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| Laboratory Tips Safety proceedures, test reagents, drilling rubber stoppers, bending glass tubes, etc. Contributed to by chemists. |
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#1
 2003-11-24, 07:08
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kelz 
Regular
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uninvited guest interupts reaction - help please
so swim is 15.5hrs into 11 g E reaction (rp/I2) and uninvited guest shows up meaning a hasty disasembling of equipment -
temp was at 180f at this time and had been for several hours,
the flask prior to this had most of the RP on bottom of flask with a small amount still in clear liquid,
the bubbles were not visible from the surface, but could be seen in small clusters near the bottom of the flask, they were tiny and the clusters of them only covered some parts of the bottom of the flask.
swim took the flask and placed it out of obvious site (reaked of rotton eggs when condensor came off) when disturbed and their it has remained for most of the day.
my question is can SWiM start the reaction back up 2morrow (because swim believes it may not quite be finished) ?
swim assumes what is in the flask is still o.k and unharmed up until this point?
thanks for any help as this will determine my next step which SWIM is unsure of at this time,
cheers all :-)
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#2
 2003-11-24, 07:35
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kirby 
Regular
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Re: uninvited guest interupts reaction - help please
15 hours will still be a good result...
carry on as though the time was right
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#3
 2003-11-24, 07:40
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kelz 
Regular
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Re: uninvited guest interupts reaction - help please
thanks for the prompt reply Kirby,
swim will carry on as if completed then,
just out of interest how come the flask cant be thrown back on and brought back to heat?
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#4
 2003-11-24, 08:06
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kirby 
Regular
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Re: uninvited guest interupts reaction - help please
hmm
ive got a feeling the reaction carries on with or without heat,,at 6 hours you have a good result,,anything more than that and it gets better but by small degrees,,,use it as a tester,,you may like 15 hour meth
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#5
 2003-11-24, 19:12
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madchemist 
Regular
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Re: uninvited guest interupts reaction - help please
It does carry on without heat.
The HI reduction carries on regardless of temperature. Heat just tremendously speeds the reaction. A reduction with HI attempted at room temperature or below will happen too slowly to be of any value.
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#6
 2003-11-24, 22:12
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Wicked_Rain 
Regular
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Re: uninvited guest interupts reaction - help please
once he removed the condensor tho the reaction came to a halt since all the HI was lost. id run it like it is and be happy 15 hrs is a good cook. if you just had to refire it maybe 3 grams of I2 and 3 grams of RP condensor back on. maybe the I2 only. id go by look and feel from experience but most likly id filter it and do post rxn workup and be done with it besides it was only 11 grams into the flask it really should be complete especially at 180. my opinion anyways.
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#7
 2003-11-24, 22:19
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kelz 
Regular
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Re: uninvited guest interupts reaction - help please
swim took a few ml's of honey from the flask and did an a/b to test the product, to determine whether to continue or go to clean up -
the end product has swim sold that its all good - so on with cleaning the rest,
thanks for all the help :-)
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#8
 2003-11-25, 17:31
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Str8_Shooter! 
Regular
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Re: uninvited guest interupts reaction - help please
At that temperature, if everything was done "right", and you were reacting under "ideal" conditions, your rxn was as complete as it will ever be at 6 hours.
You will, of course, want to heat it back up to free up the R, for easy removal (of the red from the flask, as well as the meth from the red).
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#9
 2003-11-26, 00:36
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kman 
Regular
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Re: uninvited guest interupts reaction - help please
15 hours is as long as swim has ever run a rxn, and usually less. Smoke that shit, man!
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