Author Topic: half frozen ketone  (Read 2356 times)

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darius

  • Guest
half frozen ketone
« on: September 03, 2004, 09:03:00 AM »
So swim tried the old srv, a little while back and then was distracted after doing all the hum dee lala lala and performing it seemingly without error, it was placed in the freezer. 

The vac. distillate was noted at coming over between 102-110c,  saf apx the mid 80's to 91-92.  Swim seemed satisfied. 

however, recently when swim went to check on it it was half frozen.  finely formed crystals, and when tipped on it's side there was a small amt that remained fluid. 

Before running for help all the FAQ answers were tried, it was redistilled under vac, and a more refined yellow/green fluid came over again, no forerun, only the upper fraction collected and saved, and the same shit happened!  frozen!

it seems to pass every other test swim can think of though... smells correct, casts greenish glow under UV light, rootbeerish taste that sort of numbs swims tongue, bp is almost dead on (swim is open to the fact them. may be off by a degree or two). 

what the hell?  Has this happened to other swimmers? thanks for any help.


Rhodium

  • Guest
And the mp of MDP2P is?
« Reply #1 on: September 03, 2004, 09:48:00 AM »
How cold is your freezer?

You might have the MDP2P contaminated with a sizable amount of the corresponding aldehyde ("MDP3P", bp slightly higher than MDP2P), this causing the mixture to solidify easier.


darius

  • Guest
pretty low
« Reply #2 on: September 03, 2004, 11:50:00 AM »
took swim a while to get check, but therm. doesn't record that low.  swims digital thermometer issued two asteriks and alcohol thermometer stops at -10c if swim had to guess based on continued scale of the alcohol therm. it would be close to -18c.

Alright.   Out of morbid curiousity, and since swim happens to have your attention, what precautionary measures can me taken against mdp3p formation?  is there any practical use for it?

thanks


XrLeap

  • Guest
Did you try the sodium bisulphate test?
« Reply #3 on: September 04, 2004, 11:15:00 AM »
Did you try the sodium bisulphate test?:) Come to think of it, why not just proceed to make some honey using any preferred route on a small scale to confirm this?:)

just some novice suggestions....:)


pooky

  • Guest
Rhodium..
« Reply #4 on: September 07, 2004, 11:28:00 AM »
posted a nice little write up a few months ago,demonstrating how a wash and work up with something or other would rid you of your 3P.When,what and how you'll have to search for.


Snakebyte

  • Guest
I was wondering why you didn't get back to me...
« Reply #5 on: September 07, 2004, 04:11:00 PM »
I was wondering why you didn't get back to me on those questions awhile back.  Swim's never had success with his O2 wackers and has an excellent setup.  Your distillation gap between your safrol and ketone is less than 20C, which seems much too low for that amount of vacuum.  Swim's vacuum pulls better than yours and his gap is about 35C.


Precursor2112

  • Guest
In my feebles attempts and many failures
« Reply #6 on: September 08, 2004, 08:41:00 AM »
MANY FAILURES..
if it freezes it ain't key...

Rhod has a m3p work up?  where?