Reagent grade iodine

[kewlcanuk]

Swim noticed that he has been following reciepes that use I2. He is using reagent grade iodine not from tincture and wonders if the ratios should change. 2.2I:1MBRP:2E   is what he has been using.

[SpamIam]

Equal amounts of I and E half as much rp.Although I think even more rp would be in order since your using mbrp.

S.I.A©

[geezmeister]

1:1:0.5 is probably fine if you are doing over twenty grams or so, below that I'd hedge with a little more I2; if the mbrp is done per Squidippy and has the consistency of talc and is first use, 0.5 will be fine. Most of us use a little more even for first use red just to make sure, and if it isn't the first use, I would go at least 0.75 or even 1.0. If you run the reaction wet from the start, the excess red phosphorous won't hurt you, as it can with dryer reactions, IMHO.

[wareami]

I agree with geez on all accounts....except the equalling of I₂ to E in larger rxns.
While it can be done that way...I'd still side with caution there to guarantee a higher %age of HI.
Even more so with the wetter rxn.
If it's too dilute in relation to the amount of precursors...the HI may be too weak IMHO!
In addition....it may account for any gaaks that may have slipped by the cleanup.
Not saying geez is wrong in that advice...but the little extra I₂ in relation to E suggested by the standard ratio should be equally scaled UP in larger rxns to insure full reduction.
|1-E|1.2-I₂|.08-MBRP|.05-DH₂O|
Again...IMHO!!!

Haahahahahaa Geez....I got to smack you around abit on that one.
We even!
All in fun of course!

[Jacked]

Swim always used a 1.1 : 1 : ratio with LG I2 no mater what the size. MBRP would be up there but LG would be around .3. This was the ratio for the push pull with .2ml H20 per gram.. The extra .1 was added because of the escaping HI was not returning down a condenser but getting bubbled through the water in the push tank.. At least a condenser will return what is trying to leave your reaction..

[abominator]

Jacked's above post is ,as usual, right on the money, especially the h2o amounts.  I thought I would point that out since there is much confusion on water amounts in a push/pull reaction.  With his tinc. I and MBRP swim always runs 1:1.2 pfed to iodine.  This is with MBRP levels at .08:1 MBRP:pfed, to ensure success and enough HI.  Keep in mind I am speaking of Jacked's recommend h2o amounts in a push/pull.

[wareami]

GlueBee69 and Jacked:
Way back when, ware Ibee pulled off regular shorter timed HI/RP rxns, the guiding ratio was the one jacked points out above. Never had a problem with a single one. It helped having LG RP and I₂.
Plus, 1oz LG RP afforded many extra runs before it fizzled out primarily because of the cleanliness of the feedstock at the time.
On average he'd get 4 runs before it lost it's potency. Of course those runs were incrimentally smaller each run due to the rp that was used up. To the point that extra fresh was added to the greyish RP in the last run.
Dipping into a sack for precursors sure was sweet compared to all that scraping and tinc messes!
In the begining of the LWR trials...those ratio's weren't changed until problems were encountered in the longer rxns.
Mainly the first problem encountered was drying out which led to the increase in dh₂o. After that it was noted that HI wasn't strong enough to completely reduce the pfed...then UP went the I₂, but the RP stayed the same for fear of flask fire...(once you've fried a rxn from excess RP you learn quick not to be too heavy handed)...then came the ole .
If it's wet...it won't get hot enough to fry anything and so came the optimal realization that had been handed down from those saying "slow/controlled" is more favorable than the hotter uncontrollable ones.
So UP went the RP ratio as well!
As geez points out...any unused RP is recovered post-rxn so why sell yourself short by using .06 RP and coming up with unreacted.
This evened out to the optimal LWR ratio that guarantees putting bees through the window of success.
This proved to be the case time and again.
So any confusion in ratio around here can be directly blamed on Ibee and Geez!
The P/P should be carried out with the Jacked ratio! Success will be had!
The LWR should be carried out with either the Geez ratio or the Wareami ratio! Success will be had also!
We agree to disagree because they both work and we have fun giving each other a from time to time

[kewlcanuk]

[clandestine]

one of the big underlying factors of failed RXN that isnt readily addressed is the fact that with the Rp/i2 reaction that a 100% SEAL is neaded and if there is any small leak at all your hi percentage down fast...  Even the slightest smell outside the flask and condenser of the rxn mix means your not going to get 100% out of your reagents and your possible leaking bad stuff anyways..     So be sure you rub a little grease on the joints of the glassware and tape it down after you have put it on and rotated it in place to disperse the grease...  with LWR and high temps you will have rp that gets up in the joints if you shook to hard if when it was being added it hit the sides... this leads to a leak without being greased!.  leaks cause failures too if using meager amounts of water for LWR...  so remember if you smell anything more than just a little hint of warm plastic from the tape on the top of the flask your going downhill not up!.

my 2 cents

[Jacked]

Then how does a push pull set up work?
 The molar ratios for reduction are the same as in a LWR ain't they? In a push pull the HI gassing out gets scrubbed in H2O never to return to the rxn vessel again..

[clandestine]

[memeep]

>lwr you need a tight seal..  trust swim on that.

Hydriodic acid forms a constant boiling mixture at ~57% HI. That means a mixture of HI and H₂O at that ratio will, when boiled evolve a gaseous mixture of the same ratio.
Acid of concentration greater or less than the constant boiling ratio tend to approach it by evolving more of the part of the mixture which is in excess when they are boiled. Simply put hydriodic acid of concn 60% HI will tend to lose HI until it reaches the 57% mark and hydriodic of concn 40% HI will tend to lose water until it reaches 57%HI  This is true for all the halo acids*.

*Edit:The constant boiling mixtures are different though, for HBr it is ~48% and for HCl it is ~20%.

[geezmeister]

lwr you need a tight seal..  trust swim on that.

LWR is ez too but the longer time means the smallest leak will leak the most..

One of the great advantages of the long wet reflux, aside from avoiding the creation of unwanted by products during the hot fast start, is that the reflux can be done without any pressure at all, will a condenser with an open top. Once the HI is made and largely absorbed by the water put in the reaction to absorb it all, the balloon that is useful during the early HI production stage can be removed and the reflux done without containment.

The problem I had with push pull units and hot fast cooks was that when you had a seal leak you lost too much of the HI and had inconsistent completion ratios. A leaky seal can ruin a hot dry reaction quickly. What do you think is escapting from the seals, anyway? HI is, since you don't have enough water to hold it, it escapes, and once its gone, its gone.

This is not a problem with a LWR.

[Zen]

Then how does a push pull set up work?

Most of the HI gas is "trapped" in the first tank.

As the pressure builds the H20 is pushed into the second tank.

When the reaction begins to pull back for need of hydrogen the gas trap fluid re equalizes.

The molar ratios for reduction are the same as in a LWR ain't they?

3I:3E:1RP is the magic molar ratio, no?

In a push pull the HI gassing out gets scrubbed in H2O never to return to the rxn vessel again..

Only excess volume that your gas trap can't handle bubbles across.

***A Note About Pressurized Gas Cans***

There are pressure relief grooves in the threading,
half a roll of teflon helps.

The gaskets are often low grade rubber that can be rendered useless by corrosives and solvents,
replace with silicon and graphite gaskets instead.

It's a good idea to test your apparatus a make sure it will hold constant pressure / vacuum for a duration before putting it to work.

[Jacked]

What happened to the reflux of days gone by, Once a pon a time before the push pull was popular there was a simple reflux of HI/Rp/E with a condenser that if anything only had a small peace of cotton placed in the very end but other than that was under no pressure and exposed.. Very little smell was produced and the damn thing always made good fucking dope... I don't understand what has changed over the years... (That was a smart ass comment)

The problem I had with push pull units and hot fast cooks was that when you had a seal leak you lost too much of the HI and had inconsistent completion ratios. A leaky seal can ruin a hot dry reaction quickly. What do you think is escaping from the seals, anyway? HI is, since you don't have enough water to hold it, it escapes, and once its gone, its gone.

 This is simply not true. Nothing is returning to the reaction vessel that is of any use to the reaction itself.. The tanks are not even necessary, They control smell and enable recovery of I2. Thats about it. The pull is nothing but the lack of energy and has no mystical part in the production of meth. By time the pull is noted the reduction is already over..
 A leak will expose you to HI gas which is not good, It will result in stains on the walls and everything else the gas contacts and that ain't good. One big thing is you wont get to see the dramatic pull when the second phase is wrapping up depending on the size and location of the leak and for the new bees that ain't cool at all, So leaks are defiantly not wanted. As far as hampering the reduction of E to meth, a leak just ain't going to do that. 
 



 And as for the question of how the push pull works, that was meant in reference to the on goings inside the flask itself and not to how the tanks work... The starting ratios in mass are about the same except for the amount of H2O peasant.
 

3I:3E:1RP is the magic molar ratio, no?"

 Would that be the same as 1:1:.3?
 Is that a molar ratio or a mass ratio?
This might sound stupid but here it goes anyway.
 How can a molar ratio be expressed without water being figured in as well?, I understand % of a solution and its molarity some what. I'm not to good with moles so bare with me.
 In a LWR the molarity of the HI is always changing being H2O is produced in the reaction itself. In this light it still 1:1 molar but broke down at 57% and involving many hours at reflux to reduce correct?    
 A "push pull" has lower amounts of
H2O there fore the concentration of HI is way Higher than that of a reflux resulting in a shorter time for reduction but the 1:1 ratio is the same as a reflux.
 Comparing one to the other and you will find a major difference in molarity so why isn't H2O figured into the molar ratio when it is expressed?
 I am a little confused here. I know this has been covered but WTF, help me out here...
 
 Oh yeah, one more thing on the push pull sense I'm here and don't want to look like a complete dumb ass thats been kicked by a gang of moles.

 There is hardly any pressure in a push pull set up right.. The only pressure will be determined by the weight of water that hast to be pushed from the first tank and this is short lived once its in the second tank the pressure is off. A proper set up and one should be able to blow into the hose and just with the air in your lungs push one tank into the other then your just blowing bubbles at this point with very little effort..
Sense there is a hose exiting the second bottle that is open to the atmosphere the system is not a gas trap. It a gas scrubbing tank, water being the scrubber and the gas being the scrub bee. The gas escapes the tanks cleaner than it was with less of an oder leaving a valuable precursor behind for a later recovery..

[geezmeister]

Jacked... my comments were comparing push pull cooks to reflux cooks. What I responded to as nonsense was the comment that a reflux reaction was more dependent on good seals than a push pull reaction. Its not. The reflux can run with no pressure on the seals, and the condenser will contain almost all the vapors. Keeping a balloon on the condenser after the inital HI production phase is more to prevent odor from escaping than for any other purpose.

 A push pull may not have much pressure, but it has enough pressure that a leak will let HI escape. How much HI is lost depends on how bad the leak is, and when it occurs.  With a drier reaction, there is less water for the HI to dissolve in. Without containment, the HI dissolved in the water will fume off until the concentration of HI falls below 57%; This will happen very quickly at the temperature of the reaction. With drier reactions, you can lose more HI to a leak than with a reflux, since the extra water in the reflux reaction will hold more HI in solution. Have a bad problem with a seal between the flask and push-pull tanks and you lose more HI than you would with a comparably sized wet reflux.

[clandestine]

well think though geez...  would the same size leak in a push pull leak more or less hi than an rxn of the same size and reagents than with LWR....  thats the the point im trying to pass off because its obvious... the longer time would leak a lot more...  and depnding on your flask size and setup could very easily drop your concentration level if your setup was ghetto..  expecially if your borderline on the reagents and it tips the scales into failure..  what if the h20 evaps out in small quantites through that leak too...  it all depends on the SIZE of the leak..  in swims days seeings many ghetto and glass setups.. leaks were seen in most ghettos even if its so small its hard to detect..  the nost can find it usually.

really even nice lab glass setups with sized joints have that pushy problem with the seals if the balloon inflated enough..  sometimes that tape holding the flask in hot and fast rxns gets kinda weak when its heated so much and it loses a little bit of the hold...  or maybe its just shitty tape swim seen used over the eons.

oh well either way...  swim knows from his experence...  if you skimp on the reagents to much a leak could mean failure or success in certain situations.... probly not that of a busy bee but to a newb or semi buzzy it would be a problem..    

Its not really nonsense geez if you think about the possibility of different sized leaks in ghetto setups without condensers lol.

[Zen]

Individual steps:

P4 + 6 I2 -> 4 PI3
4PI3 +4 I2 ->4 PI5
4PI5 + 16 H2O -> 4 H3PO4 + 20 HI
10 E-OH + 20 HI <-> 10  E-I + 10 H2O + 10 H I
10 E-I +  10 HI  -->> 10 M-H + 10 I2

Overall reaction:
 
P4  + 10 I2 + 16 H20 + 10 E-OH --> 10 M-H  + 10 I2  + 4 H3PO4  +  10 H20

P4 = red phosphorous
I2 =  crystal iodine
E-OH = ephedrine
E-I = iodated Ephedrine or iodated  pre meth
M-H= methamphet.

Water is used up.
P4 is turned into phosphate and lost.
Iodine is restored  (the actual catalyst) except it is part of the reaction.

[Jacked]

Geez look at it this way. In a push pull nothing is returning to the flask like in a reflux. There fore a leak is not effecting what is going on in the flask. The concentration of HI is way up there. It's the same as if a single hose was run from the reaction vessel to an outside vent. There are many bees that have done exactly this. L8ter did this all the time, I thought he was nuts but his shit turned out for him every time.. Swim has had more than his share of leaks as well and none of which effected the outcome.. I'm just relaying what Swim has actually experienced in his endeavors into this craft. I trust what he says although I might not be able to explain it very well. He explains what he thinks I will understand in order to keep me from sticking my foot in my mouth by spouting off at things I know nothing about....This is not the case right now..

[abominator]

It's the same as if a single hose was run from the reaction vessel to an outside vent. There are many bees that have done exactly this.

This bee has always done the push/pull minus the tanks.  He found that their only advantage was to control the smell.  Swim recalls on Worlock's old site he recommended running 15 ft. of hose out the window if cook under an Oz. of E.  This bee always did like to put a loop or two in the hose just to watch when suckback occured.

Jacked is right bout(or anything pertaining to the pp) a small leak not affecting the outcome, this happened to swim's buddy just last week when to cork wouldn't seal off for a few minutes.  Swim told his buddy the dope probably wouldn't bee worth a shit.  He was wrong,  the gear was just like the other two hundred rxn's before, quality meth.

[wareami]

Methro_tull, aquagirl, and others had suggested the use of a hose to just kittylitter as the odor containment device.
Ibee's belief that HI gas was an essential in rxns of any HI type, turned out to be incorrect. Aqueous HI is the essential ingredient. This in turn makes h2o a bees friend in the HI rxn.
Ibee set out to prove this to himself! Not that he didn't trust what respectable bees reported along the "uncapped" rxn lines. He just had to see for himself!
He's run rxns to completion without any balloon, condensor or tanks.
In drier short rxns, it was noticed that h2o was driven off or used up and the contents would solidify.
The rxn would complete but only percentage-wise.
The measurment of success in those cases were dependent on the level of hydration.

While Ibee never tried it, He did entertain ben_wiffens idea of flipping a bowl over the flask in an oilbath, leaving enough headroom for the rxn to breath. The bowl rim would create the seal in the oil and according to BMW, it would burp out gas on occasion.

Some may recall Ibees reports during early LWR testing that he would cook the rxn for days with very little h2o and on the last day he would add h2o to fire off complete reduction.
Ibee's cooked rxns to bonedry desert looking powder in the early daze of the 3-4-5day cooks. All produced product...Spacey as all get-out, but product.
The sevenday cooks that didn't convert at all were thought to be products of a reverse-rxn taking place.
We now know that isn't possible.
There had to be a happy medium among all the reactants in the developement of LWR. This had to take into account the HI concentration at levels needed to reduce.
With the LWR, Since a shift was implemented away from all the instruction bees had up to that point, the focus was set on determining the best apparatii and conditions suited for success.
After all, when Ibee first learned...many things defied logic surrounding the suggested parameters in the HI rxn if Ibee encountered 15 failures at his first times up to bat.
These were by-the-book rxns.
The condensor/balloon or just balloon type rxns proved to be the most consistant successful full reductions in the LWR.
Does the rxn need to be contained to complete?
No!
But the chances of full reduction are decreased if the h2o is used up before reduction takes place.
Therefore it's suggested that the rxn be carried out under cdonditions that minimize the chances of h2o being cooked  off into the air.
Be it LWR....P/P....hot/fast...it's always best to not subject yourself to rxn fumes.
If the rxn device springs a leak...plug it and continue for the best chances of success and safety purposes.
There is no right or wrong here, because the rxn will complete either way.
There is a better or worse though.