Author Topic: help with Rp/I rxn in progress,,,,  (Read 2555 times)

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Nuniabiz

  • Guest
help with Rp/I rxn in progress,,,,
« on: January 30, 2004, 04:51:00 AM »
thanx for taking a look and hope someone can give swin an idea of where swin stands at present.
swin broke loose from under the stairs again and got into the lab and started a small rp/i rxn 8 gr. very clean P-fed hcl. 12 gr. resublimed I2 from tinc. and 4 gr lab grade RP in a 125 erlemeyer flask with aprox 18" of braided hose topped woth punch ball and that covered with a couple of increasing in size bags as backups just in case,

rxn started of very vigorously as swin had forgotten to add the D h20 when the I2 was added a half a ml of d h20 was added by syrimge and rxn slowed to a crawl until heat was added and refired as happily as one could ask. after slowly raising the temps over about an hour to just below 100C sxpansion was noted as it krept nearly to the top of the flask.. was patted down and re heated this was done several times until no further expansion was noted at which point the heat was kicked to 120 C and let cook until  swin noticed squarish  crystals forming in the braided. he was unsure if these were HI crystals but thought the odds wereon that side so added a ml of d h20 and washed the x tals into the rxn and has cntinued refulx to this point the rxn fluid is pretty much clear except for the RP can be seen and it boils with large free floating bubbled the obvious question is would this be signs of completion also there was marked white smoke before the d h20 was added. and in reading Jackeds post on a rxn he stated that this wold be the sign she was finito but better safe than unreacted yuckiness any input would be greatly apreaciated.... not swins first rxn by any means but he has complained he has had a couple of rxn seem finiched to him only to find it was about half reacted and the rest Iodometh and iut was not a pleasant expererience so he has been backing off the larger rxn's till he has this problem out of his system thanx in advance
stay safe
Nunia

jemma_jamerson

  • Guest
worlok fail safe
« Reply #1 on: January 30, 2004, 05:34:00 AM »
would be to make sure there is enough of a liquid mass or if not add a tiny amount of water and put it on a light boil for 8 hours. to make sure there is no unreduced gear in there

thats just the fail safe option..you might want to wait for another bee to answer,but thats what i would do. :P


Nuniabiz

  • Guest
forgot to add....
« Reply #2 on: January 30, 2004, 05:51:00 AM »
In re reading swins post a friend noticed that a certain pertanent paraneter had been left out. after the expansion of rxn had been shaken down several times the heat was increased to 120 c and it has been a total now of 11 hours. swin was going to take zib's advice of a nine hour run for a rxn of this size but after the xtals were washed from the up tube swin thought it prudent to allow it to reflux for awhile. the logic being if those were HI Xtals they weren't in the rxn to raise the conc to the required 57-58% so it has been allowed to continue to reflux fo another couple of hours with all xtals in the mix. To swins eye things are ready but swins eye of late has been not the most accurately calabrated of measuring devices so to be sure he has allowed the extra time and will continue to reflux until he hears otherwise from a more knowledgable bee then he. thanx for the re there jemma < one of my favorite actresses as well?
stay safe
Nunia

geezmeister

  • Guest
suggestions
« Reply #3 on: January 30, 2004, 04:04:00 PM »
1) add enough water to rinse the PI3 crystals down into the flask. This will make HI and let your reaction continue.

2) Add enough water next time to let this reaction work. You are obviously using good enough precursors. Now do a long wet reflux and enjoy the quality of the dope.

3) Use some water next time.

4) Use some water every time.

5) Water is cheap. Feel free to use a little more

6) Some water in the reaction is actually a good idea.

7) Don't forget to add some water.

Oh, and one other thing---

Use more water next time.


gluecifer69

  • Guest
Just curious......
« Reply #4 on: January 30, 2004, 05:12:00 PM »
Wondering whether swin set out to perform a push/pull or reflux, sounds like a push pull.  The starter amount of water recommended for a pp would be 4 mL/oz of E

There is a distinct dfference in water amounts in the two.
Follow Geezmeister's advice next time and reflux for a long ass time, it is worth it!!!


Stonium

  • Guest
One more thought on water...
« Reply #5 on: January 30, 2004, 09:45:00 PM »
Don't use too much, either.  :P

On another note:

Follow Geezmeister's advice next time and reflux for a long ass time, it is worth it!!!
Speaking of a long ass time...

This advice has been not only geezmeister's, but that of all sorts of others in the know around here for what seems like forever.

Obviously, it takes some of you a bit longer to listen than it does others.