11-12-02 18:22
No 379131
Hey
When makin methylamine.hcl you can do this
Clean the blue paraformaldehyde with 3-5gallons of H2O and a few alcohol soaks. This will leave the paraformaldhyde free of most of the dye (still light blue) but usable in the synth.
Also instead of buyin the good ole ammonium chloride you can make a conc. sol of NH4Cl from conc. ammonia solution and muriatic acid. This will leave a sol which some NH4Cl precipitates and the rest is a saturated sol (35g/100ml H2O) at room temp. This can be directly pluged into the brighstar synth!!
The methylamine.hcl will be slighty blue but in the Osmium al/hg it doesnt get in the final product and the yields are high~!
Sink or SWIM
(Hive Addict)
11-12-02 20:31
No 379157
Is the dye from an OTC source of paraformaldehyde? And couldn't all these posts about your success have been in the same thread?
there's a big difference between criticizing your government and criticizing your country
(Hive Bee)
11-12-02 20:41
No 379158
Yes, there is an OTC source of paraformaldehyde which contains a blue dye.
sorry about the multiple threads!
Sink or SWIM
(Synaptic Self-Mutilator)
11-14-02 07:09
No 379611
Once you try it compared to the HCHO/NH4Cl, you won't go back.
(Old P2P Cook)
11-14-02 07:13
No 379615
Why, what is the difference?
Baseline Does Not Exist.
(Hive Bee)
11-14-02 13:26
No 379712
swim needs a source first! p-CH2O is fiiine so far
Sink or SWIM
(Synaptic Self-Mutilator)
11-15-02 08:46
No 380013
I'd prefer handling 31% HCl over 40% HCHO. Also it's easier and cheaper to find hexamine and hydrochloric acid than to find formaldehyde and to *make* NH4Cl as in the post. Plus there's more "NH4Cl equiv" (ie as HCl/hexamine) used in the hexamine reaction, and according to K.C. Nicolau it's a good thing "to suppress the dimethylamine formation". Perhaps K.C. Nicolau (an old school bee, if you recall him) got that wrong?
(Old P2P Cook)
11-15-02 10:32
No 380048
I'd prefer handling 31% HCl over 40% HCHO. Also it's easier and cheaper to find hexamine and hydrochloric acid than to find formaldehyde and to *make* NH4Cl as in the post.
Yes, if you can only acquire OTC chems then perhaps you can't get formaldehyde so hexamine is the only way to go. If you can acquire simple but non OTC chems then paraformaldehyde and (store bought) ammonium chloride is the way to go. "Stinkiness" doesn't seem to factor anywhere into the decision.
Plus there's more "NH4Cl equiv" (ie as HCl/hexamine) used in the hexamine reaction,
IIRC, the ratio of ammonia to formaldehyde in hexamine is exactly the same as is called for in the Org. Syn. and Vogel preparations of methylamine.
and according to K.C. Nicolau it's a good thing "to suppress the dimethylamine formation".
I haven't a clue as to who K.C. Nicolau is but Vogel says the same thing so it must be true.
Perhaps K.C. Nicolau (an old school bee, if you recall him) got that wrong?
Whenever possible I prefer to get my information from closer to the source - Vogel, Org. Syn. etc.
Baseline Does Not Exist.
(Chief Bee)
11-15-02 11:17
No 380059
I would really reccommend using ammonium chloride/paraformaldehyde. The yield is 85%, and you don't need to handle ANY smelly/corrosive liquids...
Instructions: ../rhodium /methyla
(Hive Addict)
11-15-02 20:18
No 380162
Would Chromic's method of heating the second time until ammonium chloride sublimes be a better workup than just heating until half remains? I seem to have difficulty knowing when all the ammonium chloride is removed, since it looks no different to me.
Life is not measured by the number of breaths we take but by the moments that take our breath away.
(Old P2P Cook)
11-15-02 21:39
No 380173
You should follow either the procedure in Vogel or the procedure in Organic Syntheses.
Baseline Does Not Exist.
(Newbee)
11-15-02 21:57
No 380176
>> I seem to have difficulty knowing when all the ammonium chloride is removed, since it looks no different to me.
When checking the final product, rub a little in between 2 fingers. If it disapears, it's MeAm, and most likely pretty pure. If it's grindy, almost descriptively fitting of the word "griemey" then it probably contains some ammonium chloride. I found this to be helpful when I thought making methylamine was fun.