Balloon ruptured on LWR, advice needed plz

[kuskus]

Hello

Before SWIM begins, he would like to say that he danced with TFSE for a while before posting, but could find no information specific to his peculiar problem.

SWIM is in the process of doing a LWR, after several successful short cooks under SWIM's belt (first try too).

SWIM's reaction vessel is a converted lava lamp with a balloon on top, and a 40W bulb that gets to around 110C on the surface of the bulb.
SWIM is using MBRP, I2 from tinct, and pseudo from pills.

The amounts of each reagent that was used are:
- approx 5.5 gm pseudo
- approx 3 gm rP
- approx 6.5 gm I2
- 4ml dH2O

Now, SWIM set it all up, and everything was going fine so he went to sleep for a couple of hours.. When SWIM woke up 6-7 hours later he saw that the balloon was limp.. Uppon further inspection SWIM saw that there was a big rip in the balloon, where the ballon meets the vessel. SWIM then took the vessel off the heat and let cool, added about 1.5ml of dH2O, and put 2 fresh ballons on (one inside the other). The vessel was then returned to the heat. After a couple of minutes the reaction started up again and seemed to be going just fine. There was a good amount of HI gas whisping around inside the vessel.

However, an hour or two later, there was no more HI gas to be seen inside the vessel, and the condensation on the sides had mostly kinda dried up, whereas before it was plentiful and running fairly freely down the sides.
The ballon is still standing up.

Would any of you knowledgeable gentlemen have any advice for SWIM? Or is everything fine in your opinion?

Any help would be greatly appreciated.

[wareami]

Add 1g I2
Add .5g RP
Stir....recap and cook for 30-48hrs!
However long your patients can sit still...but ot less than 30 in Ibee opinion!
Especially since adding new precursor!
It's those precursors that create side reactions and time in a properly ratio'd rxn is what cooks them off or lessens them!
No more dh2o should be necessary since adding the 1.5ml after the mishap..

Check rxn after 8 hours to determine the moisture level.
If still fluid and liquidy...keep running!
Every 8 hours following uncap and stir, knocking down side creepers!

[kuskus]

Thanks pal. SWIM added 1g of I2, but had no clean rP so skipped that. SWIM put it back on the heat, and its doing much better (HI gas is visible).

BTW, is it just SWIM or is wetdreams down today?

[kuskus]

OK so this is kinda weird..

Shortly after SWIM got the reaction going again, it promptly died again. So SWIM opened it up again, squirted .5ml of water in, and the reaction started up again, only to die out again shortly after.
Oh SWIM forgot to mention in his last post that he added .5ml of dh2o then too. Also SWIM should probably have mentioned the white-ish residue that was left on the side of the vessel when the condensation dried up the first time.
So SWIM has just added another 1ml of dh2o to get things going again, gas was visible for a couple of minutes, then not. Balloon still stood up though.

SWIM has a theory about this situation. The vessel that SWIM is using is quite long, like 12". Could it be that water is condensing on the side, but due to the fact that there is not much of it compared to surface area on which it can condense, that leaves no water in the rxn fluid?

EDIT: Ok now THIS is weird.. SWIM just pulled the balloon off without taking the vessel off the heat. What does SWIM see? A cloud of smoke immediately appeared in the vessel, so SWIM wrestled the balloons back on, which was shortly followed by... Can you guess? Smoke went byebye. SWIM hit the bong.

[wareami]

And leave the rxn alone!
Swim has 20 plus hours to GO.
In a LWR your not suppose to gauge the rxn by it'sactivity but by your inactivity!
And quit opening the rxn except at the specified checkoints for the specified reasons only!
There should be plenty of RP in the rxn as that won't escape as readily as I or HI.
The suggestion to add .5rp was only to give a KICKSTART to the new I2 added!
Done properly, the LWR is akin to watching grass grow! It's not meant to provide amusement to the cook!

[CharlieBigpotato]

removing the balloon decreased the inside pressure, allowing some vapors to exit the fluid; sort of like popping a beer can.
visable fumes are not needed, nor very helpful, as it is in the rxn where the HI is needed.
even bubbling isn't needed.
its hard to beelieve that something so boring to beehold, could bee illegal.

[kuskus]

Hey guys..

Ok so SWIM is getting ready to do his post rxn workup soon.. SWIM thinks there is a very good chance that there is some of the new gakk in there.. He used the TCE/Japan drier method, but that doesn't get rid of the new gakk right?
Any suggestions on what SWIM might do now to get his shit squeeky clean?
I guess steam distillation would be one way.. But SWIM does not have a distillation setup.. SWIM did read about using like a sauce pan or something, with the lid inverted and full of ice, and a receptacle in the pan to catch the condensed vapors.. Sort of like how a hickman condenser works.. Would that work inyour opinion?

Thanks guys.

[wareami]

The new gaak after it undergoes the conditions of the rxn makes it the nastiest xtal inhibitor on the market.
Ibee's attempts to rid this new gaak on the frontside extract with just JD/TETRA failed miserably.
That fact alone was enough to stimulate Ibee's paranoia psycho-sis into beelieving the newest gaak is a diabolical conspiracy plot aimed at Ibee's methods  making them madness!  
But seriously...The work-up should be carried out as normal to claim whats claimable and to get a taste of what's beeing dealt with.
That seems harsh and cruel but oneday you'll see why.
This is what you'll get from titration:
An oily Evapped end result. It won't xtal. That's okay...because now you'll have to learn recrystalling.
Re-xtal what is obtained.
One can still distill to get the product and Ibee isn't familiar enough with your proposed ghetto rig to say it will or won't work.
Ibee says titrate then rextal until higher skill levels are achieved through reading and practice.
Make certain to wash the post-rxn fluid with NP prior to basing for best results.
You'll bee living UP to yer name in no time kuskus  

[SHORTY]

Don't try to distill that way or you will not have anything.  That type of distillation is meant for distilling water not meth.  Follow wareami's advice.

[kuskus]

Hey guys, SWIM would have posted sooner, but SWIM was at GF's house all weekend enjoying the fruits of his labor.

SWIM is not so sure the pills were neo-gakked (shaddap) after all.. Or perhaps SWIM inadvertently got rid of it somehow..

The former would be more likely.. But SWIM was under the impression that pretty much any pill (esp. the 120's) with a >;;;;2006 expiration date would have the new gakk.. Most of SWIM's pills had >;;;;2006 exp date.

So just for the hell of it SWIM will write a very informal and likely innacurate report on this latest reaction of his.

Well you know the details of the reaction itself except it's length, which was about 30 hours (minus a few hours from the various problems that occurred, SWIM would guess).
SWIM really wanted to let it go the full 48 hrs, but was really pressed for time.

Ah there is actually another detail that may be of interest; for the last 6 or 7 hours of the reaction (which SWIM reminds you, in case you forgot, was carried out in a lava lamp) SWIM switched the 40W bulb for a 60W one.
The temperature on the surface of the bulb was approx 140C.
SWIM is sorry, but he does not know the temp of the rxn fluid itself, nor does he know how to derive it from the temperature value of the surface of the bulb. If SWIM was to pull a value out of his ass, it would probably be 130C, but he has no reason whatsoever for thinking that. SWIM just has a gut feeling.. Or perhaps SWIM should lay off the baked beans (amongst other things)..

Anyway, SWIM did this because he knew that he would not be able to let it go 48hrs, and figured it could help a lot to raise the temp in the flask to speed it up a little. SWIM can't really say whether this worked in his favor or not.
SWIM became aware of some past discussions on rxn temp, and its effect on the presence of undesirable compounds in the end product. It was too late to turn back really, so SWIM said "fuck it".. SWIM was then made to wash his mouth out with soap.

Oh BTW, SWIM did not "reset the timer", so to speak, on addition of new precursors (well, just I2 really) as was suggested by ware. Again, time was scarce.

SWIM also read about using UV and whatnot to help the rxn.
SWIM was in an experimantal mood, so he set up a small fluorecent light to shine in the vessel. This continued for a couple of hours, then the rxn vessel was placed in full sunlight on the windowsill for about 4 hrs until the end of the rxn.
The sunlight seemed to have quite a noticeable effect on the rxn, which SWIM could only describe as an increase in vigor. 

Post reaction, SWIM washed the living fuck out of the rxn fluid, on account of the vast amounts of I2 left in there after filtering a couple of times. SWIM started with about 4 or 5 xylene washes.. SWIM didn't keep count unfortunately.. SWIM is starting to see the value in recording details in a notebook as one proceeds.

After the (now crimson) xylene washes, SWIM washed with TCE, which turned pink and caused much annoyance by being heavier than water.

This was followed shortly by a couple more xylene washes, as the color of the rxn fluid was still somewhat darker than considered ideal, and finally a couple of hot naphtha washes.

Btw SWIM WAS aware of the boiling trick used by some to get rid of excess I2, but SWIM only thought of it AFTER diluting the fluid with hot dh2O.

SWIM's A/B was in the form of a kerplunk type thing with naphtha as the NP. SWIM did 2 pulls. Washed twice with plain dh2o.

SWIM titrated, and ended up with some excellent (by SWIM's standards) product. It is sparkly as hell, and just as potent (hence this giant rambling post). Seems pretty clean to SWIM, but what does SWIM know.. SWIM has yet to rxtal due to time constraints, but will be doing that either tonight or tomorrow.. Will let you know.. whether you like it or not..

Thanks to ware and shawtey for the tips..

Lata fewlz