The Possible Dream.......

[DarkSky]

Once upon a dream there was someone with 15gE/17.5gI2/16gH3PO. In this dream they combined 15mlDH2O, 16gH3PO & 17.5gI2 in a 500ml flat bottom bottle. A "getto" condenser was connected to this and it was placed in a pot filled with sand and oil.

Once HI had been made it was allowed to cool (untile the ballon collapsed) and then the 15gE was poured in a little at a time and swirled. The bottle was sealed again and placed back in the pot of sand. The temperature of the oil was slowly raised to 165°C (SWIM estimates that there was a 20/25° differance between bottle temp and oil temp) at which time everything started to bubble very nicely. After an hour the temperature of the oil was maintaining at 165/170 and activity was visible. At this point the dream takes a turn for the worse.

The bottle and "getto" condenser that SWIM was dreaming of consisyed of a 500ml small milk bottle with a cap attached, though the cap there was a PVC 1/4" hoes bib adapter affixed  with 16" of 1/4" braided hose to which a balloon was attached. SWIM had used this set-up before for a RP/I rxn and had not had a problem.

Well, whether the hose adapter had been weakened from the heat in the previous rxn or it was just not able to substain the heat for this H3PO rxn is unclear but was is clear is the hose seperated from the cap after 7 hours of rxn time. When SWIM found this a portion of the Fluid had managed to make its way out of the bottle and now had the oil in the pan colored a dark black. SWIM removed the bottle, sealed it up and has set it aside.

It will probably be a few days before SWIM can finish this dream so here are his questions, please bear with SWIM because this is only his second rxn and his first H3PO rxn;

1) SWIM has a bottle which containes approximately 3/4 of the mixture that he originally started with and it's the color of motor oil after 7 hours of heat. Is this normal?

2) Can SWIM restart this rxn in a few days after he figures out how to fix up another attachment for his bottle?

3) If so, will SWIM need to add any additional H3PO or I2 at the time he restarts the rxn and how much?

The feed stock was cleaned via the IDEA method from dollar a pack 60's, I2 was from tinture and H3PO was 98% flakes and fresh.

Any and all help offered SWIM with his dream will be appreciated

[DarkSky]

Sorry, H3PO3 is what I ment

[biotechdude]

IMHO the reaction should be done at 140'C reaction temp for 7 hours (so no need to restart or add extras).  Your ghetto condenser (a braided hose) is not recommended at such temps (as swix's proper condenser condenses to half-way up).  The hot-cooked gear will be 'hard' and smell like a hypo cook.

HOWEVER in the future, a longer cooler reaction would also suffice.  BOS suggested 90-100'C for 14hrs (no vissible bubbling will occur).  These parameters are more appropriate for your equipment and produce similar yields.

Lastly, what is your post reaction workup? 

I'll assume you won't be steam distilling (as no condenser).  Let reaction cool and dilute with some dH20(when cool; flask will darken and may see solid phosphoric sediment). Then np wash 3x. Then base with 50% NaOH solution and extract to dry np 3x. Wash np with salty, hot and cold dH20 (IMPORTANT - as not ridding your extraction of extra salt(able) ions will cause a funny taste and whitish appearance to your end product).  Then titrate or gas np and evap slowly.  Flash with acteone to rid of excess h20, then recrystalise or use as is.

Hope this helps and good luck

[DarkSky]

SWID does not think the stuff is ready...either that or he has royally screwed up! The stuff in the bottle is black, the color of oil and now that it has set for some time it is no longer liquid, at least not most of it. There is a little liquid  with the consistency of oil on top, the bottom seems to be a mass of some sort. Please tell me there is some way to salvage this

[DarkSky]

To the bottle 1ml of DH2O has been added and a 1' long 1 1/2" dia. braided hose was attached and secured with a hose clamp. In the top of the hose a rdeucer was attached and a 1/4" dia. hose with a balloon was secured to this. The bottle has been placed back on heat and is slowly being brought back up to heat

[DarkSky]

20 minutes into cook: oil temp 86°C (estimate 20/25° differance between ouil and bottle), light white smopke apparent, balloon starting to presurize

30 minutes into cook: oil temp 104°C, light white smoke still apparent, Balloon erect

45 minutes into cook: oil temp 123°C, light white smoke still apparent, red tint to bottle and some redenind of hose, light swelling to balloon maintaining this temp for now

[Rhodium]

There is no need to post real-time reports of your experiments, as that is completely unusable to anyone. Wait until you are finished, and then post a complete report if you believe it has any information value.

[geezmeister]

Keep cooking, and raise the temp slowly as you do. What you describe suggests that you never reached a proper temperature for the H3PO3 and I2 to make HI; It sounds as if you have made it now. If the solution goes yellow, level off the heat at that point and reflux it for another eight to twelve hours. Going long on the reflux will not hurt anything, and in my experience the longer times give better yields and purer meth.

[DarkSky]

Thanks Geez, Ill follow your advice....and sorry Rhodium if I was out of line earlier. Once I have finished Ill post a detailed report

[DarkSky]

Well the results are in and it was a miserable failure! Looks like the problem started yesterday when SWID had the equipment failure. It appears like some of the PVC from the melted part managed to get into the rxn fluid and contaminate the whole batch.

When the rxn fluid was mixed with DH2O it turned a nasty greenish, cloudy white color with globs of the contaminate floating in it. It also had the odor of melted PVC. Guess enough can’t be said for having the proper equipment before you begin.

Thanks to all, I’ll dream again soon!

[livid]

that happened to swim a long time ago along with melted getto stoppers, heating problems,vessel, chems, the list goes on and on. then one day sucsess. Now failing is not an option.

[energizer_bunny]

While confidence and determination are a bees best friends, complacency and "man of steal" syndrome can lead to serious disappointment.
"Failing is not an option" .....UNTIL someone throws a monkeywrench in the works. Rxn inhibitors for example.

The IDEA method is not sufficient for removing OrangeII gaak. Judging by the work-up summary and the rxn fluid color when dh2o was added, OII gaak seems to bee the likey culprit.
If one were to add 10ml of JapanDrier to the IDEA juice(iso,denat,tetra,tone) before cleaning the finely ground pillmass, then OII gaak will be dealt with after several acetone washes of the scraped UP xtals. Remove all traces of blue before proceeding.
Hope this helps...

[livid]

swils point was,Everything under the sun that could go wrong, has gone wrong . eventually , thing start going right. you start knowing about the visuals. Knowing what to look for.Knowing what is going on at all times instead of hoping everything is going right. Sure things dont always go as planned and trouble shooting is required, swim doesn't buy meth anymore. Swim has alot to learn.