Author Topic: Won't boil....  (Read 4970 times)

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8ball

  • Guest
Won't boil....
« on: July 04, 2004, 07:24:00 PM »
The other night swim's hypo(shortys hypo mix) reaction started just like they always do so once the temp was set to 110c and evrything was boiling away swim went back to working on his bike. Maybe 3 hours later went to check and make sure everything was cool and noticed that the boiling had stopped yet the contents were still condensing and the temp was maybe 5 degrees celcius lower, so swim figures he will up the heat a little to get the contents boiling again, but even at 126 deg celcius the contents would still not boil, the only boiling that occured was when the condensation would drip back into solution from condenser. so swim decreased temp to 120 deg celcius and went back to working on bike for another 4 hours, then when swim went to check again the temp was the same maybe 1-2 deg higher and still no boil but still condensing. Anyway swim turns heat off for hour then starts to re-arrange equipment to begin distilling the honey, which went the same way as usual(time to distill and quantity) yet the quality had not been as good as usual after re-crystallizing.

Has anybody encountered this problem before or have any ideas as to the cause of the flasks contents not boiling.
all glassware was spotless and acid, iodine and pseudo quantities were the norm. Before swim left the first time 3ml of distilled was added to rinse HI crystals back into flask.

cheers any input would be appreciated.


Scottydog

  • Guest
Hypo Concentration?
« Reply #1 on: July 04, 2004, 11:05:00 PM »
The longest that Swim's hypo rxns even bother to run for is right around 3-4 hrs.

Swim is not an expert on hypo rxns and could bee wrong but maybee it is something as simple as a hypo concentration issue?

Too much water or not enough hypo? Did all of the iodine clear?

Swim had similar problems with Phosacid and narrowed it down to pill gakk.

Maybee concentrate any remaining hypo a little further, add a little more of this hypo that has not yet been diluted with any water, raise the temp a little and let it go for a few more hrs? Swim always dreams of doing this (just in case) and it always seems to remedy the problem.

Quantity of hypo, concentration of hypo, temp, excess water or pill gakk.

Not that I recommend you do this, but after a PM with another bee, Swim has always wondered if NaCl could bee used to "dehydrate" an overly diluted rxn to release gas HI from the fluid? Would this work to clear up any remaining iodine and bring a rxn to completion?


SHORTY

  • Guest
What happened when you agitated it?
« Reply #2 on: July 05, 2004, 03:26:00 AM »
Would it boil if you agitated it?  As sd stated, there are numerous possibilities however, if you did everything the same as usual then it is probably a gaak problem.  Next time add a few pieces of broken glass and see if that will get it boiling.  A little iodine will also get it going sometimes.

If it wouldn't boil at 126 and it wasn't superheating then the hypo could bee the problem.  Since phosphoric acid has a high boiling point depending on the concentration.  Was the hypo used in any other rxns or just this one?


wareami

  • Guest
Hmmmmm....
« Reply #3 on: July 05, 2004, 06:21:00 AM »
Wouldn't a fully reduced product subside activity-wise after a time?
I'm sure at those temps...miniscule bubbling would be taking place...so much so that you'd have to look very close.
Ibee would say it's done doin what it was done diddin! ;D


8ball

  • Guest
Still a strange one though
« Reply #4 on: July 05, 2004, 04:47:00 PM »
SD.  Too much water or not enough hypo? Did all of the iodine clear?

            Swim don't think that too much water was the problem as swim don't generally add water to swims hypo once it has been concentrated prefering to maybe rinse the sides of condenser down with no more than 2 - 3ml of distilled once ingredients have been combined. Swim assures that with 15g of pseudo and 30ml of hypo there was no dramas there either. And as far as the I2 no dramas there either as the smell was quite sweet and solution was almost clear bar a slight blue gray tint, and swim does mean slight. Swim agree's that reactions are normally over by the time 3 - 4 hrs have past as swim used to only let them run for 2hrs but is now a little lazy so just lets them go till he is ready to complete. But swim cannot rule out the pill gaak although he would be a little surprised.

        SHORTY   Would it boil if agitated gently

                    Yes it would but only for a very minimal amount of time, and not vigourously. Boiling chips were present from the beginning of reaction so as not to forget to put in before distilling as swim often used to forget until the bumping would start. This batch of hypo had been used only once before 2 weeks earlier and was typical of other reactions slowing considerably to just the ping pong ball effect and occasionally a vigourous boil every few minutes for 10 - 15 seconds.

         Wareami    Would'nt a fully reduced reaction cease to boil.

                       Well one would think so at temps closer to actual boiling point but at these temps you would expect some sort of movement on the surface or like you mention, at those temps there must have been at the least tiny bubbles, but no nothing yet there was a very slight reflux occurring.

Unless there is some sort of new gaak creating this problem swim would be surprised if it was in fact gaaks at all as no doubt he would have had the problem occur before, but has not.
Swim does not know what to think, but its still a strange one though...

Shit almost forgot to mention swim did add a couple of extra mls of hypo but only boiled for maybe 2 mins but did not add any extra I2..

thanks for your thoughts.