armageddon & organikum
You have both taught me a valuable lesson, and that is that a bee that is prepared to roll up his/her sleeves, put some glassware together, and do some
actual research is worth more than all the bullshitting "armchair experts" on the planet.
Nevertheless I am astonished what kind of behaviour of a certain immature member is tolerated here - I thought this forum is moderated.Do you think that the reason that I have not been, as you say, "moderated", is that I may have a point?
I am quite happy for the members to go back over this thread and make up there own minds as to who has been productive and counter productive.
Let's agree to not pollute this thread with any more of your stupidity.
To save yourselves any further public embarressment, you can P.M. your apologies to me.
Now, here is some more USEFUL information.
After reading the interesting words of abacus:
Setup for redistillation and distil again at atmospheric pressure UNTIL the flask contents temperature is OVER 150DegC, Then pour into a container and cool. This will cause the whole solution to form a solid.
in his
(EDIT - THE WORD THREAD HAS BEEN REPLACED WITH THE WORD POST, APOLOGIES FOR THIS OVERSIGHT, ALTHOUGH I ASSUME THAT MOST OF YOU WOULD HAVE BEEN INTELLIGENT ENOUGH TO WORK THIS OUT ANYWAY
) post:
Post 513530
(abacus: "Alcohol is not vital", Methods Discourse)abacus, then goes on to say:
This seems like a lot of crystallising methylamine.hcl but its not.Maybe so abacus my friend, but if you substitute the first part of the I.G.Farben patent as mentioned by BDB:
Post 500578
(Bond_DoubleBond: "Nothin special, but here ya go . . .", Methods Discourse)for the Vogel procedure you are left with a MeNH3Cl that is suitable for the Osmium Al/Hg.
Swim set about to do another experiment, using some of abacus's interesting workup.
After formate distillation, excess NH4CL removal and the 1 hour reflux, glassware was set up for distillation and the oilbath was raised to 155 Celcius (as measured by a thermometer dipping into the reaction) and held there until water distillation ceased. The distilling flask was quickly removed and the contents poured into a beaker whilst still hot.
The beaker was left to cool to room temperature and formed a hard white sheet of solids, that was crushed up and vacuumed filtered to allow for around 10 mls of liquid that was crashed out with dry acetone to give a very small amount of MeNH3Cl. The resulting dry crystals in the buchner was thoroughly rinsed again with dry acetone and vacuum filtered again and gave no appreciable weight loss. Tests done on the crystals showed them to be at least 93% weight MeNH3Cl.
This research is also in accordance with the yields noted by BDB (92% & 94%):
Post 512674
(Bond_DoubleBond: "not to worry . . .", Methods Discourse)My point is that MeNH3Cl for a standard 3 x excess Osmium Al/Hg, can be made without recrystallisation, the use if vacuum or vacuum filtering and with "ghetto" equipment if need be.
I know this might offend some of the purists out there, but please consider:
Simply add the required amount of reactants, quickly distill off the formate, reflux, filter, distill and hold reaction temp at 155 C until H2O distillation ceases, quickly pour out, let cool, crush up solids and add aqueous 25% naoh until neutral.
Easy as pie
This is just bits and pieces of other peoples techniques.
Thank god for research.