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?
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?

