Author Topic: Citric acid direct to freebase  (Read 362 times)

b6baddawg

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Re: Citric acid direct to freebase
« Reply #20 on: June 02, 2011, 11:30:52 AM »
alternate gassing-

drip conc hcl (28%) onto conc sulphuric (92%)  while been stirred, the evolved gas turns to vapour when in contact with air, swim fills the vessal with gas allowing a small "puff" to escape the tube fitted before directly gassing the boiled dry and cooled xylene.the % stated was just what was used successfully.

jobs a good un.

observations/notes

stirring the sulphuric while dripping conc hcl onto it is definately desirable, it makes the control of gas flow regular as you drip and prevents either foaming over or sudden suckback.

swim was gassing litre portions of xylene, the fine mda hcl formed was cropped and filtered in 3-4 goes. after each second "crop" the xylene would be reheated  and cooled before continuing to drive of any moisture what may have got in while filtering.

the mda.hcl would then be washed with freezing acetone.

when using the worked up "oil" portion the colour was white with hint of yellow.
the chloramine portion was pearl white.


swim asked older bees why they didnt gas so oft in the old days, it would be worth noting if in a high humidity area you might have a problem and titration be preferable.

theres a certain "magic" when titrating method thats absent when gassing dontya think?

Tsathoggua

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Re: Citric acid direct to freebase
« Reply #21 on: June 02, 2011, 05:39:22 PM »
Tsathoggua doesn't know about the rest of you...but he would not be happy using OTC solvents. He does use OTC methylated spirits to clean glassware after use, but plenty of OTCs are crap. For instance, he picked up some toluene/aromatic type stuff, which turned out to be dyed GREEN. This, needless to say was never used, and remains in the house only for use if something needs burning, or oily muck needs cleaning off metalwork, etc.

OTCs in the UK are full of crap more often than not, although some naptha is ok. There unfortunately, is pyridine in the denatured alcohol, which always contains purple dye to prevent drinking thereof. This could of course be distilled, but Tsathoggua buys pure, clean MeOH and toluene in five or ten liter jugs, and other solvents from the same supplier he gets his lab reagents at, and they always evap cleanly. He suggests other hymenoptera of all descriptions do the same...there is no substitute in his opinion for clean reagents and solvents.
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