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how does one recover MeOH from the basified remains of a AlHg workup?
after basifying with aq. NaOH, and extracting with toluene, you are left with a solution of MeOH, H2O, and sludge. filter out the sludge.
now, how does one distill the MeAm infused MeOH from the H2O and MeOH azetrope (as recommended by Osmium in his MeAm writeup? (https://www.thevespiary.org/rhodium/Rhodium/chemistry/alhg.osmium.html (https://www.thevespiary.org/rhodium/Rhodium/chemistry/alhg.osmium.html)
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Don't Basify.
- After Adding Nitro/MeNH2, add a little solid NaOH to speed up
- Let sludge settle
- Filter off sludge
- Distill Off Methanol/Methylamine(Bottle & Re-use)
- Add dilute Hcl to leftover residue until ~P.H. 3
- Do 3x N/P washes
- Basify
- Take up in N/P, Gas, recrystallise, dry, Send sample to abolt :)
how does one distill the MeAm infused MeOH from the H2O and MeOH azetrope (as recommended by Osmium in his MeAm writeup?
Methanol and Water have no azeotrope, check page 8 of this link:
http://www.methanex.com/methanol/Methanex_TISH_Guide.pdf (http://www.methanex.com/methanol/Methanex_TISH_Guide.pdf)
(Rhodium, this link has excellent info on the properties of Methanol. You might consider putting it on your page.)
Just keep your distillation temp below 80.Celcius. ;)
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too late for all the stored up remains SWIM has been holding on to.
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I have archived the document linked above at my page:
Technical Information & Safe Handling Guide for Methanol (https://www.thevespiary.org/rhodium/Rhodium/pdf/chemical-data/methanol.technical.info.pdf)
(https://www.thevespiary.org/rhodium/Rhodium/pdf/chemical-data/methanol.technical.info.pdf)