the stereochemical aspect.
If we had a SN2 we should have inversion of configuration, so from a R reagent we should obtain a S product, so from L-ephedrine we should obtain d-meth, and from d-ephedrine (pseudoephedrine) we should get L-meth. But this doesn't happen, so this could be another evidence against an SN2 mechanism. With SN1 we should have racemization, but we have a product of optical purity (d-meth, wether we start from ephedrine or pseudo). Shit, this is a maze, what's the answer to this?crazy
 
 
 
 
    Rhodium
(Chief Bee)
02-02-03 21:10
No 403680
      not an issue     

The stereochemical aspect is not an issue here, as the only chiral center left after the reduction (the amine-bearing carbon) is not touched by HI, only the OH, which is nixed anyway in the process.
 
 
 
 
    Worlock
(Tweaker God)
02-02-03 21:37
No 403698
      You are good at this     

SWIA-C has got to be careful , all reports in the past approached from the point of view that it all was the same reaction.
However depending upon the environment I /RP /E /water  seem to be able to take a variety of paths , all of them going on at once but with some mechanisms predominating in different enviromnments at different times Phosphorous behaving  strangely at different temperatures, Iodine never sure if it wants to be a metal, or a salt or just evaporate into thin air , only to show up somewhere else red again


So, if we consider the steric effect, we could say that a SN2 would be not favoured in the formation of iodomethamphetamine.



hmmm  a very good point, SwiW always wondered how the I- could get in so close to the Alpha carbon. SwiA-C answer is , general it  won't


Water, HI, hypo or phosphorous acids, polar medium anyway, even if we use RP. For these reasons I think SN1 way is more probable.



hmmm this would lead one to think that the Sn2 mechanism is a hold over from earlier liturature and SwiA-C is right again,

The splitting of I2 into 2I- in the presence of P4 is a farce without a source of easy to get protons, supplied by water or an acid.

But the SN1 reaction is initiated with a simple acids  addition of H+ and not a redox reaction.


Obviously in acidic water and low temperature elimination is not favoured and substitution should be the main reaction.



Your logic is outstanding, makes ,much sense,

SwiW called the cold reaction "Cold Lazy Arse method"
SwiW knows that when they used a 1 hour cook, it always would get a bitterness, when vaporized in a glass tube, that requiires re-crystalization to remove,  With the Cold Lazy Arse method, under 110F SwiW has not had to recrystaslize , since it was not bitter. The bitterness was present in samples taken before the Cold L A method had finished, Indicating that some chemical has not finished cooking, the obviouis choice would be epherdrine, but E has a distinktive taste anmd it must be that  Ephedrine and pseudoephedrine have different taste and reaction rates.. In fact they are seeming to be much less similar than we have been led to believe. It is no wonder extractions are harder, they add things that will block one or both from being extracted , complicating a once simple process. .

Swi-Us may have to extract ephedrine ,then go back and extract pseudo with different conditions.

formation of Ephedrine from pseudo would be apparent in much higher yelds  20-25% improved , but AwiW has not done enough to yet be certain what is going on there. It is possible and it may prove out  in the end, somewhere near the 48 hour point.
Unfortunately, precursors are becoming scarce and another approach may need  to replace this.

Thanks for your insight, It has cleared up much and has left SwiW with a new set of problems, Always gaining ground, the playing field keeps changing.


Worlockium
 
 
 
 
    Worlock
(Tweaker God)
02-02-03 22:11
No 403711
      Stereo     

The SN1 May Be occuring on the surface of an I- charged Phosphorous particle, The RP does not dissolve. This fact forces the reaction to o be a surface effect since the P4 loads up with Iodide.

The E also has to apptoach with the proper bonds exposed,
and in the proper configuration.
I have been able to model only two stable forms of the Ephed / pseudo  molecules

1. One is relatively flat and long
2. The other is L shaped with the ring at a 90 degree offset from the rest of the molecule , in the L shaped form m the stable isomer has the oxygen sticking outward and ro one side at the bend of the L. leaving an opening at the alpha carbon
If the reaction occured at this opening , although the bonds can rotate, they won't, it is too crowded for them to begin spinning and flipping.
Heat may force more I- to leave the RP particle, making it easier to reconfigure abd also making the molecules more energetic and able to reconfigure.
This would explain the violence in the 1 hour reaction at 190 F
I- ions and not HI  would suddenly become abundant, and most of the reaction occurs away feom yje phos particles damaging a potion rotating and not rotating achieving equilibriom based  mainly on stereo chemical probability with a minor influence  from the precurserd configuration.

i'LL TOSS UP PICTURES IN A WHILE
  they are revealing about the nature of the isomers of E


Worlockium
 
 
 
 
    Rhodium
(Chief Bee)
02-02-03 22:12
No 403712
      more pathways
(Rated as: good read)
    

The splitting of I2 into 2I- in the presence of P4 is a farce without a source of easy to get protons, supplied by water or an acid.

I wouldn't say so, 2 P + 3 I2 2 PI3 happens easily with a little heat, and the hydroxyl group of (pseudo)ephedrine then performs a nucleophilic attack on PI3 and with a little I- shuffling and elimination of HPOI2 we get iodoephedrine. The HPOI2 can then turn another two (pseudo)ephedrines into iodoephedrine with relative ease.

All this at the same time as more direct iodinations take place, so there are many reaction mechanisms doing their thing simultaneously...
 
 
 
 
    wareami
(Hive Addict)
02-02-03 23:50
No 403728
      Hey Now....     

Don't think ya'll are gonna ditch the Kidz that easy with all this ChemSpeak!
This HIGHly informative rally has stamped a hugh on Ibee's farhead replacing that Big "L" normally stamped there!(silly bee's...."L" = Looped nt Lunatic!wink)
Ibee's question is: Can anybee identify the governing factor that creates the racemic variety of Meth (50% l-meth/50% d-meth)in the rxn. Does this occur with ephedrine as well as pseudoephedrine?
Is it the iodo factor?
Is it heat?
Is it ratio of reactants?
Is it length of time exposed to HI or
Is it concentration of HI?
Ibee doesn't want to derail the current discussion, he's just searching for a clearer understanding if one is known.
The correct answer may help direct us all toward a consistant successful rxn method thereby directing bees toward more d-meth and less l-meth.
Peace of the REaction
Have FUN-Bee SAFE


PharmulationPhreek!
http://www.chemhead.org
 
 
 
 
    Rhodium
(Chief Bee)
02-03-03 00:10
No 403734
      Why racemate?     

Can anybee identify the governing factor that creates the racemic variety of Meth (50% l-meth/50% d-meth) in the rxn.

Where is the evidence that would be the case? In my opinion racemic meth could only be the product if the starting material used was either racemic ephedrine or racemic pseudoephedrine, which is not likely if commercial cold medication was used as a source for the starting material.
 
 
 
 
    wareami
(Hive Addict)
02-03-03 01:09
No 403746
      Loose Terminology     

Where is the evidence that would be the case?
Ibee sees that term used way too often and just assumed that most HI/RP reductions of pseudoeph resulted in the racemic mixture...incorrectly I suppose!
Upon referencing the Merck listing you posted on pseudo(thanx!cool), I see where Ibee was mistaken!
So would Ibee be correct in assuming that l-meth is excluded from the picture if the starting precursor is d-pseudo?
An unfinished reduction would then include a mixture of d-pseudo and d-meth only....correct?


PharmulationPhreek!
http://www.chemhead.org
 
 
 
 
    Worlock
(Tweaker God)
02-03-03 01:19
No 403750
      2d representation of 3d simulation of isomers...     

2d representation of 3d simulation of isomers


L shaped configuration


Flat configuration


Worlockium
 
 
 
 
    Rhodium
(Chief Bee)
02-03-03 02:05
No 403768
      Dynamic structures     

Here you have all the interesting molecules, a thick bond means the bond is pointing towards us, a dashed that it is pointing away. You can rotate the molecules individually by holding down the left mousebutton on a molecule and drag it around. Right-click and choose ball-and-stick models, animate it and whatever you want. This must make the stereochemistry clear to most.













Molecule: d-Methamphetamine ("C[C@H](NC)CC1=CC=CC=C1")


d-Methamphetamine













Molecule: l-Ephedrine ("C[C@H](NC)[C@H](O)C1=CC=CC=C1")


l-Ephedrine













Molecule: d-Pseudoephedrine ("C[C@H](NC)[C@@H](O)C1=CC=CC=C1")


d-Pseudoephedrine
 
 
 
 
    wareami
(Hive Addict)
02-03-03 02:18
No 403778
      PharmOut Rhodium : !!!!!!     

It's a good thing Ibee has TunnelVision to keep UP with all them Moles! It's funny how when the fork in tunnel bares to the Right....Ibee Gets HIGHer!tongue
IWare



PharmulationPhreek!
http://www.chemhead.org
 
 
 
 
    Worlock
(Tweaker God)
02-03-03 04:14
No 403832
      Rhodium     

First I would like to congradulate you and the Geez' on the sucessfull methamphetamine synthesis using HI without Red Phos.

Secondly - Try it, mix RP with I2, it just sits there.
The I2 slowly melts and dissipates in moist air like always, but there is no active reaction. Mix in some dry ephedrine and it might do something, but only because it can remove a proton from the hydroxode  group, still no major amount of activity will begin
 
     P4
I2  --->  I2  

             P4
I2 + 2H+   ----> 2HI

                  P4
I2 +  ROH  ----> RI + HI + 1/2(O2)- this does not go very far

Without water it is a dead reaction. you could substitute other things to provide the proton .

SwiW at one time would mix RP, I2, and E together. The reaction was started by injecting  drops of  water  into the hose that drained into the reaction flask.
This was good because it can be mixed  well before iniiating the reaction.
The other advantage was it prevented SwiW from addibg too much water, drowning the reaction, stopping it from completing in an hour.

The fast reaction was probably better on smaller amounts under 14 grams, simply because it was over sooner, and the small violemt thing was controlable,
I woud not want to see a pound of E fire off in a fast reaction, too intense, too exothermic, too much pressure and the vacuum portion would be worse than the expansile,
SwiW haa seen large fast reactions get violent appear to slow down , then come back even stronger . expand and contract several times within 5-10 seconds

There was a story, whether true or not,  about a couple who would put it in a rock tumbler to mix it super well before reacting the mixture

Worlockium
 
 
 
 
    Worlock
(Tweaker God)
02-03-03 05:09
No 403850
      There was a bee "fj" who at one time     

There was a bee "fj" who at one time worked for an ephedrine distributer
The distributer is usually also the manufacturer.
"fj" a friend of Dwarfer said, the ephedrine came in from China, they would boil it in HCl for 24 hours. This would racimise it( convert it to the different isomers) . He also added that the ratio of ephedrine and pseudo ephedrine was 60/40 but he did not know which was the 60 and which was the 40.

L-ephedrine makes D-methamphetamine this is not configuration but optical activity. The only change is the removal of oxygen , no rearrangement occurs to change the L to D/

L methamphetamine is present in vicks inhailers, it is called desoxy-ephedrine but probablt should be named either L-desoxy-ephedrine or desoxy pseuso ephedrine . These would all be incorrectly names also.
there is
L-ephed  and D-ephed or  ((-)ephed  and (+)ephed) respectively
L-pseudo and D pseudo or ((-)pseudo and (+)pseudo)respectively

[1R,2S] or (-) or (L) ephedrine are the same
[1S,2R] or (+) or (R) ephedrine are the same
[1S,2S] or (+) or (D) pseudo are the same
[1R,2R] or (-) or (L) pseudo are the same




Worlockium
 
 
 
 
    zibarium
(The Abyss)
02-03-03 05:57
No 403861
      much thanks; great illustration     

without water; no rxn

what substitutes might bee worth consideration, for proton providers?

any attempts with inert mediums to provide better fluid dynamics in water substitutes?

isn't the proton doner doing double duty, in a sense, in providing the viscosity that is needed?
in rp/i, swiz felt an urge to have it sloppy 'wet' without much water, and wondered how to try.

seems detrimental, by way of possible overheating, to have a slurry so thick as to get hung up on the sides of a flask.

peace, bees
 
 
 
 
    Worlock
(Tweaker God)
02-03-03 06:21
No 403867
      I have dragged around the stick figures.     




Here you have all the interesting molecules, a thick bond means the bond is pointing towards us, a dashed that it is pointing away. You can rotate the molecules individually by holding down the left mousebutton on a molecule and drag it around. Right-click and choose ball-and-stick models, animate it and whatever you want. This must make the stereochemistry clear to most.




First -L-ephedrine and D-pseudoephedrine do not have identical configurations

Second - I have dragged around the stick figures. And come ip with a very different conclusion  this picture is too simplistic,  as long as we continue using terminolgy  (D,L) (+,-)that relates to optical activity and not configuration, we will be stuck.
I have said this 2  over two years ago, repeated it many times since then, sooner or later enough bees  will get past the inital shock of seeing 4 enantomers and the discussions will quit referring to useless optical terminology. Then there will be some understanding that these enantomers have a wide range of physical properties.

It is not any fun to try and deal with stereochemistry, when the topic begins with D and L because at that point, What can be said ?
only this  D and L do not accurately describe configuration they refer to optical activity

The distributer ruins the E for our purpose when they racimize it.

There are 2 chiral or assymetrical carbons in ephedrine
22=4 isomers (enanmtomers)

and since the amide N is also assymetrical( by some authors) there can be even more 23= 16

This is not my opinion this is the present way of defining configuration

Look it up 
relative diastereo isomers (diasteners)
enantomers
Chirality


Worlockium
 
 
 
 
    Rhodium
(Chief Bee)
02-03-03 10:40
No 403935
      Clarification/Correction     

See Post 401416 (Rhodium: "Hermann Emde's Ephedrine Chemistry Treatise", Stimulants) for a more in-depth discussion of ephedrine/pseudoephedrine racemization.

First -L-ephedrine and D-pseudoephedrine do not have identical configurations

l-ephedrine, d-pseudoephedrine and d-methamphetamine all have the (S)-stereoconfiguration at the amine-bearing carbon, and that's all that counts.

The distributer ruins the E for our purpose when they racimize it.

Why would they? And by what process would they racemize which stereocenter?

There are 2 chiral or assymetrical carbons in ephedrine 22=4 isomers (enanmtomers)

Yes, see below for a listing. Technically, the four are stereoisomers, not enantiomers (enantiomers are a molecule pair  differing by only one stereocenter, and diastereomers differ by two stereocenters - stereoisomers can differ by any number).

and since the amide N is also assymetrical (by some authors) there can be even more 23=16

No, that's completely incorrect. First out, there is no amide nitrogen present, only a secondary amine (but that was perhaps a typo?).

The four isomers are as follows:

(1R,2S)-1-phenyl-1-hydroxy-2-(methylamino)-propane (l-ephedrine)*
(1S,2R)-1-phenyl-1-hydroxy-2-(methylamino)-propane (d-ephedrine)
(1S,2S)-1-phenyl-1-hydroxy-2-(methylamino)-propane (d-pseudoephedrine)*
(1R,2R)-1-phenyl-1-hydroxy-2-(methylamino)-propane (l-pseudoephedrine)

*) These isomers both reduces to (S)-1-phenyl-2-(methylamino)-propane (d-methamphetamine)



I have no idea how you meant that the above molecule could have 16 stereoisomers, that is just impossible. Nitrogens are never chiral in freely rotating molecules.
 
 
 
 
    Osmium
(Stoni's sexual toy)
02-03-03 17:23
No 404000
      Rhodium, you should add hydrogens in your...     

Rhodium, you should add hydrogens in your little rotating pictures, at least those attached to the chiral C atoms to make it more clear. The way it is now it seems like the angle between the bonds is 120 and the atoms directly involved in chirality would be in the same plane. Of course these carbons are tetrahedral and the angles are more like the usual 100 or so.

I'm not fat just horizontally disproportionate.
 
 
 
 
    Rhodium
(Chief Bee)
02-03-03 21:28
No 404076
      Perhaps I should raytrace the molecules instead?     

Os: Our little molecule applet is not good enough for that, if I do what you tell me we end up with a visual like the ones below, and that's not pretty:













Molecule: l-Ephedrine ("C[C@](NC)([H])[C@](O)([H])C1=CC=CC=C1")


l-Ephedrine
 
 
 
 
    Snapdragon
(Stranger)
02-03-03 21:30
No 404078
      Please pardon what may be a stupid question,...     

Please pardon what may be a stupid question,
When I looked up this reference,
See Rhodium: "Hermann Emde's Ephedrine Chemistry Treatise"

was sent a djvu file,
How to open a (*.DJVU) file?
Looked on Rhodium's web-site.
Is there something that must be downloaded?

It is important to me.
Tanks lots
SDblushblush
 
 
 
 
    Organikum
(Hive Addict)
02-03-03 22:08
No 404085
      the distributor racemisation story     

got somehow confused by the bee telling it, Worlock.
Probably this way: The distributor cooks the ephedrine he gets from china and as a cheapass he buys it bulk, with a strong mineral acid and some nickel or zinkchloride to gain a mixture of d-pseudoephedrine and l-ephedrine.(here named in the old way for more confusion smile).
The ephedrine goes to canada to be sold in the US and the pseudo is directly marketed in the US.
This is technical and economical ok.
d-ephedrine is only needed in separating chiral compounds in chemistry. I know of no other use of it.

for the interested some racemisation and separation patents:
Patent US2608583 amphetamines
Patent US3970700
Patent US2797243
Patent DE2903589 separation
Patent GB804788
Patent GB297385


ORG

nothing special
 
 
 
 
    Worlock
(Tweaker God)
02-04-03 18:21
No 404410
      Stereochemistry ephedrine - Elder bee philosophy     

Rhodium,
Excellent, you have a quick mind. Never again will the hive be plagued with D and L
we can finally use [s]-Methamphetamine. The chief of bees sets the standard and many rally around. The internet is a role playing situation. A chief of bees can be an evil tyrant, who hordes the glory for himself, torturing the not so adept.
 However ,
the chief bee could also assume the role of a benevolent father, who nurtures the hive and gently brings others to full potential. Willing to share the limelight and good fortune because he  has more than enough. Who needs not jealously protect his position because being confident and sure. Has no problem with stepping aside now and then to let others also have their moment of glory. Being a father who is kind and considerate to his children.  He would be the most revered of all bees , The tyrant would be tolerated, smiled at publicly, but loathed in private.

Point #2
It is often the greenest New bee that is not tainted with shards of misinformation and old baggage of past drug lore. These New bees when asking  the seemingly dumbest of questions are actually peering through a veil we put over our minds  that is full of myth and misinformation. The new bee wonders at inconsistency, whereas the elder bee has accepted it, accepted an error in perception because he is standing on the shoulders of those before. It is vital to take each bee seriously as they often will pose the question that leads to the unraveling of another mystery.


Point #3
Time to get down to Stereochemistry
Let me remark on an inconsistency I have spotted, I could quote the source , but the gist of it is:

"[R,S] ephedrine and [S,S] pseudoephedrine are the precursors of [S] methamphetamine, and it is the [S] position that counts."

This is only  partially correct, Alpacenturi was just about to expound up the stereochemistry of the different types of reaction mechanism , when he was interrupted.
The availability of the reaction site, the crowding by various side groups, is of vital importance to the ways with which the different types of reactions can effect the outcome of the molecule. . Simply because the rule is that secondary alcohols behave in this or that manner , assumes that other factors are insignificant like charge on nearby atom

Even though the beta carbon is vital. The groups on the rest of the molecule determine the direction  of approach, ability to attack the main chain, or a side group. This will have a tremendous effect the configuration of the final product,. In some situations, as you well know, the tendency for rearrangement is more important than initial configuration. It is possible to start with [S,R] ephedrine , under the right conditions force the molecules to undergo a mechanism that results in reconfiguration of the molecule to {S] methamphetamine.  It is a crime to mislead others away from this potential rich area of experimentation.


Point #4
You are quite correct about the amide , and the nitrogen not being chiral,. It was not a  typo, nor was it a mistake.  I used the wrong terms purposely. You gotta chum if you want to catch fish. Trolling  ls a popular term.
I want to point out that , carbon is not the only  atom that can be considered chiral. In certain oxidation states, some bonds become locked, in other they oxidation states they are transient.

I hope Alphacenturi still has the desire to continue his discussion of Stereochemistry without feeling that he is treading in areas, that are forbidden, because after all we are not here to learn  only one point of view , but to absorb the collective knowledge of the hive.

It is said, I am a rabble rouser. The truth is I refuse to be lead into narrow minded ways of thinking. I accept everything, including my self as a source of potential missinformation.
Most of all, I scoff at attempts to socially stratify the hive into cliques. Is that rabble rousing, or not? It depending on where you stand.

  

Worlockium
 
 
 
 
    zibarium
(Naked Abyss)
02-04-03 18:48
No 404418
      we are fortunate     

to have such dialog. many thanks to you all.

wink
 
 
 
 
    Rhodium
(Chief Bee)
02-04-03 22:59
No 404474
      Better pictures     

Yes, you need a plugin from http://www.lizardtech.com/download/ to be able to read *.djvu documents.

And for the isomers, perhaps this will make it even more clear to you:



It is possible to start with [S,R] ephedrine , under the right conditions force the molecules to undergo a mechanism that results in reconfiguration of the molecule to [S] methamphetamine.

Technically - yes, practically - no. Also, you will not find (1S,2R)-ephedrine (aka d-ephedrine) anywhere but at fine chemical suppliers, and that at grossly inflated prices, as it is the unnatural form of ephedrine, and as it is not found in nature it has to be made by expensive stereoselective syntheses.

As it is very hard to convert natural (1R,2S)-ephedrine into (1S,2R)-ephedrine, you won't run into that isomer by mistake, and  thus it can be exempted from our discussions here.

You are quite correct about the amide, and the nitrogen not being chiral,. It was not a  typo, nor was it a mistake.  I used the wrong terms purposely. You gotta chum if you want to catch fish. Trolling  ls a popular term. I want to point out that, carbon is not the only  atom that can be considered chiral. In certain oxidation states, some bonds become locked, in other they oxidation states they are transient.

Yes, in rare cases, other atoms than carbon can be chiral, but as that is no issue with the stimulants we discuss here, there is no reason to confuse others by discussing that fact here and now. There are even chiral molecules containing no chiral atoms, but that is off topic. Trolling is not appreciated here, nor is posting misinformation - we even have a notice on the front door saying that such behavior is grounds for banning. If you want me to explain or clarify something to you, then please ask me to do so instead of posting errorneous things on purpose.

You are right when saying that the chirality of neighboring atoms can affect the reactions of another atom, this for example explains the difference in reactivity between ephedrine and pseudoephedrine (as you can see above, pseudoephedrine is more sterically hindered towards SN2 reactions than ephedrine as it has its methyl group sticking out on the back side. None of these things will ever change the chirality of the amine-bearing carbon though.
 
 
 
 
    raffike
(Hive Addict)
06-12-03 15:59
No 439522
      Still little confused.When l-ephedrine's OH...     

Still little confused.When l-ephedrine's OH group suddenly starts looking other way ie is S chiral,the name changes to d-pseudoephedrine,why not l-pseudoephedrine,raf thought that pseudo in front of name ephedrine means OH group position difference,why l in the name changes to d.Like why l-ephedrine is right form for bees but not l-pseudoephedrine?Raf thouht that these l's and d's mean chirality of amine bearing carbon and should always be l when dealing with (pseudo)ephderine that changes to d-methamphetamine.Raf has never read anything about isomeria,could anyone suggest some document or web page something where raf could learn about that a little?

For those about to synth,we salute you
 
 
 
 
    Rhodium
(Chief Bee)
07-04-03 04:33
No 444361
      Pseudo(ephedrine) Optical Isomers
(Rated as: good read)
    

To understand, you need to discard the obsolete 19th century d/l-nomenclature of the compounds, as they do not logically correlate to any actual arrangement of the atoms in space, but rather if a solution of the substance rotate plane-polarized light to the right (d, dextro) or the left (l, levo).

Instead, we need to use the modern chemical nomenclature, developed by Prelog-Ingold-Kahn, which designates different isomers as either R or S. Here you see the tabulated names of all four isomers:

(1R,2S)-1-Phenyl-1-hydroxy-2-(methylamino)-propane (l-Ephedrine) *
(1S,2R)-1-Phenyl-1-hydroxy-2-(methylamino)-propane (d-Ephedrine)
(1S,2S)-1-Phenyl-1-hydroxy-2-(methylamino)-propane (d-Pseudoephedrine) *
(1R,2R)-1-Phenyl-1-hydroxy-2-(methylamino)-propane (l-Pseudoephedrine)

* These isomers are the naturally occurring ones, and they will both reduce to the most wanted Methamphetamine isomer as the chemical name for it is (2S)-1-Phenyl-2-(methylamino)-propane - as they all three have the "2S" thing in their name - meaning that in all compounds the 2-carbon (the amine carbon) is in the S configuration, the shape which fits best into your brain's receptors.
 
 
 
 
    raffike
(Hive Addict)
07-04-03 13:38
No 444465
      aight,thanks chief.     

aight,thanks chief.

For those about to synth,we salute you
 
 
 
 
    Jacked
(Ancient Alchemist Delux)
08-11-03 14:40
No 452977
      Novel idea with poor results     

Worlock, Nice try. You defiantly stirred up some posting. After all is said and done this procedure is misinforming if outcomes are projected as wished. This was a good shot at stimulating a group effort, I will give you that. Some good information on isomers as well came out but with no references.. To any newbees or even old bees that are thinking about giving this idea a try I recommend not wasting time and money. Time would be better spent watching a reflux condenser circulating water instead of the trunk of an old junk car..

Sorry, But Jacked rates this post as a dud.

Tighten Up!  (UH)
 
 
 
 
    Buckshot
(Hive Bee)
07-13-04 23:42
No 519191
      10 grams cold for 2 weeks     

Ok I have had a 10 gram batch of clean ephedrine reacting in a flask with rp and I2 and a little water for almost 2 weeks. The reaction flask has had no light exposure or heat applied.
I've been excited to even smell the contents.....(I haven't opened it yet.) Until I read Jacked's post at the end of this thread.Jacked says the reaction won't work without heat. I'd like to know why? Im asking because Jacked seems like a respectable bee who kows his/her stuff. But the post has nothing to it. Nothing to back up why it wont work. Could someone explain the bad news to me, or was Jacked incorrect?
I was sure I'd have meth with the least side reaction impuraties ever.

Drop Bush! Not Bombs.
                                 


 
 
 
 
    aia2
(Newbee)
07-14-04 02:02
No 519246
      Definitely     

Yes, Jacked's post comes after a stimulating discussion of stereoisomers of ephedrine, and unexpectedly calls Worlock's procedure into question.  Zibarium's posts earlier in the thread also looked skeptical, if only because no scientific analysis was done on final products.

During the discussion of the HI reduction, alphacentauri put forth a convincing theory for the apparent correlation between long, cold reactions and pure product: Post 403630 (alphacentauri: "I think this, Worlock.", Stimulants)

So in the past 18 months have any bees tried it?  Real experimental results would be very convincing.  Worlock seems to have disappeared in the middle of this thread! (last post 2/04/03)

Buckshot: how does the visible evidence stack up against Worlock's posts?  What color do you see?  Soup or syrupy?  Are there any crystals on the flask walls?

Whether you find success or failure, details about your experiment would be great!

--aia
 
 
 
 
    Buckshot
(Hive Bee)
07-14-04 07:30
No 519311
      results will be posted     

I haven't had a chance to look at the reaction flask.The flask is sitting in a dark place at a friends cottage. I'll be going there in the next couple weekends for sure, so I can give us an update. I would never leave a reacting flask un-attened under normal reaction circumstances, but that is one of the main benefits of the cold rxn. You dont need to baby sit.

I can say that the experiment was 10 grams of very clean E, 12 grams of lab grade iodine cyrstals, with 7 grams of very clean match book red phosphorus. (I get my mbrp as clean aas it gets.) I added a touch less water then I'd use in a long wet reflux. I know thats a vague description for my dH2O amount. Its been at outside temps but its been rather hot this time of year.

No light exposure, and I've read threads with hints that suggest sunlight may stimulate the reaction. I agree that ultraviolet light would help the reaction along, but my experiment is to get the cleanest dope ever using an extremely slow "cold" reaction approach. My thinking being anything to speed the reacion along including light or external heat would cause side reactions and unwanted side products. I did NOT however pre-chill any ingredients in the freezer.

The flask isn't hooked up to a push/pull system, I used a bike tire innertube cut and tied off at one end, as a reflux, to replace those balloons. A balloon works (sometimes) for short reactions, but the acids will eat through it in a day or two (sometimes in minutes), this reflux membrane has to hold up for a couple weeks. My slight concern is that my knots on the innertube will have a slow leak....I doub it will leak. I'm hoping the sides of the flask are not red color or orange but a nice golden yellow.

I've done a variation of this before, but it was because I didn't have time to do the whole LWR at once so I heated the flask for an hour then let it sit without heat for about 3 days. During this 3 days the ballons kept breaking/leaking which probably released precious gas. After those 3 days I removed the balloon and just let it "breath" at normal atmosphere for another 3 days. That batch was 5 grams of E going in and I got about 3 grams of meth back and it ws the very best meth I ever made.

Another question is what is a good method to seal off the end of the inner-tube? I just tied a bunch of vey tight knots on the end.

I should be able to tell by the smell as usual I think. Has anyone ever had that sweet smell from a flask and not had decent end product? I never have seen poor product after smelling that "complete sweet meth" smell.

Im excited about this, I will post results for sure. Cold reacted meth.....If it works I'd like to try cooling the entire rxn. Even keeping it in an ice bath during the initial exthermic reaction phase to keep it cool as possible, then  keeping it in the fridge for 6 weeks or something.

Drop Bush and food not bombs
                                 


 
 
 
 
    wareami
(Hive Addict)
07-17-04 17:23
No 519911
      Not likely....     

Heat is a necessary component of the rxn during the critical reduction stage.
Yes, The rxn itself will start out exothermic, but loses energy and cools off by itself.
To expect a conversion to take place under cold conditions is like wishing the sun were blue because it looks prettier than the red one.
You could leave the precursors sitting in rxn for a year and they won't fully convert without some external heat.
Some bees have reported success over time just using lightbulb heat but Ibee would bet that the reduction percentage to meth was under 70%. Just enough to feel it.
Don't get your hopes UP!
If you don't want to waste all that time and chems....apply some heat for 12hrs before work-up

Remember, it's not,
"Hi, how are you?" it's
"How high are you?"
 
 
 
 
    Red_Crown
(Hive Bee)
07-19-04 19:48
No 520302
      bee so sure?     

I mean, the thermodynamically favored product is still the reduced one. The reaction is always exothermic.. Applying external heat only effects the rate -- which is a kinetic consideration.

~If you live in a warm enough area, it could work in a week, vs.  400,000 years @ the north pole. But it would still convert.~
 
 
 
 
    Jacked
(Ancient Alchemist Delux)
07-19-04 20:27
No 520305
      Then explain the second phase     

The same idea should bake a cake correct? I wouldn't want to eat that cake after it sat in the trunk of an old car for two weeks baking.
 I didn't just guess at this, A little embarrassed I didn't post up the step by step rxn that lead to a pile of unreacted gear. I figured the others following this thread would step up and declare there findings but as you see hardly anyone did. This left me even more embarrassed that I might have been one of the only ones who tried this method.....Bottom line is with RP and I2 being the body of the reaction heat is as necessary as the I2 it self. 
 Reflux is the key and you cant reflux without a heat source of some type applied, even at reflux temps it takes 48 hours, 2 days. That's 4 tweaker days mind ya.
 In the push pull the second phase of the reaction is were the reduction is carried out and it does not come about less than 190 degrees. 

 An still I wonder if you could raceamize pseudo just by letting it sit in HCl for a week or two?

 This bee ain't wondering or speculating on thermodynamic reactions, and did very little math during this whole project.  This bee is simply stating what he has seen with his own two eyes.

Buckshot I hope your experience turns out much better than mine, there is always hope and that's all I have to back you with. good luck

Tighten Up!  (UH)
 
 
 
 
    CharlieBigpotato
(goat)
07-19-04 20:46
No 520310
      insulation     

perhaps with lots of insulation, the exothermia wouldn't bee lost almost immediately. glass offers almost no resistance to the heat flow.
 
a good candidate for a sealed rxn, perhaps; with minimal surface area. conventional refluxing is not essential for sucessfull reduction.
not sure about the temp.

i hope we get a report back on this.
(yes, there is danger in a sealed rxn; use with care and knowledge)
 
 
 
 
    Buckshot
(Hive Bee)
07-20-04 23:53
No 520470
      Stressing a little over this     

Jacked, thank you for the more detailed explanation of why you don't think a cold rxn can work. Could you please tell us details of you're test experiment? More specificly how long did you let the rxn flask sit for? Did you only let the rxn flask sit for 4 days as Dwarfer suggests in this thread? Furthermore, very important information would be to know if the flask had that sweet smell when opened? Finally, did you use a membrane or a push pull system? I believe for this type of rxn the push/pull system may not be as effective as a membrane or sealed rxn.

My rxn flask is still sitting....If its gonna work it should be done by now.

I haven't had a chance to look at the rxn flask, but I can say for sure, that in the past I put a flask on the heat for an hour or two, and then let the flask sit for a week with no additional heat, and that method worked great.

And Ibee, I know you are skilled, but honestly have you even tried this or are you just speculating? Becuase you don't give any details whatsoever. You did however make a comment about wishing for the sun to change colours, which had no scientific value related to the topic. Kinda like that comparison of baking a cake without heat, which is also a statement which doesn't apply to the topic. (I wouldn't eat a cake that's cooked WITH heat for 48hrs)no offense Jacked, Im just trying to get this straight.

Regulate you're idle
                                 


 
 
 
 
    CharlieBigpotato
(goat)
07-21-04 03:11
No 520507
      forget the sweet smell     

the 'smell' is so easily overwhelmed by other smells.

christ, if someone opens a flask, post rxn, and smells HI, it doesn't mean it didn't reduce.  yet, it sure won't smell sweet!
 
 
 
 
    barkingburro
(Hive Bee)
07-21-04 04:43
No 520519
      possible methods of attaining energy needed     

swibb seems to remember somewhere that thre was once a method of making 'god speed' that was set off by the mere flash of a lightning strike. this being the case here are a couple of ideas that have come to mind that may be the methods in which this slow no heat reaction may occur. over time from start to finish we have rp+i2+h2o+pfed=>2HI+h2o+pfed=>i2+h3po3+meth+h2o=>i2+h3po4+meth+h2o now the initial rxn is from the combination of i2 and rp, plus a lil ultra violet to start the i2 decay. this initial reaction creats a significant amount of energy in the form of heat. eventually this heat is going to dissipate however and more energy is going to be needed. the UV reaction with iodine may be one source of this energy, even the slow decay of the iodine during the recycling may be enough to keep a subdued reaction going. on top of that the mixture of h3po3 and i2 and h2o is an endothermic reaction, so it is storing energy in some manner, what manner that is swibb is unsure of, but it is definately happening, swibbs felt the flask too many times after combining the 3 to be told otherwise. now, h3po3 and i2 don't become HI, so fas as known, until 87C. BUT since this IS a closed/sealed reaction, pressure equates heat, potentially, though swibb's not so sure that there's enough pressure there. just a few potential ideas.... perhaps the push and pull mechanism is providing enough pressure and kinetic energy that it is being converted?
 
 
 
 
    12cheman12
(Hive Bee)
07-21-04 08:54
No 520546
      Well i think everyone agress on that the rxn...     

Well i think everyone agress on that the rxn must reach some minimum temp for the process to start happening, so i think we have to just work out what this ideal temp is, if HI is produced at 87C then wouldnt it be perfect to keep the RXN at 87C, no higher and no less? just my thoughts
 
 
 
 
    placebo
(arrogant bee of the day)
07-21-04 10:49
No 520559
      I agree with Jacked, (hey buddy, long time no...     

I agree with Jacked, (hey buddy, long time no see) SWIM attempted this as well and did write it up above somewhere. I won't say it's impossible to work but SWIM and others say it hasn't.
However I disagree with your comment about 2 days being 4 to a tweaker. I would say it is more like 2 weeks and 1 week more like a month of waiting in tweaker terms.

In my opinoin there is definately a minimum heat requirement, what it is doesn't matter, reflux is fine and not worth the time required in testing to find out.

I'm not fat, I'm just too short for my weight.
http://www.whatreallyhappened.com
 
 
 
 
    Red_Crown
(Hive Bee)
07-21-04 22:37
No 520673
      yet another theoretical point     

Just thought I'd work this out publicly.. T'might stimulate:
(^=delta)

A quick and loose estimation of the bond enthalpies (^Hformation, in kcal/mol):
1) pseudoephedrine ~= 2796  
2) iodoephedrine   ~= 2641
3) methamphetamine ~= 2700


*albiet barely; within error margin

Hypothetical partial reactions: (^G = ^H - T^S)
Rxn.A   1 -> 2  = -155 (exothermic)
pseudoephedrine + HI(aq) -> iodoephedrine + H2O

I believe the ^S above is 0, no?


Rxn.B   2 -> 3  = +59  (endothermic) 
iodoephedrine + H2O  ->  methamphetamine + I- + OH-

And above ^S is positive. Correct?


..If so, then rxnA is both spontaneous (negative ^G) and exothermic and would occur even at very low temperatures.
And rxnB may be spontaneous depending on the precise change in entropy (and more accurate enthalpy data) and Temp.

Wouldn't it be possible to find the mechanism by creating a number of hypothetical mechs and measuring they're rate thermodynamics?   No researcher has done this for the RPI reaction?

Think it could be done in tha kitchen?
 
 
 
 
    Jacked
(Ancient Alchemist Delux)
07-23-04 07:32
No 521034
      Sweet Smell     

I think it was more like 7 days, The container was a 2000 ml RBF with a single 24/40 neck. It contained around 40gs of E with a ratio of around 1.2 I 1 E and .4 twice ran RP with approximately 8ml of H2O, added, after a brief exothermic reaction took place and it rolled over into the black liquid with bubbling subsided the cap was placed on it and taped down, It sat in the trunk of and old car just like was suggested and a week later when opened it did have the P2P smell (sweet) that you are referring too. This smell does not mean the reaction was a success, as I learned watching SWIM processing this batch. The results have been stated above. I'm not sure if some of the E was reduced but the majority was pinwheel in fashion and when burned had a sweet pseudo smell and taste. The shit was collected and reran under normal conditions with no problems.

 

You did however make a comment about
wishing for the sun to change colors, which had no scientific value related to the topic.




 That was a comparison, you should start reading things a little closer like the fact of running this reaction before you even finished the thread.
 I was informed of this through PM a week before it was posted and was asked to give it a try. It was my mistake for not posting more detail.


  but honestly have you even tried this or are you just speculating?




 Again go back and read again, the statement was make that I "was not" speculating about this. As a mater of fact I don't post speculation because I am just a chem hack and don't posses the ability to balance a reaction on paper much less talk about before it happens..
 


Kinda like that comparison of baking a cake without heat, which is also a statement which doesn't apply to the topic.




Why the reference is to cooking something in laymen terms, (comparing to something easer to understand) us simple minded guys understood that (Smile).
 It's been three days sense your post, do you have anything to say about your experience with this?
 The statement about getting stressed over this is what gets me.. You should have known there was a question with this method and sense there is very little success reported then why experiment unless you could afford the loss. Nothing to stress over if that were the case.
No offense taken, I still wish you the best of luck.
 ____________________________________________

 BB you said


swibb seems to remember somewhere that thre was once a method of making 'god speed' that was set off by the mere flash of a lightning strike. this being the case here



 Will stop right here, God speed actually "lighting speed, the method of the gods" is a fiction man, it was wrote to parallel the facts of the reaction, Which in case it did just that. I should know, I'm the one who wrote the story..
 I'm glad you have read it, a lot of people around have not and referencing to it is rair indeed....

 Maybe there is a low heat in which would work that would produce fewer impurities as what this method was about. Right now the long reflux at the 48hour mark is your best bet for fewer side products and higher % of conversion to the target molecule.. Remember this is an experiment and posting on the like should be after you have compiled the results of your experiment, especially if a couple elder bees have made statements to the contrary of its sucess.....


Tighten Up!  (UH)
 
 
 
 
    abominator
(Newbee)
07-24-04 16:06
No 521333
      God Speed and swim's cold expr.     


Will stop right here, God speed actually "lighting speed, the method of the gods" is a fiction man, it was wrote to parallel the facts of the reaction, Which in case it did just that.




Goddamned glad to finally know that Jacked.  Swim read that story on Worlocks site long ago when it first appeared and was always quite skeptical.  Thanks for putting in the final word.

Here is swim's experience with the closest thing he can call a "cold" rxn.

Swim had a buddy whom whilst after 2hrs. into the rxn the po-po came to his door with an arrest warrant and he went quietly, but all power to the rxn off.

It was placed outside in the sun during the day and beside a baseboard heater at night.   This was done for a total of three weeks.(it was middle of summer)  BTW, swim was not the one with the rxn flask, it was the brother of the guy who got took to jail.

Anyway after the fellow got out of jail, the shit was worked up.  Several NP washes were needed to get rid of the red color.  There was about a 70% return by weight which led swim to believe much of that weight was undreduced pfed.

The bioassay of the product resembled the street dope going around at that time, a bit better actually.  It was still not anywhere near if the fella had done a push/pull, much less a reflux.

To sum it all up, in swim's experience one will get a return from this method, but it is one of with much unreduced pfed and indeed a waste of precursors./Gluecifer69


  I'd like to have her right there on floor with the 'ol in/out, real savage.
 
 
 
 
    Buckshot
07-24-04 22:49
      Bad news
(Rated as: off-topic)
    
 
 
 
    ChemoSabe
07-24-04 23:39
      School Computer Systems
(Rated as: off-topic)
    
 
 
 
    barkingburro
07-25-04 01:29
      ok i do wonder why you posted this in this thread,
(Rated as: off-topic)
    
 
 
 
    Buckshot
07-26-04 18:00
      I know
(Rated as: off-topic)
    
 
 
 
    Rhodium
(Chief Bee)
07-29-04 15:30
No 522466
      activation energy     

..If so, then rxnA is both spontaneous (negative ^G) and exothermic and would occur even at very low temperatures.
And rxnB may be spontaneous depending on the precise change in entropy (and more accurate enthalpy data) and Temp.


Just because a reaction is thermodynamically favored does not mean it is spontaneous.

The reaction 2 H2 + O2 -> 2 H2O is certainly thermodynamically favored, but you can still store a 2:1 mixture of oxygen and hydrogen in a container for years at room temp without any water forming - you need to heat the mixture to get things going.

This is due to something called activation energy and corresponds to how much energy you need to make the reactants overcome the thermodynamically disfavored transition states inherent in virtually any reaction.



Example taken from http://encyclopedia.thefreedictionary.com/Activation%20energy


Fig 1. The enthalpy profile of a reaction between two hydrogen peroxide molecules to form water and oxygen.
The Transition State is the point at which the original bonds have been stretched as far as they can without breaking (this is illustrated by the structural diagram below the graph.) The energy required to reach the transition state is equal to the activation energy of the reaction.

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    CharlieBigpotato
(Bizarre pHomme de Terra)
07-29-04 18:12
No 522483
      very strange, chief     

now there's something that sure seems counter to semi-scientific reasoning. very cool.

still, one has trouble picturing a means of getting that 2:1 mix in the jar in the first place. or letting it out.
i can imagine that the energy to tear the O2 apart exceeds that which is required for the water to form, but can't picture how they could bee put in the containor in that ratio simultaneously.

ever seen it done?
such a peculiar way to store H2!
 
 
 
 
    Rhodium
(Chief Bee)
07-29-04 19:26
No 522489
      How to mix two gases in a container     

still, one has trouble picturing a means of getting that 2:1 mix in the jar in the first place. or letting it out.

Fill two balloons with hydrogen and one with oxygen, then empty all of them into an empty plastic bag through a one-way valve wink

i can imagine that the energy to tear the O2 apart exceeds that which is required for the water to form,

No, that is not the issue. For water to form, both O2 and H2 molecules needs to break apart to form free atoms before they can re-combine to form water. At room temperature, the molecules always have too little energy to break apart, as when they bump into each other they merely bounce apart. If the temperature is raised (for example by applying a burning match to the plastic bag containing the gas mixture) some of the molecules will gain enough kinetic energy (speed) to be able to break apart when crashing into other molecules, and the reaction between the atoms can proceed.

The reaction between oxygen and hydrogen is a special case, as enough energy is released when water is formed to push further O2/H2 molecules over the activation energy treshold so that they in turn can react to produce water, and even more energy is released - the reaction rate will accelerate explosively until all the molecules has reacted.

In most exothermic reactions suitable for laboratory use, the amount of heat released when the product is formed is not as large as to initiate such a chain reaction - at least the energy release is small enough for a reflux condenser to neutralize it - hence you will usually need to continue heating the reaction mixture until everything has reacted, as opposed to the O2/H2 example above, when a simple initiation is needed.

but can't picture how they could bee put in the containor in that ratio simultaneously.

ever seen it done?


Sure - at chem class demonstrations... But there is no need to introduce the gases simultaneously, as it makes no difference if you do it with one at a time.

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    CharlieBigpotato
(Bizarre pHomme de Terra)
07-30-04 05:14
No 522607
      one last question about that, please:     

if this combination of hydrogen and oxygen can bee stored together regardless of the ratio they are introduced to each other, initially; that is, at some point they could bee in the ideal ratios for water formation; yet they don't react:

does this mean that the explosions i've seen were only beecause of the pre-heated state of the H2 when it met up with the O2?
this probably isn't the right thread to attempt to understand this. but with luck, perhaps one more from rhodium on this subject.

fascinating stuff, as it runs counter to uneducated assumption.
 
 
 
 
    Rhodium
(Chief Bee)
07-30-04 10:44
No 522682
      Another example of activation energy     

does this mean that the explosions i've seen were only beecause of the pre-heated state of the H2 when it met up with the O2?

Huh??

Somehow the needed energy was aquired, such as through strong compression, a lit match etc. The Hindenburg airship met its fate due to static electricity.

But to make the argument even simpler, here is a similar example:

Beeswax is combustible, but you cannot ignite it with a match. If you make a candle out of the beeswax and ignite its wick, it slowly heats and evaporates the wax (transferring energy to it), and this can then combust in the air (the wax is oxidized to gaseous carbon dioxide and water vapor by the oxygen in the air).

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    Red_Crown
(Hive Bee)
08-12-04 17:49
No 525070
      intentions, assumptions, question, cheesy sig     

Just because a reaction is thermodynamically favored does not mean it is spontaneous.

 I didn't neglect the role of temperature, but meant to leave it as the open variable of sorts; partly thinking that standard conditions might provide the required activation energy.

-On what order is the activation energy for this reaction? 
-What is the mechanism anyway (to iodoephedrine)? Sn2? Sn1?
(It feels like it'd have to be somehow in-between.. Inversion indicates Sn2, but with an aweful OH- leaving group?? Sn1 would make for water as the leaving group, but it's trigonal bipyramidal transition state would cause racemization, no? I'm probably forgetting..) Then, couldn't any eliminations undergo a methyl shift?
-Just how much energy is ambiently 'free' at STP?
-If the reaction was perfectly insulated, beyond the initial energy of activation, wouldn't it be self-sustaining (- since even the EA would be conserved)?
-Given the observation that it IS indeed spontaneous at RT(initially anyways), might conservation of the energy from rxnA drive rxnB? (-whether by insulation or perhaps coupling the two parts in lock-step somehow..)

If I am completely off-base, you don't have to give me a chemistry lesson (unless you want to), just tell me I'm wrong and I'll work my way out..smile

got mechanism?
 
 
 
 
    CharlieBigpotato
(Bizarre pHomme de Terra)
08-13-04 02:45
No 525133
      Na in h2o:     

when dropping small slices of sodium down a tube with water in it, the liberted H2 has always exploded, w/ no spark.
i'm not sure why, now.

i better study up. thanks for the explantion, cheif.